JP5546263B2 - Cleaning liquid regenerating device and circulating cleaning device - Google Patents

Description

  The present invention relates to a cleaning liquid regenerating apparatus and a circulating cleaning apparatus, and in particular, cleaning liquid regeneration for efficiently regenerating both an aqueous cleaning liquid composed of a plurality of components and a cleaning liquid in a phase separation state composed of a plurality of components. The present invention relates to an apparatus and a circulating cleaning apparatus provided with such a cleaning liquid regenerating apparatus.

  2. Description of the Related Art Conventionally, various types of cleaning liquid regenerating devices for regenerating used cleaning liquid generated when an object to be cleaned such as a metal electronic component or a printed wiring board is cleaned using a cleaning liquid composed of a plurality of components have been proposed.

For example, a continuous distillation regeneration system using a distillation regeneration apparatus has been proposed that continuously circulates and purifies a multi-component cleaning liquid having a constant composition (see, for example, Patent Document 1).
More specifically, as shown in FIG. 15, the cleaning tanks 101 and 102 having a cleaning liquid, a distillation regenerating apparatus 103, and a pipe connecting them, the multi-component cleaning liquid having a constant composition is supplied to the cleaning tank 101, 102, and the multi-component cleaning liquid adjusted in the distillation regenerator 103 in advance so that the composition of the distillate from the distillation apparatus obtained from the vapor-liquid equilibrium diagram of the multi-component cleaning liquid is the same as that of the cleaning liquid. Is a continuous distillation regeneration system containing a specified amount.
The cleaning tanks 101 and 102 and the distillation regenerator 103 are connected by pipes provided with backflow prevention valves 106, 108, and 113, respectively. A liquid level adjusting device 110 that maintains a constant level is used to adjust the amount of distillate and the amount of inflow, and a multi-component cleaning liquid distillate having a constant composition from the distillation regenerator 103 is supplied to the cleaning tank 102, and the cleaning tank This is a continuous distillation regeneration system in which excess cleaning liquid from 101 is refluxed into the distillation regenerating apparatus 103, and a multi-component cleaning liquid having a constant composition is continuously circulated and purified.

Further, a vacuum distillation apparatus equipped with an ejector has been proposed as a vacuum distillation apparatus for regenerating a cleaning liquid composed of a non-aqueous solvent or the like (see, for example, Patent Document 2).
More specifically, as shown in FIG. 16, a distillation pot 201 that heats and evaporates the liquid to be treated under reduced pressure, a cooler 219 that condenses and liquefies the vapor of the liquid to be treated, and a distillate that is condensed and liquefied. There has been proposed a vacuum distillation apparatus 200 that includes an ejector 234 that is inserted in a circulation system 232 that circulates via a liquid storage tank 231 and a pump 233 and depressurizes the inside of the distillation pot 201.
Further, as a preferred embodiment, a heat exchanger 226 is provided between the distillation kettle 201 and the cooler 219, and the liquid storage tank 231 is for removing moisture contained in the non-aqueous solvent. A water separator 237 is provided.
Japanese Patent No. 25777857 JP-A-7-136402

  However, in the continuous distillation regeneration system disclosed in Patent Document 1, since distillation under reduced pressure is not considered, in order to obtain a sufficient amount of washing liquid without changing the composition, the distillation time tends to be long, In order to regenerate a sufficient amount of cleaning liquid, there has been a problem that the distillation regenerator tends to be large.

Moreover, although the vacuum distillation apparatus disclosed in Patent Document 2 can reduce the distillation time by vacuum distillation using an ejector, it is not intended for cleaning liquids composed of a plurality of components, but also includes moving speed, gas-liquid equilibrium, etc. Since no consideration was given to the above, problems such as a bumping phenomenon in the evaporation tank and a change in the composition of the resulting cleaning liquid were observed.
In particular, the steam taken out from the distillation kettle is directly introduced into a cooler placed at a distance to be liquefied, so that the pressure in the evaporation tank becomes excessive, causing bumping or maintaining gas-liquid equilibrium. The problem of not being able to do was seen.
In addition, not only are non-aqueous solvents originally intended, but when a water separator is provided in the liquid storage tank, there is a problem that the aqueous solvent cannot be applied.

Therefore, according to the present invention, not only the non-aqueous solvent is used by taking into consideration the moving speed of the cleaning liquid vapor, but also by vacuum distillation utilizing the vapor-liquid equilibrium between the cleaning liquid vapor as the gas phase and the liquid phase. Even if it is an aqueous solvent, it can be efficiently regenerated while maintaining the initial composition even if it is a cleaning liquid consisting of multiple components that phase separates in a stationary state and becomes cloudy when washed. An object of the present invention is to provide a simple cleaning liquid regenerating apparatus.
Further, according to the present invention, by providing a cleaning liquid regenerating apparatus that performs vacuum distillation using gas-liquid equilibrium, a circulating cleaning apparatus capable of stably circulating a cleaning liquid composed of a plurality of components over a long period of time is provided. Objective.

According to the present invention, a used cleaning liquid composed of a plurality of components derived from a distillation source liquid is heated and evaporated in a reduced pressure state, thereby generating a cleaning liquid vapor in a gas-liquid equilibrium state and condensing the cleaning liquid vapor. And a recovery unit for continuously collecting the regenerated cleaning liquid, and the generation unit contains the used cleaning liquid and is heated. An evaporator for condensing, a cooling part for condensing the cleaning liquid vapor into a regenerated cleaning liquid, and a connecting part connecting the evaporation part and the cooling part. The cooling part is provided directly above the evaporation part. with some Te, Yes respectively provided inside the same housing, recovery unit, and the cleaning solution tank reproducing cleaning liquid stored, the cleaning liquid take-out portion for taking out reproduction cleaning liquid to the outside, the reproduction cleaning liquid by the circulating pump循A circulation path that is made to flow, a suction section that is provided in the middle of the circulation path and generates a negative pressure when the regenerated cleaning liquid flows, and a decompression path that communicates between the suction section and the generation section. With the negative pressure, the generation unit is brought into a depressurized state via the decompression path, and the regenerated cleaning liquid is sucked from the storage part and introduced into the circulation path, and the opening area of the connection part is set to A (mm ² ). When the heater capacity for heating the evaporation section is B (kW), the cleaning liquid vapor transfer coefficient C defined by the following equation (1) is set to a value within the range of 100 to 30,000 mm ² / kW. A cleaning liquid regenerating apparatus characterized by the above is provided, and the above-described problems can be solved.
Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1)

That is, according to the cleaning liquid regenerating apparatus of the present invention, the distillation speed of the cleaning liquid is taken into consideration, and the vacuum distillation is performed using the cleaning liquid vapor as a gas phase and the vapor-liquid equilibrium between the liquid phase. Therefore, the initial formulation composition can be determined not only for non-aqueous solvents, but also for aqueous solvents, and even for cleaning liquids composed of a plurality of components that are phase-separated in a stationary state and become cloudy when washed. The cleaning liquid can be efficiently regenerated while substantially maintaining and preventing the bumping phenomenon.
In constructing the cleaning liquid regenerating apparatus of the present invention, when generating the cleaning liquid vapor by heating the cleaning liquid in the generating section, the evaporation section has the same composition as the cleaning liquid vapor and a gas-liquid equilibrium. It is preferable to store in advance a distilling liquid composed of a plurality of components having a composition calculated from the figure.
Furthermore, the cooling unit is provided immediately above the evaporation unit, and is configured to be provided in the same casing, thereby reducing the distance between the cooling unit and the evaporation unit as much as possible. Thus, not only the control of the moving speed of the cleaning liquid vapor but also the maintenance of the vapor-liquid equilibrium state under reduced pressure can be facilitated, and the cleaning liquid having a predetermined composition comprising a plurality of components can be more efficiently regenerated.
In addition, since the cooling unit and the evaporation unit in the generation unit are provided inside the same housing, it is possible to provide a cleaning liquid regenerating apparatus that is further simplified and miniaturized.
In addition, by configuring the recovery unit in this way, there is no need to use a vacuum pump for directly depressurizing the inside of the generation unit, a means for gas-liquid separation of the discharged gas, etc. An improved cleaning liquid regenerating apparatus can be provided.

In configuring the cleaning liquid regenerating apparatus of the present invention, the opening area (A) of the connecting portion is preferably set to a value within the range of 100 to 3,000,000 mm ² .
By limiting the opening area (A) of the connecting portion to a value within a predetermined range as described above, it becomes easier to control the moving speed of the cleaning liquid vapor, and the bumping phenomenon is caused in the vacuum distillation using gas-liquid equilibrium. It can be effectively prevented.
In addition, with such an opening area (A) of the connecting portion, it is possible to prevent the cleaning liquid regenerating apparatus from becoming excessively large and to provide a cleaning liquid regenerating apparatus of an appropriate size that can be easily attached to the cleaning apparatus.

Moreover, when comprising the washing | cleaning-liquid reproduction | regeneration apparatus of this invention, it is preferable to make a heater capacity | capacitance (B) into the value within the range of 0.1-100 kW.
By limiting the heater capacity (B) to a value within the predetermined range as described above, it becomes easier to control the moving speed of the cleaning liquid vapor, and the bumping phenomenon can be effectively performed even in vacuum distillation using gas-liquid equilibrium. Can be prevented.
Further, with such a heater capacity (B), it is possible to prevent the power consumption from becoming excessively large and to provide a cleaning liquid regenerating apparatus that is excellent in economy.

Further, in constituting the cleaning liquid regenerating apparatus of the present invention, when the cleaning liquid vapor contains water vapor, it is preferable to set the moving speed of the water vapor to a value within the range of 0.02 to 6 m / sec.
In this way, by limiting the moving speed of the water vapor to a value within a predetermined range, in the vacuum distillation using the vapor-liquid equilibrium, the bumping phenomenon can be made more effective not only with non-aqueous solvents but also with aqueous solvents. Can be prevented.

Further, in configuring the cleaning liquid regenerating apparatus of the present invention, it is preferable to set the pressure of the generation unit to a value within the range of -0.01 to -0.1 MPa.
In this way, by limiting the pressure of the generation unit to a value within a predetermined range, vacuum distillation in the generation unit can be performed efficiently, and the gas-liquid in the blending composition having greatly different cleaning liquid vapor moving speed and boiling point An equilibrium state can be stably maintained.

In configuring the cleaning liquid regenerating apparatus of the present invention, it is preferable that the cleaning liquid contains water and the content of the water is set to a value within the range of 40 to 70% by weight with respect to the total amount.
By comprising in this way, while carrying out the vacuum distillation in a production | generation part efficiently, even when a predetermined aqueous cleaning liquid is used, the gas-liquid equilibrium state in a production | generation part can be maintained stably.

Another aspect of the present invention is a cleaning device capable of cleaning an object to be cleaned with a regenerated cleaning liquid and capable of supplying a used cleaning liquid after cleaning to a generating unit, a cleaning liquid regenerating apparatus for generating a regenerated cleaning liquid, The cleaning liquid regenerating apparatus comprises a cleaning liquid vapor in a gas-liquid equilibrium state by heating and evaporating a used cleaning liquid composed of a plurality of components derived from a distillation source liquid in a reduced pressure state. A generation unit for generating and condensing the cleaning liquid vapor into a regenerated cleaning liquid and a recovery unit for continuously recovering the regenerated cleaning liquid are provided, and the generation unit accommodates the used cleaning liquid. And an evaporating part for heating, a cooling part for condensing the cleaning liquid vapor to form a regenerated cleaning liquid, and a connecting part for connecting the evaporating part and the cooling part. Set directly above With some Te, Yes respectively provided inside the same housing, recovery unit, the circulating flow and the washing liquid tank reproducing cleaning liquid stored, the cleaning liquid take-out portion for taking out reproduction cleaning liquid to the outside, the reproduction cleaning liquid by the circulating pump A suction path that is provided in the middle of the circulation path and generates a negative pressure when the regenerated cleaning liquid flows, and a decompression path that communicates between the suction section and the generation section. Negative pressure causes the generating unit to be in a depressurized state via the depressurization path, and the regenerated cleaning liquid is sucked from the storage unit and introduced into the circulation path, and the opening area of the coupling unit is set to A (mm ² ), evaporating. When the heater capacity for heating the part is B (kW), the transfer coefficient C of the cleaning liquid vapor defined by the following formula (1) is set to a value within the range of 100 to 30,000 mm ² / kW. Circulation characterized by Kiyoshi is a device.
Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1)

That is, according to the circulating cleaning device of the present invention, by providing a predetermined cleaning liquid regenerating device, the used cleaning liquid can be stably evaporated in a reduced pressure state while preventing bumping, and gas-liquid equilibrium can be achieved. Depending on the condition, not only non-aqueous solvents, but also aqueous solvents, and even a cleaning liquid consisting of a plurality of components that are phase-separated in a stationary state and become cloudy at the time of washing, are prescribed blended. In addition, the cleaning liquid can be efficiently recovered, and the object to be cleaned can be stably cleaned by using the recovered cleaning liquid recovered as described above.
In addition, by providing a cleaning liquid regenerating apparatus having such a recovery unit, a vacuum pump for directly depressurizing the inside of the generation unit, a means for separating the discharged gas from gas and liquid, and the like can be omitted. It can be set as the circulation washing apparatus provided with the washing | cleaning liquid reproduction | regeneration apparatus made into.

It is the schematic provided in order to demonstrate the washing | cleaning-liquid reproduction | regeneration apparatus of this invention. It is a figure which shows the correlation with the liquid phase composition in the operating condition of a washing | cleaning liquid reproduction | regeneration apparatus, and a gaseous-phase composition when it is set as the ideal solution of 2 components (NMP and BFG) of a washing | cleaning liquid. It is a figure which shows the correlation of the liquid phase composition in a working condition of a washing | cleaning liquid reproduction | regeneration apparatus, and a gaseous-phase composition when it is set as the ideal solution of 2 components (NMP and water) of a washing | cleaning liquid. It is a figure which shows the correlation of the liquid phase composition in a working condition of a washing | cleaning liquid reproduction | regeneration apparatus, and a gaseous-phase composition when it is set as the ideal solution of 2 components (water and BFG) of a washing | cleaning liquid. It is a figure provided in order to demonstrate the relationship between the transfer coefficient of a washing | cleaning liquid vapor | steam, and the pressure of an evaporation part. It is a figure provided in order to demonstrate the relationship between the movement coefficient of cleaning liquid vapor | steam, and the moving speed of water vapor | steam. It is the schematic provided in order to demonstrate the circulation washing apparatus of this invention. It is the schematic provided in order to demonstrate another circulation washing apparatus of this invention. It is a figure provided in order to demonstrate the influence with respect to the washability of the compounding quantity of a 1st organic solvent. It is a figure provided in order to demonstrate the influence with respect to the washability of the compounding quantity of a 2nd organic solvent. It is a figure provided in order to demonstrate the influence with respect to the washability of the compounding quantity of a 3rd organic solvent. It is a figure provided in order to demonstrate the influence with respect to drying property of the compounding quantity of a 3rd organic solvent. It is a figure provided in order to demonstrate the influence with respect to flash point of the compounding quantity of a 3rd organic solvent. It is a figure provided in order to demonstrate the influence with respect to the washability of the compounding quantity of water. It is the schematic provided in order to demonstrate the conventional circulation washing apparatus. It is the schematic provided in order to demonstrate another conventional circulation washing apparatus.

[First Embodiment]
In the first embodiment, as shown in FIG. 1, a cleaning liquid vapor 15 in a gas-liquid equilibrium state is obtained by heating and evaporating a used cleaning liquid 30 composed of a plurality of components derived from a distillation source liquid in a reduced pressure state. , And a cleaning unit for condensing the cleaning liquid vapor 15 ′ into the regenerated cleaning liquid 15 and a recovery unit 23 for continuously recovering the regenerated cleaning liquid 15. 10, the generation unit 13 contains the used cleaning liquid 30, the evaporation unit 31 for heating, the cooling unit 41 for condensing the cleaning liquid vapor 15 ′ into the regenerated cleaning liquid 15, and the evaporation And a connecting part 41c that connects the cooling part 41 and the cooling part 41, the cooling part 41 is provided immediately above the evaporation part 31, and each is provided inside the same housing . Regenerated cleaning solution 5, a cleaning liquid tank 43 in which the regenerated cleaning liquid 15 is taken out, a cleaning liquid extraction part for taking out the regenerating cleaning liquid 15 to the outside, a circulation path 47 through which the regenerated cleaning liquid 15 is circulated and flowed by the circulation pump 49a, and a recirculation path 47. A suction part 49 that generates a negative pressure when the cleaning liquid 15 flows, and a decompression path 55 that communicates between the suction part 49 and the generation part 13, and the decompression path 55 is defined by the negative pressure of the suction part 49. Thus, the generation unit 13 is brought into a reduced pressure state, and the regenerated cleaning liquid 15 is sucked from the storage unit 41b and introduced into the circulation path 47, and the opening area of the connection unit 41c is set to A (mm ² ). When the heater capacity for heating is B (kW), the transfer coefficient C of the cleaning liquid vapor 15 ′ defined by the following equation (1) is set to a value within the range of 100 to 30,000 mm ² / kW. This A cleaning liquid reproducing apparatus 10, characterized in.
Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1)
Hereinafter, the cleaning liquid regenerating apparatus 10 of the first embodiment will be specifically described with reference to FIG.

1. Cleaning liquid (1) Type 1
In FIG. 1 and the like, the used cleaning liquid 30 composed of multiple components to be processed by the cleaning liquid regenerating apparatus 10 is a mixed solution in which at least two components, preferably three or more cleaning components are mixed.
Such cleaning component types can be appropriately selected depending on the object to be cleaned.
More specifically, water, 3-methoxy-3-methyl-1-butanol (MMB), 3-methoxy-3-methylbutyl acetate (MMBAC), 3-methoxybutyl acetate (methace), propylene glycol monomethyl ether acetate (PMA), propylene glycol monopropyl ether (PFG), propylene glycol diacetate (PGDA), ethylene glycol monoisobutyl ether (iBG), ethylene glycol monoisopropyl ether (iPG), ethylene glycol monobutyl ether acetate (BGAC), propylene glycol Monobutyl ether (BFG), dipropylene glycol dimethyl ether (DMFDG), dipropylene glycol monobutyl ether (BFDG), dipropylene glycol Cole monomethyl ether (MFDG), diethylene glycol monohexyl ether (HeDG), diethylene glycol diethyl ether (DEDG), N-methyl-2-pyrrolidone (NMP), N, N-dimethylacetamide (DMAC), N, N-diethylisopa Nolamine (2FA), N-ethylethanolamine (MEM), N-methylethanolamine (MMA), N, N-diethylethanolamine (2A), N, N-dimethylethanolamine (2Mabs), 2-ethylhexylamine (2EHA), N, N-dimethylbenzylamine (DMBAN), formamide, N-methylformamide, N-ethylformamide, 1-decene, 1-dodecene, limonene, cymene, anisole, furfural, 2-heptanone 2-octanone, furfuryl alcohol (FFAL), propylene glycol (PG), tetrahydrofurfuryl alcohol (THFAL), 1-hexanol, 1-heptanol, dibutylamine (DBA), benzyl alcohol (BAL), benzylamine (BAN) , Dimethyl sulfoxide (DMSO), diethanolamine (DEA), monoisopanolamine (MIPA), pseudocumene (cumene), n-decane (decane), etc. Abbreviation.)

Therefore, as suitable combinations of cleaning liquids (used cleaning liquids) to be processed by the cleaning liquid regenerating apparatus, cumene, decane combinations, BAL, HeDG, DEA combinations, BAL, DEA combinations, PFG, DMAC, Water combination, PMA, DMAC, water combination, PMA, PFG, NMP, water combination, Metoace, PFG, NMP, water combination, MMBAC, PFG, NMP, water combination, BAN, BAL, BGAC, MIPA, Water combination, decane, BAN, BAL, BGAC, MIPA, water combination, PMA, metace, PGDA, MMB, DMSO, NMP, water combination, MEM, iBG, BFG, water combination, iBG, BFG, water Combination, MEM, 1-decene, MP, 1-hexanol, the combination of MAK, DMBAN, anisole, BAL, the combination of water, 2FA, 1-decene, the combination of iBG, MMB, MEM, a combination of water, PFG, the combination of water and the like.
In addition, although the example of the detergent composition which phase-separates and wash | cleans in a cloudy state is included partially, it demonstrates in detail in 2nd Embodiment.

2. Generation Unit (1) Basic Configuration Further, the generation unit 13 shown in FIG. 1 contains a used cleaning liquid (hereinafter sometimes referred to as a distillation source liquid) 30 and the distillation source liquid 30 is heated by a heating means 31a. An evaporation unit 31 for heating by the cooling unit, a cooling unit 41 for condensing the cleaning liquid vapor 15 ′ into the regenerated cleaning liquid 15, and a connecting unit 41 c connecting the evaporation unit 31 and the cooling unit 41. The cooling unit 41 is provided directly above the evaporation unit 31 and is provided inside the same casing.
And in the pressure_reduction | reduced_pressure state of the production | generation part 13, the distillation original liquid 30 stored by the evaporation part 31 and the washing | cleaning liquid vapor | steam 15 '(namely, obtained regenerated washing | cleaning liquid 15) are the structures which are in a gas-liquid equilibrium state.
The generation unit 13 cleans an object to be cleaned (not shown), and thereby discharges contaminants such as solid or liquid accumulated in the evaporation unit 31 to the outside through the valve 37a. , And is configured to enable stable reproduction.

(2) Distillation source liquid Although the distillation original liquid 30 shown in FIG. 1 contains all the compounding components that constitute the cleaning liquid before use (regenerated cleaning liquid), it has a different composition from the cleaning liquid. The cleaning liquid vapor 15 ′ generated by evaporation under the temperature and pressure conditions of the generation unit 13 is a liquid material prepared in advance so as to have the same composition as the regenerated cleaning liquid 15.
That is, the distillation source liquid 30 is a liquid having a blended composition in which a gas-liquid equilibrium state is established between the distillation source liquid 30 and the cleaning liquid vapor 15 ′ having the composition of the regenerated cleaning liquid 15 under the operating conditions of the generation unit 13. It is a thing.
Even when the used cleaning liquid is supplied to and mixed with the original distillation liquid, the mixture may be referred to as the original distillation liquid or used in the steady state of the cleaning liquid regenerating apparatus. Sometimes referred to as a finished cleaning solution (the same applies hereinafter).

  In addition, in order to set the blending composition of the distillation source liquid 30, it is possible to repeat a preliminary test or the like under the operating conditions of the generating unit 13. For example, for the cleaning liquid having a desired composition, the cleaning liquid It is also possible to calculate based on the vapor-liquid equilibrium diagram of the ideal solution of each component.

Here, when the blending composition of the distillation source liquid 30 is calculated for a cleaning liquid composed of two components, a vapor-liquid equilibrium diagram of the cleaning liquid composed of two components is obtained in advance, and the blending in the gas becomes the blending component of the cleaning liquid. In each case, the mixing ratio in the liquid phase is determined and used as the distillation source liquid.
For example, as shown in FIG. 2, based on a gas-liquid equilibrium diagram (XY diagram of NMP-BFG) showing the correlation between the liquid phase composition of the NMP-BFG solution and the gas phase composition under the operating condition of the cleaning liquid regenerating apparatus. Thus, the mixing ratio in the liquid phase in the case where the gas phase composition coincides with the mixing ratio of the NMP-BFG solution as the desired cleaning agent is obtained and used as the distillation source liquid.
Similarly, as shown in FIG. 3, a vapor-liquid equilibrium diagram (XY of H ₂ O-NMP) showing the correlation between the liquid phase composition of the H ₂ O-NMP solution and the gas phase composition under the operating conditions of the cleaning liquid regenerator. Based on the diagram), the mixing ratio in the liquid phase when the gas phase composition matches the mixing ratio of the H ₂ O-NMP solution as the desired cleaning agent is obtained, and this is used as the distillation source liquid It is.
Furthermore, as shown in FIG. 4, a vapor-liquid equilibrium diagram (XY line of H ₂ O-BFG) showing the correlation between the liquid phase composition of the H ₂ O-BFG solution and the gas phase composition under the operating conditions of the cleaning liquid regenerating apparatus. Based on the figure), the mixing ratio in the liquid phase when the gas phase composition coincides with the mixing ratio of the H ₂ O-BFG solution as the desired cleaning agent is obtained and used as the distillation source liquid. is there.

In addition, as described above, in the case of a distillate source liquid consisting of a plurality of components, the vapor-liquid equilibrium state between the cleaning liquid vapor consisting of the plurality of components changes little even if the ambient temperature or pressure changes somewhat. Without it, it has been found separately that it is stable.
More specifically, when the distillation source liquid is, for example, A component: B component: C component is present at a normal temperature and a strip pressure in a weight ratio of A: B: C, For example, it was found that the weight ratio of A component: B component: C component is substantially A: B: C even at −0.01 to −0.1 MPa, for example, at 50 to 200 ° C. and low pressure. Yes.

Moreover, even when a cleaning liquid consisting of three or more components is targeted, one of the cleaning liquids consisting of a plurality of components is used as a reference component, and this reference is determined based on a vapor-liquid equilibrium diagram with other compounding components. By determining the mixing ratio of the component and the other compounding component in the cleaning liquid, the composition of the distillation source liquid 30 composed of three or more components can be determined.
That is, assuming a two-component ideal solution of the reference component and each of the other components, the liquid composition from which the vapor of the mixing ratio can be obtained from each vapor-liquid equilibrium diagram.

Next, the liquid composition of each of the other components with respect to the reference component obtained for the ideal solution of the two-component system is combined so that the total amount becomes 100% corresponding to the existing ratio in the cleaning liquid. By performing correction for application to the above, the blend composition as the distillation source liquid can be determined.
Specifically, the blending ratio of the A component, the B component, and the C component is Ya (wt%): Yb (wt%): Yc (wt%) when the total amount of each is 100 wt%. In the case of a cleaning liquid, A component is used as a reference component, a two-component ideal solution (A-B solution) of A component and B component, and a two-component ideal solution (A-C solution) of A component and C component ).
In this case, the mixing ratios in the AB solution are Ya / (Ya + Yb) and Yb / (Ya + Yb), and the mixing ratios in the AC solution are Ya / (Ya + Yc) and Yc / (Ya + Yc).

  Next, the blending ratio of the component A in the distillation source liquid is calculated from the vapor-liquid equilibrium diagram of the AB solution and the following equation (2).

Here, Ya is a blending ratio of the component A in the gas phase made of the cleaning liquid in the cleaning apparatus. Therefore, for example, when the blending ratio of the component A in the cleaning liquid is 1.8% by weight, Ya = 1.8.
The blending ratio of the A component in the liquid phase means the blending ratio of the A component with respect to the total amount of the A component and the B component in the regeneration tank (Ya / (Ya + Yb)). Therefore, when the weight ratio of the A component to the B component in the cleaning liquid is 83:17, for example, the blending ratio of the A component in the liquid phase composed of the cleaning liquid in the regeneration tank is 0.17.

  Further, the blending ratio of the A component in the gas phase is a value obtained from the vapor-liquid equilibrium diagram of the AB solution with respect to the blending ratio of the A component in the liquid phase. Therefore, for example, the blending ratio of the A component in the liquid phase composed of the cleaning liquid in the regeneration tank is 0.17, and in the vapor-liquid equilibrium diagram of the AB solution, the gas phase value corresponding to the numerical value is 0. In the case of 38, this 0.38 is used as the blending ratio of the component A in the gas phase consisting of the cleaning liquid in the cleaning tank.

  Further, the correction coefficient is tentatively calculated as a blending ratio Ya ′ (%) of the A component calculated with the correction coefficient set to 1, and similarly, the vapor-liquid equilibrium diagram of the AB solution and the following equation (3) (correction coefficient) B component blending ratio Yb '(%) calculated from 1), the vapor-liquid equilibrium diagram of the AC solution and the following formula (4) (correction coefficient is assumed to be 1) The ratio Yc ′ (%) is calculated according to the following formula (5).

Correction coefficient = (Ya ′ + Yb ′ + Yc ′) / 100 (5)

  By using the liquid whose blending ratio is determined in this way as the distillation source liquid, during the operation of the cleaning liquid regenerating apparatus 10, each blending component continuously changes the blending composition of the regenerated cleaning liquid 15 from the evaporation unit 31. Each of the cleaning liquid vapors 15 'is continuously evaporated. Then, after a predetermined time has passed, the cleaning liquid regenerating apparatus 10 is in a steady state, and the used cleaning liquid is continuously supplied from the pipe 17b to the evaporation unit 31 in a predetermined amount. It will be maintained substantially constant.

(3) Cooling unit The cooling unit 41 in the generation unit 13 is integrally provided above the evaporation unit 31 including the evaporation tank and the like, and condenses the cleaning liquid vapor 15 ′ generated in the evaporation unit 31. It is a part of.
Therefore, after the vapor | steam from the evaporation part 31, for example, an evaporation tank rises, it is cooled by the cooling pipe 41a, and the condensed liquid which flows down is temporarily collected in the storage part 41b, it is sucked in it. It is configured to be guided by the portion 49.
Therefore, it is preferable that the cooling unit 41 in the generation unit 13 is provided immediately above the evaporation unit 31.
That is, by considering the position of the cooling unit 41 in the generation unit 13 in this way, the distance between the cooling unit 41 and the evaporation unit 31 is made relatively short, and the cleaning liquid evaporated upward from the evaporation unit 31. This is because the vapor 15 ′ is immediately liquefied, so that the gas-liquid equilibrium state in the generation unit 13 can be maintained more stably.

(4) Connection part Moreover, as shown in FIG. 1, the connection part 41c is provided between the cooling part 41 in the production | generation part 13, and the evaporation part 31, and it is the opening part 41d provided in the said connection part 41c. The cleaning liquid vapor 15 ′ is preferably configured to move from the evaporating unit 31 to the cooling unit 41 via
This is because the cooling part 41 and the evaporation part 31 are clearly separated by the connecting part 41c, and the moving speed of the cleaning liquid vapor 15 'is controlled by controlling the opening area of the opening part 41d in the connecting part 41c. This is because, as a result, the bumping phenomenon of the cleaning liquid in the evaporation unit 31 can be effectively prevented.

When the opening area of the connecting portion 41c is A (mm ² ) and the heater capacity for heating the evaporation portion 31 is B (kW), the cleaning liquid vapor 15 ′ defined by the following equation (1) The movement coefficient C is set to a value in the range of 100 to 30,000 mm ² / kW.

  Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1)

The reason for this is that, as shown in FIG. 5, when the transfer coefficient of the cleaning liquid (cleaning liquid vapor) 15 ′ is less than 100 mm ² / kW, the pressure in the evaporation section becomes remarkably large, and the distillation source liquid 30 is likely to bump. Because.
Further, as shown in FIG. 6, when the transfer coefficient of the cleaning liquid (cleaning liquid vapor) 15 ′ is less than 100 mm ² / kW, the moving speed of the water vapor is remarkably increased. This is because it becomes easier to bump.
On the other hand, as shown in FIG. 5, when the transfer coefficient of the cleaning liquid (cleaning liquid vapor) 15 ′ exceeds 30,000 mm ² / kW, the pressure in the evaporation section decreases, and the distillation source liquid 30 is bumped. This is because although the area of the opening of the connecting portion 41c becomes excessive, the cleaning liquid regenerating apparatus can be easily increased in size.
Similarly, as shown in FIG. 6, when the transfer coefficient of the cleaning liquid (cleaning liquid vapor) 15 ′ exceeds 5,000 mm ² / kW, the moving speed of the water vapor decreases, which is the case with an aqueous cleaning agent. Even if it exists, although the bumping of the distillation original liquid 30 can be prevented, the area of the opening part of the connection part 41c becomes excessive, and the cleaning liquid regenerating apparatus is easily increased in size.
Accordingly, the washing solution is preferably set to a value within the range of 1,000~20,000mm ² / kW to transfer coefficient C of (cleaning liquid vapor) 15 ', a value in the range of 1,000~5,000mm ² / kW More preferably.

In the cleaning liquid regenerating apparatus, the opening area (A) of the connecting portion is preferably set to a value within the range of 100 to 3,000,000 mm ² .
The reason for this is that by restricting the opening area (A) of the connecting portion to a value within a predetermined range, it becomes easier to control the moving speed of the cleaning liquid vapor, and in vacuum distillation using gas-liquid equilibrium. This is because the bumping phenomenon can be effectively prevented.
In addition, with such an opening area (A) of the connecting portion, the cleaning liquid regenerating apparatus can be prevented from becoming excessively large, and a cleaning liquid regenerating apparatus of an appropriate size that can be easily attached to the cleaning apparatus can be obtained. It is.
Accordingly, the cleaning liquid reproducing apparatus, the opening area of the connecting portion (A) is more preferably set to a value within the range of 1,000～1,000,000Mm ^2, in the range of 10,000～150,000Mm ² More preferably, it is a value.

Moreover, when water vapor | steam is contained in cleaning liquid vapor | steam, it is preferable to make the moving speed of the water vapor | steam in the opening part in a connection part into the value within the range of 0.02-6m / sec.
The reason for this is that by limiting the moving speed of water vapor to a value within a predetermined range in this way, in vacuum distillation using gas-liquid equilibrium, not only non-aqueous solvents but also water-based solvents can cause bumping phenomenon. This is because it can be more effectively prevented.
Therefore, it is more preferable to set the moving speed of water vapor at the opening in the connecting portion to a value within the range of 0.03 to 0.6 m / sec, and a value within the range of 0.1 to 0.6 m / sec. More preferably.

(5) Heating means The heating means 31a in the production | generation part 13 shown in FIG. 1 supplies the calorie | heat amount which can maintain the distillation original liquid 30 stored in the evaporation tank 31 at predetermined temperature.
Therefore, for example, it is configured by a steam flow path, a heater, or the like that can heat the distillation source liquid 30 by ventilating the heating steam.
Further, such a heating means 31a may supply a constant amount of heat when the amount of liquid in the evaporation tank 31 is maintained constant or substantially constant, When the amount of liquid varies with time, or when the temperature of the used cleaning liquid supplied from the pipe 17b varies with time, the amount of heat may be adjustable according to the amount of liquid and the temperature. .
Furthermore, it is possible to use a temperature sensor or the like (not shown) to adjust the amount of heat to be supplied.

Moreover, regarding a heating means, it is preferable to make a heater capacity | capacitance (B) into the value within the range of 0.1-100 kW.
The reason for this is that by limiting the heater capacity (B) to a value within the predetermined range, the control of the moving speed of the cleaning liquid vapor becomes easier, and even in vacuum distillation using gas-liquid equilibrium, bumping This is because the phenomenon can be effectively prevented.
Further, with such a heater capacity (B), it is possible to prevent the power consumption from becoming excessively large and to provide a cleaning liquid regenerating apparatus excellent in economy.
Therefore, the heater capacity (B) is more preferably set to a value within the range of 0.1 to 50 kW, and further preferably set to a value within the range of 1 to 30 kW.

Further, the temperature (evaporation temperature) in the generation unit 13 can be appropriately selected depending on the cleaning liquid and pressure to be used, but is preferably maintained at a constant temperature during operation.
More specifically, it is preferable to keep the evaporation temperature in the generation part at a value within the range of 50 to 200 ° C.
This is because the selection range of the cleaning liquid used in the cleaning liquid regenerating apparatus can be remarkably increased by setting the temperature range.
That is, when the evaporation temperature in the generating unit is less than 50 ° C., the types of usable cleaning agents may be excessively limited.
On the other hand, when the evaporation temperature in the generation unit exceeds 200 ° C., similarly, the types of cleaning agents that can be used are excessively limited, the constituent materials in the generation unit are excessively limited, and the generation unit is maintained. This is because management may be difficult.
Therefore, it is preferable to set the evaporation temperature in the generation part to a value in the range of 50 to 180 ° C, and more preferably to a value in the range of 60 to 160 ° C.
Note that the evaporation temperature in the generating unit is basically a value determined and determined by the degree of pressure reduction in the generating unit, the composition of the cleaning liquid, or the like.

(6) Discharge Unit The discharge unit 37 shown in FIG. 1 is a part for discharging the contaminants brought into the evaporation tank 31 in a state of being mixed in the used cleaning liquid out of the system.
Therefore, it has the discharge pipe 37a opened to the bottom part of the evaporation tank 31, and the on-off valve 37b for opening and closing the discharge pipe 37a.
The contaminants are liquids and solids other than the cleaning components constituting the cleaning liquid, and are accumulated in the evaporation tank 31 over time without evaporating during the operation of the cleaning liquid regenerating apparatus 10, and in this embodiment, the evaporation tank 31 stays at the bottom.
Therefore, it is possible to discharge from the bottom of the evaporation tank 31 periodically or when the amount of staying contaminants increases.
However, without providing such a discharge part, the influence of contaminants can be eliminated by replacing the evaporation tank 31 in the generation part with a new evaporation tank after a predetermined time has elapsed.

(7) Liquid level adjustment means In addition, in this production | generation part 13, in order to keep the storage amount of the distillation original liquid 30 stored by the evaporating tank 31, constant or substantially constant, for example, a liquid level is predetermined range, Preferably It is preferable to provide a liquid level adjusting means for keeping the position constant.
As such a liquid level adjusting means, for example, it is preferable to mechanically adjust the opening of the flow rate adjusting valve 17d by a predetermined operation (vertical operation) of the float 31b as shown in FIG.
Further, based on the liquid level detected by the liquid level sensor, the opening degree of the flow rate adjusting valve 17d provided in the pipe 17b may be adjusted based on an electric signal from a microprocessor (not shown). Good.

3. Recovery Unit (1) Basic Configuration The recovery unit 23 in the cleaning liquid regenerator 10 shown in FIG. 1 is a part for continuously recovering the regenerated cleaning liquid 15 via the cleaning liquid tank 43.
Accordingly, the cleaning liquid tank 43 in which the regenerated cleaning liquid 15 is stored, the circulation path 47 in which the regenerated cleaning liquid 15 in the cleaning liquid tank 43 is circulated and flowed by the circulation pump 49a, and the cleaning liquid 15 provided in the circulation path 47 flows. The suction part 49 that generates a negative pressure and the suction part 49 communicate with each other through the cooling part 41 so that the suction part 49 sucks the gas or liquid in the cooling part 41 and the generation part 13. And a decompression path 55 including a check valve 53b.
The cleaning liquid tank 43 is provided with a pipe 17a including a check valve 17c as a cleaning liquid extraction part for extracting the stored regenerated cleaning liquid 15 to the outside.

(2) Cleaning liquid tank The cleaning liquid tank 43 is provided as a container for storing the regenerated cleaning liquid 15 having a predetermined composition.
The amount of the cleaning liquid stored in the cleaning liquid tank 43 is a volume that can sufficiently secure the amount of cleaning liquid supplied from the pipe 17a to the cleaning device (not shown) in a state where the cleaning liquid is constantly circulated in the circulation path 47. I just need it.
However, when the amount of the cleaning liquid becomes excessive, it becomes difficult to contribute to simplification and miniaturization of the cleaning liquid regenerating apparatus. That is, if the cleaning liquid stored in the cleaning liquid tank 43 is excessively large, the amount of the regenerated cleaning liquid 15 used in the cleaning liquid regenerating apparatus 10 tends to be unnecessarily increased, and the cleaning liquid regenerating apparatus itself tends to be large. Because.
The cleaning liquid tank 43 is preferably provided with a cooling device, a heating device or the like in order to keep the regenerated cleaning liquid at a predetermined temperature.

(3) Circulation path The circulation path 47 is a pipe line in which the inlet 47a and the outlet 47b are provided in the cleaning liquid tank 43, and the cleaning liquid is passed through the suction part 49b by the circulating pump 49a provided in the middle. The cleaning liquid in the tank 43 is configured to always flow from the inlet 47a to the outlet 47b.
The pressure in the circulation path 47 is monitored and maintained by a pressure gauge 49c provided at the suction point 49b.
Since the circulation pump 49a is a pump that continuously circulates the cleaning liquid at a constant flow rate, for example, the circulation pump 49a is preferable because the negative pressure generated at the suction location 49b can be easily maintained by the ejector effect.

(4) Suction part The suction part 49 provided in the middle of the circulation path 47 is a part that generates a negative pressure by flowing the regenerated cleaning liquid 15 and sucks the liquid or gas. It comprises a circulation pump 49a, a suction location 49b, and a pressure gauge 49c.
That is, according to the suction unit 49, a negative pressure is generated by the ejector effect, so that the regenerated cleaning liquid (which may include cleaning liquid vapor) stored in the storage unit 41 b in the cooling unit 41 via the pressure reducing path 55 may be included. .) 15 can be aspirated.
Therefore, the sucked regenerated cleaning liquid 15 is introduced as it is into the regenerated cleaning liquid 15 flowing through the circulation path 47 in the suction section 49 and supplied to the cleaning liquid tank 43.

Further, in the cleaning liquid regenerating apparatus 10, the inside of the generation unit 13 is decompressed by the regenerating cleaning liquid 15 and the cleaning liquid vapor being sucked by the suction part 49 via the storage part 41b.
In this embodiment, the pressure of the generation unit 13 can be sucked by the suction unit 49 so as to have a value within a range of, for example, −0.01 to −0.1 MPa, and thereby the cleaning liquid regenerating apparatus. The degree of freedom in the selection range of the configuration of the cleaning liquid used in 10 is high.
However, if the pressure is excessively reduced, the size of the suction unit may be increased in order to increase the capacity of the suction unit.
Therefore, it is more preferable that the pressure of the generation unit 13 is set to a value within the range of −0.06 to −0.095 MPa by the suction unit 49.
In addition, although the structure of the suction part 49b in the suction part 49 is sufficient if it is a T-shaped tube, it may be configured by an ejector, an aspirator, or the like.

4). Basic Operation Next, the basic operation of the cleaning liquid regenerating apparatus 10 shown in FIG. 1 will be described.
In the cleaning liquid regenerating apparatus 10, the distillation source liquid 30 is stored in the generation unit 13 in advance, and is heated by the heating unit 31 a such as a heater in the evaporation tank 31.
In addition, the regenerated cleaning liquid 15 is stored in advance in the cleaning liquid tank 43 of the recovery unit 23, and the regenerated cleaning liquid 15 is circulated and flowed counterclockwise in the circulation path 47 by the circulation pump 49a. The generation unit 13 is in a reduced pressure state due to the negative pressure generated by.
Thereby, the inside of the production | generation part 13 is maintained by the operating condition which has the predetermined | prescribed temperature and pressure according to the mixing | blending component and composition of the reproduction | regeneration washing | cleaning liquid 15 desired.

Next, the used cleaning liquid guided by the pipe 17b is supplied to the generation unit 13 and mixed with the distillation source liquid 30, so that the compounding components constituting the regenerated cleaning liquid 15 are the cleaning liquid under the operating conditions of the generation unit 13. It evaporates as vapor 15 '.
And it is possible to generate the cleaning liquid vapor 15 ′ having the blended composition of the regenerated cleaning liquid while the distillation source liquid 30 is mixed with the used cleaning liquid supplied through the pipe 17 b in advance under the operating condition of the generation unit 13. In addition, since the gas-liquid balance is adjusted, the generation unit 13 generates the cleaning liquid vapor 15 ′ having a predetermined composition.

On the other hand, in the generation unit 13, the cleaning liquid vapor 15 ′ in a gas-liquid equilibrium state is continuously generated while being held in a predetermined reduced pressure state by the function of the suction unit 49, and each compounding component is reduced from the distillation source liquid 30. However, as the used cleaning liquid is continuously supplied from the pipe 17b, each component is replenished at a rate corresponding to the blended composition of the regenerated cleaning liquid.
And the liquid composition is kept constant or substantially constant, so that the blending composition and the storage amount of the distillation source liquid 30 are kept constant or substantially constant.

In the suction section 49, the sucked cleaning liquid vapor 15 ′ and the regenerated cleaning liquid 15 are introduced into the regenerated cleaning liquid 15 already flowing in the circulation path 47 and transferred to the cleaning liquid tank 43.
As a result, the cleaning liquid vapor 15 ′ generated by the generation unit 13 is all stored in the cleaning liquid tank 43 as the regenerated cleaning liquid 15 without being discharged out of the system. Therefore, the used cleaning liquid regeneration process is completed, and the cleaning liquid can be supplied again from the pipe 17a to the cleaning device 11 as a cleaning liquid.

According to the cleaning liquid regenerating apparatus 10 described above, by providing the predetermined suction part 49, the cleaning liquid 15 in the cleaning liquid tank 43 circulates and flows through the circulation path 47, so that a negative pressure is generated, and the generation unit 13 is brought into a reduced pressure state. At the same time, the cleaning liquid vapor 15 ′ and the regenerated cleaning liquid 15 generated in the generation unit 13 are sucked through the storage unit 41 b and introduced into the regenerated cleaning liquid 15 flowing through the circulation path 47. Without discharging each component out of the system, it is possible to perform a regeneration process in which the used cleaning liquid is evaporated and recovered in a reduced pressure state.
In addition, in the cleaning liquid regenerating apparatus 10, the distillation source liquid 30 stored in the generation unit 13 is subjected to cleaning liquid vapor and gas having the composition of the cleaning liquid 15 at the pressure and temperature of the generation unit 13 based on the negative pressure of the suction unit 49. Since the composition has a liquid equilibrium, the composition of the cleaning liquid 15 is unlikely to fluctuate, and the regeneration process can be stably performed by maintaining the cleaning liquid 15 at a desired composition.

Further, since the regeneration process is performed in a reduced pressure state, there is an advantage that a sufficient amount of the cleaning liquid 15 can be easily regenerated at a lower temperature.
Furthermore, it is not necessary to use a means for exhausting gas in order to depressurize the inside of the generation unit 13 or a means for gas-liquid separation of the exhausted gas. Therefore, the configuration of the cleaning liquid regenerating apparatus 10 can be simplified and downsized.

In addition, in this cleaning liquid regenerator 10, if the circulation pump 49a continuously circulates the cleaning liquid 15 at a predetermined flow rate and the generation unit 13 is maintained at a predetermined temperature, the operation of the generation unit 13 is performed. Conditions can be maintained stably.
Therefore, it is possible to generate the cleaning liquid vapor in a stable amount from the generation unit 13, and the generation unit 13 is configured to continuously mix a predetermined amount of the used cleaning liquid. By combining the amount and the mixed amount of the used cleaning liquid, it is possible to maintain the desired composition and continue the regeneration process of the cleaning liquid 15 for a long period of time.

[Second Embodiment]
In the second embodiment, as shown in FIG. 7, a cleaning device capable of cleaning an object to be cleaned (not shown) with the regenerated cleaning liquid 15 and supplying the used cleaning liquid 30 after cleaning to the generation unit 13. 11 is a circulating cleaning device 12 including a cleaning liquid regenerating apparatus 10 that generates a regenerating cleaning liquid 15.
Then, the cleaning liquid regenerator 10 heats and evaporates the used cleaning liquid 30 composed of a plurality of components derived from the distillation source liquid in a reduced pressure state, thereby generating a cleaning liquid vapor 15 ′ in a gas-liquid equilibrium state, The production | generation part 13 for condensing the said washing | cleaning liquid vapor | steam 15 'and making it the reproduction | regeneration washing | cleaning liquid 15 and the collection | recovery part 23 for collect | recovering the reproduction | regeneration washing | cleaning liquid 15 continuously are provided, and the production | generation part 13 is used. While containing the cleaning liquid 30, the evaporation section 31 for heating, the cooling section 41 for condensing the cleaning liquid vapor 15 ′ into the regenerated cleaning liquid 15, and the connecting section 41 c connecting the evaporation section 31 and the cooling section 41 It provided with a cooling unit 41, along with some provided immediately above the evaporation portion 31, Yes respectively provided inside the same housing, recovery unit 23, the cleaning liquid tank reproducing cleaning liquid 15 is stored 3, a cleaning liquid extraction unit for taking out the regenerated cleaning liquid 15 to the outside, a circulation path 47 for circulating the regenerated cleaning liquid 15 by the circulation pump 49 a, and a part of the circulation path 47. A suction part 49 that generates a negative pressure, and a decompression path 55 that communicates between the suction part 49 and the generation part 13, and the generation part 13 is connected to the generation part 13 via the decompression path 55 by the negative pressure of the suction part 49. A heater capacity for heating the evaporation unit 31 with the decompression state, suctioning the regenerated cleaning liquid 15 from the storage unit 41b and introducing it into the circulation path 47, setting the opening area of the connection unit 41c to A (mm ² ). And B (kW), the circulation coefficient C of the cleaning liquid vapor 15 ′ defined by the following formula (1) is set to a value within the range of 100 to 30,000 mm ² / kW. Device 1 It is.
Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1)
In the circulating cleaning device 12 shown in FIG. 7, as described in the first embodiment, the same cleaning liquid regenerator 10 shown in FIG. 1 can be used as it is. Explained.

1. Cleaning Device The cleaning device 11 shown in FIG. 7 introduces the cleaning liquid 15a supplied from the pipe 17a into the cleaning unit 11b including the cleaning tank 62 through the rinse unit 11a including the rinse tank 60 and the check valve 65. Using this, the cleaning object can be cleaned, and the used cleaning liquid 15b used for cleaning can be supplied to the cleaning liquid regenerator 10 via the pipe 17b.
As such a cleaning apparatus 11, it is preferable that substantially all of the regenerated cleaning liquid 15 supplied from the pipe 17a can be supplied to the cleaning liquid regenerating apparatus 10.
Therefore, there may be inevitable consumption such that the cleaning liquid 15 adheres to the object to be cleaned and is discharged to the outside of the system. However, it is preferable that the configuration is such that it is not discharged from the system other than the pipe 17b.

In addition, the cleaning device 11 includes a rinsing unit 11a including the rinsing tank 60 and a cleaning unit 11b including the cleaning tank 62, and a check valve 65 for preventing a backflow of the regenerated cleaning liquid 15b therebetween. Is provided.
Therefore, first, in the cleaning tank 62, the object to be cleaned is immersed in the cleaning liquid 30 and cleaned using it to remove solder, flux residue, and the like. When the cleaning liquid 15b stored in the cleaning tank 62 is contaminated more than a predetermined amount by solder, flux residue, or the like, the cleaning liquid 15b (30) containing the solder, flux residue, or the like is supplied to the cleaning liquid regenerator 10. It is.
On the other hand, the object to be cleaned that has been cleaned in the cleaning tank 62 is moved from the cleaning tank 62 to the rinsing tank 60, where the regenerated cleaning liquid 15a as a clean rinsing liquid is used to efficiently remove contaminants attached to the surface. To do. Since the regenerated cleaning liquid 15a regenerated in the cleaning liquid regenerating apparatus 10 is supplied to the rinsing tank 60 in a steady or non-steady manner, it can be stably rinsed using this as a rinsing liquid.
In addition, a part of the regenerated cleaning liquid 15a regenerated in the cleaning liquid regenerating apparatus 10 and supplied to the rinsing tank 60 overflows and is introduced into the cleaning tank 62 and used for cleaning the object to be cleaned. Since the check valve 65 is provided, the structure does not return to the rinsing tank 60.
In the cleaning device 11 shown in FIG. 7, for the sake of convenience, a rinsing section 11a including a rinsing tank 60, a cleaning section 11b including a cleaning tank 62, and a cleaning liquid regenerating apparatus 10 are sequentially arranged from the left. The cleaning liquid regenerating apparatus 10 is disposed below, above, or to the left of the rinsing portion 11a including the rinsing tank 60, and the rinsing portion 11a is disposed on the right side of the cleaning portion 11b. 65 may be provided.

2. Circulating Cleaning Device (1) Basic Configuration Further, as a basic configuration of the circulating cleaning device 12 shown in FIG. 7, an object to be cleaned is cleaned with the regenerated cleaning liquid 15 and the used cleaning liquid 30 after cleaning is supplied to the generation unit 13. Although the cleaning device 11 and the cleaning solution regeneration device 10 for generating the regeneration cleaning solution 15 are provided, the cleaning device 11 and the cleaning solution regeneration device 10 may be provided in a one-to-one correspondence. Good.
Alternatively, although not shown, a plurality of cleaning liquid regeneration devices may be provided for one cleaning device, and further, a single cleaning liquid regeneration device may be provided for a plurality of cleaning devices. .

Further, although the circulating cleaning device 12 includes the cleaning device 11 and the cleaning liquid regenerating device 10, as shown in FIG. 8, a part 10 b of the cleaning liquid regenerating device 10 rinses the cleaning device 11. You may be comprised so that the part 11a may be shared.
That is, the circulating cleaning apparatus 12 shown in FIG. 8 is an example in which the cleaning liquid tank 43 in the recovery unit 23 of the cleaning liquid regenerating apparatus 10 shown in FIG. 1 also serves as the rinse tank 60 in the cleaning apparatus 11.
Therefore, in the case of such a circulating cleaning device 12, such a rinsing tank 60 is used as a rinsing place for the object to be cleaned, and a main cleaning tank 62 for the object to be cleaned is provided on the right side of the rinsing tank 60. Therefore, the circulation cleaning device can be downsized as a whole.

(2) Basic Operation Next, the basic operation of the circulating cleaning apparatus 12 as shown in FIG. 7 will be described.
When the circulating cleaning device 12 is continuously operated, the cleaning device 11 sequentially supplies the regenerated cleaning liquid 15 from the cleaning liquid tank 43 guided by the pipe 17a to the rinse tank 60 while the flow rate is adjusted by the flow rate adjusting valve 17c. As a result, the rinse liquid 15a partially flows out of the rinse tank 60 and flows into the cleaning tank 62 to become the cleaning liquid 15b.
Therefore, the object to be cleaned is accommodated in the cleaning tank 62, and the object to be cleaned is cleaned by the cleaning liquid 15b there.
In this cleaning, the contaminants made of solid or liquid adhering to the object to be cleaned are transferred to the cleaning liquid, and the used cleaning liquid 30 in a state where the contaminants are mixed in the cleaning liquid is discharged from the cleaning device 11. The used cleaning liquid 30 is guided to the cleaning liquid regenerator 10 through the pipe 17b.

That is, in the cleaning liquid regenerating apparatus 10, the distillation source liquid 30 is stored in the generation unit 13 in advance and is heated by the heating unit 35 in the evaporation tank 31. In addition, the regenerated cleaning liquid 15 is stored in the cleaning liquid tank 43 of the recovery unit 23 in advance, and the regenerated cleaning liquid 15 is circulated and flowed in the circulation path 47 by the circulation pump 49 a, and is generated by the negative pressure generated by the suction unit 49. The part 13 is in a reduced pressure state.
Thereby, the inside of the production | generation part 13 is maintained by the operating condition which has the predetermined temperature and pressure according to the component and composition of the washing | cleaning liquid 15. FIG.

Then, in the circulating cleaning device 12 using such a cleaning liquid regenerating apparatus 10, the cleaning object is cleaned with the regenerating cleaning liquid 15 (rinsing liquid 15a, cleaning liquid 15b) from the pipe 17a of the cleaning liquid regenerating apparatus 10, and the rinse treatment is performed. It can be performed.
At the same time, since it includes the cleaning device 11 that supplies the contaminated used cleaning liquid 30 after cleaning to the generation unit 13 of the cleaning liquid regeneration device 10, between the cleaning device 11 and the cleaning liquid regeneration device 10, The regenerated cleaning solution 15 can be repeatedly circulated for use.

  At that time, the cleaning liquid regenerating apparatus 10 can perform a regeneration process for evaporating and recovering the used cleaning liquid without discharging each component of the regenerating cleaning liquid 15 out of the system. It can be used in a circulating manner.

In addition, in the generation unit 13 of the cleaning liquid regenerating apparatus 10, the respective blending components corresponding to the blending composition of the cleaning liquid 15 from the distillation source liquid 30 are continuously evaporated without using bumping and utilizing the gas-liquid equilibrium state. Therefore, since each compounding component corresponding to the cleaning liquid 15 is continuously and stably replenished as a used cleaning liquid to the generating unit 13, the mixing composition of the distillation source liquid 30 of the generating unit 13 can be maintained. it can.
Therefore, even if the cleaning liquid is circulated and used for a long period of time, a regenerated cleaning liquid having a predetermined composition can be continuously regenerated without performing any special component adjustment. The mixed cleaning liquid can be continuously supplied to the cleaning device for a long period of time to clean the workpiece.

(3) Cleaning liquid As the cleaning liquid, the same liquid as described in the first embodiment can be used. Further, a predetermined stock solution for a cleaning composition is prepared, and a predetermined amount of water is added thereto. It is also preferable to add it after use and use it as a cloudy cleaning liquid (cleaning agent composition).
That is, it is a stock solution for a cleaning composition for cleaning an object to be cleaned as a white turbid cleaning composition containing a predetermined amount of water, and the composition of the first organic solvent A hydrocarbon compound or aromatic compound having an SP value in the range of 6.5 to 12, and a nitrogen-containing compound having an SP value in the range of 8 to 15 as the second organic solvent, or A sulfur-containing compound and an ester compound having a SP value in the range of 8 to 12 as the third organic solvent, and the second organic solvent with respect to 100 parts by weight of the first organic solvent. Is a composition for a cleaning liquid having a value within the range of 5 to 1400 parts by weight and a blending amount of the third organic solvent within a range of 5 to 1400 parts by weight.
By comprising in this way, before adding a predetermined amount of water, it is a homogeneous solution, and after adding a predetermined amount of water, it is phase-separated and used as a white turbid cleaning solution, such as flux residue and solder paste An excellent detergency can be exhibited for an object to be cleaned.
That is, a hydrocarbon compound (for example, an aliphatic hydrocarbon) or an aromatic compound (for example, an aromatic hydrocarbon) having a SP value in the range of 6.5 to 12 as the first organic solvent The ester compound having an SP value in the range of 8 to 12 as the third organic solvent is a combination that is hardly compatible with each other. However, by including a predetermined amount of a nitrogen-containing compound (for example, an amine compound) or a sulfur-containing compound (for example, a sulfoxide compound) whose SP value as the second organic solvent is a value within the range of 8 to 15, In the stock solution for cleaning composition, the first organic solvent and the third organic solvent are compatible with each other to form a uniform solution.
And, when a predetermined amount of water is added later to the stock solution for the detergent composition, the effect of the second organic solvent changes, and the first organic solvent and the third organic solvent are: When incompatible and left to stand, the phases will separate. Although it becomes cloudy when it is put in a predetermined stirring state, it can show an excellent detergency against flux residue, solder paste and the like.
In addition, although the right or wrong of the cloudiness state in a cleaning composition can also be judged sensuously by visual observation, it can be quantitatively determined by the light transmittance of the cleaning composition as described later.

In addition, since such a stock solution for a detergent composition can be used by mixing with a relatively large amount of water, it efficiently provides a detergent composition excellent in environmental safety, handling, and reprocessing. can do.
More specifically, since it is possible to contain 60% by weight or more of water with respect to the total amount, it does not correspond to a dangerous material of the Fire Service Act.
Similarly, since a relatively large amount of water is contained, even if the cleaning composition is contaminated by use, it can be efficiently recycled and used.
Furthermore, with such a detergent composition stock solution, the user can change the blending ratio of the detergent composition stock solution and water in accordance with the degree of contamination in the object to be cleaned, etc. In addition, it is possible to efficiently provide a cleaning composition having different cleaning properties.

  Next, the first organic solvent, the second organic solvent, and the third organic solvent that constitute the stock solution for the detergent composition will be specifically described.

(First organic solvent)
Further, the first organic solvent constituting the stock solution for the detergent composition is a hydrocarbon compound or an aromatic compound having an SP value in the range of 6.5 to 12, and exhibits a predetermined detergency. This is an organic solvent to be blended.
That is, by using a hydrocarbon compound or aromatic compound having a predetermined SP value as the first organic solvent, the second organic solvent and the third organic solvent are mixed in a wide temperature range before mixing with a predetermined amount of water. When a uniform solution is composed together with an organic solvent and a predetermined amount of water is added afterwards, it becomes a white turbid cleaning composition and can exhibit a further excellent detergency.

  More specifically, the first organic solvent is a hydrocarbon compound or an aromatic compound that does not correspond to any of the second and third organic solvents or the fourth organic solvent described later. For example, anisole (SP value: 9.3, boiling point: 152 ° C., flash point: 52 ° C.), furfural (SP value: 10.2, boiling point: 162 ° C., flash point: 62 ° C.), methylstyrene (SP value) : 8.8, boiling point: 164 ° C, flash point: 54 ° C, myrcene (SP value: 7.7, boiling point: 167 ° C, flash point: 54 ° C), cumene (SP value: 9.0, boiling point: 169) , Flash point: 50 ° C., menthane (SP value: 7.2, boiling point: 170 ° C., flash point: 63 ° C.), phenetole (SP value: 9.0, boiling point: 170 ° C., flash point: 63 ° C.) Decane (SP value: 7.7, boiling point: 170 ° C., flash point: 53 ), Limonene (SP value: 7.8, boiling point: 175 ° C., flash point: 48 ° C.), cymene (SP value: 8.7, boiling point: 177 ° C., flash point: 47 ° C.), terpinene (SP value: 8) 0.0, boiling point: 180 ° C., flash point: 71 ° C., n-paraffin L (SP value: 8.9, boiling point: 189-229 ° C., flash point: 71 ° C.), indene (SP value: 6.8, Boiling point: 182 ° C, flash point: 78 ° C) Toluidine (SP value: 9.8, boiling point: 202 ° C, flash point: 85 ° C), durene (SP value: 9.2, boiling point: 192 ° C, flash point: 65 ° C.), benzylamine (SP value: 9.9, boiling point: 185 ° C., flash point: 72 ° C.), benzyl ethyl ether (SP value: 8.9, boiling point: 189 ° C., flash point: 73 ° C.), thio Anisole (SP value: 8.8, boiling point: 188 ° C, flash point: 72 ° C), dimethylaniline SP value: 9.9, boiling point: 188 ° C., flash point: 63 ° C., linalool (SP value: 9.4, boiling point: 198 ° C., flash point: 83 ° C.), methyl benzoate (SP value: 9.9) Boiling point: 199 ° C., flash point: 82 ° C., diisopropylbenzene (SP value: 8.3, boiling point: 202 ° C., flash point: 85 ° C.), swazole (SP value: 9.5, boiling point: 180-208 ° C., Flash point: 64 ° C), guaiacol (SP value: 10.2, boiling point: 205 ° C, flash point: 87 ° C), benzyl alcohol (SP value: 11.6, boiling point: 205 ° C, flash point: 93 ° C), Tetralin (SP value: 9.2, boiling point: 208 ° C, flash point: 77 ° C), N-methylbenzylamine (SP value: 9.5, boiling point: 180 ° C, flash point: 77 ° C), N, N- Dimethylbenzylamine (SP value: 9.8, boiling point: 181 ° C., Flash point: 60 ° C., α-phenylethylamine (SP value: 9.7, boiling point: 192 ° C., flash point: 79 ° C.), and phenethylamine (SP value: 9.7, boiling point: 198 ° C., flash point: 90) At least one aliphatic hydrocarbon or aromatic compound selected from the group consisting of benzylamine and benzyl alcohol. ) Is preferable.

In particular, the first organic solvent includes anisole, furfural, cumene, phenetole, decane, limonene, cymene, terpinene, n-paraffin, benzylamine, benzylethyl ether, methyl benzoate, diisoprobenzene, benzyl alcohol, toluidine, N It is preferably at least one selected from the group consisting of -methylbenzylamine, N, N-dimethylbenzylamine, α-phenylethylamine and phenethylamine.
The reason for this is that by using such a first organic solvent of this kind, excellent detergency can be obtained even with a relatively small amount of blending, and a decrease in drying property is relatively reduced. .
Therefore, the SP value in the first organic solvent is preferably set to a value within the range of 7 to 12, and more preferably set to a value within the range of 8 to 11.

Moreover, it is preferable to make the compounding quantity of a 1st organic solvent into the value within the range of 0.25 to 55 weight% with respect to the whole quantity.
The reason for this is that when the blending amount of the first organic solvent is less than 0.25% by weight, the cleaning effect on the flux or the like may be significantly reduced. On the other hand, if the blending amount of the first organic solvent exceeds 55% by weight, the amount of combustible liquid may exceed the predetermined amount, and may be handled as a hazardous material under the Fire Service Law. .
Therefore, in consideration of the balance between the cleanability and handleability, the blending amount of the first organic solvent is more preferably set to a value within the range of 1 to 50% by weight with respect to the total amount. More preferably, the value is within the range of 3 to 30% by weight.

FIG. 9 shows the results of studying the influence of the blending amount of the first organic solvent on the cleaning properties.
That is, the horizontal axis of FIG. 9 shows the blending amount (% by weight) of the first organic solvent in the detergent composition (including moisture) using the detergent composition stock solution according to Example 1. On the vertical axis, the evaluation results (relative values) of the detergency when using the detergent composition stock solution according to Example 1 are shown.
And the evaluation result (relative value) of detergency is represented by an evaluation score of 0 to 10, and the evaluation standard is as follows after setting the cleaning temperature of the flux to 70 ° C.
Evaluation point 10: The flux cleaning time is 0 to less than 10 minutes.
Evaluation point 9: The flux cleaning time is less than 10 to 12 minutes.
Evaluation point 8: The flux cleaning time is less than 12 to 15 minutes.
Evaluation point 7: The flux cleaning time is less than 15 to 17 minutes.
Evaluation point 6: The flux cleaning time is less than 17 to 20 minutes.
Evaluation point 5: The flux cleaning time is less than 20 to 25 minutes.
Evaluation point 4: The flux cleaning time is less than 25 to 30 minutes.
Evaluation point 3: The flux cleaning time is less than 30 to 40 minutes.
Evaluation point 2: The flux cleaning time is less than 40 to 50 minutes.
Evaluation point 1: The flux cleaning time is less than 50 to 60 minutes.
Evaluation point 0: The flux cleaning time is 60 minutes or more.

As shown in the characteristic curve of FIG. 9, the blending amount of the first organic solvent in the detergent composition stock solution is, for example, 0.25 to 55% by weight indicated by range A in the figure with respect to the total amount. If it is the range of this, when it is set as the cleaning composition which contains a predetermined amount of water, favorable detergency is acquired.
On the other hand, when the blending amount of the first organic solvent is less than 0.25% by weight or exceeds 55% by weight, the cleaning performance when a cleaning composition containing a predetermined amount of water is used. It is understood that the evaluation result is significantly reduced.
In addition, even in consideration of differences in blending components and blending amounts, it is understood that even better detergency can be obtained, for example, within the range of 1 to 50% by weight indicated by range B in the figure. The
Accordingly, by limiting the blending amount of the first organic solvent in the detergent composition stock solution to a value within a predetermined range, a good detergency can be obtained when the detergent composition contains a predetermined amount of water. It is understood.
Therefore, it can be said that it is preferable to limit the blending amount of the first organic solvent in the detergent composition stock solution of the present invention to a predetermined range from the detergency when a cleaning composition containing a predetermined amount of water is used.

(Second organic solvent)
The second organic solvent is a nitrogen-containing compound (for example, an amine compound or a pyrrolidone compound) or a sulfur-containing compound (for example, a sulfoxide compound) having an SP value in the range of 8 to 15, or any one of them. A compound.
That is, the second organic solvent improves the detergency when it is used as a cleaning composition, and before mixing with a predetermined amount of water, phase separation between the first organic solvent and the third organic solvent is performed. It is an organic solvent to be blended in order to effectively prevent water and provide a stock solution for a detergent composition as a uniform solution.

  More specifically, the second organic solvent is a nitrogen-containing compound or sulfur-containing compound that does not correspond to any of the first and third organic solvents or the fourth organic solvent described later. For example, 2-ethylhexylamine (SP value: 8.4, boiling point: 168 ° C, flash point: 53 ° C), monoisopropanolamine (SP value: 12.7, boiling point: 160 ° C, flash point: 74 ° C), N-ethylethanolamine (SP value: 11.4, boiling point: 169 ° C, flash point: 71 ° C), N, N-dimethylacetamide (SP value: 11.1, boiling point: 166 ° C, flash point: 70 ° C) N-methylformamide (SP value: 11.8, boiling point: 183 ° C, flash point: 98 ° C), dimethyl sulfoxide (SP value: 13.0, boiling point: 189 ° C, flash point: 95 ° C), N-methyl -2-Pyro At least selected from the group consisting of dong (SP value: 11.2, boiling point: 204 ° C., flash point: 91 ° C.), and diethanolamine (SP value: 14.4, boiling point: 269 ° C., flash point: 134 ° C.) One amine compound or pyrrolidone compound.

In particular, as the second organic solvent, at least one amine compound selected from the group consisting of 2-ethylhexylamine, monoisopropanolamine, dimethyl sulfoxide, N-methyl-2-pyrrolidone, diethanolamine, N, N-dimethylacetamide And pyrrolidone compounds are preferred.
The reason for this is that by using the second organic solvent of this kind, before mixing with a predetermined amount of water, the first organic solvent and the third organic solvent are mixed in a wide temperature range. This is because it effectively prevents phase separation and composes a uniform solution, and when a predetermined amount of water is added afterwards, it becomes a cloudy detergent composition and can exhibit further superior detergency. is there.
Therefore, the SP value in the second organic solvent is preferably set to a value within the range of 9 to 14, and more preferably set to a value within the range of 10 to 13.5.

Moreover, let the compounding quantity of a 2nd organic solvent be a value within the range of 5-1400 weight part with respect to 100 weight part of 1st organic solvents.
The reason for this is that when the blending amount of the second organic solvent is less than 5 parts by weight, the detergency of the cleaning composition may be significantly reduced.
On the other hand, when the blending amount of the second organic solvent exceeds 1400 parts by weight, the cleaning property and drying property of the cleaning composition may be significantly reduced.
Therefore, it is more preferable to set the blending amount of the second organic solvent to a value within the range of 10 to 600 parts by weight with respect to 100 parts by weight of the first organic solvent, and within a range of 30 to 350 parts by weight. More preferably, it is a value.

Moreover, the result of having examined the influence with respect to the washability of the compounding quantity of a 2nd organic solvent in FIG. 10 is shown.
That is, the horizontal axis of FIG. 10 shows the blending amount (parts by weight) of the second organic solvent in the detergent composition stock solution according to Example 1, and the vertical axis shows the detergent composition. The evaluation results (relative values) of the detergency in the detergent composition using the stock solution are shown.
And the evaluation result (relative value) of the washing | cleaning property is represented by the evaluation score of 0-10, The evaluation criteria are the same as that of the case of FIG.
And as the characteristic curve of this FIG. 10 shows, the compounding quantity of the 2nd organic solvent in detergent composition undiluted | stock solution is 5 to 5 shown with the range A with respect to 100 weight part of 1st organic solvents, for example. If it is in the range of 1400 parts by weight, good detergency with an evaluation score of 8 or more is obtained.
On the other hand, it is understood that when the blending amount of the second organic solvent becomes a value less than 5 parts by weight or exceeds 1400 parts by weight, the detergency evaluation result is remarkably lowered.
In addition, even if the difference in the blending components and the variation in the blending amount are taken into account, for example, if the range is 10 to 600 parts by weight indicated by the range B, a better cleaning property with an evaluation score of about 10 can be obtained. Is understood.
Therefore, it is understood that good detergency can be obtained by limiting the blending amount of the second organic solvent in the detergent composition stock solution to a value within a predetermined range.

(Third organic solvent)
Moreover, the 3rd organic solvent which comprises the stock solution for cleaning composition is an ester compound whose SP value is the value within the range of 8-12, Comprising: The drying property at the time of setting it as a cleaning composition improves Therefore, it is an organic solvent to be blended.
And the 3rd organic solvent is an organic solvent mix | blended in order to provide the stock solution for cleaning composition as a uniform solution with the 1st and 2nd organic solvent before mixing with predetermined amount of water. .
More specifically, the third organic solvent is an ester compound that does not fall into any of the first to second organic solvents and the fourth organic solvent described later, and includes, for example, propylene glycol monomethyl. Ether acetate (SP value: 9.2, boiling point: 146 ° C., flash point: 47 ° C.), 3-methoxybutyl acetate (SP value: 9.3, boiling point: 173 ° C., flash point: 63 ° C.), 3-methoxy -3-methylbutyl acetate (SP value: 9.2, boiling point: 188 ° C, flash point: 73 ° C), propylene glycol diacetate (SP value: 10.4, boiling point: 190 ° C, flash point: 93 ° C), Ethylene glycol monobutyl ether acetate (SP value: 9.0, boiling point: 192 ° C., flash point: 88 ° C.), butyl lactate (SP value: 10.5, boiling point: 188 ° C., flash point: 71 ), Methyl acetoacetate (SP value: 11.6, boiling point: 172 ° C., flash point: 77 ° C.), ethyl acetoacetate (SP value: 10.7, boiling point: 181 ° C., flash point: 75 ° C.), anhydrous propion Acid (SP value: 10.5, boiling point: 167 ° C, flash point: 74 ° C), butyric anhydride (SP value: 9.7, boiling point: 199 ° C, flash point: 88 ° C), diethyl oxalate (SP value: At least one ester selected from the group consisting of 10.8, boiling point: 189 ° C, flash point: 76 ° C, and octanoic acid ester (SP value: 8.4, boiling point: 208 ° C, flash point: 75 ° C) A compound.

In particular, the third organic solvent is selected from the group consisting of propylene glycol monomethyl ether acetate, 3-methoxybutyl acetate, 3-methyl-3-methoxybutyl acetate, propylene glycol diacetate, and ethylene glycol monobutyl ether acetate. Preferably, it is at least one ester compound.
The reason for this is that by using the third organic solvent of this kind, before mixing with a predetermined amount of water, a uniform solution is formed together with the first organic solvent and the second organic solvent in a wide temperature range. This is because when a predetermined amount of water is added after composition, a more excellent detergency can be exhibited as a cloudy detergent composition.
Therefore, the SP value in the third organic solvent is preferably set to a value within the range of 8.5 to 11.5, and more preferably set to a value within the range of 9 to 11.

Moreover, let the compounding quantity of a 3rd organic solvent be the value within the range of 5-1400 weight part with respect to 100 weight part of 1st organic solvents.
This is because when the blending amount of the third organic solvent is less than 5 parts by weight, the drying property when the cleaning composition is constituted from the cleaning composition stock solution may be significantly reduced. is there.
On the other hand, when the blending amount of the third organic solvent exceeds 1400 parts by weight, the detergency when the detergent composition is constituted from the detergent composition stock solution may be significantly reduced. .
Therefore, it is more preferable to set the blending amount of the third organic solvent to a value within the range of 10 to 600 parts by weight with respect to 100 parts by weight of the first organic solvent, and within a range of 30 to 350 parts by weight. More preferably, it is a value.

FIG. 11 shows the results of studying the influence of the blending amount of the third organic solvent on the cleaning properties.
That is, the horizontal axis of FIG. 11 shows the blending amount (parts by weight) of the third organic solvent in the detergent composition stock solution according to Example 1, and the vertical axis shows the detergent composition. The evaluation results (relative values) of the detergency in the detergent composition using the stock solution are shown.
Moreover, the evaluation result (relative value) of the detergency is expressed by evaluation points of 0 to 10, and the evaluation criteria are the same as those in FIG.
And as the characteristic curve of this FIG. 11 shows, as the compounding quantity of the 3rd organic solvent in detergent composition undiluted | stock solution shows with the 1st organic solvent 100 weight part, for example, with the range A If the value is 1400 parts by weight or less, a good cleaning property with an evaluation score of 8 or more is obtained. As shown by the range B, if the value is 600 parts by weight or less, the evaluation score is 10 or more. Detergency is obtained.
However, it is understood that the evaluation result of the detergency is good even when the blending amount of the third organic solvent is 0 part by weight.

On the other hand, in FIG. 12, the result of having examined the influence with respect to drying property of the compounding quantity of a 3rd organic solvent is shown.
That is, the horizontal axis of FIG. 12 shows the blending amount (parts by weight) of the third organic solvent in the detergent composition stock solution according to Example 1, and the vertical axis shows the detergent composition. The evaluation result (relative value) of the drying property in the cleaning composition using the stock solution is shown.
And the evaluation result (relative value) of dryness is represented by the evaluation score of 0-10, and the evaluation criteria are as follows in the conditions of the drying temperature of 100 degreeC.
Evaluation point 10: Drying time is 0 to less than 5 minutes.
Evaluation point 9: The drying time is less than 5 to 7 minutes.
Evaluation point 8: The drying time is less than 7 to 10 minutes.
Evaluation point 7: The drying time is less than 10 to 12 minutes.
Evaluation point 6: The drying time is less than 12 to 15 minutes.
Evaluation point 5: The drying time is less than 15 to 17 minutes.
Evaluation point 4: The drying time is 17 to less than 20 minutes.
Evaluation point 3: The drying time is 20 to less than 22 minutes.
Evaluation point 2: The drying time is less than 22 to 25 minutes.
Evaluation point 1: The drying time is less than 25 to 30 minutes.
Evaluation point 0: The drying time is 30 minutes or more.

As shown in the characteristic curve of FIG. 12, if the blending amount of the third organic solvent in the detergent composition stock solution is a value of 10 parts by weight or more as shown by the range A with respect to the total amount, Good dryability with an evaluation score of 8 or more is obtained, and as shown by the range B, if the value is 20 parts by weight or more, even better dryability with an evaluation score of about 10 is obtained.
Therefore, it is understood that good drying properties can be obtained by limiting the blending amount of the third organic solvent in the detergent composition stock solution to a value within a predetermined range.
Therefore, when the evaluation result of the cleaning property described above is taken into consideration, by limiting the blending amount of the third organic solvent in the cleaning agent composition stock solution to a value within a predetermined range, it is possible to achieve good cleaning properties and drying properties. Can balance.

FIG. 13 shows the results of examining the influence of the blending amount of the third organic solvent on the flash point of the detergent composition stock solution.
That is, the horizontal axis of FIG. 13 shows the blending amount (parts by weight) of the third organic solvent in the detergent composition stock solution according to Example 1, and the vertical axis shows the detergent composition. The flash point (° C) of the stock solution is taken.
As shown in the characteristic curve of FIG. 13, if the blending amount of the third organic solvent in the detergent composition stock solution is, for example, a value of 50 parts by weight or more with respect to the total amount, it is 75 ° C. or more. A relatively high flash point value is obtained.
Therefore, in addition to the evaluation results of the cleaning property and drying property described above, by limiting the blending amount of the third organic solvent in the detergent composition stock solution to a value within a predetermined range, not only the flash point, A balance between good cleanability and dryness can be achieved.

(4th organic solvent)
Further, when constituting the stock solution for the detergent composition, as the fourth organic solvent, a glycol ether or alcohol compound having an SP value in the range of 8.5 to 12 is further added, and the fourth organic solvent is added. The blending amount of the organic solvent is preferably set to a value in the range of 5 to 600 parts by weight with respect to 100 parts by weight of the first organic solvent.
The reason for this is that by adding a predetermined amount of such a fourth organic solvent, the second organic solvent is supplemented, and phase separation between the first organic solvent and the third organic solvent is performed. This is because it can be effectively prevented.

Here, the fourth organic solvent is a glycol ether or an alcohol compound that does not correspond to any of the first to third organic solvents.
More specifically, propylene glycol monopropyl ether (SP value: 9.6, boiling point: 150 ° C., flash point: 48 ° C.), propylene glycol monobutyl ether (SP value: 9.0, boiling point: 171 ° C., flash point: 62 ° C.), dipropylene glycol dimethyl ether (SP value: 8.7, boiling point: 171 ° C., flash point: 65 ° C.), ethylene glycol monoisobutyl ether (SP value: 9.1, boiling point: 161 ° C., flash point: 56) ° C), ethylene glycol monoisopropyl ether (SP value: 10.9, boiling point: 142 ° C, flash point: 46 ° C), furfuryl alcohol (SP value: 11.9, boiling point: 171 ° C, flash point: 65 ° C) , And 3-methoxy-3-methyl-1-butanol (SP value: 10.5, boiling point: 174 ° C, flash point: 68 ° C), etc. That.

Moreover, it is preferable to make the compounding quantity of a 4th organic solvent into the value within the range of 5-600 weight part with respect to 100 weight part of 1st organic solvents.
This is because when the amount of the fourth organic solvent is less than 5 parts by weight, the addition effect may not be exhibited.
On the other hand, when the blending amount of the fourth organic solvent exceeds 600 parts by weight, the detergency may be remarkably deteriorated.
Therefore, it is more preferable to set the blending amount of the fourth organic solvent to a value within the range of 10 to 250 parts by weight with respect to 100 parts by weight of the first organic solvent, and within a range of 15 to 150 parts by weight. More preferably, it is a value.

(Surfactant)
Further, the surfactant is added to emulsify or solubilize the above-described first to third organic solvents or the first to fourth organic solvents in water. In order to improve the affinity with respect to and, as a result, improve the cleaning property, it is preferable to mix in the cleaning composition.
Here, as preferable examples of the surfactant, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene polypropylene alkyl ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene which are nonionic surfactants are used. A single type of glycol fatty acid ester, polyoxyethylene alkylamine, polyoxyethylene benzyl alcohol, polyglycerin fatty acid ester, or a combination of two or more types may be mentioned.

Moreover, it is preferable to make the compounding quantity of surfactant into the value within the range of 0.01 to 5 weight% with respect to the whole quantity of a cleaning composition, for example.
The reason for this is that when the amount of the surfactant is less than 0.01% by weight, the compatibility of the first to third organic solvents described above becomes insufficient, and the stock solution for the detergent composition is used. This is because it may be easy to separate.
On the other hand, if the amount of the surfactant exceeds 5% by weight, the amount remaining on the object to be cleaned increases, and a rinsing step becomes essential, or the electrical characteristics of the object to be cleaned are deteriorated. Because there is.
Accordingly, in consideration of the balance between the emulsifiability and the persistence, the amount of the surfactant is more preferably set to a value in the range of 0.05 to 2% by weight with respect to the total amount. More preferably, the value is in the range of 0.1 to 2% by weight.

(amount of water)
When the multi-component cleaning composition (used cleaning composition) contains water as a blending component, the water content in the cleaning composition is 40 to 40% of the total amount. A value within the range of 90% by weight is preferred.
This is because, when the water content is less than 40% by weight, the low VOC property, safety, handleability, etc. in the cleaning composition may be significantly reduced.
On the other hand, when the content of water exceeds 90% by weight, the cleaning property and the regenerating property in the cleaning composition may be remarkably deteriorated.
Therefore, the content of water in the cleaning composition is more preferably set to a value in the range of 60 to 90% by weight, and a value in the range of 65 to 90% by weight with respect to the total amount. Further preferred.

In addition, with respect to the amount of water, a predetermined amount of water is post-added to the stock solution for the detergent composition to form a predetermined detergent composition in order to be in a cloudy state and exhibit excellent detergency.
That is, by adding a relatively large amount of water to the stock solution for the detergent composition, the effect of the second organic solvent is changed, and the first organic solvent, the third organic solvent, Separation can be promoted to become a cloudy detergent composition, which can exhibit excellent detergency.
In addition, since it contains a relatively large amount of water, it is possible to efficiently provide a cleaning composition excellent in environmental safety, handleability, and reprocessing.
In addition, the user can change the blending ratio of the detergent composition stock solution and water according to the degree of contamination and the type of contaminants in the object to be cleaned. A cleaning composition can be provided.

Moreover, it is preferable to make the compounding quantity of water into the value within the range of 50-1900 weight part with respect to 100 weight part of stock solutions for cleaning composition.
The reason for this is that when the amount of water is less than 50 parts by weight, not only the washability is deteriorated, but also the safety and the handleability may be lowered.
On the other hand, if the amount of water exceeds 1900 parts by weight, the detergency may be significantly reduced.
Therefore, the amount of water is more preferably set to a value in the range of 150 to 900 parts by weight, and a value in the range of 175 to 600 parts by weight with respect to 100 parts by weight of the stock solution for the detergent composition. More preferably.

Here, in FIG. 14, the result of having examined the influence of the compounding quantity of water with respect to 100 weight part of undiluted | determinated solutions for cleaning compositions in a washability is shown.
That is, the horizontal axis of FIG. 14 shows the amount of water blended (parts by weight) with respect to 100 parts by weight of the detergent composition stock solution according to Example 1, and the vertical axis shows the detergent composition stock solution. The evaluation results (relative values) for the detergency in the cleaning composition composed of
As shown in the characteristic curve of FIG. 14, the amount of water to 100 parts by weight of the detergent composition stock solution is within the range of 50 to 1900 parts by weight with respect to the total amount, for example, as shown by Range A. If it is the value of this, the favorable detergency of the evaluation point 8 or more is obtained.
For example, as shown by the range B, if the value is in the range of 65 to 900 parts by weight, good cleanability of the evaluation point 10 is obtained.
Therefore, it is understood that, by limiting the blending amount of water with respect to 100 parts by weight of the detergent composition stock solution to a value within a predetermined range, good cleaning properties can be obtained in the cleaning composition obtained therefrom.

(Light transmittance)
Moreover, it is preferable to set the light transmittance (visible light / 750 nm standard) that is a standard of the cloudiness state of the cleaning composition to a value within 80%.
The reason for this is that when the light transmittance exceeds 80%, the solution becomes close to a uniform solution, or the phase separation becomes excessive, and the white turbid state cannot be maintained. This is because there may be a significant decrease.
On the other hand, if the light transmittance of such a cleaning composition is excessively small, phase separation becomes insufficient, and it may be difficult to control the cleaning properties, or the cleaning effect on flux or the like may be reduced. Because there is.
Therefore, the light transmittance of the cleaning composition is more preferably set to a value within the range of 0.5 to 60%, and further preferably set to a value within the range of 3 to 40%.
In addition, the light transmittance with respect to visible light of a cleaning composition can be measured as described in Example 1 using a spectrophotometer.

[Example 1]
In Example 1, as shown in FIG. 1, using a cleaning liquid having a composition in which water, N-methylpyrrolidone (NMP), and propylene glycol monobutyl ether (BFG) are 15:20:65 wt%. It was confirmed whether or not the composition of the cleaning liquid could be stably maintained by configuring the circulating cleaning device and operating continuously.
Therefore, each compounding component was mixed at a ratio as shown in Table 1 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
In addition, since the cleaning liquid of Example 1 has a uniform composition without phase separation, its light transmittance was 100%.

Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Furthermore, the light transmittance of the cleaning liquid (cleaning agent composition) was measured as follows. That is, 200 g of the obtained cleaning composition was accommodated in a beaker having a capacity of 300 ml. The magnetic stirrer in the beaker was then rotated at about 700 rpm. Next, the cleaning composition in that state was quickly accommodated in a spectrophotometer cell and allowed to stand for 5 minutes, and the light transmittance at that time was measured based on the following conditions.
Measuring device: Spectrophotometer (manufactured by Hitachi, Ltd.)
Measurement light: Visible light (wavelength 750 nm)
Measurement temperature: Room temperature (25 ° C)

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 1 and charged into the evaporation tank.
Here, since the composition of the temporary distillation source liquid fluctuates at the start of operation of the circulating washing apparatus, the temporary distillation source liquid was prepared to be an appropriate distillation source liquid when reaching a steady state. This temporary distillation source liquid is based on FIGS. 2 to 4 which are correlation diagrams between the liquid phase composition and the gas phase composition under the operating condition of the cleaning liquid regenerating apparatus, and the above-described equations (2) to (5). The blending composition of the distillation source liquid was calculated so as to establish a vapor-liquid equilibrium with the cleaning liquid vapor having the cleaning liquid composition, and the amount charged was set.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the agglomeration unit are measured over time, and in the cleaning solution tank. The composition of the stored cleaning liquid was measured over time. The results are shown in Table 1.
Further, the number of bumps generated between 1 hour and 1 hour after the start, the number of bumps generated between 10 hours and 11 hours, and the number of bumps generated between 100 hours and 101 hours were measured.

As is apparent from the results in Table 1, the composition of the regenerated cleaning liquid stored in the cleaning liquid tank has a light transmittance of 100% even after the circulating cleaning apparatus is continuously operated for 10 hours and 100 hours, respectively. It was confirmed that the initial composition of the cleaning liquid was substantially maintained.
In addition, since the value at the start of operation of the blend composition of the distillation source liquid is a value before the used cleaning liquid is started to be supplied to the generation unit, although the initial fluctuation is large, it is stable after the start of operation. It was. Therefore, after reaching a steady state, it became a liquid having a blending composition of water: NMP: BFG = 2: 43: 55 wt% as an appropriate distillation source liquid.
Therefore, according to this circulating cleaning apparatus, it has been confirmed that the desired composition of the cleaning liquid can be maintained even if it is continuously operated for a long period of time.
Further, according to the specification of the circulating cleaning apparatus of Example 1, it was confirmed that the bumping phenomenon does not occur even after a long period of time as well as the initial stage.

[Example 2]
In Example 2, except that the specification of the circulating cleaning apparatus of Example 1 was changed as follows, the circulating cleaning apparatus was driven in the same manner as in Example 1, and the composition of the cleaning liquid was measured over time. The number of bumps was measured. The obtained results are shown in Table 2.
In addition, since the cleaning liquid of Example 2 has a uniform composition without phase separation, the light transmittance was 100%.
Opening area (A) of connecting part: 9,000 mm ²
Heater capacity (B): 1.5 kW
Cleaning fluid vapor transfer coefficient (C): 6,000 mm ² / kW
Water vapor transfer coefficient (D): 0.1 m / sec

As is clear from the results in Table 2, the composition of the regenerated cleaning liquid stored in the cleaning liquid tank is light transmissive even after the circulating cleaning apparatus in Example 2 is continuously operated for 10 hours and 100 hours, respectively. It was confirmed that the initial composition of the cleaning liquid having a rate of 100% was maintained.
Moreover, according to the specification of the circulating cleaning apparatus of Example 2, it was confirmed that the bumping phenomenon does not occur even after a long period of time as well as the initial stage.

[Example 3]
In Example 3, except that the specification of the circulating cleaning apparatus of Example 1 was changed as follows, the circulating cleaning apparatus was driven in the same manner as in Example 1, and the composition of the cleaning liquid was measured over time. The number of bumps was measured. The obtained results are shown in Table 3.
In addition, since the cleaning liquid of Example 3 has a uniform composition without phase separation, its light transmittance was 100%.
Opening area (A) of connecting part: 15,000 mm ²
Heater capacity (B): 5kW
Cleaning fluid vapor transfer coefficient (C): 3,000 mm ² / kW
Water vapor transfer coefficient (D): 0.2 m / sec

As is apparent from the results in Table 3, the composition of the regenerated cleaning liquid stored in the cleaning liquid tank is such that the light transmittance is maintained even after the circulating cleaning apparatus in Example 3 is continuously operated for 10 and 100 hours, respectively. It was confirmed that the initial blending composition of the cleaning liquid with 100% was maintained.
Moreover, according to the specification of the circulating cleaning apparatus of Example 3, it was confirmed that the bumping phenomenon does not occur even after a long period of time as well as the initial stage.

[Example 4]
In Example 4, as shown in FIG. 7, using a cleaning liquid having a composition of water, N, N-dimethylacetamide (DMAC), and propylene glycol monobutyl ether (BFG) at 15:40:45 wt%. It was confirmed whether the composition of the cleaning liquid could be stably maintained by configuring a simple circulating cleaning device and operating continuously.
Therefore, each compounding component was mixed at a ratio as shown in Table 4 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
In addition, since the cleaning liquid of Example 4 has a uniform composition without phase separation, its light transmittance was 100%.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 4 and charged into the evaporation tank.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the agglomeration unit are measured over time, and in the cleaning solution tank. The composition of the stored cleaning liquid was measured over time. The results are shown in Table 4.
Further, the number of bumps generated between 1 hour and 1 hour after the start, the number of bumps generated between 10 hours and 11 hours, and the number of bumps generated between 100 hours and 101 hours were measured.

As is clear from the results in Table 4, the composition of the cleaning liquid stored in the cleaning liquid tank has a light transmittance of 100% even after the circulating cleaning apparatus is continuously operated for 10 hours and 100 hours, respectively. The initial composition of the cleaning liquid could be substantially maintained.
Therefore, according to this circulating cleaning apparatus, it was confirmed that the composition of the desired cleaning liquid can be maintained even if it is continuously operated for a long period of time.
Moreover, according to the specification of the circulating cleaning apparatus of Example 4, it was confirmed that the bumping phenomenon does not occur even after a predetermined time has passed, not to mention the initial stage.

[Example 5]
In Example 5, 69: 10: 1: 15 water, monoisopanolamine (MIPA), benzylamine (BAN), ethylene glycol monobutyl ether acetate (BGAC), and benzyl alcohol (BAL) : Using a cleaning liquid having a blending composition of 5% by weight, a circulating cleaning apparatus as shown in FIG. 7 is configured and continuously operated, so that the blending composition of the cleaning liquid in a cloudy state (light transmittance 5%) It was confirmed whether it could be maintained stably.
Therefore, each compounding component was mixed at a ratio as shown in Table 5 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 5 and charged into the evaporation tank. Here, the temporary distillate solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 5.

[Example 6]
In Example 6, water, N-methyl-2-pyrrolidone (NMP), dimethyl sulfoxide (DMSO), 3-methoxy-3-methyl-1-butanol (MMB), and propylene glycol diacetate (PGDA) FIG. 7 shows a cleaning solution having a composition of 70: 2: 2: 7: 9: 9: 2 wt% of methoxybutyl acetate (Metace) and propylene glycol monomethyl ether acetate (PMA). By configuring such a circulating cleaning apparatus and continuously operating, it was confirmed whether or not the initial blending composition of the cleaning liquid that becomes a cloudy state (light transmittance of 10%) during cleaning can be stably maintained.
Therefore, each compounding component was mixed at a ratio as shown in Table 6 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 6 and charged into the evaporation tank. In addition, a temporary distillation source solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 6.

[Comparative Example 1]
In Comparative Example 1, except that the specification of the circulating cleaning apparatus of Example 1 was changed as follows, the circulating cleaning apparatus was driven and the blending composition of the cleaning liquid was measured over time, as in Example 1. The number of bumps was measured. The results obtained are shown in Table 7.
Opening area (A) of connecting part: 300 mm ²
Heater capacity (B): 5kW
Cleaning liquid vapor transfer coefficient (C): 60 mm ² / kW
Water vapor transfer coefficient (D): 9 m / sec

As is apparent from the results in Table 7, the composition of the regenerated cleaning liquid stored in the cleaning liquid tank is the original composition after the circulating cleaning apparatus in Comparative Example 1 was continuously operated for 10 hours and 100 hours, respectively. It was confirmed that the ratio deviated considerably.
Further, according to the specification of the circulating cleaning apparatus of Comparative Example 1, it was confirmed that a predetermined number of bumping phenomena occurred not only in the initial stage but also after a long period of time.

[Comparative Example 2]
In Comparative Example 2, except that the specification of the circulating cleaning apparatus of Example 4 was changed as follows, the circulating cleaning apparatus was driven and the blending composition of the cleaning liquid was measured over time, as in Example 1. The number of bumps was measured. Table 8 shows the obtained results.
Opening area (A) of connecting part: 180 mm ²
Heater capacity (B): 5kW
Cleaning fluid vapor transfer coefficient (C): 36 mm ² / kW
Water vapor transfer coefficient (D): 15 m / sec

As is clear from the results in Table 8, the composition of the regenerated cleaning liquid stored in the cleaning liquid tank is the original composition after the circulating cleaning apparatus in Comparative Example 2 was continuously operated for 10 hours and 100 hours, respectively. A slight deviation from the ratio was confirmed.
Moreover, according to the specification of the circulating cleaning apparatus of Comparative Example 2, it was confirmed that a predetermined number of bumping phenomena occur not only in the initial stage but also after a long period of time.

[Example 7]
In Example 7, water, N-ethylethanolamine (MEM), propylene glycol monobutyl ether (BFG), and ethylene glycol monoisobutyl ether (iBG) were blended at 70: 2: 19: 9% by weight. By constructing a circulating cleaning device as shown in FIG. 7 using the cleaning liquid of the composition and continuously operating, the initial composition of the cleaning liquid that becomes white turbid (10% light transmittance) at the time of cleaning is stably maintained. I confirmed that it was possible.
Therefore, each compounding component was mixed at a ratio as shown in Table 9 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 9 and charged into the evaporation tank. In addition, a temporary distillation source solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 9.

[Example 8]
In Example 8, water, 1-decene, N-ethylethanolamine (MEM), N-methyl-2-pyrrolidone (NMP), 1-hexanol, and 2-heptanone (MAK) are 70: 17.1: 0.1: 4.3: 4.2: 4.3% by weight, using a cleaning solution having a blending composition, configure a circulating cleaning device as shown in FIG. 7 and operate continuously. Thus, it was confirmed whether or not the initial blending composition of the cleaning liquid that becomes a cloudy state (light transmittance of 5%) during the cleaning can be stably maintained.
Therefore, each compounding component was mixed at a ratio as shown in Table 10 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 10 and charged into the evaporation tank. In addition, a temporary distillation source solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 10.

[Example 9]
In Example 9, as shown in FIG. 7, using a cleaning liquid having a composition in which water, propylene glycol monobutyl ether (BFG), and ethylene glycol monoisobutyl ether (iBG) are 70:17:13 wt%. By configuring a circulating cleaning device and continuously operating, it was confirmed whether or not the initial blending composition of the cleaning liquid that becomes a cloudy state (light transmittance 30%) at the time of cleaning can be stably maintained.
Therefore, each compounding component was mixed at a ratio as shown in Table 11 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 11 and charged into the evaporation tank. In addition, a temporary distillation source solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 11.

[Example 10]
In Example 10, a cleaning liquid having a composition in which water, 3-methoxy-3-methyl-1-butanol (MMB), and N-ethylethanolamine (MEM) are 70: 28: 2 wt% is used. Then, it was confirmed whether or not the initial blending composition of the cleaning liquid can be stably maintained by configuring a circulating cleaning apparatus as shown in FIG. 7 and operating continuously.
Therefore, each compounding component was mixed at a ratio as shown in Table 12 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
In addition, since the cleaning liquid of Example 10 has a uniform composition without phase separation, the light transmittance was 100%.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 12, and charged into the evaporation tank. In addition, a temporary distillation source solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 12.

[Example 11]
In Example 11, a circulating cleaning apparatus as shown in FIG. 7 was constructed using a cleaning liquid having a composition in which water and propylene glycol monopropyl ether (PFG) were 60: 40% by weight. By operating, it was confirmed whether the initial composition of the cleaning liquid could be stably maintained.
Therefore, each compounding component was mixed at a ratio as shown in Table 13 to prepare a cleaning liquid, which was put into a cleaning liquid tank.
In addition, since the cleaning liquid of Example 11 has a uniform composition without phase separation, the light transmittance was 100%.
Moreover, the specification of the circulating cleaning apparatus was as follows.
Opening area (A) of connecting part: 5,000 mm ²
Heater capacity (B): 0.5 kW
Transfer coefficient of cleaning liquid vapor (C): 10,000 mm ² / kW
Water vapor transfer coefficient (D): 0.06 m / sec

Next, a temporary distillation source liquid corresponding to the cleaning liquid charged in the cleaning liquid tank was prepared as shown in Table 13, and charged into the evaporation tank. In addition, a temporary distillation source solution was prepared according to the method of Example 1.
In this state, the circulating cleaning device is operated, and after reaching a substantially steady state, the temperature and pressure of the generation unit and the flow rate of the condensate from the generation unit are measured over time, and in the cleaning liquid tank. The composition of the stored cleaning liquid was measured over time. In addition, the number of bumps that occurred between 1 hour and 1 hour after the start, the number of bumps that occurred between 10 hours and 11 hours, and the number of bumps that occurred between 100 hours and 101 hours were measured. The results are shown in Table 13.

According to the cleaning liquid regenerating apparatus of the present invention, not only the non-aqueous solvent but also the non-aqueous solvent is taken into account by taking into consideration the moving speed of the cleaning liquid vapor and by vacuum distillation using the vapor-liquid equilibrium between the cleaning liquid vapor as the gas phase and the liquid phase. Even if it is a water-based solvent, and even if it is a cleaning liquid consisting of a plurality of components that are in a phase separation state (white turbid state at the time of cleaning) in a stationary state, it is efficient while substantially maintaining the initial composition. It became possible to reproduce automatically.
Moreover, according to the circulating cleaning apparatus of the present invention, by providing a predetermined cleaning liquid regenerating apparatus that performs vacuum distillation using gas-liquid equilibrium, even in the case of an aqueous solvent, the phase separation state ( It has become possible to provide a circulating cleaning apparatus that can be stably circulated over a long period of time even with a cleaning liquid composed of a plurality of components that are in a cloudy state at the time of cleaning.
In addition, it is a predetermined type, and by using it as a stock solution for a cleaning composition using an organic solvent having a predetermined SP value, it contains a predetermined amount of water, and in a stationary state, it is in a phase-separated state (at the time of cleaning, a cloudy state) Since the cleaning liquid consisting of a plurality of components can be in a uniform state without phase separation before a predetermined amount of water is added, there is no possibility that the blending composition, the cleaning power, and the like vary depending on the storage conditions and the transport conditions.
Therefore, according to the cleaning liquid regenerating apparatus and the circulating cleaning apparatus of the present invention, in particular, metal such as flux residue and solder paste cleaning, screen plate cleaning, cutting oil, and press oil in electronic parts that require high reliability. In cleaning parts, it is possible to provide a cleaning composition and a cleaning method that are excellent in cleaning performance.

10: Cleaning liquid regenerating apparatus, 11: Cleaning apparatus, 11a: Rinsing section, 11b: Cleaning section, 12: Circulating cleaning apparatus, 13: Generation section, 15: Regenerating cleaning liquid, 15a: Rinsing liquid (regenerating cleaning liquid), 15b: Cleaning liquid ( Regenerated cleaning liquid), 15 ': cleaning liquid vapor, 17a: cleaning liquid take-out section, 17b: piping, 17c, 17d: flow rate adjusting valve, 23: recovery section, 30: used cleaning liquid (distillation source liquid), 31: evaporation section (evaporation) Tank), 31a: heating means (heater), 41: cooling unit (water-cooled pipe), 41b: storage unit, 41c: opening, 43: cleaning liquid tank, 47: circulation path, 49: suction unit, 49a: circulation pump, 49b: suction part, 49c: pressure gauge, 51: piping, 53a: suction valve, 53b: check valve, 55: pressure reducing path, 60: rinsing tank, 62: washing tank

Claims (7)

A used cleaning liquid composed of a plurality of components derived from the distillation source liquid is heated and evaporated under reduced pressure to generate a cleaning liquid vapor in a gas-liquid equilibrium state, and the cleaning liquid vapor is condensed to form a regenerated cleaning liquid. A generation unit for
A recovery unit for continuously recovering the regenerated cleaning liquid, and a cleaning liquid regenerating apparatus comprising:
The generator is
While containing the used cleaning liquid, an evaporation unit for heating,
A cooling unit for condensing the cleaning liquid vapor to obtain a regenerated cleaning liquid;
A connecting part connecting the evaporation part and the cooling part;
With
The cooling unit is provided immediately above the evaporation unit, and each cooling unit is provided in the same casing.
The collection unit
A cleaning liquid tank in which the regenerated cleaning liquid is stored;
A cleaning liquid outlet for taking out the regenerated cleaning liquid to the outside;
A circulation path for circulating and flowing the regenerated cleaning liquid by a circulation pump;
A suction part that is provided in the middle of the circulation path and generates a negative pressure by flowing the regenerated cleaning liquid;
A decompression path communicating between the suction unit and the generation unit,
With the negative pressure of the suction part, the generation part is brought into a reduced pressure state via the pressure reduction path, and the regenerated cleaning liquid is sucked from the storage part and introduced into the circulation path,
When the opening area of the connecting portion is A (mm ² ) and the heater capacity for heating the evaporation portion is B (kW), the cleaning liquid vapor transfer coefficient C defined by the following equation (1) is A cleaning liquid regenerating apparatus having a value in a range of 100 to 30,000 mm ² / kW.
Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1) Cleaning liquid reproducing apparatus according to claim 1, characterized in that a value within the range opening area of the connecting portion (A) of 100~3,000,000mm ^2.   The cleaning liquid regenerating apparatus according to claim 1 or 2, wherein the heater capacity (B) is set to a value within a range of 0.1 to 100 kW.   The cleaning liquid regeneration according to any one of claims 1 to 3, wherein when the cleaning liquid vapor contains water vapor, a moving speed of the water vapor is set to a value within a range of 0.02 to 6 m / sec. apparatus. The cleaning liquid regenerating apparatus according to claim 1 , wherein the pressure of the generation unit is set to a value within a range of −0.01 to −0.1 MPa. The said cleaning liquid contains water, and makes content of the said water into the value within the range of 40 to 70 weight% with respect to the whole quantity, The Claim 1 characterized by the above-mentioned. The cleaning liquid regenerating apparatus as described. A circulating cleaning apparatus comprising a cleaning device capable of cleaning an object to be cleaned with a regenerated cleaning liquid and capable of supplying a used cleaning liquid after cleaning to a generating unit, and a cleaning liquid regenerating apparatus for generating a regenerated cleaning liquid,
The cleaning liquid regenerator comprises:
A used cleaning liquid composed of a plurality of components derived from the distillation source liquid is heated and evaporated under reduced pressure to generate a cleaning liquid vapor in a gas-liquid equilibrium state, and the cleaning liquid vapor is condensed to form a regenerated cleaning liquid. A generation unit for
A recovery unit for continuously recovering the regenerated cleaning liquid,
The generator is
While containing the used cleaning liquid, an evaporation unit for heating,
A cooling unit for condensing the cleaning liquid vapor to obtain a regenerated cleaning liquid;
A connecting part connecting the evaporation part and the cooling part;
With
The cooling unit is provided immediately above the evaporation unit, and each cooling unit is provided in the same casing.
The collection unit
A cleaning liquid tank in which the regenerated cleaning liquid is stored;
A cleaning liquid outlet for taking out the regenerated cleaning liquid to the outside;
A circulation path for circulating and flowing the regenerated cleaning liquid by a circulation pump;
A suction part that is provided in the middle of the circulation path and generates a negative pressure by flowing the regenerated cleaning liquid;
A decompression path communicating between the suction unit and the generation unit,
Due to the negative pressure of the suction part, the generation part is brought into a reduced pressure state through the pressure reducing path,
When the opening area of the connecting portion is A (mm ² ) and the heater capacity for heating the evaporation portion is B (kW), the cleaning liquid vapor transfer coefficient C defined by the following equation (1) is A circulating cleaning apparatus having a value in a range of 100 to 30,000 mm ² / kW.
Cleaning fluid vapor transfer coefficient (C) = opening area (A) / heater capacity (B) (1)

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