WO2019093251A1 - Procédé et dispositif de recyclage pour nettoyer une composition de solvant, et procédé et système de nettoyage pour objet à nettoyer - Google Patents

Procédé et dispositif de recyclage pour nettoyer une composition de solvant, et procédé et système de nettoyage pour objet à nettoyer Download PDF

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Publication number
WO2019093251A1
WO2019093251A1 PCT/JP2018/040909 JP2018040909W WO2019093251A1 WO 2019093251 A1 WO2019093251 A1 WO 2019093251A1 JP 2018040909 W JP2018040909 W JP 2018040909W WO 2019093251 A1 WO2019093251 A1 WO 2019093251A1
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Prior art keywords
cleaning
solvent composition
cleaning solvent
regenerating
component
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PCT/JP2018/040909
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English (en)
Japanese (ja)
Inventor
敬二 安藤
菅原　充
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日本ゼオン株式会社
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Priority to CN201880069532.7A priority Critical patent/CN111278578A/zh
Priority to JP2019552767A priority patent/JPWO2019093251A1/ja
Publication of WO2019093251A1 publication Critical patent/WO2019093251A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/04—Breaking emulsions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/14—Removing waste, e.g. labels, from cleaning liquid; Regenerating cleaning liquids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/26—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22—Organic compounds
    • C11D7/28—Organic compounds containing halogen
    • C11D7/30—Halogenated hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50—Solvents

Definitions

  • the present invention relates to a method of regenerating a cleaning solvent composition used for cleaning an object to be cleaned such as precision machine parts, electric / electronic parts, optical parts and the like, and a method of cleaning an object to be cleaned using the reclamation method It is.
  • the present invention also relates to a device for regenerating a cleaning solvent composition used to clean objects to be cleaned such as precision machine parts, electrical and electronic components, optical components, and a cleaning system for objects to be cleaned including the regenerating device. It is a thing.
  • processing oil for example, cutting oil, press oil, squeeze oil, rolling, etc.
  • rustproof oil for example, waxes, greases, fluxes, etc.
  • a mixed solution containing a fluorine-based solvent and a predetermined organic solvent is used from the viewpoint of achieving high washability with low environmental load. See, for example, Patent Documents 1 to 4.
  • Patent Documents 1 and 2 after dirt components are deposited from the cleaning solvent composition by addition of a poor solvent or cooling in a dirt removal tank, the deposited dirt components are surfaced in the dirt removal tank. By separating it, the cleaning solvent composition is regenerated. Then, the regenerated cleaning solvent composition obtained in the soil removal tank is sent from the soil removal tank to the cleaning tank for cleaning the object to be cleaned, and is reused for the cleaning of the object to be cleaned.
  • Patent Documents 3 and 4 after the dirt component is precipitated from the cleaning solvent composition by addition of a poor solvent and cooling in the dirt separation tank, the deposited dirt component is connected to the dirt separation tank and the washing tank.
  • the separated cleaning agent composition separated by the fiber separation filter installed in the liquid transfer path and separated from the soil components by the separation filter is sent to the cleaning tank to wash the soil components dissolved.
  • the solvent composition is recycled and reused.
  • an object of this invention is to provide the reproduction
  • Another object of the present invention is to provide a method and a system for cleaning an object to be cleaned using a regenerated cleaning solvent composition obtained by efficiently separating dirt components.
  • the present inventors deposit the dirt component from the washing solvent composition in which the dirt component is dissolved, and then deposit the washing solvent composition containing the deposited dirt component against the dirt component. It has been found that the soil component can be coarsely grained and the soil component can be efficiently separated by contacting the soil component affinity material having higher affinity than the cleaning solvent composition, and the present invention is completed. I did.
  • the object of the present invention is to advantageously solve the above-mentioned problems, and according to the present invention, the following regeneration methods (1) to (10), the following cleaning method (11), 12) A regenerating apparatus of (13) and a cleaning system of (14) below are provided.
  • a method of regenerating a cleaning solvent composition in which dirt components are dissolved The cleaning solvent composition contains a fluorine-based solvent and a flammable organic solvent, Step (A) of depositing a dirt component from the washing solvent composition in which the dirt component is dissolved, and obtaining a mixture containing the deposited dirt component and the washing solvent composition; Contacting the mixture with a soil component compatible material (B); Step (C) of removing the dirt component from the mixture brought into contact with the dirt component compatible material to obtain a regenerated cleaning solvent composition;
  • a method of regenerating a cleaning solvent composition comprising: (2) performing the step (B) and the step (C) while circulating the mixture between the contact portion having the soil component affinity material and the separation portion for removing the soil component from the mixture (1)
  • the fluorinated solvent is 1,1,2,2,3,3,4-heptafluorocyclopentane, The method for regenerating a cleaning solvent composition according to any one of the above (1) to (5), wherein the flammable organic solvent is an aromatic alcohol.
  • a regenerating apparatus for regenerating a cleaning solvent composition in which dirt components are dissolved contains a fluorine-based solvent and a flammable organic solvent, A deposition portion for depositing the dirt component from the cleaning solvent composition in which the dirt component is dissolved; A contact portion for bringing a mixture containing the deposited dirt component and the cleaning solvent composition, obtained in the deposition portion, into contact with the dirt component compatible material; A separation unit for removing a dirt component from the mixture brought into contact with the dirt component affinity material at the contact portion;
  • An apparatus for regenerating a cleaning solvent composition comprising: (13) The apparatus for regenerating a cleaning solvent composition according to (12), further comprising a circulation line for circulating the mixture between the contact portion and the separation portion.
  • An apparatus for regenerating the cleaning solvent composition as described in (12) or (13) above, A regeneration line for delivering a cleaning solvent composition in which dirt components are discharged, which is discharged from the cleaning apparatus, to the regeneration apparatus;
  • the washing system for washing objects provided with
  • the “flammable organic solvent” is an organic solvent having a flash point by any method when the flash point is measured by the tag sealing method and the Cleveland open method according to JIS K2265.
  • the term "soil component compatible material” means that the turbidity value measured by a turbidimeter is 5 or more in 50 ml of the cleaning solvent composition in which the soil component is dissolved to a concentration of 6% by mass. After cooling until rising to obtain 50 ml of the cleaning solvent composition in which the dirt component is deposited, 25 ml of the dirt component affinity material is added while maintaining the temperature, and mixing is performed at a stirring speed of 300 rpm, and then it is immersed for 30 minutes.
  • the reduction rate of the concentration of dirt components is 10% or more.
  • concentration of the dirt component at the time of soaking for 30 minutes is 30% or more in a dirt component affinity material.
  • the dirt component can be efficiently separated from the cleaning solvent composition in which the dirt component is dissolved, and the cleaning solvent composition can be efficiently regenerated.
  • an object to be cleaned can be efficiently cleaned using a regenerated cleaning solvent composition obtained by efficiently separating dirt components.
  • the method for cleaning an object to be cleaned according to the present invention is used when cleaning an object to be cleaned to which a dirt component adheres with a cleaning solvent composition.
  • the step (a) of washing with the washing solvent composition and the washing solvent composition in which the dirt component formed in the step (a) is dissolved is regenerated using the method of regeneration of the washing solvent composition of the present invention described later in detail.
  • the method is characterized by including a step (b) and a step (c) of washing the to-be-cleaned material to which the dirt component adheres using the regenerated washing solvent composition obtained in the step (b).
  • the reclaimed cleaning solvent composition obtained in the step (b) is reused to clean the object to be cleaned, so that the cost required for cleaning the object to be cleaned Can be effectively reduced.
  • the object to be cleaned is not particularly limited, and examples thereof include various materials such as metal materials, ceramic materials, plastics materials, intermediate products and final products.
  • the dirt component is not particularly limited, and, for example, processing oil (for example, cutting oil, press oil, throttling oil, rolling oil, etc.), lubricating oil, rust preventive oil, wax And greases and fluxes.
  • processing oil for example, cutting oil, press oil, throttling oil, rolling oil, etc.
  • lubricating oil for example, rust preventive oil, wax And greases and fluxes.
  • the processing oil may be either a water-soluble processing oil or an oil-soluble processing oil, but is preferably an oil-soluble processing oil such as a hydrocarbon-based processing oil.
  • the cleaning solvent composition used in the present invention contains a fluorine-based solvent and a flammable organic solvent, and optionally, an alcohol and / or phenol which is azeotroped with the fluorine-based solvent It further contains a system antioxidant and the like. Also, the cleaning solvent composition used in the present invention may optionally further contain an epoxy compound. And it is preferable that a washing
  • “does not have flammable” means that the flash point is measured by the tag sealing method and the Cleveland opening method according to JIS K2265, and the flash point is not recognized by any method. Point to.
  • fluorine-based solvent contained in the cleaning solvent composition are not particularly limited, and methyl perfluorobutyl ether, methyl perfluoroisobutyl ether, methyl perfluoropentyl ether, ethyl perfluorobutyl ether, ethyl Hydrofluoroethers such as perfluoroisobutyl ether; Hydrofluorocarbons such as 1,1,1,3,3-pentafluorobutane; Hydrofluorochloroolefins such as 1-chloro-3,3,3-trifluoropropene And hydrofluorocyclocarbons such as 1,1,2,2,3,3,4 heptafluorocyclopentane; and the like.
  • fluorocarbon solvents hydrofluorocarbons and hydrofluorocyclocarbons are preferable, and 1,1,1,3,3-pentafluorobutane and 1,1,2,2,3,3,3,4- Heptafluorocyclopentane is more preferred.
  • fluorine-type solvent mentioned above can be used individually by 1 type or in mixture of 2 or more types.
  • flammable organic solvent contained in the cleaning solvent composition are not particularly limited, and dipropylene glycol monobutyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monomethyl ether, dipropylene glycol mono Glycol ethers such as butyl ether and 3-methoxy-3-methyl butanol; Glycol ether acetates such as 3-methoxy-3-methyl butyl acetate; Aliphatic alcohols such as butanol, propanol, heptanol, hexanol, decanol and nonanol; Benzyl alcohol, methyl benzyl alcohol, ethyl benzyl alcohol, methoxy benzyl alcohol, ethoxy benzyl alcohol, hydroxy benzyl alcohol, 3-phenyl ester Aromatic alcohols such as panol, cumyl alcohol, furfuryl alcohol, phenethyl alcohol, methoxyphenethyl alcohol
  • butyl acetate, butyl propionate Mention may be made of esters such as methyl caproate and butyl caproate; carbonates such as dimethyl carbonate, diethyl carbonate and propyl carbonate; and lactones such as ⁇ -butyl lactone.
  • esters such as methyl caproate and butyl caproate
  • carbonates such as dimethyl carbonate, diethyl carbonate and propyl carbonate
  • lactones such as ⁇ -butyl lactone.
  • glycol ethers and aromatic alcohols are preferable, and 3-methoxy-3-methylbutanol, benzyl alcohol and phenethyl alcohol are more preferable.
  • the flammable organic solvent preferably has a boiling point higher than that of the fluorinated solvent.
  • the flammable organic solvent is particularly preferably an aromatic alcohol, and benzyl alcohol and It is more preferable to contain / or phenethyl alcohol.
  • the flammable organic solvent mentioned above can be used individually by 1 type or in mixture of 2 or more types.
  • the alcohol which can be used in the cleaning solvent composition and which forms an azeotropic mixture with the fluorine-based solvent is not particularly limited, and any alcohol such as tert-amyl alcohol can be used.
  • the fluorinated solvent is 1,1,2,2,3,3,4-heptafluorocyclopentane
  • the cleaning solvent composition is a tert-amyl alcohol as an alcohol which is azeotroped with the fluorinated solvent. Is preferred.
  • the phenol-based antioxidant that can be used for the cleaning solvent composition is not particularly limited, and phenol, 2,6-di-t-butylphenol, 2,6-di-t-butyl-p- Cresol, butyl hydroxyl anisole etc. can be mentioned. Among these, 2,6-di-t-butyl-p-cresol is preferable as a phenol-based antioxidant from the viewpoint of a high antioxidant effect.
  • the phenolic antioxidant mentioned above can be used individually by 1 type or in mixture of 2 or more types.
  • epoxy compounds which can be used for the cleaning solvent composition are not particularly limited, and butylene oxide, penten oxide, hexene oxide, heptene oxide, octene oxide, cyclopentene oxide, cyclohexene oxide, cycloheptene oxide And cyclooctene oxide, glycidol, methyl glycidyl ether, ethyl glycidyl ether, propyl glycidyl ether, butyl glycidyl ether and the like.
  • the epoxy compound mentioned above can be used individually by 1 type or in mixture of 2 or more types.
  • the proportions of the fluorine-based solvent and the flammable organic solvent contained in the cleaning solvent composition, and the alcohols, phenol-based antioxidants and epoxy-based compounds that azeotrope with the fluorine-based solvent that is an optional component It can be appropriately set according to the type of component and the like.
  • the cleaning of the object to be cleaned to which the dirt component adheres and the object to be cleaned is immersed in the cleaning solvent composition, or the cleaning solvent composition is sprayed onto the object to be cleaned, It can be carried out by dissolving the dirt components in At this time, the temperature of the cleaning solvent composition to be used can be appropriately set according to the solubility of the dirt component, and the cleaning solvent composition used for cleaning may be boiling.
  • the rinse of the object to be cleaned washed with the cleaning solvent composition is not particularly limited, and the object to be cleaned is dipped in the rinse solution, or the rinse liquid is sprayed onto the object to be washed and adheres to the object to be cleaned. It can be carried out by replacing the cleaning solvent composition and / or the cleaning solvent composition containing the soil component with a rinse solution.
  • the temperature of the rinse solution used is preferably kept as low as possible.
  • the temperature of the rinse solution is 20 times higher than the temperature of the steam used in steam cleaning. It is preferable that the temperature be lower than ° C.
  • the object to be cleaned in the rinse may be irradiated with ultrasonic waves, or physical force such as jet flow or peristalsis is used. You may add it.
  • the rinse solution is not particularly limited, and it is preferable to use a solvent containing the above-mentioned fluorine-based solvent as a main component (that is, a solvent containing 50 mass% or more of the fluorine-based solvent).
  • a solvent containing the fluorine-based solvent as a main component does not impair the rinse property and the vapor cleaning property, and in addition to the fluorine-based solvent, the solvent which forms an azeotrope with the flammable organic solvent and / or the fluorine-based solvent described above You may include the kind.
  • the solvent which has a fluorine-type solvent as a main component may further contain the epoxy-type compound mentioned above in the range which does not inhibit rinse property and steam cleaning property.
  • the solvent which has a fluorine-type solvent as a main component forms an azeotropic composition from a viewpoint of the predictability of flash point.
  • the fluorine-based solvent, the flammable organic solvent as an optional component, the alcohol which forms an azeotropy with the fluorine-based solvent, and the epoxy-based compound contained in the solvent containing the above-mentioned fluorine-based solvent as a main component It is preferred to use the same ones contained in the cleaning solvent composition used to wash the wash.
  • the vapor cleaning of the object to be cleaned rinsed with the rinse solution is not particularly limited, and can be performed by exposing the object to be cleaned to the vapor of the fluorine-based solvent described above as the main component. Then, in the vapor cleaning, due to the temperature difference between the vapor and the object to be cleaned, the vapor mainly composed of the vapor of the fluorine-based solvent becomes a condensate on the surface of the object to be cleaned, and the cleaning solvent composition etc. Be done.
  • the steam cleaning can be finished at the timing when the surface temperature of the object to be cleaned becomes the same as the temperature of the steam and the condensation of the vapor mainly composed of the vapor of the fluorinated solvent stops.
  • cleaning of a to-be-cleaned thing which has as a main component the vapor
  • the change in the composition of the cleaning solvent composition used for cleaning the object to be cleaned is evaporation of a solvent mainly composed of a fluorine-based solvent such as a rinse solution. This can be suppressed by feeding the cleaning solvent composition in an amount approximately equal to the amount.
  • cleaning arbitrarily can be dried using a well-known drying method, without being limited.
  • Process (b) Contamination components are mixed into the cleaning solvent composition used in the step (a) by cleaning the object to be cleaned. Then, since the cleaning solvent composition in which the dirt component is mixed has a reduced detergency, if the cleaning solvent composition is continued to be used for washing as it is, the dirt component tends to remain on the object to be washed. Therefore, in the method for cleaning the object to be cleaned according to the present invention, the cleaning solvent composition in which the dirt component formed in step (a) is dissolved is regenerated using the method for regenerating the cleaning solvent composition of the present invention described later. Ensure sufficient cleaning ability of the composition.
  • the concentration of the dirt component in the cleaning solvent composition to be regenerated in the step (b) can be appropriately set according to the cleaning power required for the cleaning solvent composition. That is, the cleaning solvent composition to be regenerated may be one in which the removal power of the dirt component is completely lost or may be one having a removal power of the dirt component to a certain extent.
  • the cleaning of the object to be cleaned using the regenerated cleaning solvent composition is not particularly limited, and the cleaning solvent containing the regenerated cleaning solvent composition as the cleaning solvent composition used for cleaning the object to be cleaned is used. Except using a composition, it can carry out like the process (a) mentioned above. That is, the washing of the object to be washed in the step (c) may be carried out using only the regenerated washing solvent composition, or the other washing solvent composition which has not been subjected to regeneration in the step (b). It may be carried out using a mixture of the cleaning solvent composition and the regenerated cleaning solvent composition.
  • the cleaning solvent composition not subjected to regeneration in the step (b) It is preferable to wash the material to be washed using a mixture with the regenerated washing solvent composition.
  • a step of regenerating the cleaning solvent composition in which the dirt component is dissolved in the step (c) in the same manner as the step (b) and d) repeatedly performing the step (e) of washing the object to be washed using the mixture of the washing solvent composition not subjected to regeneration in the step (d) and the regenerated washing solvent composition.
  • step (d) and step (e) are repeated after step (b) and step (c), the concentration of the dirt component in the cleaning solvent composition used for cleaning the object to be cleaned is
  • the object to be cleaned can be cleaned continuously and efficiently while maintaining the concentration below the desired concentration. And as a result, the wash which is excellent in cleanliness can be obtained.
  • the method of regenerating the cleaning solvent composition of the present invention is used in regenerating the cleaning solvent composition by separating and removing the soil components from the cleaning solvent composition in which the soil components are dissolved. And depositing the dirt component from the washing solvent composition in which the dirt component is dissolved, and obtaining the mixture containing the deposited dirt component and the washing solvent composition, and the mixture obtained in step (A) being a dirt component
  • the method comprises the steps of: (B) contacting with the affinity material; and (C) removing the soil component from the mixture brought into contact with the soil material compatible material in the step (B) to obtain a regenerated cleaning solvent composition. It is characterized by And, according to the method for regenerating the cleaning solvent composition of the present invention, since the mixture containing the deposited dirt component and the cleaning solvent composition is brought into contact with the dirt component compatible material, the dirt components can be separated efficiently. be able to.
  • the method of regenerating the cleaning solvent composition of the present invention is particularly preferably used when the cleaning solvent composition is regenerated in the step (b) and the step (d) of the method of cleaning an object to be cleaned of the present invention described above.
  • the method of regenerating the cleaning solvent composition of the present invention may be used for applications other than the method of cleaning the object of the present invention described above.
  • the dirt component is precipitated from the washing solvent composition in which the dirt component is dissolved, and a mixture containing the deposited dirt component and the washing solvent composition is obtained.
  • the method of precipitating the dirt component is not particularly limited, and examples thereof include cooling, addition of a poor solvent, and a combination thereof. Among them, there is no need to separate and remove the poor solvent when reusing the regenerated cleaning solvent composition, and from the viewpoint that the dirt component can be deposited by a simple operation, the dirt component is the dirt component It is preferable to carry out by cooling the dissolved cleaning solvent composition.
  • the poor solvent is not particularly limited, and the above-mentioned fluorine-based solvent, rinse solution, and the like can be used.
  • the poor solvent it is preferable to use a fluorine-based solvent or a solvent containing a fluorine-based solvent as a main component, and it is more preferable to use the same fluorine-based solvent as the fluorine-based solvent contained in the cleaning solvent composition.
  • the added poor solvent may be recovered from the mixture after removing the dirt component in step (C) using a known method such as distillation. it can.
  • the poor solvent is recovered from the mixture after the removal of the dirt component, the composition of the regenerated cleaning solvent composition is prevented from being changed by the addition of the poor solvent, and the regenerated cleaning solvent composition is obtained. It can be easily reused.
  • step (B) the mixture containing the deposited soil component and the cleaning solvent composition obtained in the step (A) is brought into contact with the soil component compatible material to enhance the separation of the deposited soil component. Specifically, in the step (B), the mixture is brought into contact with the soil component compatible material to coarsen the soil component, thereby enabling efficient separation of the soil component in the step (C).
  • step (B) it is necessary to make the mixture of the state in which the dirt component precipitated contact a dirt component affinity material. Therefore, when dirt components are precipitated by cooling in step (A), the temperature of the mixture in step (B) is preferably below the temperature at which dirt components were precipitated in step (A).
  • the stain component affinity material although depending on the type of the stain component, for example, polyethylene resin, polypropylene resin, nylon resin, polyester resin, phenol resin, ion exchange resin, etc. can be mentioned. Among them, polyethylene resin and / or ion exchange resin is preferable as the stain component affinity material for hydrocarbon stain components such as hydrocarbon type processing oil. And as an ion exchange resin, the ion exchange resin which made the base material the copolymer of styrene and divinylbenzene is not particularly limited. Moreover, as an ion exchange resin, strongly acidic cation exchange resin or weak basic ion exchange resin is preferable, and strongly acidic ion exchange resin is more preferable. In addition, the dirt component affinity material mentioned above can be used individually by 1 type or in mixture of 2 or more types.
  • the shape of the stain component affinity material is not particularly limited, but is preferably in the form of particles, and more preferably in the form of spheres.
  • the particle diameter of the stain affinity material is preferably 0.05 mm or more, more preferably 0.1 mm or more, and preferably 2.0 mm or less. If the particle diameter is equal to or more than the above lower limit value, the stain component affinity material may have a sufficient size as compared to the deposited dirt component, so the mixture containing the deposited dirt component and the cleaning solvent composition is stained. When contacting with the component compatible material, it is possible to suppress an increase in pressure loss and clogging. Therefore, the workability and economic efficiency at the time of regenerating the cleaning solvent composition can be improved. In addition, when the particle diameter is equal to or less than the above upper limit value, the contact area with the mixture can be sufficiently secured.
  • a contact with the mixture in a process (B) and dirt ingredient affinity material can be performed using an arbitrary contact method, without being limited in particular.
  • the contact method it is preferable to use a method in which the mixture is caused to flow in a container filled with a soil component compatible material such as a packed column.
  • the speed is preferably 5 m / h or more, more preferably 8 m / h or more, preferably 25 m / h or less, and more preferably 15 m / h or less.
  • the space velocity at the time of distributing the mixture in a container filled with soil components affinity material such as packed tower it is preferably 10h -1 or more, and 16h -1 or more more preferably, it is preferable that 30h is less than -1, and more preferably 26h -1.
  • step (C) the soil component is removed from the mixture brought into contact with the soil component compatible material in step (B) to obtain a regenerated cleaning solvent composition.
  • the dirt component that has precipitated is coarsened. Therefore, in the step (C), the dirt component can be easily removed from the mixture, for example, by utilizing the difference in specific gravity between the deposited dirt component and the cleaning solvent composition.
  • the specific gravity of the stain component is smaller than the specific gravity of the cleaning solvent composition, the stain component floating in the mixture brought into contact with the stain component compatible material is removed.
  • step (C) when the specific gravity of the soil component is larger than the specific gravity of the cleaning solvent composition, by removing the soil component precipitated in the mixture brought into contact with the soil component compatible material; Alternatively, by removing the washing solvent composition as the supernatant liquid, the soil components deposited in the step (A) can be removed from the mixture to obtain a regenerated washing solvent composition.
  • the cleaning solvent composition may be regenerated by a one-pass method in which the step (C) described above is carried out in the separation unit for removing the water, but the above steps (B) and (B) Preferably, the cleaning solvent composition is regenerated in a circulating manner to carry out C). If the cleaning solvent composition is regenerated while circulating the mixture between the contact portion and the separation portion, the deposited dirt components can be separated and removed while being coarsened more favorably, so the dirt components can be removed. It is possible to separate more efficiently.
  • the cleaning system for objects to be cleaned according to the present invention is used when cleaning an object to be cleaned to which dirt components adhere, with the cleaning solvent composition.
  • An apparatus for cleaning the cleaning target to which the component is adhered using a cleaning solvent composition an apparatus for regenerating the cleaning solvent composition of the present invention to be described in detail later, and a cleaning apparatus discharged from the cleaning apparatus It is characterized by comprising a regeneration line for sending the cleaning solvent composition to the regeneration device, and a recycling line for sending the regenerated cleaning solvent composition discharged from the regeneration device to the cleaning device.
  • the regenerated cleaning solvent composition discharged from the regenerating apparatus can be sent to the cleaning apparatus to be reused, so it is necessary to clean the object to be cleaned. Cost can be reduced effectively.
  • the apparatus for regenerating the cleaning solvent composition of the present invention is used when the cleaning solvent composition is regenerated by separating and removing the soiling component from the cleaning solvent composition in which the soiling component is dissolved, and the cleaning with the soiling component dissolved.
  • a separator for removing dirt from the mixture in contact with the affinity material since the contact portion is provided, the dirt component can be efficiently separated in the separation portion.
  • the apparatus for regenerating the cleaning solvent composition of the present invention can be particularly suitably used as the apparatus for regenerating the cleaning system for the object to be cleaned of the present invention described above, the apparatus for regenerating the cleaning solvent composition of the present invention is It may be used for cleaning systems other than the cleaning system of the thing to be washed of the present invention mentioned above, and may be used independently, without incorporating in a cleaning system.
  • cleaned material of this invention and the reproducing
  • cleaning solvent composition are not specifically limited, For example, it has a structure as shown in FIG.
  • the cleaning system 100 for the object to be cleaned shown in FIG. 1 is discharged from the cleaning device 10 for cleaning the object to be cleaned to which the dirt component adheres, the regenerating device 20 for the cleaning solvent composition, and the cleaning device 10.
  • the cleaning solvent composition in which the object to be cleaned, the soil component, the cleaning solvent composition and the soil component are dissolved the same method as the method for cleaning the object to be cleaned of the present invention described above can be used. I omit explanation.
  • the cleaning device 10 is not particularly limited, and is, for example, a two-tank type cleaning device, in which the cleaning solvent composition is stored, the cleaning tank 11 for cleaning the object to be cleaned, and the rinse liquid is stored. And 11 a rinse tank 12 for rinsing the object to be cleaned.
  • the cleaning apparatus 10 further includes an overflow pipe 13 for feeding the rinse liquid from the rinse tank 12 to the cleaning tank 11 and a heater 14 for heating the cleaning solvent composition in the cleaning tank 11.
  • a cooling coil 16 is provided above the cleaning tank 11 and the rinse tank 12 in the cleaning apparatus 10, and the upper part of the cleaning tank 11 and the rinse tank 12, more specifically, the cleaning tank 11 and the rinse tank 12
  • a vapor phase 15 is formed between the cooling coil 16 and the vapor heated by the heater 14 and accumulated therein.
  • the cleaning apparatus 10 further includes a water separator 17 that removes water from the condensate of the steam cooled by the cooling coil 16 and sends the obtained liquid to the rinse tank 12. Even if the cleaning tank 11 of the cleaning apparatus 10 is equipped with a sensor (for example, a thermometer, a hydrometer, a liquid level meter, etc.) for controlling the concentration of the flammable organic solvent in the cleaning solvent composition. Good.
  • a sensor for example, a thermometer, a hydrometer, a liquid level meter, etc.
  • the vapor obtained by heating the cleaning solvent composition with the heater 14 usually contains the vapor of the fluorinated solvent as the main component. And the condensate of the said vapor has a fluorine system solvent as a main component, and may contain water.
  • the regenerating apparatus 20 contacts the soil component affinity material with a mixture containing the deposition tank 21 as a deposition portion for depositing the soil component from the cleaning solvent composition in which the soil component is dissolved, and the deposited soil component and the cleaning solvent composition.
  • the separation vessel 22 as a separation part which removes a dirt component from the mixture which contacted the dirt component affinity material in the filling container 24 is provided.
  • the regeneration device 20 is a pump that extracts the mixture containing the deposited dirt component and the cleaning solvent composition from the lower part of the separation tank 22 and sends it to the filling container 24 to flow the mixture into the filling container 24 in upward flow.
  • the precipitation tank 21 of the regenerating apparatus 20 is connected to the lower portion of the cleaning tank 11 of the cleaning apparatus 10 through the regeneration line 18. Moreover, the precipitation tank 21 is equipped with the cooler which is not shown in figure. And in the precipitation tank 21, while the washing
  • the separation tank 22 includes at least two partition plates (two in the illustrated example, the first partition plate 22A and the second partition plate 22B) in the tank. Then, in the first region located in the separation tank 22 on the opposite side (left side in the illustrated example) to the second partition plate 22B side than the first partition plate 22A, the deposited dirt component and the cleaning solvent composition As a mixture containing the mixture flows out of the precipitation tank 21, the mixture in contact with the soil component compatible material flows in via the return line 27B. Furthermore, a discharge line 25 for discharging the separated dirt component is connected to the first area.
  • a delivery line 27A is connected to the lower part of the second region located between the first partition plate 22A and the second partition plate 22B in the separation tank 22.
  • the separation tank 22 of the regenerating apparatus 20 and the cleaning apparatus are provided in the third region of the separation tank 22 located on the opposite side (right side in the illustrated example) to the first partition plate 22A side than the second partition plate 22B.
  • Reuse lines 26 are connected to connect the lower portions of the ten cleaning tanks 11.
  • the filling container 24 is filled with the stain component compatible material.
  • the filling container 24 is not particularly limited, and, for example, a filling tower or the like can be used.
  • the loading of the soil component compatible material is not particularly limited, and for example, the soil component compatible material can be filled using a mesh-like support member which allows the mixture to pass but not the soil component compatible material. It can be done by keeping it inside.
  • cleaning solvent composition of this invention mentioned above can be used as a dirt component affinity material, description is abbreviate
  • the cleaning of the object to be cleaned, the regeneration of the cleaning solvent composition, and the reuse of the regenerated cleaning solvent composition can be performed as follows.
  • the to-be-cleaned material to which the dirt component has adhered can be washed by immersing in the washing solvent composition in the washing tank 11 and dissolving the dirt component in the washing solvent composition.
  • cleaning solvent composition in the washing tank 11 can be suitably set according to the solubility of a dirt component, and the washing
  • cleaned by the washing tank 11 is immersed in the rinse liquid of the rinse tank 12 in order to rinse the washing
  • the object to be cleaned may be irradiated with ultrasonic waves, or physical force such as jet flow or peristalsis may be applied.
  • the temperature of the rinse solution in the rinse tank 12 is not particularly limited, but is preferably kept as low as possible to enhance the steam cleaning property, and is preferably 20 ° C. or more lower than the temperature of the steam of the vapor phase 15 .
  • the object to be cleaned is pulled from the rinse tank 12 to the vapor phase 15 and is vapor-cleaned. And the to-be-washed
  • the composition and the amount of the cleaning solvent composition and the rinse liquid are generated by the vapor of the fluorinated solvent generated by heating by the heater 14 as the main component by the cooling coil 16 It is cooled to form a condensate, which is removed by the water separator 17 and returned to the rinse tank 12 so that a rinse solution mainly composed of a fluorinated solvent having an amount substantially equivalent to the amount of evaporation overflows the overflow pipe 4 By flowing into the cleaning tank 11 through the, it can be maintained substantially uniform.
  • a part of the cleaning solvent composition in which the dirt component is mixed by the cleaning of the object to be cleaned is sent from the cleaning tank 11 to the regenerating apparatus 20, and is regenerated as follows. Specifically, the cleaning solvent composition in the cleaning tank 11 is sent to the precipitation tank 21 through the regeneration line 18, and is cooled in the precipitation tank 21 to a temperature at which the dirt components are precipitated. Next, the mixture containing the deposited dirt component and the cleaning solvent composition is sent to the separation tank 22 and then from the separation tank 22 to the filling container 24 via the pump 23 and the delivery line 27A, and the dirt component Contact with affinity material. Furthermore, the mixture that has flowed out of the filling container 24 is returned to the separation tank 22 and circulates between the separation tank 22 and the filling container 24.
  • the dirt component finely dispersed in the mixture is coarsened by contact with the dirt component compatible material, and is easily separated due to the difference in specific gravity with the cleaning solvent composition.
  • the deposited dirt components float on the upper side in the first region and the second region of the separation tank 22 and are collected and discharged from the discharge line 25 to any treatment facility such as a waste liquid tank and discarded.
  • the cleaning solvent composition (the regenerated cleaning solvent composition) from which the dirt component has been separated and removed and the detergency recovered is transferred from the third region of the separation tank 22 to the cleaning tank 11 through the reuse line 26. It is sent and reused to wash the objects to be cleaned.
  • the specific gravity of the dirt component is smaller than the specific gravity of the cleaning solvent composition and the dirt component floats up in the separation tank 22 is described here, the specific gravity of the dirt component is higher than the specific gravity of the cleaning solvent composition In the case of a large size, the dirt component that has settled in the separation tank 22 may be pulled out from the lower part of the separation tank 22.
  • the cleaning solvent composition is extracted from the cleaning tank 11 in an amount determined by the amount of the dirt component to be removed and the solubility of the dirt component and the cleaning solvent composition, etc. Even when the cleaning product is continuously cleaned, the concentration of the dirt component in the cleaning solvent composition can be kept constant or less, and the cleaning ability of the cleaning solvent composition can be sufficiently secured. As a result, efficient cleaning of the object to be cleaned can be realized.
  • the cleaning system and the cleaning solvent composition regenerating apparatus of the present invention have been described above using an example, but the cleaning system and the cleaning solvent composition regenerating apparatus of the present invention according to the present invention It is not limited to the example described above.
  • the number of cleaning tanks and rinsing tanks may be two or more as needed.
  • the return destination of the regenerated cleaning solvent composition is not limited to the cleaning tank 11. Even if the regenerated cleaning solvent composition is used for cleaning the cleaning object in the separately prepared cleaning tank, etc. Good.
  • the dirt component may be precipitated by the addition of a poor solvent.
  • the deposition tank 21 may be provided with a poor solvent addition mechanism, and the recycling line 26 may be provided with an apparatus for recovering a poor solvent such as a distillation apparatus.
  • the cleaning solvent composition may be cooled in the separation tank 22 to precipitate the dirt component without providing the precipitation tank 21.
  • the separation tank 22 may be provided with an inclined plate for accelerating the separation of the dirt component.
  • the deposition tank 21 and the filling container 24 may be directly connected without providing the delivery line 27A and the return line 27B.
  • the present invention will be more specifically described based on examples and comparative examples, but the present invention is not limited to the following examples.
  • concentration of the dirt component was measured as follows.
  • the concentration of the dirt component was determined using a calibration curve method. Specifically, first, 25 ml of a cleaning solvent composition in which a dirt component having a known concentration is dissolved is prepared, and the mass at 25 ° C. is measured to determine the density. In addition, 25 ml of the cleaning solvent composition containing no dirt component is prepared, and the mass at 25 ° C. is measured to determine the density. Then, a calibration curve is created using the density of the cleaning solvent composition that does not contain the dirt component and the density of the cleaning solvent composition in which the dirt component is dissolved. Next, for 25 ml of the cleaning solvent composition to be measured, the mass at 25 ° C. is measured to determine the density. Then, the concentration of the dirt component in the cleaning solvent composition to be measured is determined from the calculated density using a calibration curve.
  • Example 1 Using the combination (1) shown in Table 4 as the soil component, the cleaning solvent composition and the filler, a regeneration test of the cleaning solvent composition was conducted. Specifically, first, Lilia-cut DS-10 as a dirt component is added to 1 L of the washing solvent composition (1) at 6% by mass, the solution is boiled and cooled to room temperature, and the test solution (washing with dirt components dissolved) Solution composition was obtained.
  • the test solution was withdrawn from the glass bottle from the bottom of the bottle using a circulation pump, and the test solution flowing out of the top of the packed column was returned to the middle of the bottle.
  • C Removal rate is less than 10%
  • Example 2 The cleaning solvent composition was subjected to a regeneration test in the same manner as in Example 1 except that the temperature in the test solution and the packed column was changed to 4 ° C. and the circulation conditions were changed as shown in Table 6. And evaluation was performed in the same manner as in Example 1. The results are shown in Table 6.
  • Example 3 Using the combination (2) shown in Table 4 as the dirt component, the washing solvent composition and the filler, 10 mass% of Cut Arbus KZ 216 as the dirt component is added to 1 L of the washing solvent composition (1) to prepare a test solution Further, a regeneration test of the cleaning solvent composition was conducted in the same manner as in Example 1 except that the circulation conditions were changed as shown in Table 7. And evaluation was performed in the same manner as in Example 1. The results are shown in Table 7.
  • Example 4 A cleaning solvent composition was prepared in the same manner as in Example 1 except that the combination (3) shown in Table 4 was used as the dirt component, the cleaning solvent composition and the filler, and the circulation conditions were changed as shown in Table 8. The regeneration test was performed. And evaluation was performed in the same manner as in Example 1. The results are shown in Table 8.
  • Example 5 Using the combination (4) shown in Table 4 as the dirt component, the washing solvent composition and the filler, 10 mass% of Cut Arbus KZ 216 as the dirt component is added to 1 L of the washing solvent composition (2) to prepare a test solution
  • the cleaning solvent composition was subjected to a regeneration test of the washing solvent composition in the same manner as in Example 1 except that the temperature in the test solution and the packed column was changed to 5 ° C., and the circulation conditions were changed as shown in Table 9. And evaluation was performed in the same manner as in Example 1. The results are shown in Table 9.
  • Example 6 In the test device 30 shown in FIG. 2, the continuous regeneration test of the cleaning solvent composition was conducted using the combination (1) shown in Table 4 as the dirt component, the cleaning solvent composition and the filler. Specifically, first, 6% by mass of Lilia cut DS-10 as a dirt component is added to the washing solvent composition (1), the mixture is boiled and cooled to room temperature, and the test solution (washing solution in which the dirt component is dissolved) The composition was obtained. Next, the test solution was put into the container 34 (volume: 3.2 L, the partition plate 36 and the inclined plate 37 were installed) of the test apparatus 30 shown in FIG. 2 from the test solution supply port 31 and cooled to 5 ° C.
  • the test solution was put into the container 34 (volume: 3.2 L, the partition plate 36 and the inclined plate 37 were installed) of the test apparatus 30 shown in FIG. 2 from the test solution supply port 31 and cooled to 5 ° C.
  • the cleaning solvent composition in the container 34 has a linear velocity of 10.2 m / h in the packed tower 38 in the order of the circulating fluid intake 35, the packed tower 38 and the circulating fluid outlet 33, and the space velocity is It was circulated at 18 h -1 and circulated for 50 minutes.
  • test solution cooled to 5 ° C. was continuously supplied from the test solution supply port 31 to the container 34 at a flow rate of 1.8 L / h.
  • cleaning solvent composition which flowed out from the sampling port 32 was measured, it carried out similarly to Example 1, calculation of the removal rate of dirt components and evaluation of the removal efficiency of dirt components were performed. The results are shown in Table 10.
  • Example 2 The test solution prepared in Example 1 was cooled to 5 ° C. to be in an opaque state and allowed to stand for 30 minutes. As a result, the test solution remained in an opaque state, and the dirt component did not float and separate.
  • the dirt component can be efficiently separated from the cleaning solvent composition in which the dirt component is dissolved, and the cleaning solvent composition can be efficiently regenerated.
  • an object to be cleaned can be efficiently cleaned using a regenerated cleaning solvent composition obtained by efficiently separating dirt components.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Emergency Medicine (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

La présente invention concerne un procédé de recyclage pour une composition de solvant de nettoyage grâce auquel des contaminants peuvent être efficacement séparés. Un procédé de recyclage pour une composition de solvant de nettoyage dans lequel des contaminants sont dissous, la composition de solvant de nettoyage contenant un solvant à base de fluor et un solvant organique inflammable, et ledit procédé comprenant : une étape (A) pour précipiter des contaminants à partir de la composition de solvant de nettoyage dans laquelle les contaminants sont dissous pour obtenir un mélange comprenant les contaminants précipités et la composition de solvant de nettoyage; une étape (B) pour amener le mélange en contact avec un matériau ayant une affinité pour les contaminants; et une étape (C) pour éliminer les contaminants du mélange qui a été mis en contact avec le matériau ayant une affinité pour les contaminants afin d'obtenir une composition de solvant de nettoyage recyclée.
PCT/JP2018/040909 2017-11-10 2018-11-02 Procédé et dispositif de recyclage pour nettoyer une composition de solvant, et procédé et système de nettoyage pour objet à nettoyer WO2019093251A1 (fr)

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CN201880069532.7A CN111278578A (zh) 2017-11-10 2018-11-02 清洗溶剂组合物的再生方法和再生装置、以及被清洗物的清洗方法和清洗系统
JP2019552767A JPWO2019093251A1 (ja) 2017-11-10 2018-11-02 洗浄溶剤組成物の再生方法および再生装置、並びに、被洗浄物の洗浄方法および洗浄システム

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