JP4104602B2 - Method for cleaning and removing contaminants or impurities of fine porous material with a high-pressure fluid in a sealed container - Google Patents

Description

  The present invention relates to a method for cleaning and removing contaminants or impurities of a microporous material with a high-pressure fluid in a sealed container, and includes a high-pressure fluid technology (supercritical fluid and liquid carbon dioxide), a cleaning technology, and processing of a microporous material. In particular, the present invention relates to a method that does not require a large amount of cleaning water and does not cause environmental protection problems due to wastewater discharge.

  In general, parts such as bearings, filters, silencers, and coolers formed of metal materials, polymer materials, ceramic materials, and composite materials thereof have a considerable number of holes. For example, bearing holes are used to store lubricating oil, and when the equipment is operated, the lubricating oil is released by heat to lubricate the rotating shaft, reducing wear and noise, and when cooling, the lubricating oil is the principle of pores This is a characteristic of powder metallurgy products.

  These miniaturized porous materials have a problem that contaminants or impurities remaining after processing or use cause clogging of parts.

The problems existing in the current cleaning method are as follows.
1. Uses a large amount of acid solution, alkali solution or water, and consumes time and energy.
2. The surface tension of water is large and does not immediately penetrate from the material outer layer to the inner layer, and does not penetrate unless an external force such as air pressure is combined.
3. At the time of cleaning, water is sent from the outer layer to the interior and is easily adsorbed into the fine porous structure, and it is necessary to send air for drying treatment or to heat and dry it separately.

  The present invention provides a method for cleaning and removing contaminants or impurities of a microporous material in a sealed container with a high-pressure fluid in order to protect the environment, simplify the manufacturing process of the microporous material, and increase production efficiency. To do.

  The technical means applied by the present invention and the effects of the conventional technology are as follows. That is, by using a high-pressure fluid in a closed container, and having a high diffusion coefficient and high penetration ability, a solvent ability to have under a specific temperature and pressure, and rapidly accumulating contaminants or impurities, Overcoming the problems in the above known cleaning methods, i.e. improving the problem of using large amounts of organic chemical water, solvent and cleaning water, as well as increasing the quality and life of products using micronized porous materials, cleaning Shorten drying steps and time, reduce operating costs.

Advantages when carbon dioxide is used in the present invention are as follows.
1. There is no bad physiological effect. In other words, carbon dioxide is present in both carbonated water and human metabolism, and is a generally recognized safety substance and is approved for use.
2. Harmless to the environment, non-flammable, non-explosive, non-corrosive, stable chemical, high purity, non-toxic.
3. It is inexpensive and can be obtained in large quantities, is not affected by the petrochemical industry, and can be stored in large quantities in liquid form.
4). It has considerable volatility and therefore can be separated from solutes very easily and safely, i.e. the recovery of solutes and solvents is easy, there are no residual problems, the reaction can take place at low temperatures and the thermosensitive substances can be destroyed. Absent.
5. Liquid carbon dioxide solvent properties are close to hydrocarbon solvents.

The invention according to claim 1, placing the fine porous material in the reaction tank of the closed container, along with utilizing a high pressure pump and the high-pressure pipe accessory for introducing a fluid in the fluid storage tank during the reaction tank, the temperature and pressure By controlling and adjusting the density, high-density, high-diffusion, low-viscosity, low-dielectric constant and extremely low surface tension can be used to remove contaminants or impurities in the microporous material .
The reaction tank is connected to a separation tank using a high-pressure pipe accessory and a high-pressure valve, the separation tank is connected to a fluid recovery pump via a high-pressure pipe accessory and a high-pressure valve, and the fluid recovery pump is stored as a fluid using a high-pressure pipe accessory and a high-pressure valve. Of a microporous material characterized in that it is connected to a tank, thus forming a main circuit, and a separation tank and a fluid storage tank are connected using a high-pressure pipe accessory and a high-pressure valve to form a sub-circuit . It is a method of cleaning and removing contaminants or impurities with a high-pressure fluid in a sealed container.
According to the second aspect of the present invention , a pressure meter and a high-pressure valve are provided above and below the fluid storage tank, reaction tank, and separation tank, respectively, and the fluid is discharged and collected through the high-pressure pipe accessory. The method according to claim 1, wherein the contaminants or impurities of the microporous material are deposited and collected by an opening operation of the high-pressure valve.
According to a third aspect of the present invention , there is provided a temperature control device provided outside the fluid storage tank, the reaction tank, and the separation tank. It is a method of washing and removing with a high-pressure fluid in a sealed container.
The invention according to claim 4, the operating temperature is determined by the properties of the fine porous material, characterized in that it is a 4 to 120 ± 1 ° C, contamination of the fine porous material according to claim 1 In this method, substances or impurities are washed away with a high-pressure fluid in a sealed container.
The invention of claim 5 is characterized in that the operating pressure is determined by the characteristics of the refined porous material, and is 10 to 300 kg / cm ² . Alternatively, the impurities are washed away with a high-pressure fluid in a sealed container.
The invention according to claim 6 is characterized in that the fluid is carbon dioxide, propane, xenon, nitrous oxide, hydrogen, nitrogen, and the contaminants or impurities of the microporous material according to claim 1 are sealed. In this method, the container is cleaned and removed with a high-pressure fluid.

  The present invention puts a fine porous material in a closed container, controls and adjusts temperature and pressure, and provides high pressure fluid density, high diffusivity, low viscosity, low dielectric constant and extremely low surface tension solvent properties. The high-pressure fluid is made to enter the inner layer through the microporous structure from the outer layer of the microporous material, and the contaminants or impurities remaining after processing or use are dissolved. Release through finer porous material to achieve the purpose of cleaning and removing contaminants or impurities of the finer porous material, save processing and cleaning water, reduce wastewater treatment and pollution discharge problems, reduce operation time In addition, contaminants and impurities can be removed and separated and collected at the same time, and it is not necessary to consume a large amount of power and dry the microporous material.

  FIG. 1 is a collection type system display diagram of the present invention. The high pressure pipe accessory 1 connects the fluid storage tank 10, the high pressure pump 20, the reaction tank 30, the separation tank 40, and the fluid recovery pump 50 to form a main circuit, and the separate high pressure pipe accessory 2 separates the fluid storage tank 10 from the fluid storage tank 10. The tanks 40 are connected to form a sub circuit. High-pressure valves V2, V3, V5, V7, and V9 are provided between the main circuit fluid storage tank 10, the high-pressure pump 20, the reaction tank 30, the separation tank 40, and the fluid recovery pump 50. And a separation tank 40 are provided with a high-pressure valve V8. In addition, pressure meters P1 to P3 and high pressure valves V1, V4, and V6 are provided above and below the fluid storage tank 10, the reaction tank 30, and the separation tank 40, respectively.

Among them, the fluid storage tank 10 is used for storage of fluid (including liquid and gas), and a temperature control device 11 is provided. The fluid storage tank 10 is used for pressurization and recovery storage of fluid, and pressure operation range is 10~150kg / cm ^2.

The high-pressure pump 20 is used for pressurization of fluid (including liquid and gas), and the pressure operation range is 10 to 300 kg / cm ² .

The reaction tank 30 is provided with a high-pressure tank 32 provided with a lid 31 that can be opened and closed for batch operations, and a temperature control device 33 is provided in the high-pressure tank 32 to provide a temperature control range of 4 to 80 degrees Celsius, 10 to 300 kg. In a pressure operating range of / cm ^2, a microporous material (not shown) is accommodated, and the operation of removing contaminants or impurities is performed after fluid pressurization.

Separation tank 40 comprises a high-pressure tank 42 and the temperature control device 43, equipped with cap 41 that do not need to be opened and closed at all times, the temperature control range of 4 to 80 degrees Celsius, a pressure operating range of the 10~300kg / cm ^2, The fluid and the contaminants or impurities are separated, and the fluid is discharged and collected from the pipe line at the upper end of the separation tank 40, and the contaminants or impurities are accumulated in the lower part of the separation tank 40, and collected by opening and closing the high-pressure valve V6.

The fluid recovery pump 50 is used for recovery of fluid (including liquid and gas), and the pressure operation range is 10 to 300 kg / cm ² .

  The system used in the method of cleaning and removing the contaminants or impurities of the fine porous material provided by the present invention with a high-pressure fluid in a sealed container can omit the fluid recovery pump 50, and the fluid storage tank 10 generally includes Steel cylinder 10 'can be used.

  FIG. 2 is a diagram showing the separation type system of the present invention, and the contaminants and fluid separated after the reaction are directly discharged and not recovered, and are therefore called separation type.

  The apparatus used for the method of cleaning and removing the contaminants or impurities of the fine porous material provided by the present invention with a high-pressure fluid in a sealed container can omit the separation tank 40 and the fluid storage tank 10. The fluid storage tank 10 can use a general steel cylinder 10 ', and FIG. 3 shows a basic system display diagram of the present invention. After the reaction, the contaminants and fluid are directly discharged and not separated and recovered, and are therefore referred to as the basic type.

  In actual cleaning, the recovery type is the most preferred embodiment, and the operation steps are as follows.

Before operation, check that all high pressure valves V1 to V9 are closed, as well as all tanks (fluid storage tank 10, reaction tank 30, separation tank 40), high pressure pipe accessories 1, 2, high pressure pump 20, The fluid recovery pump 50 and the pressure meters P1 to P3 are inspected for abnormalities, and the pressure value of the pressure meter P1 of the fluid storage tank 10 is inspected to be 50 kg / cm ² or more. The valve V1 is connected to a gas supply steel cylinder outside the system to supply gas necessary for normal operation of the system.

After confirming that the system is operating properly, execute the following operations.
1. warm up. That is, the temperature of the fluid storage tank 10 is controlled to 2-4 degrees Celsius, the temperature of the reaction tank 30 is controlled to 40-80 ± 1 degrees Celsius, and the temperature of the separation tank 40 is controlled to 4-80 ± 1 degrees Celsius.
2. A refined porous material, for example, a bearing is inspected and confirmed to be normal, and the temperature is already set in a reaction tank 30 having reached a set value of 40 to 80 ± 1 degrees Celsius.
3. The lid 31 of the reaction tank 30 is closed, the high pressure valves V2 and V3 are opened, and the pressure is increased with carbon dioxide gas. When the pressure value of the pressure meter P2 reaches 200 kg / cm ² , the high pressure valves V2 and V3 are turned on. Close and start timing for 5-20 minutes.
4). When the operation time is over, the high-pressure valves V5, V7, V8 and V9 are opened to separate the contaminants or impurities from the gas, and to perform the first-stage recovery / circulation operation of the gas.
5. After the pressure values of the pressure meters P2 and P3 are not lowered, the high pressure valve V8 is closed and the fluid recovery pump 50 is opened to perform the second stage gas recovery operation.
6). When the pressure values of the pressure meters P1 and P2 are smaller than 10 kg / cm ² , the high pressure valves V5, V7, V9 are closed, and the high pressure valve V4 is opened to discharge the gas remaining in the reaction tank 30, and the pressure meter When the pressure value of P2 reaches 0 kg / cm ² , the lid 31 of the reaction tank 30 is opened, the bearing sample is taken out, and the cleaning operation for contaminants or impurities by the primary high-pressure fluid is completed.

  At present, bearings are generally washed with ultrasonic vibration and then dried, but if the water molecules encapsulated in the microporous structure in the bearing cannot be completely removed, the bearing is likely to rust. , Bearing quality and normal service life are impaired.

  The method of cleaning and removing the contaminants or impurities of the microporous material provided by the present invention with a high-pressure fluid in a sealed container has been confirmed to achieve the expected effects by actually performing repeated operation tests. It is a novel invention that is not present in the market and has industrial utility value.

It is a collection type | system | group system display figure of this invention. It is a separation type system display figure of the present invention. It is a system display figure of the basic type of the present invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 High pressure pipe accessory 2 High pressure pipe accessory 10 Fluid storage tank 10 'Steel cylinder 11 Temperature control apparatus 20 High pressure pump 30 Reaction tank 31 Lid 32 High pressure tank 33 Temperature control apparatus 40 Separation tank 41 Lid 42 High pressure tank 43 Temperature control apparatus 50 Fluid recovery Pump V1-V9 High pressure valve P1-P3 Pressure meter

Claims (6)

Place the micronized porous material in the reaction tank of the sealed container, introduce the fluid in the fluid storage tank into the reaction tank using a high pressure pump and high pressure pipe accessories, and control and adjust the temperature and pressure to increase the Removes contaminants or impurities in micronized porous materials with gas or liquid fluids with density, high diffusivity, low viscosity, low dielectric constant and very low surface tension ,
The reaction tank is connected to a separation tank using a high-pressure pipe accessory and a high-pressure valve, the separation tank is connected to a fluid recovery pump via a high-pressure pipe accessory and a high-pressure valve, and the fluid recovery pump is stored as a fluid using a high-pressure pipe accessory and a high-pressure valve. Of a microporous material characterized in that it is connected to a tank, thus forming a main circuit, and a separation tank and a fluid storage tank are connected using a high-pressure pipe accessory and a high-pressure valve to form a sub-circuit . A method of cleaning and removing contaminants or impurities with a high-pressure fluid in a sealed container. A pressure meter and a high-pressure valve are provided above and below the fluid storage tank, reaction tank, and separation tank, respectively, and fluid is discharged and collected through the high-pressure pipe accessory, and contaminants or impurities are deposited on the bottom, and The method for cleaning and removing contaminants or impurities of a finely porous material according to claim 1, wherein the contaminant or impurities are collected by an opening operation. The temperature control device is provided outside the fluid storage tank, the reaction tank, and the separation tank. How to wash away. The operating temperature is determined by the characteristics of the microporous material and is set to 4 to 120 ± 1 degrees Celsius. Cleaning and removing with high pressure fluid. The operating pressure is determined by the characteristics of the micronized porous material, 10 to 300 kg / cm ²  The method for cleaning and removing contaminants or impurities of the fine porous material according to claim 1 with a high-pressure fluid in a sealed container. 2. The fine porous material contaminants or impurities according to claim 1, wherein the fluid is carbon dioxide, propane, xenon, nitrous oxide, hydrogen, nitrogen, and is cleaned with a high-pressure fluid in a sealed container. How to remove.

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