CN113214425B - Modified polytetrafluoroethylene and preparation method and application thereof - Google Patents
Modified polytetrafluoroethylene and preparation method and application thereof Download PDFInfo
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- CN113214425B CN113214425B CN202110521598.9A CN202110521598A CN113214425B CN 113214425 B CN113214425 B CN 113214425B CN 202110521598 A CN202110521598 A CN 202110521598A CN 113214425 B CN113214425 B CN 113214425B
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- deionized water
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- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 149
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 139
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 139
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 59
- 239000008367 deionised water Substances 0.000 claims abstract description 56
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000006185 dispersion Substances 0.000 claims abstract description 49
- 239000007787 solid Substances 0.000 claims abstract description 45
- 239000007789 gas Substances 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000000314 lubricant Substances 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 6
- 230000003797 telogen phase Effects 0.000 claims abstract description 6
- 239000003607 modifier Substances 0.000 claims description 12
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 11
- KDRUZFPAMQCIGS-UHFFFAOYSA-N 1-ethyl-4-(1,2,2-trifluoroethenoxy)benzene Chemical compound CCC1=CC=C(OC(F)=C(F)F)C=C1 KDRUZFPAMQCIGS-UHFFFAOYSA-N 0.000 claims description 9
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000007639 printing Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000004519 grease Substances 0.000 claims description 2
- 230000001050 lubricating effect Effects 0.000 claims description 2
- HVUFSELLSNXJCA-UHFFFAOYSA-N 1,2,2-trifluoroethenoxybenzene Chemical compound FC(F)=C(F)OC1=CC=CC=C1 HVUFSELLSNXJCA-UHFFFAOYSA-N 0.000 claims 1
- ZESXUEKAXSBANL-UHFFFAOYSA-N trifluoromethyl prop-2-enoate Chemical compound FC(F)(F)OC(=O)C=C ZESXUEKAXSBANL-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 36
- 230000000052 comparative effect Effects 0.000 description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000012535 impurity Substances 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- 229910001220 stainless steel Inorganic materials 0.000 description 12
- 239000010935 stainless steel Substances 0.000 description 12
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 9
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 9
- 239000007983 Tris buffer Substances 0.000 description 8
- LOYYAPWQNHOYQA-UHFFFAOYSA-N methyl 2,3,3-trifluoroprop-2-enoate Chemical compound COC(=O)C(F)=C(F)F LOYYAPWQNHOYQA-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- NZXVPCQHQVWOFD-UHFFFAOYSA-N 1,1,2,2-tetrafluoro-1,2-diiodoethane Chemical compound FC(F)(I)C(F)(F)I NZXVPCQHQVWOFD-UHFFFAOYSA-N 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 7
- 238000005406 washing Methods 0.000 description 6
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 125000001153 fluoro group Chemical group F* 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- AJCMVKBTUWFCKH-UHFFFAOYSA-N 2,2,3-trifluorooxirane Chemical compound FC1OC1(F)F AJCMVKBTUWFCKH-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- ADKBGLXGTKOWIU-UHFFFAOYSA-N butanediperoxoic acid Chemical compound OOC(=O)CCC(=O)OO ADKBGLXGTKOWIU-UHFFFAOYSA-N 0.000 description 3
- 229920006335 epoxy glue Polymers 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- TYCFGHUTYSLISP-UHFFFAOYSA-M 2-fluoroprop-2-enoate Chemical compound [O-]C(=O)C(F)=C TYCFGHUTYSLISP-UHFFFAOYSA-M 0.000 description 1
- MKTOIPPVFPJEQO-UHFFFAOYSA-N 4-(3-carboxypropanoylperoxy)-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OOC(=O)CCC(O)=O MKTOIPPVFPJEQO-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 238000013532 laser treatment Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—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
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—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
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
- C08F214/262—Tetrafluoroethene with fluorinated vinyl ethers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on 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; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on 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; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M147/00—Lubricating compositions characterised by the additive being a macromolecular compound containing halogen
- C10M147/04—Monomer containing carbon, hydrogen, halogen and oxygen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/16—Monomers containing no hetero atoms other than the ether oxygen
- C08F216/165—Carbocyclic compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/22—Esters containing halogen
- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
- C10M2213/06—Perfluoro polymers
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a modified polytetrafluoroethylene and a preparation method and application thereof; the preparation method comprises the following steps: s1: adding deionized water and a dispersing agent into a reaction kettle, regulating pH, heating, replacing a system with nitrogen, replacing with tetrafluoroethylene monomer, regulating the pressure of the system with tetrafluoroethylene gas, and stirring for reaction to obtain a mixture A; s2: adding a compound of the general formula (I) or (II), a telogen, an initiator and deionized water into the mixture A, stirring and reacting to obtain modified polytetrafluoroethylene aqueous dispersion, condensing and drying to obtain the modified polytetrafluoroethylene aqueous dispersion. The modified polytetrafluoroethylene is represented by the general formula (I)Or of the general formula (II)Copolymerizing with tetrafluoroethylene to obtain; the prepared modified polytetrafluoroethylene has excellent dispersion stability, and the modified polytetrafluoroethylene is used as a component of a solid lubricant, so that the microhardness, compressive strength and wear resistance of the solid lubricant are improved, and meanwhile, the bonding performance of the modified polytetrafluoroethylene serving as a bonding material can be improved.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to modified polytetrafluoroethylene, and a preparation method and application thereof.
Background
Polytetrafluoroethylene (PTFE) has excellent temperature resistance and excellent chemical resistance, and is thus widely used in the fields of electronics, machinery, aerospace, biomedicine, and the like. Polytetrafluoroethylene has very excellent chemical properties, and thus has wide application in industrial production. However, polytetrafluoroethylene has low surface energy, poor wettability, printing and dyeing properties and adhesion properties, and poor radiation resistance, which limits its application. Therefore, the polytetrafluoroethylene is modified, the service performance of the polytetrafluoroethylene is improved, and the application range of the polytetrafluoroethylene is widened.
The PTFE is processed into ultrafine powder (even PTFE nanometer powder) which has wide application in factories, and the PTFE ultrafine powder can be added into other polymers as a filler in the aspect of solid materials to remarkably improve the corrosion resistance and other performances. In the aspect of liquid, PTFE ultrafine powder is used as an antiwear agent to be added into lubricating oil and other grease, and PTFE emulsion has a great market in the aspects of coating, additive and the like. However, there are many applications for PTFE powders in liquid form, particularly in aqueous form, where improvements are desired. At present, the PTFE grafting modification method is more and mainly comprises two main types of grafting modification after chemical treatment and grafting modification after physical treatment. The former has simple process and low cost, but the reaction process is difficult to control, has great influence on the performance of PTFE and can bring about environmental problems; the latter (including plasma treatment technology, electron beam irradiation technology, excimer laser treatment technology, high-energy irradiation technology, etc.) can improve physical and chemical properties of the original polymer without changing the inherent properties thereof, and thus, is receiving much attention.
Disclosure of Invention
The invention aims to provide modified polytetrafluoroethylene with excellent dispersion stability, which is used as a component of a solid lubricant, so that the microhardness, compressive strength and wear resistance of the solid lubricant are improved, and meanwhile, the adhesive property of the modified polytetrafluoroethylene serving as an adhesive material can be improved.
The technical scheme adopted by the invention for achieving the purpose is as follows:
a modified polytetrafluoroethylene obtained by copolymerizing at least one compound selected from the following general formulae (I) and (II); wherein,,
the structural formula of (I) is as follows:
in the general formula (I), X 1 、X 2 、X 3 Represents a hydrogen atom or a fluorine atom; r is R 1 、R 2 、R 3 Represents one of a hydrogen atom, a fluorine atom, an alkyl group having 1 to 5 carbon atoms, and a fluoroalkyl group having 1 to 5 carbon atoms;
(II) the structural formula is:
in the general formula (II), X 4 、X 5 、X 6 Represents a hydrogen atom or a fluorine atom, and at least one fluorine atom is contained; r is R 4 Represents one of a hydrogen atom, a hydroxyl group and a compound containing a benzene ring group.
The invention adopts the compound in the general formula (I) or the general formula (II) to be copolymerized and modified with tetrafluoroethylene to prepare the modified polytetrafluoroethylene, which improves the dispersion stability of the polytetrafluoroethylene, so that the polytetrafluoroethylene can be easily dispersed in other matrix materials to obtain materials with excellent mechanical properties and bonding properties.
Preferably, formula (I) is one of methyl trifluoroacrylate, perfluoroalkyl ethyl acrylate or 2-fluoroacrylate.
Preferably, formula (II) is one of trifluoroethylene ether, 1-tris (4-trifluorovinyloxyphenyl) ethane.
The invention also discloses a preparation method of the modified polytetrafluoroethylene, which comprises the following steps:
s1: adding deionized water and a dispersing agent into a reaction kettle, regulating the pH value, heating the reaction kettle to 60-75 ℃, replacing the system for 3-5 times by adopting nitrogen, replacing the system for 2-4 times by adopting tetrafluoroethylene monomer, regulating the pressure of the system by adopting tetrafluoroethylene gas, and stirring to obtain a mixture A;
s2: and (3) adding a compound of a general formula (I) or (II), a telogen, an initiator and deionized water into the mixture A, stirring and reacting for 8-16 h to obtain modified polytetrafluoroethylene aqueous dispersion, condensing and drying to obtain modified polytetrafluoroethylene.
Preferably, the deionized water is 40 to 60 parts, the dispersing agent is 0.025 to 0.055 part, the tetrafluoroethylene is 15 to 20 parts, the compound of the general formula (I) or (II) is 0.02 to 0.5 part, the telogen is 0.01 to 0.02 part, and the initiator is 0.005 to 0.015 part by weight.
Preferably, in step S1, the pH value of the system is adjusted to 8-9, and the stirring speed is 250-350 rpm.
Preferably, in step S1, the system pressure is adjusted to 0.7-2.5 MPa by using tetrafluoroethylene gas, so that the components can fully contact and react.
More preferably, the dispersing agent is one or two of perfluorocarbonate, perfluorocarbonic acid or diethyl carbonate.
More preferably, the telogen is one or a mixture of two of ethane, methyl iodide or 1, 2-diiodotetrafluoroethane.
More preferably, the initiator is one or a mixture of two of persulfate, ferrous salt or succinic acid peroxide.
Preferably, the solids content of the aqueous dispersion of modified polytetrafluoroethylene is 25 to 35% by weight.
Preferably, in the step S2, the drying temperature is 150-200 ℃ and the drying time is 12-18 h; specifically, the drying temperature is selected from 155 ℃, 165 ℃, 175 ℃, 185 ℃, 200 ℃.
Preferably, the shape of the modified polytetrafluoroethylene is powdery.
The invention also discloses the application of the modified polytetrafluoroethylene in preparing lubricants, printing ink, coating and/or release agent.
Preferably, the compressive strength of the solid lubricant to which the modified polytetrafluoroethylene is added is higher than 50MPa.
The invention adopts the compound in the general formula (I) or the general formula (II) to be copolymerized and modified with tetrafluoroethylene to prepare the modified polytetrafluoroethylene, thus having the following beneficial effects: the prepared modified polytetrafluoroethylene has good dispersion stability, can be easily dispersed in other matrix materials to obtain a material with excellent mechanical properties and bonding properties, so that the modified polytetrafluoroethylene with excellent dispersion stability is used as a component of a solid lubricant, the microhardness, compressive strength and wear resistance of the solid lubricant are improved, and the bonding properties of the modified polytetrafluoroethylene serving as a bonding material are improved.
Drawings
FIG. 1 shows the Zeta potential of modified polytetrafluoroethylene;
FIG. 2 is the coefficient of friction of a solid lubricant;
FIG. 3 is microhardness of a solid lubricant;
FIG. 4 is a graph of the compressive strength of a solid lubricant;
fig. 5 is a graph of the tensile shear strength of the bonding material.
Detailed Description
The technical scheme of the invention is further described in detail below with reference to the specific embodiments and the attached drawings:
example 1
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 35 parts by weight of deionized water and 0.025 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.5 by adopting 5% sodium hydroxide, heating the reaction kettle to 65 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.76MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 250rpm and the temperature is kept to 65 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.025 parts by weight of perfluoroalkyl ethyl acrylate, 0.01 parts by weight of methyl iodide, 0.008 parts by weight of sodium persulfate and 20 parts by weight of deionized water were added, reacted for 8 hours under the condition that the stirring rate was 250rpm and the temperature was kept at 65℃and the pressure in the system was kept constant at 0.76MPa by supplying tetrafluoroethylene gas to obtain an aqueous dispersion of modified polytetrafluoroethylene, wherein the solid content of the aqueous dispersion of modified polytetrafluoroethylene was 25.8% by weight, deionized water was added to the aqueous dispersion of modified polytetrafluoroethylene, and the aqueous dispersion was continuously stirred until it solidified, washed 3 times with deionized water and dried at 155℃for 12 hours to obtain modified polytetrafluoroethylene.
Example 2
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 40 parts by weight of deionized water and 0.045 part by weight of ammonium perfluor carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.7 by adopting 5% sodium hydroxide, heating the reaction kettle to 75 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 3 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.84MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 300rpm and the temperature is kept at 75 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.1 part by weight of methyl trifluoroacrylate, 0.015 part by weight of methyl iodide, 0.008 part by weight of peroxysuccinic acid and 15 parts by weight of deionized water were added, reacted for 10 hours at a stirring rate of 300rpm at a temperature of 75℃and the pressure in the system was kept constant at 0.84MPa by supplying tetrafluoroethylene gas to obtain an aqueous dispersion of modified polytetrafluoroethylene having a solid content of 27.5% by weight, and deionized water was added to the aqueous dispersion of modified polytetrafluoroethylene, followed by washing with deionized water 3 times and drying at 165℃for 12 hours to obtain a modified polytetrafluoroethylene.
Example 3
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 35 parts by weight of deionized water and 0.025 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.2 by adopting 5% sodium hydroxide, heating the reaction kettle to 65 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.75MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 350rpm and the temperature is kept to 65 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.055 parts by weight of trifluoroethylene ether, 0.01 parts by weight of 1, 2-diiodotetrafluoroethane, 0.008 parts by weight of sodium persulfate and 20 parts by weight of deionized water were added, reacted for 8 hours under the conditions of a stirring rate of 350rpm and a temperature of 65℃and the pressure in the system was kept constant at 0.75MPa by supplying tetrafluoroethylene gas to obtain an aqueous dispersion of modified polytetrafluoroethylene, wherein the solid content of the aqueous dispersion of modified polytetrafluoroethylene was 29.6% by weight, deionized water was added to the aqueous dispersion of modified polytetrafluoroethylene, stirred continuously until solidification was attained, and then washed 3 times with deionized water, and dried at 155℃for 12 hours to obtain modified polytetrafluoroethylene.
Example 4
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 25 parts by weight of deionized water and 0.035 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.5 by adopting 5% sodium hydroxide, heating the reaction kettle to 70 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.79MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 250rpm and the temperature is kept at 70 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.025 parts by weight of 1, 1-tris (4-trifluorovinyloxyphenyl) ethane, 0.02 parts by weight of 1, 2-diiodotetrafluoroethane, 0.012 parts by weight of sodium persulfate and 30 parts by weight of deionized water were added, reacted for 12 hours at a stirring rate of 250rpm at a temperature of 70℃and a pressure in the system was set to 0.85MPa, to obtain an aqueous dispersion of modified polytetrafluoroethylene having a solid content of 28.6% by weight, and deionized water was added to the aqueous dispersion of modified polytetrafluoroethylene, stirred continuously until it solidified, washed 3 times with deionized water, and dried at 175℃for 12 hours, to obtain a modified polytetrafluoroethylene.
In order to further improve the properties of the modified polytetrafluoroethylene, preferred measures to be taken further include:
in the preparation process, 0.02-0.04 weight part of modifier 2, 2-bis (4-trifluoro vinyl oxyphenyl) 1, 3-hexafluoropropane is added, and the modifier and the compound in the general formula (I) or the general formula (II) are copolymerized with tetrafluoroethylene to obtain modified polytetrafluoroethylene, so that the performance of the modified polytetrafluoroethylene is further improved.
Example 5
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 35 parts by weight of deionized water and 0.025 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.5 by adopting 5% sodium hydroxide, heating the reaction kettle to 65 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.76MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 250rpm and the temperature is kept to 65 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.025 parts by weight of perfluoroalkyl ethyl acrylate, 0.01 parts by weight of methyl iodide, 0.008 parts by weight of sodium persulfate and 20 parts by weight of deionized water were added, and when the mixture was reacted for 6 hours at a stirring rate of 250rpm and a temperature of 65 ℃, 0.02 parts by weight of 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane as a modifier was further added, and the reaction was continued for 2 hours, and the pressure in the system was kept constant at 0.76MPa by supplying tetrafluoroethylene gas, whereby an aqueous dispersion of modified polytetrafluoroethylene was obtained, wherein the solid content of the aqueous dispersion of modified polytetrafluoroethylene was 26.3% by weight, and deionized water was added to the aqueous dispersion of modified polytetrafluoroethylene, and the aqueous dispersion was continuously stirred until solidification was attained, and then washed 3 times with deionized water and dried at 155℃for 12 hours.
Example 6
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 40 parts by weight of deionized water and 0.045 part by weight of ammonium perfluor carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.7 by adopting 5% sodium hydroxide, heating the reaction kettle to 75 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 3 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.84MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 300rpm and the temperature is kept at 75 ℃ to obtain a mixture A;
s2: adding 0.1 part by weight of methyl trifluoroacrylate, 0.015 part by weight of methyl iodide, 0.008 part by weight of peroxysuccinic acid and 15 parts by weight of deionized water into the mixture A, reacting for 8 hours under the conditions that the stirring speed is 300rpm and the temperature is kept at 75 ℃, adding 0.02 part by weight of modifier 2, 2-bis (4-trifluoro-vinyloxyphenyl) 1, 3-hexafluoropropane, continuing to react for 2 hours, and keeping the pressure in the system constant at 0.84MPa by providing tetrafluoroethylene gas to obtain a modified polytetrafluoroethylene aqueous dispersion, wherein the solid content of the modified polytetrafluoroethylene aqueous dispersion is 27.8wt%, adding deionized water into the modified polytetrafluoroethylene aqueous dispersion, continuously stirring until solidification, then washing 3 times by using deionized water, and drying for 12 hours at 165 ℃ to obtain the modified polytetrafluoroethylene.
Example 7
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 35 parts by weight of deionized water and 0.025 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.2 by adopting 5% sodium hydroxide, heating the reaction kettle to 65 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.75MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 350rpm and the temperature is kept to 65 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.055 parts by weight of trifluoroethylene ether, 0.01 parts by weight of 1, 2-diiodotetrafluoroethane, 0.008 parts by weight of sodium persulfate and 20 parts by weight of deionized water were added, and when the mixture was reacted for 6 hours under the conditions that the stirring rate was 350rpm and the temperature was kept at 65 ℃, 0.02 parts by weight of modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane was further added, the reaction was continued for 2 hours, and the pressure in the system was kept constant at 0.75MPa by supplying tetrafluoroethylene gas, whereby a modified polytetrafluoroethylene aqueous dispersion having a solid content of 29.7% by weight was obtained, and deionized water was added to the modified polytetrafluoroethylene aqueous dispersion to be coagulated, followed by washing 3 times with deionized water and drying at 155℃for 12 hours, to obtain a modified polytetrafluoroethylene aqueous dispersion.
Example 8
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 25 parts by weight of deionized water and 0.035 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.5 by adopting 5% sodium hydroxide, heating the reaction kettle to 70 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.79MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 250rpm and the temperature is kept at 70 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.025 parts by weight of 1, 1-tris (4-trifluorovinyloxyphenyl) ethane, 0.02 parts by weight of 1, 2-diiodotetrafluoroethane, 0.012 parts by weight of sodium persulfate and 30 parts by weight of deionized water were added, and when the reaction was carried out for 10 hours at a stirring rate of 250rpm and a temperature of 70 ℃, 0.02 parts by weight of 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane as a modifier was further added, the reaction was continued for 2 hours, and the pressure in the system was set to 0.85MPa, whereby an aqueous dispersion of modified polytetrafluoroethylene was obtained, wherein the solid content of the aqueous dispersion of modified polytetrafluoroethylene was 28.9% by weight, and deionized water was added and stirred until solidification was continued, followed by washing 3 times with deionized water and drying at 175℃for 12 hours.
Comparative example 1
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 35 parts by weight of deionized water and 0.025 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.5 by adopting 5% sodium hydroxide, heating the reaction kettle to 65 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.76MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 250rpm and the temperature is kept to 65 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.01 parts by weight of methyl iodide, 0.008 parts by weight of sodium persulfate and 20 parts by weight of deionized water were added, reacted for 8 hours at a stirring rate of 250rpm at a temperature of 65℃and the pressure in the system was kept constant at 0.76MPa by supplying tetrafluoroethylene gas to obtain an aqueous polytetrafluoroethylene dispersion having a solid content of 25.5% by weight, deionized water was added to the aqueous modified polytetrafluoroethylene dispersion and stirred continuously until it solidified, and then washed 3 times with deionized water and dried at 155℃for 12 hours to obtain a modified polytetrafluoroethylene.
Comparative example 2
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 40 parts by weight of deionized water and 0.045 part by weight of ammonium perfluor carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.7 by adopting 5% sodium hydroxide, heating the reaction kettle to 75 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 3 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.84MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 300rpm and the temperature is kept at 75 ℃ to obtain a mixture A;
s2: adding 0.015 weight part of methyl iodide, 0.008 weight part of peroxysuccinic acid and 15 weight parts of deionized water into the mixture A, reacting for 10 hours under the conditions that the stirring speed is 300rpm and the temperature is kept at 75 ℃, and providing tetrafluoroethylene gas to keep the pressure in the system constant at 0.84MPa to obtain modified polytetrafluoroethylene aqueous dispersion, wherein the solid content of the modified polytetrafluoroethylene aqueous dispersion is 27.2 weight percent, adding deionized water into the modified polytetrafluoroethylene aqueous dispersion, continuously stirring until the mixture is solidified, washing the mixture with deionized water for 3 times, and drying the mixture at 165 ℃ for 12 hours to obtain the modified polytetrafluoroethylene.
Comparative example 3
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 35 parts by weight of deionized water and 0.025 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.2 by adopting 5% sodium hydroxide, heating the reaction kettle to 65 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.75MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 350rpm and the temperature is kept to 65 ℃ to obtain a mixture A;
s2: to the above mixture A, 0.055 parts by weight of 1, 2-diiodotetrafluoroethane, 0.008 parts by weight of sodium persulfate and 20 parts by weight of deionized water were added, reacted for 8 hours under the condition that the stirring rate was 350rpm and the temperature was kept at 65℃and the pressure in the system was kept constant at 0.75MPa by supplying tetrafluoroethylene gas to obtain an aqueous dispersion of modified polytetrafluoroethylene, wherein the solid content of the aqueous dispersion of modified polytetrafluoroethylene was 29.1% by weight, deionized water was added to the aqueous dispersion of modified polytetrafluoroethylene, stirred continuously until it solidified, and then washed 3 times with deionized water, and dried at 155℃for 12 hours to obtain modified polytetrafluoroethylene.
Comparative example 4
The preparation method of the modified polytetrafluoroethylene comprises the following steps:
s1: adding 25 parts by weight of deionized water and 0.035 part by weight of diethyl carbonate into a stainless steel reaction kettle with stirring slurry and a temperature adjusting sleeve, adjusting the pH of the system to 8.5 by adopting 5% sodium hydroxide, heating the reaction kettle to 70 ℃, displacing the system for 3 times by adopting nitrogen, displacing the system for 2 times by adopting tetrafluoroethylene monomer to remove oxygen and other gas impurities in the system, adjusting the pressure in the system to 0.79MPa by adopting tetrafluoroethylene gas, and uniformly stirring under the conditions that the stirring speed is 250rpm and the temperature is kept at 70 ℃ to obtain a mixture A;
s2: adding 0.02 weight part of 1, 2-diiodotetrafluoroethane, 0.012 weight part of sodium persulfate and 30 weight parts of deionized water into the mixture A, reacting for 12 hours under the condition that the stirring speed is 250rpm and the temperature is kept at 70 ℃, setting the pressure in the system to be 0.85MPa, and obtaining modified polytetrafluoroethylene aqueous dispersion, wherein the solid content of the modified polytetrafluoroethylene aqueous dispersion is 28.6 weight percent, adding deionized water into the modified polytetrafluoroethylene aqueous dispersion, continuously stirring until solidification, washing for 3 times by using the deionized water, and drying for 12 hours at 175 ℃ to obtain the modified polytetrafluoroethylene.
Test example 1:
1. determination of the Dispersion stability of modified polytetrafluoroethylene
The sample was prepared into a solution with a mass concentration of 0.5% by using a ZEN 3690 type instrument from Malvern, england, and 1mL of the solution was placed in a quartz sample cell with electrodes, respectively, and each sample was measured 3 times by setting up the procedure.
FIG. 1 shows the Zeta potential of modified polytetrafluoroethylene. As can be seen from fig. 1, the Zeta potential absolute value of the modified polytetrafluoroethylene in examples 1-4 is higher than 52.5mV, and the Zeta potential values in examples 1 and comparative example 1, examples 2 and comparative example 2, examples 3 and comparative example 3, examples 4 and comparative example 4 are respectively lower than those in examples 1, examples 2, examples 3 and example 4, that is, the absolute values are respectively higher than those in examples 1, comparative example 2, comparative example 3 and comparative example 4, which means that the modified polytetrafluoroethylene obtained by copolymerization modification of the polytetrafluoroethylene with methyl trifluoroacrylate, perfluoroalkyl ethyl acrylate, fluorovinyl phenyl ether, 1-tris (4-trifluorovinyloxyphenyl) ethane respectively has good dispersion stability; comparative examples 1 and 5, examples 2 and 6, examples 3 and 7, examples 4 and 8, examples 1 and 5, examples 2 and 6, and examples 3 and 7, respectively, show that the Zeta potential values of the modified polytetrafluoroethylene obtained by further modifying the modified polytetrafluoroethylene with the modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane have little influence on the dispersion stability, and that the modified polytetrafluoroethylene obtained by further modifying the modified polytetrafluoroethylene has excellent dispersion stability.
Test example 2
Use of modified polytetrafluoroethylene in lubricants;
mixing the prepared sample with graphite, molybdenum disulfide, bronze powder, carbon fiber and polyimide according to the weight ratio of 10:4:2:1:0.5:0.3 for 10min at the rotating speed of 15000r/min, carrying out cold pressing and sintering according to the conventional technical parameters and steps to obtain a solid lubricant cylinder, wherein the experimental conditions of each group of experiments are the same, and further measuring each performance of each group of solid lubrication.
1. Influence of modified polytetrafluoroethylene on friction coefficient of solid lubricant
Solid lubricant by using pin-disc type friction and wear testing machineIs a pin, 45# steel->The test conditions were a friction speed of 1.2m/s, a test time of 30min and a load of 60N for the discs.
Fig. 2 is a graph showing the friction coefficient of the solid lubricant. As can be seen from fig. 2, the friction coefficients of examples 1-4 are lower than 0.1, and the friction coefficients of comparative examples 1 and 1, comparative examples 2 and 2, example 3 and 3, and example 4 and comparative example 4 are lower than those of comparative examples 1,2, 3 and 4, respectively, which shows that the modified polytetrafluoroethylene is obtained by copolymerizing methyl trifluoroacrylate, perfluoroalkyl ethyl acrylate, fluorovinyl phenyl ether, 1-tris (4-trifluorovinyloxyphenyl) ethane and tetrafluoroethylene, respectively, and the wear resistance is improved by using the modified polytetrafluoroethylene as a component of a solid lubricant; examples 5-8 have a coefficient of friction lower than 0.09, examples 1 and 5, examples 2 and 6, examples 3 and 7, examples 4 and 8, example 5 has a coefficient of friction lower than example 1, example 6 has a coefficient of friction lower than example 2, example 7 has a coefficient of friction lower than example 3, and example 8 has a coefficient of friction lower than example 4, which means that the modified polytetrafluoroethylene is further modified with the modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane, respectively, and used as a component of the solid lubricant, thereby improving the wear resistance of the solid lubricant and providing it with better lubricating properties.
2. Influence of modified polytetrafluoroethylene on microhardness of solid lubricant
The microhardness of the sample was measured by using a Laitz polarization microscope (LEICA Co.).
Fig. 3 is microhardness of a solid lubricant. As can be seen from fig. 3, the microhardness of examples 1-4 is higher than 12.25Hv, and the microhardness of examples 1 and 1, examples 2 and 2, examples 3 and 3, and examples 4 and 4 is higher than that of examples 1,2, 3 and 4, respectively, which shows that the microhardness of the solid lubricant is improved by copolymerizing methyl trifluoroacrylate, perfluoroalkyl ethyl acrylate, fluorovinyl phenyl ether, 1-tris (4-trifluorovinyl oxyphenyl) ethane with tetrafluoroethylene to obtain modified polytetrafluoroethylene, and using the modified polytetrafluoroethylene as a component of the solid lubricant; examples 5-8 have a microhardness higher than 14.17Hv, comparative examples 1 and 5, examples 2 and 6, examples 3 and 7, examples 4 and 8, example 5 has a microhardness higher than example 1, example 6 has a microhardness higher than example 2, example 7 has a microhardness higher than example 3, and example 8 has a microhardness higher than example 4, which means that the modified polytetrafluoroethylene is further modified with the modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane, respectively, and used as a component of a solid lubricant to increase the microhardness of the solid lubricant.
3. Impact of modified polytetrafluoroethylene on compressive strength of solid Lubricants
The compressive strength of the samples was measured using an MTS-810 type material tester (MTS Co., USA).
Fig. 4 shows the compressive strength of the solid lubricant. As can be seen from fig. 4, the compressive strength of examples 1-4 is higher than 50MPa, and the compressive strengths of comparative examples 1 and 1, comparative examples 2 and 2, example 3 and 3, and example 4 and comparative example 4 are higher than those of comparative examples 1,2, 3 and 4, respectively, which indicates that the use of methyl trifluoroacrylate, perfluoroalkyl ethyl acrylate, fluorovinyl phenyl ether, 1-tris (4-trifluorovinyloxyphenyl) ethane and tetrafluoroethylene for copolymerization modification respectively to obtain modified polytetrafluoroethylene, which is used as a component of a solid lubricant, improves the compressive strength of the solid lubricant; examples 5-8 have microhardness higher than 52.05MPa, and comparative examples 1 and 5, examples 2 and 6, examples 3 and 7, and examples 4 and 8, with example 5 having higher compressive strength than example 1, example 6 having higher compressive strength than example 2, example 7 having higher compressive strength than example 3, and example 8 having higher compressive strength than example 4, which means that modified polytetrafluoroethylene is further modified with modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane, respectively, and used as a component of a solid lubricant, and the compressive strength of the solid lubricant is improved to have excellent mechanical properties.
Test example 3
Use of modified polytetrafluoroethylene in a binding material.
1. Influence of modified polytetrafluoroethylene on the adhesive properties of adhesive materials
And pressing the prepared test sample into a flake shape, mixing and stirring the epoxy resin, the curing agent and a proper solvent uniformly, mixing the resin and the curing agent according to a mass ratio of 100:100, and standing to remove bubbles in the adhesive. Epoxy glue is coated on the surface and the steel sheet respectively, bonding is carried out after the solvent volatilizes, certain pressure is applied under the condition of keeping dislocation free, the epoxy glue is placed at room temperature for days, after the emulsion is solidified, the contact area of the epoxy glue is measured, the shear strength is tested on a material testing machine, the testing temperature is room temperature, and the stretching speed is 5mm/min.
Fig. 5 is a graph of the tensile shear strength of the bonding material. As can be seen from FIG. 5, examples 1 to 4 have tensile shear strength higher than 305N/cm -2 Comparative examples 1 and 1,2 and 2, 3 and 3, and 4 have higher tensile shear strength than comparative examples 1,2, 3 and 4, respectively, indicating that the modified polytetrafluoroethylene is obtained by copolymerizing methyl trifluoroacrylate, perfluoroalkyl ethyl acrylate, fluorovinyl phenyl ether, 1-tris (4-trifluorovinyl oxyphenyl) ethane and tetrafluoroethylene, respectively, to improve the tensile shear strength of the bonding material containing the modified polytetrafluoroethylene and to provide excellent bonding performance; comparative examples 1 and 5, examples 2 and 6, examples 3 and 7, examples 4 and 8, and example 5 shows little difference in tensile shear strength from example 1, example 6 shows little difference in tensile shear strength from example 2, example 7 shows little difference in tensile shear strength from example 3, and example 8 shows little difference in tensile shear strength from example 4, indicating that the modified polytetrafluoroethylene is further modified with the modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane, respectively, and the adhesive properties of the modified polytetrafluoroethylene in the adhesive material are not greatly affected.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art, and are not described herein.
The above embodiments are merely for illustrating the present invention and not for limiting the same, and various changes and modifications may be made by one of ordinary skill in the art without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also fall within the scope of the invention, the scope of which is defined by the claims.
Claims (9)
1. A modified polytetrafluoroethylene, characterized by: the modified polytetrafluoroethylene is prepared by copolymerizing at least one compound selected from modified compounds with tetrafluoroethylene; wherein,,
the modified compound is trifluoro methyl acrylate, perfluoroalkyl ethyl acrylate, trifluoro vinyl phenyl ether, 1-triss (4-trifluoro vinyl oxyphenyl) ethane.
2. The method for preparing the modified polytetrafluoroethylene as claimed in claim 1, comprising the following steps:
s1: adding deionized water and a dispersing agent into a reaction kettle, regulating the pH value, heating the reaction kettle to 60-75 ℃, replacing the system for 3-5 times by adopting nitrogen, replacing the system for 2-4 times by adopting tetrafluoroethylene monomer, regulating the pressure of the system by adopting tetrafluoroethylene gas, and stirring to obtain a mixture A;
s2: and adding a modified compound, a telogen, an initiator and deionized water into the mixture A, stirring and reacting for 8-16 h to obtain modified polytetrafluoroethylene aqueous dispersion, condensing and drying to obtain modified polytetrafluoroethylene.
3. The method for preparing the modified polytetrafluoroethylene as claimed in claim 2, wherein: the weight portions of deionized water are 40 to 60 portions, dispersant is 0.025 to 0.055 portion, tetrafluoroethylene is 15 to 20 portions, modified compound is 0.02 to 0.5 portion, telogen is 0.01 to 0.02 portion, and initiator is 0.005 to 0.015 portion.
4. The method for preparing the modified polytetrafluoroethylene as claimed in claim 2, wherein: the system pressure is regulated to be 0.7-2.5 MPa by adopting tetrafluoroethylene gas.
5. A process for producing a modified polytetrafluoroethylene according to claim 2 or 3, characterized by: the dispersing agent is one or two of perfluorocarbonate, perfluorocarbonic acid or diethyl carbonate.
6. The method for preparing the modified polytetrafluoroethylene as claimed in claim 2, wherein: the solid content of the modified polytetrafluoroethylene aqueous dispersion is 25-35%.
7. The method for preparing the modified polytetrafluoroethylene as claimed in claim 2, wherein: in the step S2, 0.02-0.04 part by weight of a modifier 2, 2-bis (4-trifluorovinyloxyphenyl) 1, 3-hexafluoropropane is additionally added.
8. Use of the modified polytetrafluoroethylene as defined in claim 1 for the preparation of lubricating grease, printing ink, coating and/or release agent.
9. Use according to claim 8, characterized in that: the compressive strength of the solid lubricant added with the modified polytetrafluoroethylene is higher than 50MPa.
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| WO2020226178A1 (en) * | 2019-05-08 | 2020-11-12 | ダイキン工業株式会社 | Fluoropolymer production method and fluoropolymer |
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