CN116655982B - Preparation method of perfluoro rubber product with non-adhesive surface - Google Patents
Preparation method of perfluoro rubber product with non-adhesive surface Download PDFInfo
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- CN116655982B CN116655982B CN202310796550.8A CN202310796550A CN116655982B CN 116655982 B CN116655982 B CN 116655982B CN 202310796550 A CN202310796550 A CN 202310796550A CN 116655982 B CN116655982 B CN 116655982B
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- perfluororubber
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- rubber
- heating
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 66
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 17
- 239000000853 adhesive Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- -1 perfluoro Chemical group 0.000 title abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 55
- 238000000576 coating method Methods 0.000 claims abstract description 55
- 238000004381 surface treatment Methods 0.000 claims abstract description 55
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 238000005507 spraying Methods 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- 238000007788 roughening Methods 0.000 claims abstract description 9
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- 239000000839 emulsion Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 13
- 229920001577 copolymer Polymers 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 239000004695 Polyether sulfone Substances 0.000 claims description 8
- 229920006393 polyether sulfone Polymers 0.000 claims description 8
- 230000003746 surface roughness Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 150000002902 organometallic compounds Chemical class 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 239000000945 filler Substances 0.000 abstract description 3
- 238000004073 vulcanization Methods 0.000 description 23
- 239000004636 vulcanized rubber Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 229920001973 fluoroelastomer Polymers 0.000 description 12
- 238000000227 grinding Methods 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 description 11
- MSTZGVRUOMBULC-UHFFFAOYSA-N 2-amino-4-[2-(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropan-2-yl]phenol Chemical compound C1=C(O)C(N)=CC(C(C=2C=C(N)C(O)=CC=2)(C(F)(F)F)C(F)(F)F)=C1 MSTZGVRUOMBULC-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 125000002560 nitrile group Chemical group 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 239000004962 Polyamide-imide Substances 0.000 description 7
- 229920002312 polyamide-imide Polymers 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 229920005992 thermoplastic resin Polymers 0.000 description 7
- PCAXITAPTVOLGL-UHFFFAOYSA-N 2,3-diaminophenol Chemical group NC1=CC=CC(O)=C1N PCAXITAPTVOLGL-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000005488 sandblasting Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 230000001680 brushing effect Effects 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 3
- 229920002313 fluoropolymer Polymers 0.000 description 3
- 239000004811 fluoropolymer Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000007799 cork Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000007590 electrostatic spraying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002335 surface treatment layer Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- YEECOJZAMZEUBB-UHFFFAOYSA-N 2,2,3,3,6,6,7,7-octamethyloctane Chemical compound CC(C)(C)C(C)(C)CCC(C)(C)C(C)(C)C YEECOJZAMZEUBB-UHFFFAOYSA-N 0.000 description 1
- 150000003923 2,5-pyrrolediones Chemical class 0.000 description 1
- 239000010963 304 stainless steel Substances 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 1
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- 229920001774 Perfluoroether Polymers 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000005870 Ziram Substances 0.000 description 1
- 125000004453 alkoxycarbonyl group Chemical group 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical group BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 150000002916 oxazoles Chemical class 0.000 description 1
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 1
- 229920005548 perfluoropolymer Polymers 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920003192 poly(bis maleimide) Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 150000003557 thiazoles Chemical class 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/10—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C08J2300/102—Polymers characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use 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; Derivatives of such polymers
- C08J2427/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
Abstract
The invention relates to the technical field of layered products, in particular to a preparation method of a perfluoro rubber product with a non-adhesive surface, which comprises the following steps: s1, preparing a perfluororubber product: mixing the raw perfluororubber with a filler or a vulcanizing agent to obtain a rubber compound; vulcanizing the rubber compound to obtain a perfluorinated rubber product; s2, surface treatment: surface roughening and degreasing treatment are carried out on the perfluorinated rubber product; s3, one-step surface treatment: spraying or dipping the coating a on the surface of the perfluororubber product, and heating to obtain the perfluororubber product with the pretreated surface; s4, two-step surface treatment: spraying or dipping non-adhesive coating a on the surface of the perfluorinated rubber product with the pretreated surface, and heating to obtain the perfluorinated rubber product with the non-adhesive surface. The surface treatment method can improve the problem of surface tackiness of the perfluororubber product, and the surface coating can not fall off under the action of external force.
Description
Technical Field
The invention relates to the technical field of layered products, in particular to a preparation method of a perfluoro rubber product with a non-adhesive surface.
Background
The perfluororubber product has the characteristics of high cleanliness, heat resistance, chemical resistance, plasma resistance and the like, and is also applied to semiconductor and liquid crystal manufacturing equipment, but the perfluororubber product is often adhered to the surfaces of materials such as metal, silicon wafers and the like which are contacted with the perfluororubber product, so that the perfluororubber product cannot be torn off, the semiconductor and liquid crystal manufacturing equipment cannot normally run at the position where the switch operation is frequently executed, and the products such as the silicon wafers, the perfluororubber product and the production equipment are damaged when the mechanical force is adopted for tearing off, so that the production efficiency and the yield of the products are reduced, and the performance of the equipment is further influenced.
The current method for surface non-tackiness treatment of perfluororubber articles comprises: (1) adding a low melting point or low molecular weight additive material; (2) subjecting the fluororubber article to plasma treatment; (3) Coating the surface of the fluororubber product by adopting a silane coupling agent, reactive silicone resin or a coating prepared by amorphous fluoropolymer resin; (4) The perfluororesin is blended with the perfluororubber green stock to provide non-tackiness by utilizing the perfluoroplastic enriched areas of the surface of the final article. The adoption of the treatment method has certain problems, and needs to be further improved, including that the addition of the additive can cause the release of gas or introduce new pollutants, which has fatal influence on the application field with high purity requirement; the bonding problem between different materials of the perfluororubber and the reactive silicone resin also exists, and the mechanical strength of the silicone resin of the surface treatment layer is not high, and the performances of solvent resistance, oil resistance and chemical resistance are slightly poor, so that the use occasion of the perfluororubber sealing member is affected; and the amorphous perfluorinated resin has very high price and low yield, and the method of coating with amorphous fluoropolymer cannot be used on a large scale. The method of blending and modifying the perfluororubber and the perfluororesin is relatively easy to realize for the raw material manufacturers of the fluororubber/the fluororesin, because the blending of the two types of fluoropolymer materials in the original form just polymerized is relatively easy to realize, and is difficult to realize for the manufacturers at the rear end.
Chinese patent with the patent application number of CN200810074222. X discloses a water-based polyether sulfone non-stick paint composition without perfluoro caprylic acid and a preparation method thereof, which is used for non-stick coating of an electric cooker and is not used for surface coating treatment of fluororubber products. Therefore, the preparation method of the perfluoro rubber product with the non-adhesive surface is a technical problem which needs to be solved at present.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a perfluororubber product having a surface non-tackiness, comprising the steps of: s1, preparing a perfluororubber product: mixing the raw perfluororubber with a vulcanizing agent to obtain a rubber compound; vulcanizing the rubber compound at high temperature to obtain a perfluorinated rubber product;
s2, surface treatment: surface roughening and degreasing treatment are carried out on the perfluorinated rubber product;
s3, one-step surface treatment: FEP emulsion, aqueous dispersion of polyether sulfone and SiO 2 Uniformly mixing to obtain a coating a, spraying or dipping the coating a on the surface of the perfluororubber product, and heating to obtain the perfluororubber product with the pretreated surface;
s4, two-step surface treatment: spraying or dipping non-adhesive coating a on the surface of the perfluorinated rubber product subjected to surface pretreatment, and heating to obtain the perfluorinated rubber product with the surface non-adhesive property;
the surface roughness Ra of the perfluororubber product after the surface rough treatment of the perfluororubber product in the step S2 is larger than 5 mu m;
the temperature of the heating in S4 is set below 360 ℃.
In the step S2, the surface of the perfluororubber product is roughened by sand blasting, rough grinding, water grinding and other methods, the particles remained on the surface are brushed off, and degreasing is performed by using an organic solvent.
Further, in the step S2, acetone is adopted to degrease the surface of the perfluororubber product.
In order to solve the problem of surface tackiness of the perfluororubber product, the applicant has unexpectedly found in experiments that by carrying out surface roughening and degreasing treatment on the perfluororubber product and then carrying out two-step surface treatment, especially when the surface roughness Ra of the perfluororubber product after the treatment is larger than 5 μm, the bonding fastness of the surface of the perfluororubber product and the coating can be improved, the problem that the surface coating falls off under the action of external force can not occur, especially when the external force is carried out in high-temperature water, the surface coating of the perfluororubber product can not fall off, no particles fall off, the fastness of the surface coating is high, the permanent service life of the perfluororubber product is prolonged, the surface non-tackiness effect of the perfluororubber product in the use process is good, especially when the surface of the perfluororubber product is contacted with the surfaces of materials such as metal, silicon chips and the like under pressure, the damage of products such as the perfluororubber product, the production equipment and the like can not be caused, and the production efficiency and the yield of the products are improved.
Preferably, the high temperature vulcanization in S1 is a vulcanization process using primary mold press vulcanization and secondary vulcanization.
Further, placing the rubber compound at 160-180 ℃ and heating for 10-20min, and simultaneously, keeping the pressure of 5MPa for one-time mould pressing vulcanization to obtain vulcanized rubber a; and (3) placing the vulcanized rubber a to 280-300 ℃ and heating for at least 20h for secondary vulcanization to obtain the perfluororubber product.
Further, placing the rubber compound at 170 ℃ and heating for 15min, and simultaneously keeping the temperature under 5MPa for one-time mold pressing vulcanization to obtain vulcanized rubber a; and (3) placing the vulcanized rubber a at 290 ℃ and heating for at least 20 hours for secondary vulcanization to obtain the perfluororubber product.
Preferably, the perfluororubber used in S1 may comprise 45 to 80mol% tetrafluoroethylene monomer units, 15 to 55mol% perfluoroether monomer units, and 0.1 to 5mol% crosslinking point monomer units of the perfluororubber.
Preferably, the crosslinking point monomer unit of the perfluorinated rubber contains one or a combination of several functional groups such as C-X (X is iodine or bromine), nitrile group, carboxyl group or alkoxycarbonyl group.
Preferably, the filler comprises an organic filler or an inorganic filler.
Further, the filler comprises one or two of carbon black and silicon dioxide.
Preferably, the vulcanizing agent comprises one or more combinations of organometallic compounds, amino-containing organic compounds, or functionalized derivatives thereof.
Further, the vulcanizing agent is a bis-aminophenol vulcanizing agent.
Preferably, the raw materials for preparing the perfluororubber product in the step S1 further comprise a vulcanization accelerator.
Preferably, the vulcanization accelerator comprises one or more combinations of multifunctional maleimides, N' -m-phenylene bismaleimides, triallyl isocyanurate.
Preferably, the raw material for preparing the coating a is at least one selected from fluororesin, fluororubber raw rubber, tackifying composition and dispersing agent.
Preferably, the fluororubber raw rubber may be in the form of particles, powder or liquid dispersion, and depending on the form of the coating material for coating, the powder and dispersion forms are preferable, respectively.
Preferably, the melting point of the fluororesin is 250 to 350 ℃.
Preferably, the fluororesin form may be a powder or a liquid dispersion.
Preferably, the fluororesin is selected from one or more of polytetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl ether copolymer, tetrafluoroethylene hexafluoropropylene copolymer, ethylene-tetrafluoroethylene copolymer.
Preferably, the tackifying composition comprises a thermoplastic resin, a vulcanizing agent.
Further, the content of the tackifying component is 0.05wt% to 5wt%, preferably 0.1wt% to 2wt%.
Preferably, the vulcanizing agent is selected from one or more of organic peroxides, inorganic peroxides, aminobenzene, bisaminophenols, oxazoles, imidazoles, thiazoles, triazines.
Preferably, the adhesion promoting composition may further comprise a vulcanization accelerator; the vulcanization accelerator is one or more selected from polyfunctional maleimide PAPI, N' -m-phenylene bismaleimide and triallyl isocyanurate.
Preferably, the dispersing agent is at least one selected from water, organic solvents, surfactants, and modifying additives.
The inventor finds that the adopted raw material components can jointly form a uniformly dispersed liquid composition by adopting a dispersing agent in the experimental process, the viscosity, the solid content and the surface tension of the liquid composition can be further adjusted, the coating a can be further uniformly dispersed on the surface of the perfluororubber product and can be uniformly adhered to the surface of the perfluororubber product, and the coating a can form a film layer with uniform thickness and good adhesiveness when being cured.
Further, the thermoplastic resin has a heat distortion temperature greater than 200 ℃.
Further, the thermoplastic resin comprises one or a combination of more of amide groups, imide groups, thioether groups, sulfonyl groups, ether groups and phenylene groups.
Further, the thermoplastic resin is selected from one or more of polyamide imide, polyphenylene sulfide, polyether sulfone and liquid crystal polymer.
Further, the thermoplastic resin is one or two of polyethersulfone and polyamide imide.
Further, the fluororesin in the coating a is selected from one or more of polytetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl ether copolymer, tetrafluoroethylene hexafluoropropylene copolymer and ethylene-tetrafluoroethylene copolymer.
Preferably, nitrile groups may be included in the raw fluororubber.
As a preferred example, the raw fluororubber may be selected from FFKM1 and FFKM2.
FFKM1 is nitrile-containing perfluororubber, and the manufacturer of FFKM1 is 3M company in the United states, and the model is PFE-131TZ.
FFKM2 is a heat-resistant perfluororubber, and its manufacturer and model are Suwei (Solvay) in the United states and PFR 95 in the model.
Preferably, the non-stick coating a is prepared from a fluororesin having a melting point of 250-350 ℃.
Preferably, the non-stick coating a is in the form of a powder or emulsion.
Preferably, the fluororesin is selected from one or more of polytetrafluoroethylene, tetrafluoroethylene-perfluoroalkyl ether copolymer, tetrafluoroethylene hexafluoropropylene copolymer, ethylene-tetrafluoroethylene copolymer.
As examples of the fluororesin in one embodiment, there may be mentioned PFA powder having a particle size of about 5 to 50 μm of MJ-102 of Sanjingke, japan, FEP emulsion of Shanghai Sanyi FR463.
The PFA is tetrafluoroethylene-perfluoroalkyl ether copolymer.
The FEP is tetrafluoroethylene hexafluoropropylene copolymer.
Preferably, the heating temperature in S4 is 10-60 ℃ higher than the melting point of the resin material contained in the non-stick coating a.
Further, the heating temperature in the step S4 is set to be 20-50 ℃ higher than the melting point temperature of the non-adhesive coating material, and is controlled to be lower than the temperature at which the fluororubber material starts to degrade and deteriorate.
In order to improve the bonding fastness between the coating layers after the two-step surface treatment of the perfluororubber product, the applicant creatively found in experiments that the coating a is adopted to carry out the one-step surface treatment when the one-step surface treatment is carried out, and the raw materials for preparing the coating a comprise fluororesin, fluororubber raw rubber, tackifying composition and dispersing agent, wherein the resin content is 30-95wt%, the fluororubber content is 0-40wt%, and the thermoplastic resin is 0-5wt%, and the polyether sulfone or polyamide imide with the heat distortion temperature being more than 200 ℃ is adopted as the thermoplastic resin when the rest of the dispersing agent is adopted to carry out the one-step surface treatment on the perfluororubber product, the intermediate bonding layer is formed on the outer layer of the perfluororubber product by drying the surface treatment at the temperature higher than the melting point of the fluororesin and the vulcanization temperature of the fluororubber when the two-step surface treatment is carried out, and the powder or emulsion fluororesin adopted when the two-step surface treatment is carried out, the melting point of the fluororesin is 250-350 ℃ and the heating temperature is set to be lower than 360 ℃, so that the bonding between the two-step surface treatment after the perfluororubber product is carried out the two-step surface treatment can be improved, and the problem of the bonding between the coating layers after the two-step surface treatment can not occur under the high temperature of the peeling of the coating layer. And can improve the yellowing problem of the perfluororubber product during high-temperature treatment.
Drawings
Fig. 1 is a view of an O-ring shape.
FIG. 2 is a surface treatment layer falling state diagram of the surface-non-tacky perfluororubber product prepared in example 2.
FIG. 3 is a yellowing chart of the substrate of the surface-non-tacky perfluororubber product prepared in example 5.
Advantageous effects
1. The surface treatment method can improve the problem of surface tackiness of the perfluororubber product, and the surface coating can not fall off under the action of external force, thereby realizing the effect of permanent sealing.
2. By adopting the surface treatment method defined in the invention, the surface coating of the perfluororubber product can not fall off due to the external force action of the perfluororubber product in high temperature water, and the surface coating has high fastness.
3. By adopting the surface treatment method defined in the invention, the service life of the perfluororubber product is prolonged.
4. By adopting the surface treatment method defined in the invention, the surface non-tackiness effect of the perfluororubber product in the use process is good, and particularly when the perfluororubber product is contacted with the surface of materials such as metal, silicon wafer and the like under pressure, the perfluororubber product is easy to tear off, the products such as the silicon wafer, the perfluororubber product, production equipment and the like are not damaged, and the production efficiency and the yield of the products are improved.
5. By adopting the surface treatment method defined in the invention, the bonding fastness between the coating layers of the perfluorinated rubber product after two-step surface treatment is improved.
Detailed Description
Example 1
A method for preparing a perfluororubber article having a surface non-tackiness, comprising the steps of:
s1, preparing a perfluororubber product: mixing 1g of a bisaminophenol vulcanizing agent and 100g of nitrile group-containing perfluoro rubber raw rubber on an open mill to obtain a rubber compound; heating the rubber compound at 170 ℃ for 15min, and simultaneously, carrying out primary mould pressing vulcanization under the pressure of 5MPa to obtain vulcanized rubber a; heating vulcanized rubber a to 290 ℃ for 20 hours for secondary vulcanization to obtain a perfluorinated rubber product;
s2, surface treatment: carrying out surface roughening treatment on the surface of a perfluororubber product by adopting methods such as sand blasting, rough grinding, water grinding and the like, brushing off particles remained on the surface, degreasing by adopting acetone, and carrying out surface treatment in the step S2, wherein the surface roughness Ra of the perfluororubber product is more than 5 mu m;
s3, one-step surface treatment: uniformly mixing 100g of PFA powder, 20g of FFKM1 rubber powder micro powder and 0.3g of bisaminophenol vulcanizing agent to obtain a coating a, spraying the coating a on the surface of a perfluororubber product by an electrostatic spraying method, heating the perfluororubber product to 320 ℃ at a heating rate of 2 ℃/min, and keeping the temperature for 15min to obtain the perfluororubber product with the pretreated surface;
s4, two-step surface treatment: coating PFA powder on the surface of the surface-pretreated perfluororubber product by utilizing an electrostatic spraying method, heating to 330 ℃ at a heating rate of 2 ℃/min, and keeping at 330 ℃ for 10min to obtain the perfluororubber product with the surface non-tackiness.
The manufacturer of the nitrile group-containing perfluororubber raw rubber in S1 is FFKM1 of 3M company in the United states, and the model is PFE-131TZ.
The bis-aminophenol vulcanizing agent in the S1 is 2, 2-bis (3-amino-4-hydroxyphenyl) -hexafluoropropane, and the CAS number is 83558-87-6.
In the one-step surface treatment process in the step S3, the spraying amount of the coating a is 100g/m 2 。
The PFA is tetrafluoroethylene-perfluoroalkyl ether copolymer.
The PFA powder adopted in the step S3 is purchased from Mitsui Cork, model MJ-102, and particle size of about 5-50 μm.
The bis-aminophenol vulcanizing agent in the S3 is 2, 2-bis (3-amino-4-hydroxyphenyl) -hexafluoropropane, and the CAS number is 83558-87-6.
In the two-step surface treatment process in the step S4, the spraying amount of the PFA powder is 100g/m 2 。
The PFA powder adopted in the S4 is purchased from Mitsui Cork, model MJ-102, and particle size of about 5-50 μm.
Example 2
A method for preparing a perfluororubber article having a surface non-tackiness, comprising the steps of:
s1, preparing a perfluororubber product: mixing 100g of raw perfluororubber, 20g of carbon black, 10g of silicon dioxide and 3g of vulcanizing agent on an open mill to obtain a mixed rubber; heating the rubber compound at 170 ℃ for 15min, and simultaneously, carrying out primary mould pressing vulcanization under the pressure of 5MPa to obtain vulcanized rubber a; heating vulcanized rubber a to 290 ℃ for 20 hours for secondary vulcanization to obtain a perfluorinated rubber product;
s2, surface treatment: carrying out surface roughening treatment on the surface of a perfluororubber product by adopting methods such as sand blasting, rough grinding, water grinding and the like, brushing off particles remained on the surface, degreasing by adopting acetone, and carrying out surface treatment in the step S2, wherein the surface roughness Ra of the perfluororubber product is more than 5 mu m;
s3, one-step surface treatment: 100g of FEP emulsion, 20g of raw rubber dispersion liquid of perfluororubber, 1g of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane, 3g of triallyl isocyanurate, 10g of silicon dioxide and 30g of organic solvent are uniformly mixed by using a homogenizer to obtain a coating a, the coating a is sprayed on the surface of a perfluororubber product, and the surface-pretreated perfluororubber product is obtained by heating to 280 ℃ and keeping for 10 min;
s4, two-step surface treatment: spraying FEP emulsion on the surface of the perfluoro rubber product with the surface pretreatment, and heating at 290 ℃ for 10min to obtain the perfluoro rubber product with the surface non-tackiness.
The raw perfluororubber adopted in the S1 is heat-resistant perfluororubber, and the manufacturer of the heat-resistant perfluororubber is Suwei (Solvay) in the United states, and the model is PFR 95.
The manufacturer adopting carbon black in the S1 is cabot in the U.S. and the model is N330.
And the manufacturer adopting the silicon dioxide in the S1 is winning AEROSIL cube R-208.
The S1 adopts 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide with CAS number of 78-63-7.
The FEP is tetrafluoroethylene hexafluoropropylene copolymer.
The manufacturer adopting FEP emulsion in the S3 is Shanghai Sanyi Fu, and the model is FR463. The dispersion of the raw rubber of the perfluororubber used in the step S3 comprises 30wt% of the raw rubber of the perfluororubber and 70wt% of an aqueous solution containing a fluorosurfactant.
The mass ratio of the fluorosurfactant to the water in the aqueous solution of the fluorosurfactant is 0.5:100.
The manufacturer of the fluorine-containing surfactant is Henan ziram new material technology Co., ltd, and the model of the perfluorohexyl amine oxide CF386N.
The manufacturer of the perfluororubber raw rubber is Sovier (Solvay) in the United states and the model is PFR 95.
The organic solvent adopted in the step S3 is butanol and ethyl acetate; the weight ratio of butanol to ethyl acetate is 1:1.
the manufacturer adopting FEP emulsion in the S4 is Shanghai Sanyi Fu, and the model is FR463. In the one-step surface treatment process in the step S3, the spraying amount of the coating a is 100g/m 2 。
In the two-step surface treatment process in the step S4, the spraying amount of the FEP emulsion is 100g/m 2 。
Example 3
A method for preparing a perfluororubber article having a surface non-tackiness, comprising the steps of:
s1, preparing a perfluororubber product: mixing 1g of a bisaminophenol vulcanizing agent and 100g of nitrile group-containing perfluoro rubber raw rubber on an open mill to obtain a rubber compound; heating the rubber compound at 170 ℃ for 15min, and simultaneously, carrying out primary mould pressing vulcanization under the pressure of 5MPa to obtain vulcanized rubber a; heating vulcanized rubber a to 290 ℃ for 20 hours for secondary vulcanization to obtain a perfluorinated rubber product;
s2, surface treatment: carrying out surface roughening treatment on the surface of a perfluororubber product by adopting methods such as sand blasting, rough grinding, water grinding and the like, brushing off particles remained on the surface, degreasing by adopting acetone, and carrying out surface treatment in the step S2, wherein the surface roughness Ra of the perfluororubber product is more than 5 mu m;
s3, one-step surface treatment: will be 100g FEP emulsion, 5g aqueous dispersion of polyethersulfone and 10g SiO 2 Uniformly mixing to obtain a coating a, spraying the coating a on the surface of a perfluororubber product, heating to 280 ℃ and keeping for 10min to obtain the perfluororubber product with the pretreated surface;
s4, two-step surface treatment: spraying FEP emulsion on the surface of the perfluoro rubber product subjected to surface pretreatment, and heating at 300 ℃ for 10min to obtain the perfluoro rubber product with the surface non-tackiness.
The manufacturer of the nitrile group-containing perfluororubber raw rubber in S1 is FFKM1 of 3M company in the United states, and the model is PFE-131TZ.
The bis-aminophenol vulcanizing agent in the S1 is 2, 2-bis (3-amino-4-hydroxyphenyl) -hexafluoropropane, and the CAS number is 83558-87-6.
The FEP is tetrafluoroethylene hexafluoropropylene copolymer.
The manufacturer adopting FEP emulsion in the S3 is Shanghai Sanyi Fu, and the model is FR463. The manufacturer of the aqueous dispersion of polyethersulfone in S3 is quark WP-421.
SiO in S3 2 The purchase manufacturer and model number of the matrix is winning AEROSIL R-208.
The manufacturer adopting FEP emulsion in the S4 is Shanghai Sanyi Fu, and the model is FR463.
In the one-step surface treatment process in the step S3, the spraying amount of the coating a is 100g/m 2 。
In the two-step surface treatment process in the step S4, the spraying amount of the FEP emulsion is 100g/m 2 。
Example 4
A method for preparing a perfluororubber article having a surface non-tackiness, comprising the steps of:
s1, preparing a perfluororubber product: mixing 1g of a bisaminophenol vulcanizing agent and 100g of nitrile group-containing perfluoro rubber raw rubber on an open mill to obtain a rubber compound; heating the rubber compound at 170 ℃ for 15min, and simultaneously, carrying out primary mould pressing vulcanization under the pressure of 5MPa to obtain vulcanized rubber a; heating vulcanized rubber a to 290 ℃ for 20 hours for secondary vulcanization to obtain a perfluorinated rubber product;
s2, surface treatment: carrying out surface roughening treatment on the surface of a perfluororubber product by adopting methods such as sand blasting, rough grinding, water grinding and the like, brushing off particles remained on the surface, degreasing by adopting acetone, and carrying out surface treatment in the step S2, wherein the surface roughness Ra of the perfluororubber product is more than 5 mu m;
s3, one-step surface treatment: uniformly mixing 100g of PTFE emulsion and 1g of polyamide-imide aqueous dispersion to obtain a coating a, spraying the coating a on the surface of a perfluororubber product, and heating the perfluororubber product in an oven at 340 ℃ for 10min to obtain a perfluororubber product with a pretreated surface;
s4, two-step surface treatment: immersing the surface-pretreated perfluororubber product in PTFE emulsion for 20s, and heating the immersed perfluororubber product in an oven at 340 ℃ for 10min to obtain the perfluororubber product with non-adhesive surface.
The manufacturer of the nitrile group-containing perfluororubber raw rubber in S1 is FFKM1 of 3M company in the United states, and the model is PFE-131TZ.
The bis-aminophenol vulcanizing agent in the S1 is 2, 2-bis (3-amino-4-hydroxyphenyl) -hexafluoropropane, and the CAS number is 83558-87-6.
And the manufacturer and model of the PTFE emulsion adopted in the step S3 are Sanyi Fu FR303A.
The manufacturer and model of the aqueous dispersion of the polyamide-imide adopted in the step S3 are quark new material SI-308.
And the manufacturer and model of the PTFE emulsion adopted in the S4 are Sanyi Fu FR303A.
In the one-step surface treatment process in the step S3, the spraying amount of the coating a is 100g/m 2 。
Example 5
A method for preparing a perfluororubber article having a surface non-tackiness, comprising the steps of:
s1, preparing a perfluororubber product: mixing 1g of a bisaminophenol vulcanizing agent and 100g of nitrile group-containing perfluoro rubber raw rubber on an open mill to obtain a rubber compound; heating the rubber compound at 170 ℃ for 15min, and simultaneously, carrying out primary mould pressing vulcanization under the pressure of 5MPa to obtain vulcanized rubber a; heating vulcanized rubber a to 290 ℃ for 20 hours for secondary vulcanization to obtain a perfluorinated rubber product;
s2, surface treatment: carrying out surface roughening treatment on the surface of a perfluororubber product by adopting methods such as sand blasting, rough grinding, water grinding and the like, brushing off particles remained on the surface, degreasing by adopting acetone, and carrying out surface treatment in the step S2, wherein the surface roughness Ra of the perfluororubber product is more than 5 mu m;
s3, one-step surface treatment: uniformly mixing 100g of PTFE emulsion and 1g of polyamide-imide aqueous dispersion to obtain a coating a, spraying the coating a on the surface of a perfluororubber product, and heating the perfluororubber product in an oven at 340 ℃ for 10min to obtain a perfluororubber product with a pretreated surface;
s4, two-step surface treatment: immersing the surface-pretreated perfluororubber product in PTFE emulsion for 20s, and heating the immersed perfluororubber product in a baking oven at 360 ℃ for 10min to obtain the perfluororubber product with non-adhesive surface.
The manufacturer of the nitrile group-containing perfluororubber raw rubber in S1 is FFKM1 of 3M company in the United states, and the model is PFE-131TZ.
The bis-aminophenol vulcanizing agent in the S1 is 2, 2-bis (3-amino-4-hydroxyphenyl) -hexafluoropropane, and the CAS number is 83558-87-6.
And the manufacturer and model of the PTFE emulsion adopted in the step S3 are Sanyi Fu FR303A.
The manufacturer and model of the aqueous dispersion of the polyamide-imide adopted in the step S3 are quark new material SI-308.
And the manufacturer and model of the PTFE emulsion adopted in the S4 are Sanyi Fu FR303A.
In the one-step surface treatment process in the step S3, the spraying amount of the coating a is 100g/m 2 。
Performance testing
1. Coating fastness test:
10 pieces of the surface non-adhesive perfluororubber products prepared in examples 1-5 were placed in 100g of deionized water, boiled in water at normal pressure and 100 ℃ for 1 hour, then treated by ultrasonic waves at 70 ℃ for 15 minutes, and the particles in the deionized water were detected, filtered by a coarse sieve, dried, and the quality and the dropping condition of the solid dropping substances were tested, the maximum value and the minimum value were removed, and the average value was taken, and the test results are shown in Table 1.
The perfluororubber product is a perfluororubber sealing piece, the shape and structure of the perfluororubber product are O-shaped rings, and the shape of the O-shaped rings is shown in figure 1.
It can be seen from FIG. 2 that the surface-treated layer of the surface-non-tacky perfluororubber article prepared in example 2 was peeled off.
2. And (3) testing the adhesion:
according to the coating fastness test result, the perfluororubber products prepared in the examples without dropping solid substances are tested, specifically 10 pieces of the perfluororubber products with the surface non-tackiness prepared in the examples 1, 3 and 5 are placed in a 304 stainless steel test die with the roughness not more than 1.0 mu m, the fastening nut is screwed down to enable the deformation of the perfluororubber product (O-shaped ring) to be 25%, the perfluororubber product is taken out after being placed at 204 ℃ for 24 hours, the perfluororubber product is cooled to room temperature first, the minimum stretching force required by pulling the O-shaped ring from the die between the stainless steels is measured by a stretching tester for 3 hours, the stretching speed is 1mm/s, the measured viscosity value of the O-shaped ring under the condition is taken out, the maximum value and the minimum value are removed, the average value is taken, and the test result is shown in table 1.
3. Plasma resistance test
Using different plasma treatment gases (O 2 Carbon tetrafluoride CF 4 、O 2 And CF (compact flash) 4 Is a blend (O) having a volume ratio of 1:1 2 /CF 4 ) Testing the mass loss rate, O, of the perfluororubber products with surface non-tackiness prepared in examples 1 to 5 after 60 minutes at a temperature of 100℃and a power of 800w 2 、O 2 And CF (compact flash) 4 The vacuum set for testing the blend with the volume ratio of 1:1 as plasma processing gas was 15mtorr, CF 4 The vacuum degree at the time of the test as the plasma processing gas was 40mtorr; the gas flow rates of the plasma processing gases were all set to 80sccm; 10 pieces of the perfluororubber products having surface tackiness obtained in examples 1 to 5 were each removed from the products, and the maximum value and the minimum value were averaged to obtain the test results shown in Table 1.
TABLE 1
Claims (4)
1. A method for preparing a perfluororubber product having a non-tacky surface, comprising the steps of:
s1, preparing a perfluororubber product: mixing the raw perfluororubber with a vulcanizing agent to obtain a rubber compound; vulcanizing the rubber compound at high temperature to obtain a perfluorinated rubber product;
s2, surface treatment: surface roughening and degreasing treatment are carried out on the perfluorinated rubber product;
s3, one-step surface treatment: FEP emulsion, aqueous dispersion of polyether sulfone and SiO 2 Uniformly mixing to obtain a coating a, spraying or dipping the coating a on the surface of the perfluororubber product, and heating to obtain the perfluororubber product with the pretreated surface;
s4, two-step surface treatment: spraying or dipping non-adhesive coating a on the surface of the perfluorinated rubber product subjected to surface pretreatment, and heating to obtain the perfluorinated rubber product with the surface non-adhesive property;
the surface roughness Ra of the perfluororubber product after the surface rough treatment of the perfluororubber product in the step S2 is larger than 5 mu m;
the temperature of the heating in the step S4 is set to be lower than 360 ℃;
the preparation raw material of the non-adhesive coating a is fluororesin with the melting point of 250-350 ℃, and the non-adhesive coating a is in a powder state or an emulsion state; the fluororesin is tetrafluoroethylene hexafluoropropylene copolymer.
2. The method for producing a perfluororubber article having a surface non-tackiness according to claim 1, wherein the vulcanizing agent comprises one or a combination of two of an organometallic compound and an amino-containing organic compound.
3. The method for producing a perfluororubber article having a surface non-tackiness according to claim 1, wherein the heating temperature in said S4 is 10-60 ℃ higher than the melting point of the resin material contained in the non-tackiness coating material a.
4. The method for producing a perfluororubber article having a surface non-tackiness according to claim 3, wherein the heating temperature in said S4 is 20-50 ℃ higher than the melting point of the resin material contained in the non-tackiness coating material a.
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