JP7684064B2 - Method for producing liquid composition - Google Patents

Description

The present invention relates to a method for producing a liquid composition, and a mixing method and mixer used therein.

By subjecting a mixture of aqueous and oily components to high shear and mixing them, an emulsion can be produced in which one component is dispersed in the other. For example, Patent Document 1 discloses a method of circulating the mixture of aqueous and oily components through a pressurized centrifugal pump and circulating it through a circulation section that includes the pressurized centrifugal pump and constitutes a circulation path. Patent Document 2 discloses a method of stirring the mixture of aqueous and oily components in a tank using an intermittent jet flow generating emulsifier and circulating it through a circulation path attached to the tank. Patent Document 3 discloses a method of circulating the mixture of aqueous and oily components through fine pores.

International Publication No. 2011/49215 JP 2016-117669 A JP 2014-87788 A

The object of the present invention is to provide a method for producing a liquid composition that can obtain high mixability between a first fluid and a second fluid, at least one of which is a liquid.

The present invention is a method for producing a liquid composition in which a first fluid and a second fluid, at least one of which is a liquid, are joined together, and the mixture of the first fluid and the second fluid in a mixed state at the time of the joining is passed through a contraction section in which the contraction ratio is variable.

The present invention is a mixing method in which a first fluid and a second fluid, at least one of which is a liquid, are joined together, and the mixture of the first fluid and the second fluid in a mixed state at the time of the joining is passed through a contraction section in which the contraction ratio is variable.

The present invention is a mixer that includes a supply system having a junction where a first fluid and a second fluid, at least one of which is a liquid, join, and a contraction section that is provided downstream of the supply system and has a variable contraction ratio through which the confluence of the first fluid and the second fluid in a mixed state when supplied from the supply system and joined at the junction section flows.

According to the present invention, a mixture of a first fluid and a second fluid, at least one of which is a liquid, can be circulated in a converging section having a variable contraction ratio in a mixed state when the first and second fluids are joined, thereby achieving high mixability of the first and second fluids.

FIG. 1 is a diagram showing the configuration of a liquid composition production apparatus. 1 is a graph showing the relationship between the pipe size and the emulsion particle size in Examples 1 to 3 and Comparative Examples 1 to 3.

The following describes the embodiments in detail.

Figure 1 shows a liquid composition manufacturing apparatus A. This liquid composition manufacturing apparatus A includes a mixer 10, a first fluid supply source 21 and a second fluid supply source 22 upstream of the mixer 10, and a liquid composition recovery tank 31 downstream of the mixer 10.

The mixer 10 has a contraction section 11, a supply system 12 upstream of it, and a recovery system 13 downstream of it.

The contraction ratio of the contraction section 11 is variable. Here, the term "contraction" in this application means that a fluid flows from a wide flow path to a narrow flow path. Therefore, the contraction section 11 includes a portion where the flow path area is continuously or stepwise reduced from the upstream side to the downstream side, or a portion where the flow path area is discontinuously reduced. The "contraction ratio" in this application means the ratio of the inner diameter of the portion with the narrowest flow path area in the contraction section 11 to the inner diameter of the upstream pipe continuing to the contraction section 11. Therefore, the contraction ratio in this embodiment corresponds to the ratio of the inner diameter of the portion with the narrowest flow path area in the contraction section 11 to the inner diameter of the junction supply pipe 123 described later. Note that the inner diameter is the hydraulic diameter when the flow path is non-circular. In addition, the "variable contraction ratio" in this application is synonymous with the inner diameter of the portion with the narrowest flow path area in the contraction section 11 being variable.

The flow contraction section 11 is preferably configured with a valve from the viewpoint of being a simple component with a variable flow contraction ratio. Examples of the valves that configure the flow contraction section 11 include ball valves, butterfly valves, globe valves, and gate valves. The valves that configure the flow contraction section 11 have a variable flow contraction ratio, so that flow rate control is possible. The valves that configure the flow contraction section 11 are preferably valves that produce a single peak in the particle size distribution of the emulsion particle size when an emulsion is produced as a liquid composition. The valves that configure the flow contraction section 11 are preferably valves that do not generate a pressure difference when the opening degree is 100%. Specifically, from these viewpoints, the valves that configure the flow contraction section 11 are preferably ball valves or butterfly valves, and more preferably ball valves.

The supply system 12 includes a first fluid supply pipe 121, a second fluid supply pipe 122, and a junction supply pipe 123. The upstream end of the first fluid supply pipe 121 is connected to the first fluid supply source 21. The upstream end of the second fluid supply pipe 122 is connected to the second fluid supply source 22. The downstream end of the first fluid supply pipe 121 and the downstream end of the second fluid supply pipe 122 are connected to form a junction section 124. The upstream end of the junction supply pipe 123 is connected to this junction section 124. The downstream end of the junction supply pipe 123 is connected to the contraction section 11. From the viewpoint of obtaining uniform mixing, it is preferable that the junction supply pipe 123 has a short length so that the junction section 124 is disposed immediately before the contraction section 11. From the same viewpoint, the length of the junction supply pipe 123 is preferably 25 cm or less, more preferably 5 cm or less, and even more preferably 1 cm or less. In addition, the junction section 124 where the first fluid supply pipe 121 and the second fluid supply pipe 122 are joined may be directly connected to the contraction section 11 without including the junction supply pipe 123. In addition, the piping sizes of the first fluid supply pipe 121, the second fluid supply pipe 122, and the junction supply pipe 123 are not particularly limited.

The recovery system 13 is composed of a liquid composition recovery pipe 131. The upstream end of the liquid composition recovery pipe 131 is connected to the flow contraction section 11. The downstream end of the liquid composition recovery pipe 131 is connected to the liquid composition recovery tank 31.

The first fluid supply source 21 is composed of a liquid tank or the like when the first fluid is a liquid, and is composed of a gas tank or the like when the first fluid is a gas. Similarly, the second fluid supply source 22 is composed of a liquid tank or the like when the second fluid is a liquid, and is composed of a gas tank or the like when the second fluid is a gas. The liquid composition recovery tank 31 is composed of a liquid tank.

Next, we will explain the method for producing a liquid composition according to an embodiment using this liquid composition production device A.

In the method for producing a liquid composition according to the embodiment, a first fluid and a second fluid are mixed. At least one of the first fluid and the second fluid is liquid. Therefore, the method for producing a liquid composition according to the embodiment may be a liquid-liquid mixture in which both the first fluid and the second fluid are liquid, or a gas-liquid mixture in which one of the first fluid and the second fluid is liquid and the other is gas.

Examples of liquids constituting the first fluid or the second fluid include solvents such as water or organic solvents, solutions in which a solute is dissolved, dispersions such as slurries in which solid particles are dispersed in a dispersion medium, and emulsions in which liquid particles are dispersed in a dispersion medium. Examples of gases constituting the first fluid or the second fluid include simple gases such as oxygen, and mixed gases such as air.

When the method for producing a liquid composition according to the embodiment is a liquid-liquid mixture in which both the first fluid and the second fluid are liquid, the first fluid and the second fluid may be incompatible. Therefore, the method for producing a liquid composition according to the embodiment may produce, as the liquid composition, an oil-in-water emulsion in which an oily component is dispersed in an aqueous component, or a water-in-oil emulsion in which a water-fat component is dispersed in an oily component, by having one of the first fluid and the second fluid be a liquid aqueous component and the other be a liquid oily component.

In this case, the contents of the aqueous component include, in addition to water, for example, monoalkyl cations, water-soluble solvents, preservatives, chelating agents, inorganic salts, fragrance capsules, water-soluble polymers, fragrance precursors, etc. The contents of the oily component include ester oils, long-chain monoalcohols with 12 to 18 carbon atoms, amidoamines with 14 to 18 carbon atoms, silicones, perfume fragrances, fragrance precursors, etc. At least one of the aqueous component and the oily component may contain a surfactant. As the surfactant, various cationic surfactants, anionic surfactants, amphoteric surfactants, and nonionic surfactants can be used.

In the method for producing a liquid composition according to the embodiment, in the supply system 12, a first fluid is supplied from a first fluid supply source 21 via a first fluid supply pipe 121, and a second fluid is supplied from a second fluid supply source 22 via a second fluid supply pipe 122. As a result, the first fluid from the first fluid supply pipe 121 and the second fluid from the second fluid supply source 22 are merged at the junction 124. The junction of the first and second fluids merged at the junction 124 is supplied to the contraction section 11 via a junction supply pipe 123.

At this time, the junction of the first and second fluids flows into the contraction section 11 in the mixed state in which the first and second fluids join at the junction section 124. Here, the "mixed state in which the first and second fluids join" in this application includes the mixed state immediately after the first and second fluids join, as well as the mixed state of the first and second fluids after the first and second fluids join and are simply transported in the piping without being subjected to high shear. For example, in the case where one of the first and second fluids is a liquid aqueous component and the other is a liquid oily component, when the first and second fluids join at the junction section 124, the resulting junction immediately flows into the contraction section 11, so that emulsification does not substantially proceed in the junction supply pipe 123, and the first and second fluids flow into the contraction section 11 in the phase-separated mixed state in which they join.

The flow velocity of the junction of the first and second fluids is preferably 0.5 m/s or more and 2 m/s or less. When one of the first and second fluids is a liquid aqueous component and the other is a liquid oily component, the ratio of the oily component to the total flow rate is preferably 30% or less.

Then, the mixture of the first and second fluids in a mixed state when they are joined is passed through the flow contraction section 11. At this time, the mixture of the first and second fluids passes through the part of the flow contraction section 11 with a reduced flow area and is subjected to high shear, promoting their mixing and producing a liquid composition. When one of the first and second fluids is a liquid aqueous component and the other is a liquid oil component, the mixture of the first and second fluids in a phase-separated mixed state passes through the flow contraction section 11 and is emulsified by being subjected to high shear, producing an emulsion liquid composition.

The pressure difference before and after the contraction section 11 at this time is preferably 5 kPa or more, more preferably 50 kPa or more, even more preferably 100 kPa or more, and is preferably 2000 kPa (2.0 MPa) or less, more preferably 1000 kPa or less, even more preferably 500 kPa or less.

The liquid composition produced by flowing through the flow contraction section 11 is then recovered in the liquid composition recovery tank 31 via the liquid composition recovery pipe 131 of the recovery system 13.

According to the above-described method for producing a liquid composition, the first and second fluids, at least one of which is liquid, are passed through the contraction section 11, which has a variable contraction ratio, in the mixed state when they are joined, thereby obtaining high mixability of the first and second fluids. In particular, when one of the first and second fluids is a liquid aqueous component and the other is a liquid oily component, and an emulsion is produced as a liquid composition, an emulsion with the same emulsion particle size can be produced by adjusting the magnitude of the differential pressure before and after the contraction section 11, even if the scale of the device is changed. Furthermore, if the scale of the device is the same, the emulsion particle size of the emulsion to be produced can be controlled only by manipulating the contraction ratio of the contraction section 11 without replacing the contraction section 11. Moreover, the control of the emulsion particle size of this emulsion can be performed centrally, regardless of the composition of the first and second fluids, as long as their properties are similar.

In the above embodiment, two types of fluids, a first fluid and a second fluid, are mixed, but this is not limited to this, and three or more types of fluids may be mixed.

(Production of emulsion)
1, emulsions were produced in the following Examples 1 to 13 and Comparative Examples 1 to 6. The respective configurations are also shown in Tables 1 and 2.

Example 1
In Example 1, 15A size pipes were used as the first fluid supply pipe, the second fluid supply pipe, the junction supply pipe, and the liquid composition recovery pipe, and a ball valve for 15A size pipes was used as the flow contraction section. For the first and second fluids, Formulation A was used, in which the first fluid was composed of an aqueous component of a predetermined composition, and the latter was composed of an oily component of a predetermined composition containing a quaternary ammonium salt of a cationic surfactant and a polyoxyethylene lauryl ether of a nonionic surfactant.

Then, the aqueous component of the first fluid was supplied from the first fluid supply source to the first fluid supply pipe at a flow rate of 17 L/min, and the oily component of the second fluid was supplied from the second fluid supply source 22 to the second fluid supply pipe at a flow rate of 4 L/min. As a result, the junction of these fluids at the junction 124 was caused to flow at a flow rate of 1.4 m/s in the junction supply pipe, and the junction was caused to flow into the ball valve of the flow contraction section. The opening of the ball valve was set to 37%, so that the pressure difference before and after it was controlled to 30 kPa. The emulsion generated by flowing through the ball valve was collected in the liquid composition collection tank via the liquid composition collection pipe.

<Examples 2 and 3>
In Example 2, 40A size pipes were used as the first fluid supply pipe, the second fluid supply pipe, the junction supply pipe, and the liquid composition recovery pipe, and a ball valve for 40A size pipes was used as the flow contraction section. The flow rates of the aqueous component and the oily component were set to 100 L/min and 22 L/min, respectively, so that the junction was caused to flow in the junction supply pipe at a flow velocity of 1.4 m/s, and the same operations were carried out as in Example 1.

In Example 3, 80A size pipes were used as the first fluid supply pipe, the second fluid supply pipe, the junction supply pipe, and the liquid composition recovery pipe, and a ball valve for 80A size pipes was used as the flow contraction section. The flow rates of the aqueous component and the oily component were set to 373 L/min and 83 L/min, respectively, and the junction was caused to flow in the junction supply pipe at a flow rate of 1.4 m/s. The same operations as in Example 1 were performed.

<Examples 4 and 5>
In Example 4, the first fluid and the second fluid were prepared using prescription B, in which the first fluid was composed of an aqueous component of a predetermined composition, and the latter was composed of an oil component of a predetermined composition containing a quaternary ammonium salt of a cationic surfactant and a polyoxyethylene lauryl ether of a nonionic surfactant, and the opening degree of the ball valve was set to 47%, thereby controlling the pressure difference between the front and rear of the ball valve to 10 kPa. The same operations as in Example 1 were performed, except that the opening degree of the ball valve was set to 47%, thereby controlling the pressure difference between the front and rear of the ball valve to 10 kPa.

In Example 5, the same operation as in Example 4 was performed, except that the opening of the ball valve was set to 32%, and the pressure difference between before and after the ball valve was controlled to 60 kPa.

<Examples 6 to 8>
In Example 6, the same operations as in Example 4 were carried out, except that formulation C was used for the first and second fluids, in which the first fluid was composed of an aqueous component of a predetermined composition, and the latter was composed of an oily component of a predetermined composition containing a quaternary ammonium salt of a cationic surfactant and a polyoxyethylene lauryl ether of a nonionic surfactant.

In Example 7, the same operation as in Example 6 was performed, except that the opening of the ball valve was set to 37%, and the pressure difference between the front and rear of the valve was controlled to 30 kPa.

In Example 8, the same operation as in Example 6 was performed, except that the opening of the ball valve was set to 33%, and the pressure difference between before and after the ball valve was controlled to 50 kPa.

In Example 9, the same operation as in Example 6 was performed, except that the pressure difference before and after the ball valve was controlled to 330 kPa.

<Examples 10 to 12>
In Example 10, the first fluid and the second fluid were prepared by using a formulation D in which the first fluid was composed of an aqueous component of a predetermined composition, and the latter was composed of an oil component of a predetermined composition containing a quaternary ammonium salt of a cationic surfactant and a polyoxyethylene lauryl ether of a nonionic surfactant. The flow rates of the aqueous component and the oil component were set to 6.6 L/min and 0.7 L/min, respectively, so that the mixture was caused to flow in the mixture supply pipe at a flow rate of 0.5 m/s, and the differential pressure before and after the ball valve was controlled to 15 kPa. The same operations as in Example 1 were performed.

In Example 11, the same operation as in Example 10 was performed, except that the flow rates of the aqueous and oily components were set to 20 L/min and 2 L/min, respectively, and the mixture was caused to flow through the mixture supply pipe at a flow rate of 1.5 m/s.

In Example 12, the same procedure as in Example 10 was carried out, except that the flow rates of the aqueous and oily components were set to 26 L/min and 3 L/min, respectively, and the mixture was caused to flow through the mixture supply pipe at a flow rate of 2.0 m/s.

<Example 13>
In Example 13, the same operation as in Example 4 was carried out, except that a globe valve for piping of 15A size was used as the flow contraction portion.

<Comparative Examples 1 to 3>
In Comparative Examples 1 to 3, the same operations as in Examples 1 to 3 were carried out, respectively, except that a static mixer having six mixing elements arranged in series in the fluid flow direction was used instead of the ball valve in the contraction section.

<Comparative Example 4>
In Comparative Example 4, the same operation as in Comparative Example 3 was carried out, except that the number of mixing elements in the static mixer was two.

<Comparative Examples 5 and 6>
In Comparative Examples 5 and 6, a milder was used instead of the ball valve in the flow contraction section, and the flow rates of the aqueous component and the oily component were 1.7 L/min and 0.4 L/min, respectively. In Comparative Example 5, mixing was performed under relatively low emulsification conditions, and in Comparative Example 6, mixing was performed under relatively high emulsification conditions.

(Test method and results)
The emulsion particle size of each of Examples 1 to 13 and Comparative Examples 1 to 6 was determined from the light scattering intensity measured by a particle size/zeta potential measuring device Zetasizer Nano ZS (manufactured by Malvern Instruments) using the emulsion obtained diluted 1500 times by mass with ion-exchanged water and adjusted to 20° C. In addition, the particle size distribution of the emulsion particle size of each of the obtained emulsions was also determined for each of Examples 1 to 13 and Comparative Examples 5 and 6. The results are shown in Tables 1 and 2.

Comparing Examples 1 to 3 with Comparative Examples 1 to 3, as shown in FIG. 2, in Examples 1 to 3 using a ball valve, even if the piping size increases and the scale of the equipment changes, it is possible to produce emulsions with the same emulsion particle size by regulating the flow rate of the junction and the pressure difference before and after the ball valve. In contrast, in Comparative Examples 1 to 3 using a static mixer, it is possible to produce emulsions with roughly the same emulsion particle size by regulating the flow rate of the junction and the pressure difference before and after the ball valve when the piping size increases and the scale of the equipment changes, even if the flow rate of the junction is regulated. In addition, comparing Examples 1 to 13, it is possible to produce emulsions with roughly the same emulsion particle size by regulating the flow rate of the junction and the pressure difference before and after the ball valve, even if the formulation of the aqueous and oily components changes.

Comparing Examples 6 to 9 with Comparative Examples 3 and 4, it can be seen that in Examples 6 to 9, which use a ball valve, the emulsion particle size of the emulsion produced can be controlled by simply adjusting the opening of the ball valve without replacing the ball valve, while keeping the equipment scale the same. On the other hand, in Comparative Examples 3 and 4, which use a static mixer, it is necessary to replace the static mixer in order to control the emulsion particle size.

Comparing Examples 10 to 12, it can be seen that even if the flow rate of the combined liquid is different, it is possible to control the emulsion particle size by the pressure difference before and after the ball valve.

Comparing Example 4 and Example 13, both Example 4 using a ball valve and Example 9 using a globe valve produced emulsions with similar particle sizes, but the particle size distribution of the emulsion particles in the former was a single peak, whereas the particle size distribution of the emulsion particles in the latter was a double peak. This shows that the ball valve can achieve more uniform mixing than the globe valve.

It is possible to control the emulsion particle size by mixing using a milder as in Comparative Examples 5 and 6, but the ball valves and globe valves used in Examples 1 to 9 do not require power like a milder, so the device configuration can be simplified.

The present invention is useful in the technical fields of a method for producing a liquid composition, and a mixing method and a mixer used therein.

A Liquid composition producing apparatus 10 Mixer 11 Flow contraction section 12 Supply system 121 First fluid supply pipe 122 Second fluid supply pipe 123 Junction supply pipe 124 Junction section 13 Recovery system 131 Liquid composition recovery pipe 21 First fluid supply source 22 Second fluid supply source 31 Liquid composition recovery tank

Claims (4)

1. A method for producing a liquid composition, comprising: joining a first liquid fluid and a second liquid fluid at a joining section ; and subsequently, flowing a mixture of the first fluid and the second fluid in a mixed state at the time of the joining through a joining supply pipe extending from the joining section to a ball valve constituting a contraction section having a variable contraction ratio ,
one of the first fluid and the second fluid is an aqueous component and the other is an oily component, at least one of the first fluid and the second fluid contains a surfactant, and the liquid composition is an oil-in-water emulsion in which the oily component is dispersed in the aqueous component, or a water-in-oil emulsion in which the aqueous component is dispersed in the oily component,
The pressure difference before and after the ball valve constituting the contraction section is 5 kPa or more and 2000 kPa or less,
The method for producing a liquid composition, wherein the particle size distribution of emulsion particle diameters of the oil-in-water emulsion or water-in-oil emulsion which is the liquid composition has a single peak . The method for producing a liquid composition according to claim 1 , wherein a ratio of the oil component to a total flow rate of the first fluid and the second fluid is 30% or less. 3. The method for producing a liquid composition according to claim 1, wherein a flow velocity of the confluence of the first fluid and the second fluid flowing into the ball valve constituting the flow contraction section is 0.5 m/s or more and 2 m/s or less. A mixing method for obtaining a liquid composition, comprising: joining a first liquid fluid and a second liquid fluid at a joining section , and subsequently flowing a mixture of the first fluid and the second fluid in a mixed state at the time of the joining through a joining supply pipe extending from the joining section to a ball valve constituting a contraction section having a variable contraction ratio , the method comprising the steps of:
one of the first fluid and the second fluid is an aqueous component and the other is an oily component, at least one of the first fluid and the second fluid contains a surfactant, and the liquid composition is an oil-in-water emulsion in which the oily component is dispersed in the aqueous component, or a water-in-oil emulsion in which the aqueous component is dispersed in the oily component,
The pressure difference before and after the ball valve constituting the contraction section is 5 kPa or more and 2000 kPa or less,
The mixing method according to claim 1, wherein the particle size distribution of the emulsion particle diameter of the oil-in-water emulsion or the water-in-oil emulsion which is the liquid composition has a single peak .

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