WO2023176922A1 - Matériau électret, filtre et mélange maître - Google Patents

Matériau électret, filtre et mélange maître Download PDF

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Publication number
WO2023176922A1
WO2023176922A1 PCT/JP2023/010280 JP2023010280W WO2023176922A1 WO 2023176922 A1 WO2023176922 A1 WO 2023176922A1 JP 2023010280 W JP2023010280 W JP 2023010280W WO 2023176922 A1 WO2023176922 A1 WO 2023176922A1
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WIPO (PCT)
Prior art keywords
electret material
charge
thermoplastic resin
group
electret
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PCT/JP2023/010280
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English (en)
Japanese (ja)
Inventor
和樹 酒見
伊万理 中村
秀之 清谷
周三 田川
怡 王
鋼 徐
旻杰 徐
佳能 周
Original Assignee
ダイキン工業株式会社
ダイキン フルオロケミカルズ （チャイナ） カンパニー リミテッド
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Publication of WO2023176922A1 publication Critical patent/WO2023176922A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C3/00—Separating dispersed particles from gases or vapour, e.g. air, by electrostatic effect
    • B03C3/28—Plant or installations without electricity supply, e.g. using electrets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/20—Carboxylic acid amides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/16—Homopolymers or copolymers or vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18—Homopolymers or copolymers or tetrafluoroethene
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G7/00—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture
    • H01G7/02—Electrets, i.e. having a permanently-polarised dielectric

Definitions

  • the present disclosure relates to electret materials, filters, and masterbatches.
  • Patent Document 1 describes electret fibers containing additives such as polyvinylidene fluoride.
  • Patent Document 2 describes an electret fiber sheet containing a perfluoroalkyl compound such as an acrylic acid-based compound.
  • Patent Document 3 describes an electret in which a compound such as n-C 10 F 22 is attached to the surface of a carrier by vapor deposition or the like.
  • Patent Documents 4 and 5 describe electret fibers containing fatty acid metal salts and hindered amine compounds.
  • the present disclosure aims to provide an electret material with excellent collection performance, a filter using the same, and a masterbatch for producing the electret material.
  • the present disclosure provides an electret material comprising a thermoplastic resin and a charge reinforcing agent contained in the thermoplastic resin,
  • the above charge enhancer relates to an electret material containing at least one fluorine charge enhancer selected from the group consisting of polytetrafluoroethylene and vinylidene fluoride polymer and at least one hydrocarbon charge enhancer. .
  • the fluorine-based charge enhancer is preferably a low molecular weight polytetrafluoroethylene and a vinylidene fluoride polymer.
  • the vinylidene fluoride polymer is preferably at least one selected from the group consisting of polyvinylidene fluoride and vinylidene fluoride/tetrafluoroethylene copolymers.
  • the hydrocarbon charge enhancer is preferably at least one selected from the group consisting of metal soaps, hindered amine compounds, triazine compounds, clarifying agents, and low-molecular amide compounds.
  • the hydrocarbon charge enhancer is preferably a metal soap or a low molecular weight amide compound.
  • the metal soap is preferably a metal salt of group 2 of the periodic table of fatty acids.
  • the low molecular weight amide compound is preferably at least one selected from the group consisting of fatty acid amides and fatty acid bisamides.
  • the mass ratio (fluorine/hydrocarbon) of the fluorine-based charge enhancer and the hydrocarbon-based charge enhancer is 1/99 to 99/1.
  • thermoplastic resin is preferably a polyolefin resin.
  • the electret material preferably has a ratio (F/C) of F element content to C element content on the surface of the electret material measured by XPS (X-ray photoelectron spectroscopy) of 0.20% or less. .
  • the total amount of the charge reinforcing agent is preferably 0.01 to 5.0% by mass based on the thermoplastic resin.
  • the electret material is a fiber sheet.
  • the present disclosure also relates to a filter using the above electret material.
  • the filter is for a dust mask.
  • the present disclosure is a masterbatch for producing an electret material, comprising: comprising a thermoplastic resin and a charge reinforcing agent contained in the thermoplastic resin,
  • the charge enhancer includes at least one fluorine charge enhancer selected from the group consisting of polytetrafluoroethylene and vinylidene fluoride polymer, and at least one hydrocarbon charge enhancer,
  • the present invention also relates to a masterbatch in which the total amount of the charge reinforcing agent is more than 5.0% by mass and not more than 50% by mass based on the thermoplastic resin.
  • an electret material with excellent collection performance it is possible to provide an electret material with excellent collection performance, a filter using the same, and a masterbatch for producing the electret material.
  • the present disclosure is an electret material comprising a thermoplastic resin and a charge enhancer contained in the thermoplastic resin, wherein the charge enhancer is selected from the group consisting of polytetrafluoroethylene and vinylidene fluoride polymer.
  • the present invention relates to an electret material containing at least one selected fluorine charge enhancer and at least one hydrocarbon charge enhancer.
  • the electret material of the present disclosure has the ability to collect particles such as NaCl particles and PAO (polyalphaolefin) particles (for example, PF value).
  • thermoplastic resin examples include polyolefin resins such as polyethylene and polypropylene; polyester resins such as polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, and polylactic acid; polycarbonate resins; polystyrene resins; polyphenylene sulfide resins. ; Fluororesins; thermoplastic elastomers such as polystyrene elastomers, polyolefin elastomers, polyester elastomers, polyamide elastomers, and polyurethane elastomers; and copolymers or mixtures thereof.
  • polyolefin resins such as polyethylene and polypropylene
  • polyester resins such as polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, and polylactic acid
  • polycarbonate resins polystyrene resins
  • polyphenylene sulfide resins examples include Fluororesin
  • polyolefin resins are preferably used.
  • Polyolefin resins have high volume resistivity and low water absorption, so they have strong chargeability and charge retention when made into fibers. Therefore, high collection efficiency can be achieved.
  • polystyrene resin examples include homopolymers such as polyethylene, polypropylene, polybutene, and polymethylpentene. Further, a copolymer obtained by copolymerizing these homopolymers with different components, or a blend of two or more different polymers can also be used. Among these, polypropylene and polymethylpentene are preferably used from the viewpoint of charge retention. Further, from the viewpoint of being available at low cost, polypropylene is more preferably used.
  • the above-mentioned polypropylene preferably has a melt flow rate (MFR) of 600 g/10 min or more, and 800 g/10 min or more, since a melt-blown nonwoven fabric with good spinnability and good mechanical strength such as tensile strength can be obtained. It is more preferable that it is 1100g/10min or more, it is still more preferable that it is 2500g/10min or less, it is more preferable that it is 1800g/10min or less, and it is still more preferable that it is 1500g/10min or less. preferable.
  • MFR melt flow rate
  • the above MFR is measured at 230° C. and a load of 2160 g in accordance with ASTM D-1238.
  • the charge enhancer includes at least one fluorine-based charge enhancer selected from the group consisting of polytetrafluoroethylene (PTFE) and vinylidene fluoride (VdF) polymer.
  • PTFE polytetrafluoroethylene
  • VdF vinylidene fluoride
  • the fluorine-based charge enhancer has excellent heat resistance.
  • the PTFE is a low molecular weight PTFE.
  • the low molecular weight PTFE has a melt viscosity of 1.0 ⁇ 10 2 to 7.0 ⁇ 10 5 Pa ⁇ s at 380°C.
  • "low molecular weight” means that the melt viscosity is within the above range.
  • the above melt viscosity is preferably 1.5 ⁇ 10 3 Pa ⁇ s or more, and preferably 3.0 ⁇ 10 5 Pa ⁇ s or less, and 1.0 ⁇ 10 5 Pa ⁇ s or less. It is more preferable that there be.
  • the above melt viscosity was measured in accordance with ASTM D 1238, using a flow tester (manufactured by Shimadzu Corporation) and a 2 ⁇ -8L die, using a 2g sample that had been preheated at 380°C for 5 minutes under a load of 0.7MPa. This is the value measured while maintaining the above temperature.
  • the low molecular weight PTFE preferably has a melting point of 320 to 340°C, more preferably 324°C or higher, and more preferably 336°C or lower.
  • the above melting point was determined by using a differential scanning calorimeter (DSC), calibrating the temperature in advance using indium and lead as standard samples, and then placing about 3 mg of low molecular weight PTFE in an aluminum pan (crimp container) and 200 ml/ The temperature is raised at a rate of 10°C/min in a temperature range of 250 to 380°C under an air flow of 100°C/min, and the minimum point of the heat of fusion in the above range is defined as the melting point.
  • DSC differential scanning calorimeter
  • the low molecular weight PTFE preferably has an average particle diameter of 0.1 to 100 ⁇ m in terms of suppressing clogging of a melt blowing die.
  • the above average particle diameter is more preferably 50 ⁇ m or less, even more preferably 10 ⁇ m or less, particularly preferably 6 ⁇ m or less, and more preferably 0.5 ⁇ m or more, 1.0 ⁇ m or more. It is more preferable that
  • the above average particle diameter was measured using a laser diffraction particle size distribution analyzer (HELOS&RODOS) manufactured by JEOL Ltd., without using a cascade, and at a dispersion pressure of 1.0 bar. It is assumed to be equal to the particle size corresponding to %.
  • HELOS&RODOS laser diffraction particle size distribution analyzer
  • the low molecular weight PTFE may be a TFE homopolymer consisting only of tetrafluoroethylene (TFE) units, or a modified PTFE containing TFE units and modified monomer units based on a modified monomer copolymerizable with TFE. Good too.
  • the content of the modified monomer units is preferably 0.001 to 1% by mass, more preferably 0.01% by mass or more, and 0.5% by mass of the total monomer units. The following is more preferable, and 0.1% by mass or less is even more preferable.
  • the modified monomer unit refers to a portion of the molecular structure of modified PTFE that is derived from the modified monomer, and the term "all monomer units" refers to all monomer units in the molecular structure of modified PTFE. It means a part that comes from the body.
  • the content of the modified monomer unit can be determined by a known method such as Fourier transform infrared spectroscopy (FT-IR).
  • the modified monomer is not particularly limited as long as it can be copolymerized with TFE; for example, perfluoroolefins such as hexafluoropropylene [HFP]; chlorofluoroolefins such as chlorotrifluoroethylene [CTFE]; Examples include hydrogen-containing fluoroolefins such as trifluoroethylene and vinylidene fluoride [VDF]; perfluorovinyl ether; perfluoroalkyl ethylene; and ethylene. Furthermore, the number of modified monomers used may be one or more than one.
  • perfluoro organic group means an organic group in which all hydrogen atoms bonded to carbon atoms are replaced with fluorine atoms.
  • the perfluoro organic group may have an ether oxygen.
  • perfluorovinyl ether examples include perfluoro(alkyl vinyl ether) [PAVE] in which Rf in the general formula (1) represents a perfluoroalkyl group having 1 to 10 carbon atoms.
  • the perfluoroalkyl group preferably has 1 to 5 carbon atoms.
  • perfluoroalkyl group in PAVE examples include perfluoromethyl group, perfluoroethyl group, perfluoropropyl group, perfluorobutyl group, perfluoropentyl group, perfluorohexyl group, etc.
  • Purple oro(propyl vinyl ether) [PPVE] in which the group is a perfluoropropyl group is preferred.
  • perfluorovinyl ether further includes those in the above general formula (1) in which Rf is a perfluoro(alkoxyalkyl) group having 4 to 9 carbon atoms, and Rf is the following formula:
  • Rf is a group represented by the following formula:
  • n an integer of 1 to 4.
  • Perfluoroalkylethylene is not particularly limited, and examples thereof include (perfluorobutyl)ethylene (PFBE), (perfluorohexyl)ethylene, and (perfluorooctyl)ethylene.
  • the modified monomer in the modified PTFE is preferably at least one selected from the group consisting of HFP, CTFE, VDF, PPVE, PFBE, and ethylene. More preferably, it is at least one selected from the group consisting of PPVE, HFP, and CTFE.
  • the VdF polymer is preferably at least one selected from the group consisting of polyvinylidene fluoride (PVdF) and VdF/TFE copolymers.
  • the above-mentioned PVdF may be a homopolymer consisting only of polymerized units based on VdF, or may be composed of polymerized units based on VdF and polymerized units based on a monomer ( ⁇ ) copolymerizable with VdF. Good too.
  • the monomer ( ⁇ ) may have an ethylenically unsaturated double bond.
  • specific examples of the above monomer ( ⁇ ) include fluorine-containing monomers [e.g., vinyl fluoride (VF), trifluoroethylene (TrFE), hexafluoropropene (HFP), 1-chloro-1-fluoroethylene (1, 1-CFE), 1-chloro-2-fluoroethylene (1,2-CFE), 1-chloro-2,2-difluoroethylene (CDFE), chlorotrifluoroethylene (CTFE), trifluorovinyl monomer, 1, 1,2-trifluorobutene-4-bromo-1-butene, 1,1,2-trifluorobutene-4-silane-1-butene, perfluoropropyl vinyl ether (PPVE), perfluoroacrylate, 2,2,2 -trifluoroethyl acrylate, 2-(perfluorohexyl)ethyl acrylate)], fluorine-free
  • ⁇ -olefins e.g. ethylene, propylene); , maleic anhydride
  • vinyl ether e.g. ethyl vinyl ether
  • allyl ether e.g. allyl glycidyl ether
  • vinyl ester e.g. vinyl acetate
  • acrylic acid or its ester methacrylic acid or its ester
  • methacrylic acid or its ester it includes one type or a combination of two or more types.
  • the PVdF may contain repeating units derived from the monomer ( ⁇ ) in an amount of, for example, 10 mol% or less, preferably 5 mol% or less, of the repeating units derived from all monomers. Moreover, it can be contained preferably within the range of 0.01 mol% or more.
  • the PVdF preferably has a weight average molecular weight (in terms of polystyrene) of 50,000 to 2,000,000.
  • the weight average molecular weight is more preferably 80,000 or more, and more preferably 1,900,000 or less.
  • the weight average molecular weight can be measured by gel permeation chromatography (GPC) using N,N-dimethylformamide as a solvent at 50°C.
  • the PVdF preferably has a number average molecular weight (in terms of polystyrene) of 150,000 to 1,400,000.
  • the number average molecular weight is more preferably 200,000 or more, and more preferably 1,300,000 or less.
  • the above number average molecular weight can be measured by gel permeation chromatography (GPC) using N,N-dimethylformamide as a solvent at 50°C.
  • the molar ratio of the repeating unit derived from VdF (-CH 2 -CF 2 -) and the repeating unit derived from TFE (-CF 2 -CF 2 -) ((-CH 2 -CF 2 -)/(-CF 2 -CF 2 -)) can be, for example, in the range of 50/50 to 99/1, although it is not limited thereto.
  • the molar ratio is preferably 55/45 or more, more preferably 60/40 or more, even more preferably 70/30 or more, and preferably 97/3 or less, 95/40 or more. It is more preferable that it is /5 or less, and even more preferable that it is 90/10 or less.
  • the VdF/TFE copolymer may be a copolymer consisting only of VdF and TFE, or may be a copolymer consisting essentially of VdF and TFE.
  • the VdF/TFE copolymer may also contain a repeating unit derived from a monomer ( ⁇ ) copolymerizable with VdF and TFE.
  • Examples of the monomer ( ⁇ ) include the same monomers as the monomer ( ⁇ ) described for the PVdF.
  • the VdF/TFE copolymer contains repeating units derived from the monomer ( ⁇ ) in an amount of, for example, 10 mol% or less, preferably 5 mol% or less of the repeating units derived from all monomers. be able to. Moreover, it can be contained preferably within the range of 0.01 mol% or more.
  • the VdF/TFE copolymer preferably has a weight average molecular weight (in terms of polystyrene) of 50,000 to 2,000,000.
  • the weight average molecular weight is more preferably 80,000 or more, still more preferably 100,000 or more, and more preferably 1,950,000 or less, even more preferably 1,500,000 or less.
  • the weight average molecular weight can be measured by gel permeation chromatography (GPC) using N,N-dimethylformamide as a solvent at 50°C.
  • the VdF/TFE copolymer preferably has a number average molecular weight (in terms of polystyrene) of 10,000 to 1,400,000.
  • the number average molecular weight is more preferably 16,000 or more, still more preferably 20,000 or more, and more preferably 1,300,000 or less, even more preferably 1,200,000 or less.
  • the above number average molecular weight can be measured by gel permeation chromatography (GPC) using N,N-dimethylformamide as a solvent at 50°C.
  • the above VdF polymer is preferably the above VdF/TFE copolymer.
  • the VdF polymer it is also preferable to use a mixture of the PVdF and the VdF/TFE copolymer.
  • the mass ratio [(VdF/TFE copolymer)/PVdF] is preferably 5/95 or more, more preferably 10/90 or more, and even more preferably 20/80 or more. Also, it is preferably 90/10 or less, more preferably 85/15 or less.
  • the fluorine-based charge enhancer is preferably the PTFE and the VdF polymer, more preferably the low molecular weight PTFE and the VdF polymer, and the low molecular weight PTFE, the PVdF, and the VdF/TFE polymer. More preferably, it is a polymer.
  • the collection performance is further improved when the mass ratio of the PTFE and the VdF polymer (PTFE/VdF polymer) is 1/99.
  • the ratio is preferably 70/30.
  • the mass ratio is more preferably 5/95 or more, even more preferably 10/90 or more, and particularly preferably 15/85 or more.
  • the mass ratio is more preferably 60/40 or less, even more preferably 50/50 or less, even more preferably 40/60 or less, and especially 30/70 or less. preferable.
  • the charge enhancer includes at least one hydrocarbon charge enhancer.
  • the hydrocarbon charge enhancer may be a non-fluorine charge enhancer.
  • hydrocarbon charge enhancer examples include metal soaps, hindered amine compounds, triazine compounds, clarifying agents, and low-molecular amide compounds.
  • the metal soap may be a fatty acid metal salt. It is believed that the fatty acid metal salt effectively traps charges that reach the thermoplastic resin composition from, for example, an ion stream emitted from a corona electrode when the composition is converted into an electret.
  • the number of carbon atoms in the fatty acid in the fatty acid metal salt is preferably 10 to 50, more preferably 12 or more, even more preferably 16 or more, and more preferably 30 or less, and 22 It is more preferable that it is the following.
  • the fatty acids include linear saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, and behenic acid; linear unsaturated fatty acids such as oleic acid and erucic acid. Among these, linear saturated fatty acids are preferred, and stearic acid is more preferred.
  • Examples of the metal in the fatty acid metal salt include metals of group 2 of the periodic table such as magnesium and calcium; metals of group 12 of the periodic table such as zinc; and metals of group 13 of the periodic table such as aluminum.
  • Group 2 metals of the periodic table are preferred, magnesium or calcium is more preferred, and magnesium is even more preferred.
  • the melting point of the fatty acid metal salt is preferably 80°C or higher, more preferably 100°C or higher, and may be 300°C or lower. Further, the thermal decomposition temperature is preferably 200°C or higher, and may be 300°C or lower.
  • the number of fatty acid chains bonded to the metal may be 1 to 3, but preferably 2.
  • the metal soap is preferably a metal salt of group 2 of the periodic table of fatty acids, more preferably a metal salt of group 2 of the periodic table of linear saturated fatty acids, and magnesium salt or calcium salt of linear saturated fatty acids.
  • a salt is more preferred, magnesium stearate or calcium stearate is even more preferred, and magnesium stearate is particularly preferred. It is also preferable that the metal soap is a fatty acid magnesium salt.
  • hindered amine compounds examples include poly[(6-(1,1,3,3-tetramethylbutyl)imino-1,3,5-triazine-2,4-diyl)((2,2,6 ,6-tetramethyl-4-piperidyl)imino)hexamethylene ((2,2,6,6-tetramethyl-4-piperidyl)imino)] (for example, "Kimasorb” (registered) manufactured by BASF Japan Ltd.
  • the above-mentioned hindered amine compound preferably has a triazine structure, and poly[(6-(1,1,3,3-tetramethylbutyl)imino-1,3,5-triazine-2,4-diyl)( (2,2,6,6-tetramethyl-4-piperidyl)imino)hexamethylene ((2,2,6,6-tetramethyl-4-piperidyl)imino)] (for example, manufactured by BASF Japan Ltd. , "KimaSorb" (registered trademark) 944LD) is more preferred.
  • triazine compounds examples include poly[(6-(1,1,3,3-tetramethylbutyl)imino-1,3,5-triazine-2,4-diyl)((2,2,6 ,6-tetramethyl-4-piperidyl)imino)hexamethylene ((2,2,6,6-tetramethyl-4-piperidyl)imino)] (for example, “Kimasorb” (registered trademark) manufactured by BASF Japan Ltd.
  • the above triazine compound may not have a hindered amine structure.
  • the clarifying agent may be a crystal nucleating agent.
  • the crystal nucleating agents include sorbitol-based nucleating agents, nonitol-based nucleating agents, xylitol-based nucleating agents, phosphoric acid-based nucleating agents, triaminobenzene derivative nucleating agents, and carboxylic acid metal salt nucleating agents.
  • sorbitol-based nucleating agent examples include dibenzylidene sorbitol (DBS), monomethyldibenzylidene sorbitol (for example, 1,3:2,4-bis(p-methylbenzylidene) sorbitol (p-MDBS)), dimethyldibenzylidene sorbitol (p-MDBS), and dibenzylidene sorbitol (DBS). Sorbitol (e.g.
  • 1,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol (3,4-DMDBS)), 1,3:2,4-bis-O-(4-methylbenzylidene)- Examples include D-sorbitol, and commercially available products include "Millad” (registered trademark) 3988 (manufactured by Milliken Japan Co., Ltd.) and "Gelol” (registered trademark) E-200 (manufactured by Shin Nippon Chemical Co., Ltd.). ) etc.
  • nonitol-based nucleating agent examples include 1,2,3-trideoxy-4,6:5,7-bis-[(4-propylphenyl)methylene]-nonitol, and commercially available products include " Millad” (registered trademark) NX8000 (manufactured by Milliken Japan Co., Ltd.).
  • Examples of the xylitol-based nucleating agent include bis-1,3:2,4-(5',6',7',8'-tetrahydro-2-naphthaldehydebenzylidene)1-allylxylitol.
  • Examples of the phosphoric acid-based nucleating agent include aluminum-bis(4,4',6,6'-tetra-tert-butyl-2,2'-methylene diphenyl-phosphate)-hydroxide, which is commercially available.
  • Examples of the products include "ADEKA STAB” (registered trademark) NA-11 (manufactured by ADEKA Corporation) and "ADEKA STAB” (registered trademark) NA-21 (manufactured by ADEKA Corporation).
  • triaminobenzene derivative nucleating agent examples include 1,3,5-tris(2,2-dimethylpropanamide)benzene, and commercially available products include "Irgaclear” (registered trademark) XT386 (BASF Japan). Co., Ltd.), etc.
  • carboxylic acid metal salt nucleating agent examples include sodium benzoate and 1,2-cyclohexanedicarboxylic acid calcium salt.
  • the above-mentioned clarifying agent is at least selected from the group consisting of sorbitol-based nucleating agent, nonitol-based nucleating agent, xylitol-based nucleating agent, phosphoric acid-based nucleating agent, triaminobenzene derivative nucleating agent, and carboxylic acid metal salt nucleating agent.
  • One type is preferable, at least one type selected from the group consisting of sorbitol-based nucleating agents and phosphoric acid-based nucleating agents is more preferable, sorbitol-based nucleating agents are even more preferable, and 1,3:2,4-bis-O-( Particularly preferred is 4-methylbenzylidene)-D-sorbitol.
  • the low molecular weight amide compound preferably has a molecular weight of 100 to 1000, more preferably 200 or more, even more preferably 500 or more, and more preferably 800 or less, and 700 or less. It is even more preferable that there be.
  • the above molecular weight can be determined from the structure (chemical formula) of the molecule.
  • Examples of the low molecular weight amide compound include fatty acid amide, fatty acid bisamide, and the like.
  • the number of carbon atoms in the fatty acid in the fatty acid amide and the fatty acid bisamide is preferably 8 to 60, more preferably 10 or more, even more preferably 20 or more, particularly preferably 30 or more, Further, it is more preferably 50 or less, and even more preferably 40 or less.
  • the above fatty acids include linear saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, and behenic acid; branched saturated fatty acids such as isostearic acid; linear unsaturated fatty acids such as oleic acid and erucic acid. etc. Among these, linear saturated fatty acids are preferred, and stearic acid is more preferred.
  • the above fatty acid amides include lauric acid amide, palmitic acid amide, stearic acid amide, behenic acid amide, hydroxystearic acid amide, N-lauryl lauric acid amide, N-palmityl palmitic acid amide, N-stearyl stearic acid amide, -stearyl-hydroxystearamide, oleic acid amide and the like.
  • stearamide is preferred.
  • the fatty acid bisamides mentioned above include methylene bisstearamide, methylene bislauric acid amide, methylene bishydroxystearic acid amide, ethylene biscaprylic acid amide, ethylene biscapric acid amide, ethylene bislauric acid amide, ethylene bis stearic acid amide, and ethylene biscaprylic acid amide.
  • Bisisostearamide ethylenebishydroxystearamide, ethylenebisbehenamide, hexamethylenebisstearamide, hexamethylenebisbehenamide, hexamethylenebishydroxystearamide, butylenebishydroxystearamide, N,N '-Distearyl adipamide, N,N'-distearyl sebacic acid amide, methylene bis oleic acid amide, ethylene bis oleic acid amide, ethylene bis erucic acid amide, hexamethylene bis oleic acid amide, N,N'-dio Examples include leyladipic acid amide, N,N'-dioleylsebacic acid amide, m-xylylene bisstearic acid amide, N,N'-distearylisophthalic acid amide and the like. Among these, alkylene bis fatty acid amides such as ethylene bis stearic acid amide are preferred.
  • the low-molecular amide compound is preferably at least one selected from the group consisting of fatty acid amide and fatty acid bisamide, more preferably fatty acid bisamide, and even more preferably alkylene bis fatty acid amide, Particularly preferred is ethylene bisstearamide.
  • the hydrocarbon charge enhancer is preferably at least one selected from the group consisting of metal soaps, hindered amine compounds, triazine compounds, clarifying agents, and low-molecular amide compounds; , more preferably at least one selected from the group consisting of a clarifying agent and a low-molecular amide compound, and still more preferably at least one selected from the group consisting of a metal soap and a low-molecular amide compound, Particularly preferred are metal soaps and low molecular weight amide compounds. Moreover, it is also preferable that it is at least one selected from the group consisting of metal soaps, hindered amine compounds, clarifying agents, and low-molecular amide compounds.
  • amide is preferably 30/70 to 99/1.
  • the mass ratio is more preferably 40/60 or more, still more preferably 50/50 or more, even more preferably 60/40 or more, and particularly preferably 70/30 or more.
  • the mass ratio is also more preferably 95/5 or less, still more preferably 90/10 or less, and particularly preferably 85/15 or less.
  • the mass ratio of the metal soap and the clarifying agent is also preferably within the above range.
  • the mass ratio (fluorine/hydrocarbon) of the fluorine-based charge enhancer and the hydrocarbon-based charge enhancer is 1/99 to 99, in that the collection performance is further improved. /1 is preferable.
  • the mass ratio is more preferably 10/90 or more, still more preferably 20/80 or more, even more preferably 30/70 or more, and particularly preferably 40/60 or more.
  • the mass ratio is also more preferably 90/10 or less, even more preferably 80/20 or less, even more preferably 70/30 or less, and especially 60/40 or less. preferable.
  • the total amount of the charge enhancer is the same as that of the thermoplastic resin. It is preferably 0.01 to 5.0% by mass.
  • the above total amount is more preferably 0.10% by mass or more, even more preferably 0.20% by mass or more, even more preferably 0.30% by mass or more, and 0.40% by mass. It is particularly preferable that it is above.
  • the above-mentioned total amount is also more preferably 1.0% by mass or less, even more preferably 0.8% by mass or less, even more preferably 0.7% by mass or less, and even more preferably 0.6% by mass or less. It is particularly preferable that it is less than % by mass.
  • the charge reinforcing agent is contained in the thermoplastic resin.
  • the electret material having such a structure can be manufactured by mixing the thermoplastic resin and the charge reinforcing agent, so there is no need to attach the charge reinforcing agent by post-processing such as vapor deposition or impregnation, and the manufacturing process is simple. The process can be simplified. Further, it is also possible to prevent deterioration in collection performance due to peeling of the charge enhancer from the surface.
  • the charge reinforcing agent may be dispersed in the thermoplastic resin.
  • the electret material of the present disclosure has a ratio (F/C) of F element content to C element content on the surface of the electret material measured by XPS (X-ray photoelectron spectroscopy) of 0.20% or less. is preferable, more preferably 0.10% or less, even more preferably 0.03% or less, and preferably 0.0005% or more, more preferably 0.0006% or more.
  • the content is preferably 0.0008% or more, and more preferably 0.0008% or more.
  • the fact that the ratio (F/C) is within the above range means that the charge reinforcing agent is contained in the thermoplastic resin (the charge reinforcing agent is not attached to the surface by post-processing). shows.
  • the electret material of the present disclosure may contain other components as long as the effects are not impaired.
  • the other components include matting agents, pigments, antifungal agents, antibacterial agents, flame retardants, heat stabilizers, weathering agents, polymerization inhibitors, and the like.
  • the electret material of the present disclosure can be obtained by mixing the thermoplastic resin, the charge reinforcing agent, and other components as necessary to prepare a resin composition, and then subjecting the resin composition to an electret treatment. can be manufactured.
  • the thermoplastic resin and the charge reinforcing agent may be mixed by mixing a masterbatch containing the thermoplastic resin and the charge reinforcing agent with the thermoplastic resin. The masterbatch will be described later.
  • the resin composition may be processed into a desired shape before the electret treatment and/or after the electret treatment.
  • melt kneading is preferred.
  • the masterbatch it is preferable to melt and knead the masterbatch and the thermoplastic resin.
  • the above-mentioned melt-kneading may be performed by a known method, for example, using a single-screw or twin-screw extruder, an open roll, a kneader, a Banbury mixer, or the like.
  • the melt-kneading temperature is preferably higher than the melting point of the thermoplastic resin, more preferably 5° C. or more higher than the melting point of the thermoplastic resin.
  • the method for the above-mentioned electret treatment can be arbitrarily selected from known charging methods such as corona charging method, liquid contact charging method, frictional charging method, electric field charging method, hot electric field charging method, and electron beam irradiation method.
  • Specific electretization methods include those using electrical effects such as polarization by high voltage, collisions of charged ions, and injection of charged particles; methods using interactions with solids such as friction and collisions; methods using contact with liquids and collisions. Conventionally known methods such as those described above can be preferably used.
  • the shape of the electret material of the present disclosure is not particularly limited, and may be fibrous, sheet, film, particle, rod, pipe, or the like.
  • the electret material of the present disclosure is preferably fibrous, and more preferably a fibrous sheet.
  • the average fiber diameter of the fibers constituting the fiber sheet is preferably 0.001 ⁇ m or more, more preferably 0.1 ⁇ m or more, even more preferably 0.2 ⁇ m or more, and even more preferably 0.5 ⁇ m or more. It is particularly preferable that there be. Moreover, it is preferably 100 ⁇ m or less, more preferably 20 ⁇ m or less, even more preferably 10 ⁇ m or less, and particularly preferably 5 ⁇ m or less.
  • the average fiber diameter of the fibers is thicker than 100 ⁇ m, it is difficult to obtain a practical collection efficiency, and the efficiency decreases significantly when the charge decays.
  • the average fiber diameter of the fibers is smaller than 0.001 ⁇ m, it is difficult to produce a charged electret.
  • the above average fiber diameter is measured as follows. Using a scanning electron microscope (product name: SU8020, manufactured by HITACHI), observe an arbitrary 25 ⁇ m x 20 ⁇ m area in an electron micrograph taken at a magnification of 5000 times, draw straight lines perpendicular to the vertical and horizontal directions, and The diameters of all fibers that cross in a straight line are measured with a ruler, and the fiber diameters ( ⁇ m) are determined by converting to scale. Next, the obtained cumulative frequency distribution of fiber diameters is log-normally plotted on log probability paper with the fiber diameter on the horizontal axis and the cumulative frequency on the vertical axis, and the value at which the cumulative frequency is 50% is determined by the average fiber diameter ( median diameter).
  • the above-mentioned fiber sheet may be a uniform product made of a single manufacturing method and material, or may be a mixture of two or more materials having different manufacturing methods, materials, and fiber diameters.
  • the basis weight of the fiber sheet is preferably 3 g/ m2 or more, more preferably 5 g/m2 or more , and 10 g/m2 or more, from the viewpoint of obtaining an electret fiber sheet with excellent air permeability and collection properties. It is more preferable that the area is at least /m 2 . Further, it is preferably 100 g/m 2 or less, more preferably 70 g/m 2 or less, and even more preferably 50 g/m 2 or less.
  • the thickness of the fiber sheet is preferably 0.01 mm or more, more preferably 0.05 mm or more, and 0.1 mm or more, from the viewpoint of obtaining an electret fiber sheet with excellent air permeability and collection properties. It is more preferable that it is above. Moreover, it is preferably 1.0 mm or less, more preferably 0.7 mm or less, and even more preferably 0.5 mm or less.
  • the fiber sheet is a nonwoven fabric.
  • Methods for obtaining the above-mentioned nonwoven fabrics include methods of forming monocomponent fibers, composite fibers such as core-sheath fibers and side-by-side fibers, and short fibers such as split fibers into sheets by carding, air-laid, wet paper-making methods, etc., and methods of forming continuous fibers into sheets by spunbonding. It is possible to use conventionally known methods, such as forming a sheet by a melt blowing method, an electrospinning method, a force spinning method, or the like.
  • melt blowing method electrospinning method, and force spinning method, which can easily obtain dense and fine fineness from the viewpoint of effectively utilizing a mechanical collection mechanism, are preferable, and the melt blowing method is preferable from the viewpoint of not requiring treatment of residual solvent.
  • melt electrospinning method, and melt force spinning method are more preferred, and melt blowing method is even more preferred.
  • the fiber sheet is preferably a melt-blown nonwoven fabric.
  • the electret material of the present disclosure preferably the fiber sheet described above, has excellent collection performance and can be suitably used for filters.
  • the present disclosure also relates to filters using the electret materials of the present disclosure.
  • the filter of the present disclosure can be used for dust collection, protection, ventilation, etc. in dust masks, various air conditioning elements, air purifiers, cabin filters, various devices, and the like. Among these, it can be suitably used for dust masks.
  • the present disclosure is a masterbatch for producing an electret material, which includes a thermoplastic resin and a charge enhancer contained in the thermoplastic resin, and the charge enhancer includes polytetrafluoroethylene and fluorine.
  • the thermoplastic resin contains at least one fluorine-based charge enhancer selected from the group consisting of vinylidene chloride polymers and at least one hydrocarbon-based charge enhancer, and the total amount of the charge enhancer is On the other hand, it also relates to a masterbatch whose content is more than 5.0% by mass and not more than 50% by mass.
  • thermoplastic resin in the masterbatch of the present disclosure the same thermoplastic resin as can be used in the electret material of the present disclosure can be used.
  • the charge enhancer in the masterbatch of the present disclosure the same charge enhancer as can be used in the electret material of the present disclosure can be used. Further, the preferred combination of charge enhancers and the preferred ratio when combining them can be the same as those of the electret material of the present disclosure.
  • the total amount of the charge reinforcing agent is more than 5.0% by mass and not more than 50% by mass based on the thermoplastic resin.
  • the above-mentioned total amount is more preferably 10% by mass or more, still more preferably 15% by mass or more, and more preferably 40% by mass or less, even more preferably 30% by mass or less. .
  • the masterbatch of the present disclosure may contain other components as necessary.
  • Other components include those similar to other components that can be included in the electret material of the present disclosure.
  • the masterbatch of the present disclosure may be non-electretized, but may be electretized.
  • the masterbatch of the present disclosure can be produced by mixing the thermoplastic resin, the charging enhancer, and other components as necessary.
  • the above-mentioned mixing can be performed using a single-screw or twin-screw extruder, an open roll, a kneader, a Banbury mixer, or the like.
  • the masterbatch of the present disclosure may be in the form of powder, granules, pellets, or the like, but it can be melt-kneaded in that the charge reinforcing agent is maintained in a finely dispersed state in the thermoplastic resin. It is preferable to use pellets obtained by The melt-kneading temperature is preferably higher than the melting point of the thermoplastic resin, more preferably 5° C. or more higher than the melting point of the thermoplastic resin.
  • the masterbatch of the present disclosure is used to produce electret materials.
  • the masterbatch may be used to produce an electret material containing a thermoplastic resin and a charge reinforcing agent contained in the thermoplastic resin, and may be used to produce the electret material of the present disclosure described above. It is preferably used for
  • PTFE Low molecular weight PTFE (average particle size: 4 ⁇ m, melt viscosity: 5.0 ⁇ 10 4 Pa ⁇ s, melting point: 329° C.).
  • Metal soap 1 Magnesium stearate (StMg)
  • Metal soap 2 Calcium stearate
  • Low molecular weight amide compound 1 Ethylene bis stearylamide (EBS)
  • Low molecular weight amide compound 2 Stearic acid amide hindered amine compound: poly[(6-(1,1,3,3-tetramethylbutyl)imino-1,3,5-triazine-2,4-diyl)((2 ,2,6,6-tetramethyl-4-piperidyl)imino)hexamethylene((2,2,6,6-tetramethyl-4-piperidyl)imino)] Clarifying agent: 1,3:2,4-bis-O-(4-methylbenzylidene)-D-sorbitol
  • Examples 1 to 18 [Preparation of masterbatch] PP and the charge enhancer listed in Table 1 or 2 are mixed so that the total amount of the charge enhancer is 10% by mass based on the PP, and a twin-screw extruder (manufactured by Toyo Seiki Seisakusho Co., Ltd., Laboplasto Mill) is used. 30C150) and melted and kneaded to obtain masterbatch pellets.
  • a twin-screw extruder manufactured by Toyo Seiki Seisakusho Co., Ltd., Laboplasto Mill
  • the obtained melt-blown nonwoven fabric sheet was subjected to corona charging treatment to obtain an electret fiber sheet.
  • the obtained electret fiber sheet was evaluated by the method described above. The results are shown in Tables 1 and 2.
  • Comparative example 1 An electret fiber sheet was produced and evaluated in the same manner as in the example using only PP. The results are shown in Table 1.
  • Comparative examples 2 to 5 An electret fiber sheet was produced and evaluated in the same manner as in the example except that the charge reinforcing agent listed in Table 1 was used. The results are shown in Table 1.

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Abstract

Le but de la présente invention est de fournir un matériau électret ayant d'excellentes performances de collecte, un filtre comprenant le matériau électret, et un mélange maître pour produire le matériau électret. Ce matériau électret comprend une résine thermoplastique et des amplificateurs de charge contenus dans la résine thermoplastique, les amplificateurs de charge comprenant au moins un amplificateur de charge fluorochimique choisi dans le groupe constitué par les polymères de polytétrafluoroéthylène et de fluorure de vinylidène et au moins un amplificateur de charge à base d'hydrocarbure.
PCT/JP2023/010280 2022-03-18 2023-03-16 Matériau électret, filtre et mélange maître WO2023176922A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0549824A (ja) * 1991-08-13 1993-03-02 Koken Kk エア・フイルタおよびその製造方法
JPH11510862A (ja) * 1995-08-14 1999-09-21 ミネソタ マイニング アンド マニュファクチャリング カンパニー エレクトレット特性が高められた繊維ウェブ
JP2003520659A (ja) * 1997-10-01 2003-07-08 ミネソタ マイニング アンド マニュファクチャリング カンパニー 耐油ミストエレクトレット物品及びフィルター
JP2018071018A (ja) * 2016-10-28 2018-05-10 東レ株式会社 エレクトレット繊維シート
CN111235666A (zh) * 2020-03-19 2020-06-05 道恩高材(北京)科技有限公司 一种长效静电保持的熔喷聚丙烯驻极体及其制备方法和应用
CN111321516A (zh) * 2020-04-02 2020-06-23 青岛科凯达橡塑有限公司 一种长效驻极pp非纺织布及其制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0549824A (ja) * 1991-08-13 1993-03-02 Koken Kk エア・フイルタおよびその製造方法
JPH11510862A (ja) * 1995-08-14 1999-09-21 ミネソタ マイニング アンド マニュファクチャリング カンパニー エレクトレット特性が高められた繊維ウェブ
JP2003520659A (ja) * 1997-10-01 2003-07-08 ミネソタ マイニング アンド マニュファクチャリング カンパニー 耐油ミストエレクトレット物品及びフィルター
JP2018071018A (ja) * 2016-10-28 2018-05-10 東レ株式会社 エレクトレット繊維シート
CN111235666A (zh) * 2020-03-19 2020-06-05 道恩高材(北京)科技有限公司 一种长效静电保持的熔喷聚丙烯驻极体及其制备方法和应用
CN111321516A (zh) * 2020-04-02 2020-06-23 青岛科凯达橡塑有限公司 一种长效驻极pp非纺织布及其制备方法

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