WO2022176696A1 - Dispositif d'élimination de particules fines et procédé d'élimination de particules fines - Google Patents

Dispositif d'élimination de particules fines et procédé d'élimination de particules fines Download PDF

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Publication number
WO2022176696A1
WO2022176696A1 PCT/JP2022/004830 JP2022004830W WO2022176696A1 WO 2022176696 A1 WO2022176696 A1 WO 2022176696A1 JP 2022004830 W JP2022004830 W JP 2022004830W WO 2022176696 A1 WO2022176696 A1 WO 2022176696A1
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Prior art keywords
membrane
size exclusion
fine particle
particle removal
chargeable
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PCT/JP2022/004830
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English (en)
Japanese (ja)
Inventor
洋一 田中
秀章 飯野
侑 藤村
孝博 川勝
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栗田工業株式会社
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Publication of WO2022176696A1 publication Critical patent/WO2022176696A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58—Multistep processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties

Definitions

  • the present invention relates to a particle removing apparatus and a particle removing method for removing particles in a liquid in a pure water or ultrapure water manufacturing process, or in an electronic component manufacturing process, a semiconductor cleaning process, or the like.
  • the present invention also relates to a pure water or ultrapure water production apparatus equipped with this fine particle removal device.
  • the present invention is highly effective in removing fine particles with a particle diameter of 50 nm or less in liquids in systems such as subsystems and water supply lines before the point of use in ultrapure water production and supply systems, and electronic component manufacturing processes and semiconductor cleaning processes. It is useful as a technique for removing
  • Size exclusion membranes such as microfiltration membranes and ultrafiltration membranes are common as filters for manufacturing semiconductors and electronic parts and filters used in the manufacturing process of semiconductors and electronic parts.
  • a positively charged membrane specifically a polyketone membrane, has one selected from the group consisting of primary amino groups, secondary amino groups, tertiary amino groups and quaternary ammonium salts.
  • a membrane having one or more cationic functional groups Patent Document 1.
  • the negatively charged membrane one or more selected from the group consisting of a sulfonic acid group, a sulfonic acid ester group, a carboxylic acid group, a carboxylic acid ester group, a phosphoric acid group, a phosphoric acid ester group, and a hydroxyl group is added to the polyketone membrane.
  • a sulfonic acid group a sulfonic acid ester group, a carboxylic acid group, a carboxylic acid ester group, a phosphoric acid group, a phosphoric acid ester group, and a hydroxyl group
  • Patent Document 2 There is also a method of using a membrane having an anionic functional group of (Patent Document 2).
  • the smaller the particles to be removed the smaller the pore size, which reduces the amount of treated water. Further, when the cumulative load amount of fine particles increases, the removal rate of fine particles decreases.
  • the present invention provides a particle removing apparatus and a particle removing method capable of improving such drawbacks of the size exclusion membrane, maintaining the particle removing performance of the size exclusion membrane for a long period of time, and prolonging the service life of the particle removing apparatus and the particle removing method.
  • An object of the present invention is to provide a pure water or ultra-pure water production device including the device.
  • the inventors of the present invention have found that by providing an electrically charged filtration membrane in series prior to the size exclusion membrane, the accumulated fine particle load of the size exclusion membrane is reduced, the fine particle removal performance is maintained for a long period of time, and the service life of the size exclusion membrane is extended. I found a way to extend it.
  • the gist of the present invention is as follows.
  • a microparticle removal device for removing microparticles in a liquid which has a chargeable filtration membrane and a size exclusion membrane disposed downstream of the chargeable filtration membrane, and the liquid is the chargeable , and a fine particle removal device characterized in that water is passed through the size exclusion membrane in this order.
  • a particle removing device characterized in that it is arranged in series and has the size exclusion membrane in the rear stage of the membrane group arranged in series.
  • a pure water or ultrapure water production device comprising the fine particle removal device according to any one of [1] to [3].
  • the present invention it is possible to reduce the cumulative particle load of the size exclusion membrane that removes particles, maintain the particle removal performance over a long period of time, and extend the service life of the membrane.
  • fine particles are stably and efficiently removed over a long period of time from water systems in general, particularly pure water and ultrapure water production processes, or from various liquids used in electronic component production and semiconductor cleaning processes to achieve high purification. can be achieved.
  • FIG. 1 is a system diagram showing an embodiment of the particulate removing apparatus of the present invention.
  • FIG. 2 is a schematic diagram illustrating a fine particle trapping mechanism by a membrane having a cationic functional group or an anionic functional group.
  • FIG. 3 is a system diagram showing a test apparatus used in Reference Examples and Comparative Examples.
  • FIG. 4 is a system diagram showing the test equipment used in the examples.
  • a film having a cationic functional group does not easily adsorb positively charged fine particles, but easily adsorbs negatively charged fine particles. Can be efficiently captured and removed.
  • the film having an anionic functional group does not easily adsorb negatively charged fine particles, but easily adsorbs positively charged fine particles. Fine particles can be efficiently captured and removed.
  • fine particles in a liquid are often positively or negatively charged. Therefore, by providing a chargeable membrane in front of the size exclusion membrane, these fine particles can be efficiently removed in advance. can reduce the particle loading of the size exclusion membrane and extend its service life.
  • the integrated fine particle load For the size exclusion membrane, it is desirable to keep the integrated fine particle load to 10% or less when the entire membrane area is 100%, in order to maintain high fine particle removal performance. Therefore, in the present invention, by providing a chargeable membrane in front of the size exclusion membrane, the ratio of the integrated fine particle load (the ratio of the total amount of fine particles loaded to the membrane area covering the membrane area) to 10% of the entire membrane area. % or less.
  • a chargeable membrane module 1 and a size exclusion membrane module 2 are provided in series.
  • An additional chargeable membrane module or a size exclusion membrane module may be arranged upstream of the chargeable membrane module 1 .
  • Another membrane module may be arranged between the chargeable membrane module 1 and the size exclusion membrane module 2 .
  • the liquid to be treated introduced through the pipe 10 is introduced into the chargeable membrane module 1 and subjected to particle removal treatment, and then introduced through the pipe 11 into the size exclusion membrane module 2. After the fine particle removal treatment, the treated water is discharged out of the system through the pipe 12 .
  • the liquid to be treated from which fine particles are removed is not particularly limited.
  • the liquid to be treated include pure water, alcohol such as isopropyl alcohol, aqueous inorganic acid such as sulfuric acid aqueous solution and hydrochloric acid aqueous solution, alkaline aqueous solution such as sodium hydroxide aqueous solution and ammonia aqueous solution, thinner, carbonated water, hydrogen peroxide solution, Hydrogen fluoride solution and the like can be mentioned.
  • the present invention can be applied to the treatment of liquids in all pH ranges of pH 1-14.
  • Liquids in the neutral pH range include ultrapure water.
  • Carbonated water, hydrochloric acid aqueous solution, hydrogen fluoride solution and the like are typical examples of acidic liquids having a pH of 7 or less.
  • Representative examples of alkaline liquids having a pH of 7 or higher include ammonia water and aqueous sodium hydroxide solution.
  • the liquid to be treated is not limited to this.
  • the present invention is effective in removing ultrafine particles with a particle size of 50 nm or less, for example, about 3 to 30 nm, in these liquids.
  • inorganic oxide fine particles such as silica, alumina, titania, and iron oxide, fluorine-based fine particles, organic resin fine particles, and the like can be mentioned.
  • the fine particle concentration in the liquid to be treated is also not particularly limited, but is usually 100 ⁇ g/L or less, or 1 to 10 10 particles/mL.
  • the pH of the liquid to be treated is preferably in a region where the zeta potential of fine particles in the liquid is not reversed (a region where the isoelectric point is not crossed).
  • the pH is preferably always 8 or less or always 8 or more. It is preferable that the silica fine particles that are negatively charged or positively charged at pH 3 are always in the range of pH 3 or less or pH 3 or more.
  • ⁇ Chargeable membrane> The chargeable membrane preferably used in the present invention will be described below.
  • a positively charged film is referred to as a "positively charged film” and a negatively charged film is referred to as a "negatively charged film”.
  • the form of the chargeable membrane may be hollow fiber membrane, flat membrane, fiber, or the like. Hollow fiber membranes are generally used as terminal membrane modules for removing fine particles in ultrapure water production processes. A pleated flat membrane can also be used for the filter attached to the process washer.
  • the porous membrane that serves as the base material of the chargeable membrane may be a polymer membrane, an inorganic membrane, or a metal membrane.
  • Polymer membranes include polyolefins such as polyethylene and polypropylene, polyethers such as polyethylene oxide and polypropylene oxide, fluororesins such as PTFE, CTFE, PFA, and polyvinylidene fluoride (PVDF), halogenated polyolefins such as polyvinyl chloride, and nylon.
  • polyolefins such as polyethylene and polypropylene
  • polyethers such as polyethylene oxide and polypropylene oxide
  • fluororesins such as PTFE, CTFE, PFA, and polyvinylidene fluoride (PVDF)
  • PVDF polyvinylidene fluoride
  • halogenated polyolefins such as polyvinyl chloride, and nylon.
  • polyamides such as nylon-66, urea resins, phenolic resins, melamine resins, polystyrene, cellulose, cellulose acetate, cellulose nitrate, polyetherketones, polyetherketoneketones, polyetheretherketones, polysulfones, polyarylsulfones, poly Materials such as ethersulfone, polyimide, polyetherimide, polyamideimide, polybenzimidazole, polycarbonate, polyethylene terephthalate, polybutylene terephthalate, polyphenylene sulfide, polyacrylonitrile, polyethernitrile, polyvinyl alcohol, and copolymers thereof can be used. However, it is not limited to this.
  • the polymer film is not limited to one type of material, and various materials can be selected as required. Other polymers such as polyolefins and polyethers may be mixed with the chargeable or conductive polymer.
  • Materials such as alumina, zirconia, and titania can be used as inorganic films, but are not limited to these.
  • Materials such as stainless steel can be used as the metal film, but it is not limited to this.
  • the charged functional groups to be introduced into the porous membrane include sulfonic acid groups, phosphoric acid groups, phosphonic acid groups, phosphinic acid groups, carboxylic acid groups, hydroxyl groups, phenol groups, quaternary ammonium groups, primary to tertiary amine groups, Examples include pyridine group and amide group, but are not limited to these. These functional groups may be not only H-type and OH-type but also salt-type such as Na.
  • a method for introducing the chargeable functional group is not particularly limited, and various methods can be adopted.
  • sulfonic acid groups can be introduced by adding an appropriate amount of paraformaldehyde to a sulfuric acid solution and heat-crosslinking.
  • a functional group can be introduced by reacting a hydroxyl group with a trialkoxysilane group, a trichlorosilane group, an epoxy group, or the like.
  • a reactive monomer such as styrene
  • the target functional group may be introduced through the process.
  • reactive monomers include, but are not limited to, glycidyl methacrylate, styrene, chloromethylstyrene, acrolein, vinylpyridine, acrylonitrile, and the like.
  • the cationization method for introducing the positively charged functional group is not particularly limited, but examples include a coating method and a combination of these methods.
  • a dehydration condensation reaction etc. are mentioned as the method by a chemical reaction. Plasma treatment, corona treatment and the like can also be used.
  • the coating method includes a method of impregnating with an aqueous solution containing a polymer.
  • chemical modification methods for imparting cationic amino groups to polyketone membranes include chemical reaction with primary amines.
  • primary amines ethylenediamine, 1,3-propanediamine, 1,4-butanediamine, 1,2-cyclohexanediamine, N-methylethylenediamine, N-methylpropanediamine, N,N-dimethylethylenediamine, N,N-dimethylpropanediamine, N Polyfunctionalized amines such as diamines, triamines, tetraamines, polyethylenimines, including primary amines such as acetylethylenediamine, isophoronediamine, N,N-dimethylamino-1,3-propanediamine, etc., have many activities. It is preferable because points can be given.
  • Substitution methods include, for example, irradiation with electron beams, ⁇ -rays, plasma, etc. After generating radicals by graft polymerization, a monomer having a reactive side chain such as glycidyl methacrylate is polymerized, and a reactive monomer having a functional group that expresses the desired function is added.
  • reactive monomers examples include derivatives of acrylic acid, methacrylic acid, vinylsulfonic acid including primary amines, secondary amines, tertiary amines, quaternary ammonium salts, allylamine, p-vinylbenzyltrimethylammonium chloride, and the like. be done.
  • More specific examples include 3-(dimethylamino)propyl acrylate, 3-(dimethylamino)propyl methacrylate, N-[3-(dimethylamino)propyl]acrylamide, N-[3-(dimethylamino) propyl]methacrylamide, (3-acrylamidopropyl)trimethylammonium chloride, trimethyl[3-(methacryloylamino)propyl]ammonium chloride and the like.
  • polymers having a positive zeta potential examples include PSQ (polysilsesquioxane), polyethyleneimine, polydiallyldimethylammonium chloride, amino group-containing cationic poly(meth) Acrylic acid ester, amino group-containing cationic poly(meth)acrylamide, polyamineamide-epichlorohydrin, polyallylamine, polydicyandiamide, chitosan, cationized chitosan, amino group-containing cationized starch, amino group-containing cationized cellulose, amino Group-containing cationized polyvinyl alcohols and acid salts of the above polymers are included. Further, the polymer or the acid salt of the polymer may be a copolymer with another polymer.
  • the anionization method for introducing the negatively chargeable functional group is not particularly limited, but the following methods may be mentioned.
  • negatively chargeable functional groups include a sulfonic acid group, a sulfonic acid ester group, a carboxylic acid group, a carboxylic acid ester group, a phosphoric acid group, a phosphoric acid ester group, One or more functional groups selected from the group consisting of hydroxyl groups are included. Examples of forms having these functional groups include chemical bonding and physical bonding states.
  • a chemical bond may be such as a covalent bond.
  • a chemically bonding substance may be a polymer or a monomer having a small molecular weight.
  • the physically bonded state includes states such as adsorption and adhesion in which intermolecular forces such as hydrogen bonding, van der Waals force, electrostatic attraction, and hydrophobic interaction are bonded without chemical bonding. be done.
  • Polymers for imparting negative zeta potential include polystyrenesulfonic acid, sodium polystyrenesulfonate, polyvinylsulfonic acid, sodium polyvinylsulfonate, poly(meth)acrylic acid, sodium poly(meth)acrylate, anionic polyacrylamide , poly(2-acrylamido-2-methyl group propanesulfonic acid), poly(2-acrylamido-2-methyl group sodium propanesulfonate), carboxymethylcellulose, anionized polyvinyl alcohol, polyvinyl phosphonic acid and the like.
  • the porous membrane may be attached or coated with a polymer having a negative zeta potential.
  • polymers having a negative zeta potential include polystyrenesulfonic acid, polystyrenesulfonic acid, sodium polystyrenesulfonate, polyvinylsulfonic acid, sodium polyvinylsulfonate, poly(meth)acrylic acid, and sodium poly(meth)acrylate.
  • anionic polyacrylamide poly(2-acrylamide-2-methyl group propanesulfonic acid), poly(2-acrylamido-2-methyl group sodium propanesulfonate), carboxymethylcellulose, anionized polyvinyl alcohol, polyvinyl phosphonic acid, etc. mentioned.
  • the polymer or the acid salt of the polymer may be a copolymer with another polymer.
  • examples of the replacement method include electron beams, gamma rays, A method of generating radicals by irradiation with plasma or the like and then adding a reactive monomer having a functional group that exhibits a desired function can be mentioned.
  • reactive monomers include sulfonic acid groups, sulfonic acid ester groups, carboxylic acid groups, carboxylic acid ester groups, phosphoric acid groups, phosphoric acid ester groups, acrylic acid containing hydroxyl groups, methacrylic acid, vinyl sulfonic acid derivatives, and the like. are mentioned.
  • More specific examples include acrylic acid, methacrylic acid, vinylsulfonic acid, styrenesulfonic acid and sodium salts thereof, 2-acrylamido-2-methylpropanesulfonic acid, 2-methacrylamido-2-methylpropanesulfonic acid , 2-acrylamido-2-methylpropanecarboxylic acid, 2-methacrylamido-2-methylpropanecarboxylic acid, and the like.
  • the fine particle removal apparatus of the present invention comprises a chargeable membrane module 1 followed by a size exclusion membrane module 2 in series.
  • the size exclusion membrane is a porous membrane that does not intentionally introduce the anionic or cationic functional group described above, or a porous membrane that is not intentionally modified to have chargeability, and has a predetermined particle size.
  • the object is to eliminate the fine particles described above. If the membrane material itself has an electric charge, it is included in the size exclusion membrane.
  • porous membrane that constitutes the size exclusion membrane the same one as in the chargeable membrane described above can be adopted.
  • the particle removal apparatus of the present invention is suitably used as a subsystem for producing ultrapure water from a primary pure water system in an ultrapure water production/supply system, particularly as a particle removal apparatus at the final stage of the subsystem.
  • the particulate removal apparatus of the present invention may be provided in a water supply line that delivers ultrapure water from a subsystem to a point of use.
  • the particle remover of the present invention can also be used as the final particle remover at the point of use.
  • the test apparatus shown in FIG. 3 prepares fine particle-containing test water by injecting fine particles from a fine particle tank 12 into a flow path 11 of a liquid to be treated by a pump P, and removes fine particles in the test water with a fine particle removal membrane module 13. It is a thing.
  • the microparticle monitors 14 and 15 provided at the inlet and outlet of the microparticle removal membrane module 13 measure the concentration of microparticles in the inlet water and the outlet water, and the microparticle removal rate is calculated from these results.
  • the test apparatus shown in FIG. 4 prepares fine particle-containing test water by injecting fine particles from a fine particle tank 12 into a flow path 11 of a liquid to be treated by a pump P, and using fine particle removal membrane modules 13A and 13B arranged in series. Fine particles in the test water are removed sequentially.
  • the microparticle concentration is measured by microparticle monitors 14 and 15 provided at the inlet of the microparticle removal membrane module 13A and the outlet of the microparticle removal membrane module 13B, respectively, and the microparticle removal rate is calculated from these results.
  • the water flow condition (water flow rate) of the liquid to be treated was set to 10 m/d.
  • the following microparticle monitors were used. Particle monitor: UDI20 (manufactured by PMS)
  • Positively charged membrane "Qyu speed D” manufactured by Asahi Kasei Medical DEA-diol (diethylamine- Diol) introduced film
  • Negatively charged film manufactured by Pall: "ABDIUPW3EH1”
  • Size exclusion membrane "APDG1HSVH3EH1K13C Ulti-pleated G2SPDR” manufactured by Nippon Pall Co., Ltd., exclusion diameter 10 nm
  • silica fine particles manufactured by Sigma-Aldrich, average particle size 22 nm
  • Alumina fine particles manufactured by Sigma-Aldrich, average particle size 22 nm
  • the particle removal performance of the positively charged membrane and the negatively charged membrane is equal to or higher than the particle removal performance of the size exclusion membrane. can efficiently remove fine particles in the liquid.
  • Example 1 Using the test apparatus shown in FIG. 4, a positively charged membrane module was arranged as the particle removal membrane module 13A, and a size exclusion membrane module was arranged as the particle removal membrane module 13B, and 1 ⁇ 10 7 particles/mL of silica particles were added to the ultrapure water. A fine particle removal test was performed on the injected test water, and changes over time in the fine particle removal rate were investigated. Table 2 shows the results.
  • Example 2 A fine particle removal test was conducted in the same manner as in Example 1, except that a negatively charged membrane module was used instead of the positively charged membrane module, and alumina fine particles were injected instead of the silica fine particles. Table 2 shows the results.
  • Example 1 Using the test apparatus shown in FIG. 3, a fine particle removal test was performed on the same test water as in Example 1, except that only the size exclusion membrane module was used. Table 2 shows the results.
  • Example 2 Using the test apparatus of FIG. 3, a fine particle removal test was conducted on the same test water as in Example 2, except that only the size exclusion membrane module was used. Table 2 shows the results.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un dispositif d'élimination de particules fines qui élimine de fines particules dans un liquide, le dispositif d'élimination de particules fines comprenant une membrane de filtration à propriété de charge électrique, et une membrane à exclusion de taille disposée à un dernier étage de la membrane de filtration à propriété de charge électrique. Le liquide traverse la membrane de filtration à propriété de charge électrique et la membrane à exclusion de taille, dans cet ordre. Une quantité de charge de particules fines cumulée de la membrane à exclusion de taille est réduite, les performances d'élimination de particules fines sont maintenues pendant une longue période et la durée de vie du dispositif d'élimination de particules fines peut être prolongée.
PCT/JP2022/004830 2021-02-18 2022-02-08 Dispositif d'élimination de particules fines et procédé d'élimination de particules fines WO2022176696A1 (fr)

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JP2021024382A JP2022126355A (ja) 2021-02-18 2021-02-18 微粒子除去装置及び微粒子除去方法
JP2021-024382 2021-02-18

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10216721A (ja) * 1997-02-07 1998-08-18 Kurita Water Ind Ltd 超純水製造装置
JP2016155052A (ja) * 2015-02-23 2016-09-01 栗田工業株式会社 水中微粒子の除去装置及び超純水製造・供給システム
JP2020062620A (ja) * 2018-10-19 2020-04-23 日東電工株式会社 水処理システム及び水処理方法
WO2020203142A1 (fr) * 2019-03-29 2020-10-08 栗田工業株式会社 Dispositif d'élimination de particules et procédé d'élimination de particules

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10216721A (ja) * 1997-02-07 1998-08-18 Kurita Water Ind Ltd 超純水製造装置
JP2016155052A (ja) * 2015-02-23 2016-09-01 栗田工業株式会社 水中微粒子の除去装置及び超純水製造・供給システム
JP2020062620A (ja) * 2018-10-19 2020-04-23 日東電工株式会社 水処理システム及び水処理方法
WO2020203142A1 (fr) * 2019-03-29 2020-10-08 栗田工業株式会社 Dispositif d'élimination de particules et procédé d'élimination de particules

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