CN116239924B - Electronic grade protective agent - Google Patents
Electronic grade protective agent Download PDFInfo
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- CN116239924B CN116239924B CN202211406840.9A CN202211406840A CN116239924B CN 116239924 B CN116239924 B CN 116239924B CN 202211406840 A CN202211406840 A CN 202211406840A CN 116239924 B CN116239924 B CN 116239924B
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- perfluoropolyether
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- 239000003223 protective agent Substances 0.000 title claims abstract description 47
- 239000000178 monomer Substances 0.000 claims abstract description 72
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 36
- 239000010702 perfluoropolyether Substances 0.000 claims abstract description 33
- 229920002313 fluoropolymer Polymers 0.000 claims abstract description 31
- 239000004811 fluoropolymer Substances 0.000 claims abstract description 31
- 125000003709 fluoroalkyl group Chemical group 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 28
- 239000011737 fluorine Substances 0.000 claims description 28
- 229920000642 polymer Polymers 0.000 claims description 9
- 150000002221 fluorine Chemical class 0.000 claims description 8
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 6
- -1 HFE-7100 Chemical compound 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- NOPJRYAFUXTDLX-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-methoxypropane Chemical compound COC(F)(F)C(F)(F)C(F)(F)F NOPJRYAFUXTDLX-UHFFFAOYSA-N 0.000 claims description 5
- DFUYAWQUODQGFF-UHFFFAOYSA-N 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane Chemical compound CCOC(F)(F)C(F)(F)C(F)(F)C(F)(F)F DFUYAWQUODQGFF-UHFFFAOYSA-N 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 3
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 claims description 3
- 229940119545 isobornyl methacrylate Drugs 0.000 claims description 3
- 239000003269 fluorescent indicator Substances 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 20
- 238000005260 corrosion Methods 0.000 abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 9
- 239000003921 oil Substances 0.000 abstract description 8
- 208000015181 infectious disease Diseases 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 238000012423 maintenance Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 16
- 239000010410 layer Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000011253 protective coating Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 125000000565 sulfonamide group Chemical group 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000011241 protective layer Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- 239000002344 surface layer Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
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- 239000000428 dust Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000005250 alkyl acrylate group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to the technical field of electronic component protection, and discloses an electronic grade protective agent, wherein the protective agent comprises a fluoropolymer and a volatile solvent, raw materials of the fluoropolymer comprise fluoromonomers and unsaturated non-fluoromonomers, and the fluoromonomers comprise perfluoropolyether monomers 1 and fluoroalkyl monomers 2; the perfluoropolyether monomer 1 has a structure shown as a structural formula (I), PFPE is a perfluoropolyether group, n is 1 or 2, m is not less than 1 and not more than 3, k is not less than 1 and not more than 12, and R 1 Selected from H, CH 3 Or CH (CH) 2 CH 3 ，R 2 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 The method comprises the steps of carrying out a first treatment on the surface of the The fluoroalkyl monomer 2 has a structure shown in a structural formula (II), rf is linear perfluoroalkyl, the carbon number of the perfluoroalkyl is not higher than 6, and R 3 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 ，R 4 Is CH 3 Or CH (CH) 2 CH 3 . The electronic protective agent has excellent water and oil repellency and corrosion resistance, and can effectively prevent the protected product from being damaged under the conditions of severe environment, water vapor infection, chemical corrosion and the like in production and use; in addition, the electronic protective agent can realize maintenance repainting.
Description
Technical Field
The invention relates to the technical field of electronic component protection, in particular to an electronic grade protective agent.
Background
Printed circuit boards (PCBs for short) are the most important components in contemporary high-end devices. The PCB is damaged by various environments during the manufacturing and using processes, such as dust and chip damage during the manufacturing process, cold and hot alternation, corrosion damage such as acid rain, salt fog, etc., and corrosion and short circuit, etc. are easily generated by unprotected precision electronic devices, so that the electrical system is paralyzed, and serious loss is caused. For example, the offshore wind power generation equipment is damaged by the ocean salt fog environment throughout the year, and the intelligent watch and the wireless earphone are corroded by sweat, water stain and the like in wearing, and the security and outdoor monitoring equipment is polluted by rain water, dust and the like for a long time.
With the rapid development of domestic communication and new energy technologies, domestic and civil electronic products (terminal products, base stations, servers and the like), automobile electronics, security protection and other electronic industries have higher and higher requirements on service life. Currently, PCBs are often extended in service life with a surface protective coating, a so-called "tri-proof paint". Conventional three-proofing coatings such as polyurethane, silicone and epoxy resin are relatively low in equivalent grid, but the coating thickness is generally more than 20-50 um or even higher, the overall cost is increased, and the three-proofing coatings do not conform to the high-end trend of light weight and miniaturization of modern electronic components, and in addition, the heat dissipation of the coatings becomes a great pain point of an integrated circuit, so that the three-proofing coatings gradually become histories. While protective coatings of fluorine-containing resins have received great attention in recent years, they have good electrical barrier properties, water-and oil-repellency, and excellent corrosion resistance. And the fluorinated acrylic protective coating has the fastest growing and successful application.
Patent application CN 110922526A discloses a fluoropolymer and a protective coating agent comprising the fluoropolymer. The polymerized monomers of the fluoropolymer include: perfluoroalkyl acrylate monomers, trifunctional acrylate monomers containing siloxane structures, alkyl acrylate monomers, and acrylate monomers containing aliphatic or aromatic rings. The fluoropolymer has a dendritic space network structure, hydrogen bond interaction can occur between amide bonds in molecules, and the introduction of a benzene ring or an alicyclic structure enables the surface of the polymer film to form a unique protective layer with the amide bonds and rigid benzene rings or alicyclic rings. The protective coating agent containing the fluoropolymer has stronger adhesive force and higher hardness, and simultaneously has excellent water and oil resistance and acid and alkali resistance. However, it belongs to a three-dimensional cross-linked structure, can be hardly reworked, and has very high use cost. Moreover, the storage conditions are very harsh, the crosslinking solidification is caused to fail in the environment of trace water and oxygen, and the corrosion resistance of the composite material is still to be improved.
Patent application CN 109897493A discloses a three-proofing paint and a preparation method thereof, wherein the three-proofing paint takes a fluorine polymer with perfluoroalkyl groups with 4-10 carbon atoms as a main component, takes a fluorine-containing solvent as a solvent, and can form a film without baking and ultraviolet curing on the premise of having good waterproof, oil-proof and antifouling performances and having no influence on the appearance of products. Although the micro-nano ultra-thin coating does not influence the heat dissipation condition in the operation of the circuit board, the corrosion resistance is only 48h, the increasingly harsh use environment cannot be met, the perfluoroalkyl monomer exceeding C8 is used, the thermal insulation coating is not easy to degrade and migrate, and the thermal insulation coating is phased out in use in the global scope.
From the prior art, the existing protective coating agent has harsh storage conditions (such as strictly controlling air, moisture and the like), poor environmental protection and safety, and cannot meet more severe performance requirements, especially service life and safety in outdoor and severe environments.
Disclosure of Invention
The invention aims to solve the problems of hydrophobic and oleophobic properties, corrosion resistance and poor heat dissipation of a protective coating agent in the prior art, and particularly the problems of short service life and poor safety in outdoor and severe environments.
In order to achieve the above object, the present invention provides an electronic grade protective agent comprising a fluoropolymer and a volatile solvent, wherein a raw material of the fluoropolymer comprises an unsaturated fluoromonomer and an unsaturated non-fluoromonomer,
the unsaturated fluorine monomer contains a perfluoropolyether-based monomer 1 and a fluoroalkyl monomer 2;
the perfluoropolyether monomer 1 has a structure shown in a structural formula (I):
in the formula (I), PFPE is a perfluoropolyether group, n is 1 or 2, m is not less than 1 and not more than 3, k is not less than 1 and not more than 12, m and k are integers, R 1 Selected from H, CH 3 Or CH (CH) 2 CH 3 ，R 2 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 ；
The fluoroalkyl monomer 2 has a structure as shown in a structural formula (II):
in the formula (II), rf is a linear perfluoroalkyl group having not more than 6 carbon atoms, R 3 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 ，R 4 Is CH 3 Or CH (CH) 2 CH 3 。
Preferably, the fluoropolymer is present in an amount of 2 to 15wt% based on the total weight of the electronic grade protectant.
Preferably, the weight average molecular weight of the fluoropolymer is 8000 to 500000.
Preferably, the perfluoropolyether group in formula (I) is Z-type, Y-type, K-type or D-type.
Preferably, the number average molecular weight of the perfluoropolyether groups in formula (I) is 500 to 2500.
Preferably, the weight ratio of the perfluoropolyether monomer 1 to the fluoroalkyl monomer 2 is 0.5-4: 1.
preferably, the unsaturated non-fluorine monomer is selected from one or more of methyl acrylate, methyl methacrylate, n-butyl acrylate, n-butyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, vinyl acetate and styrene.
Preferably, the content of the unsaturated non-fluorine monomer is 1 to 30wt% based on the total weight of the unsaturated fluorine monomer and the unsaturated non-fluorine monomer.
Preferably, the volatile solvent is selected from one or more of HFE-7200, HFE-7100, HFE-347, HFE-458, HFE-374 and HFE-356 mec.
Preferably, the electron protecting agent further comprises an auxiliary agent, and the auxiliary agent is one or more than two of a leveling agent, a defoaming agent and a fluorescence indicator.
The invention has the advantages and beneficial effects that:
(1) The protective coating formed by the electronic protective agent provided by the invention has excellent water and oil repellency; particularly, the waterproof and oil-proof performance is excellent in use, and the safe operation of components can be protected;
(2) The protective coating formed by the electronic protective agent has super-strong corrosion resistance; the protective effect on components in the open air or special environment is obvious, such as salt fog resistance, chemical infection resistance and the like;
(3) The electronic protective agent has protective performance at the micro-nano level and good heat dissipation effect;
(4) The electronic protective agent has good film forming performance, can adapt to various film forming processes, and can form a uniform protective layer by brushing, dipping, spraying and dipping;
(5) The electronic protective agent is environment-friendly and repairable, accords with the development trend of modern novel industry, and reduces the cost of replacing components due to damage of protective layers.
Drawings
FIG. 1 is a schematic illustration of the protective principle of one embodiment of an electron protective agent provided by the present invention;
FIG. 2 is a schematic diagram of an ICP-B-24 type circuit board in test example 1 of the present invention;
fig. 3 is a schematic diagram of an alarm control system of the electric bicycle in test example 2 of the present invention.
Description of the reference numerals
A substrate 1; a bottom layer 2; an intermediate layer 3; a surface layer 4; an alarm 5; a circuit board 6; a remote control 7.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides an electronic grade protective agent, which comprises a fluorine polymer and a volatile solvent, wherein the raw material of the fluorine polymer comprises an unsaturated fluorine monomer and an unsaturated non-fluorine monomer,
the unsaturated fluorine monomer contains a perfluoropolyether-based monomer 1 and a fluoroalkyl monomer 2;
the perfluoropolyether monomer 1 has a structure shown in a structural formula (I):
the fluoroalkyl monomer 2 has a structure as shown in a structural formula (II):
in the present invention, the fluoropolymer is obtained by copolymerizing an unsaturated fluoromonomer and an unsaturated non-fluoromonomer.
In the present invention, in formula (I), PFPE is a perfluoropolyether group. The perfluoropolyether monomer 1 has long-chain perfluoropolyether groups, has low surface tension, protrudes towards air in the film forming process, and is fixed in position and curled and contracted along with volatilization of volatile substances to form nanometer microprotrusions, so that the film has super-strong water and oil repellency. In a preferred embodiment, the perfluoropolyether group in formula (I) is Z-type, Y-type, K-type or D-type.
In a preferred embodiment, the perfluoropolyether groups in formula (I) have a number average molecular weight of 500 to 2500.
Specifically, the perfluoropolyether monomer 1 is formed by bonding a perfluoropolyether group and an acrylic ester group part through a hard connecting part, wherein the hard connecting part is formed by a single or a plurality of benzene rings and a sulfonamide group with stronger polarity, and the two groups are connected through straight-chain alkylene groups, and a certain distance is kept, so that the hardening function of the benzene ring part and the performance enhancement of polymer crystallization can be enhanced, and the sulfonamide group part cooperates with the sulfonamide part of the fluoroalkyl monomer 2 to further promote the crystallization of a side chain, so that a surface layer with quite hardness and regular and tight connection of the side chain is formed after the polymer is formed, and the performances of corrosion resistance, hydrophobicity, oleophobicity and the like are improved. Preferably, in formula (I), n is 1 or 2, 1.ltoreq.m.ltoreq.3, 1.ltoreq.k.ltoreq.12, m and k are integers, R 1 Selected from H, CH 3 Or CH (CH) 2 CH 3 ，R 2 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 。
In the present invention, in formula (II), rf is a linear perfluoroalkyl group. That is, the fluoroalkyl monomer 2 is composed of a sulfonamide group connecting a fluoroalkyl group with an acrylate group moiety. The linear fluoroalkyl side chain can improve the surface fluorine content of the fluoropolymer after film formation, plays a supporting role, and synergistically increases a certain hardness, and the sulfonamide group part and the sulfonamide group of the perfluoropolyether monomer 1 synergistically promote side chain crystallization, so that the performance of a film layer can be improved. Preferably, the perfluoroalkyl group has no bioaccumulation or migration of 6 or less carbon atoms, R 3 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 ，R 4 Is CH 3 Or CH (CH) 2 CH 3 。
In a further preferred embodiment, the weight ratio of the perfluoropolyether monomer 1 to the fluoroalkyl monomer 2 is 0.5 to 4:1, in particular, may be, for example, 0.5:1, 0.8:1, 1:1, 1.5:1, 1.8:1, 2:1, 3:1 or 4:1. It will be appreciated that in the present invention, the starting materials are almost lossless, and therefore, in the fluoropolymer shown, the weight ratio of the perfluoropolyether monomer 1 to the fluoroalkyl monomer 2 is also 0.5 to 4:1.
the present invention is not limited to a specific preparation method of the fluoropolymer, and may be solution copolymerization and emulsion copolymerization which are conventional in the art. In a specific embodiment of the present invention, taking solution polymerization as an example, the preparation method of the fluoropolymer includes the following steps: adding the perfluoropolyether monomer 1, the fluoroalkyl monomer 2 and the non-fluorine monomer into a jacketed kettle with a stirrer, a reflux condenser and a thermometer according to weight proportion, adding a first solvent and an initiator, replacing with nitrogen until the water content is less than or equal to 20ppm, heating to the reaction temperature (60-90 ℃) after sealing, and keeping for a specified reaction time (3-12 hours) to obtain a fluoropolymer solution with certain solid content. Wherein the first solvent is one or more of HFE-7200, HFE-7100, HFE-347, HFE-458, HFE-374 and HFE-356 mec. It will be appreciated that the specific amounts of the first solvent and initiator added, the specific reaction temperature and reaction time may be determined by the amounts and specific choices of the perfluoropolyether monomer 1, fluoroalkyl monomer 2 and non-fluorine monomer, as long as they are allowed to react completely.
When the electronic grade protective agent is used for protecting products (such as components), the electronic grade protective agent can form a protective thin layer on the surface of the protected products, and has excellent water, oil and corrosion resistance. Specifically, the electronic protective agent is suitable for protecting medium-high-end electronic and electric components of smart phones, hearing aids, wireless headphones, smart watches, laptops, notebook computers, tablet phones and Personal Digital Assistants (PDAs); meanwhile, the electronic protective agent can be used for protecting a substrate which is generally required, wherein the substrate can be silicate-containing materials such as glass, marble and the like or metal surface materials such as copper, iron, aluminum, titanium and the like; it can also be used for protecting polymer materials such as plastics, rubber, etc.
Referring to fig. 1 in combination, in one embodiment, an electron protecting agent is used for protecting a substrate 1, after the substrate 1 is formed into a film, the electron protecting agent can form a three-layer structure with similar phase separation under the synergistic effect of each component, a surface layer 4 is a curled micro-convex structure of a perfluoropolyether end, a middle layer 3 is composed of a crystallization area promoted by sulfonamide groups and a hard area with multiple benzene rings, and a bottom layer 2 is an adhesion layer containing an acrylate main chain, namely a bottom layer. In this way, the surface layer 4 of the fluorine-containing portion of the overall layer system exhibits excellent water-and oil-repellency and corrosion resistance outwards, while the intermediate layer 3 of the crystalline and hard portion increases the compactness and hardness, and increases the resistance to mechanical damage; the bottom layer 2, due to the self-delamination effect, is an acrylate backbone with low fluorine content, improving adhesion and flow thixotropy.
When the fluoropolymer in the electronic-grade protective agent is too small, the thickness of the formed protective coating is too small, even a large substrate is exposed, the protective performance is insufficient, or the secondary film forming process is required to be complex and the cost is increased; when the amount of fluoropolymer in the electron protecting agent is excessive, an automated process is not facilitated and waste is easily caused. In a preferred embodiment, the fluoropolymer is present in an amount of 2 to 15wt% based on the total weight of the electronic grade protectant, from the standpoint of both cost and process of use. It is understood that when the electron protecting agent contains only the fluoropolymer and the volatile solvent, the volatile solvent is contained in an amount of 85 to 98wt%.
When the molecular weight of the fluoropolymer is too small, the film forming property is poor and even a film structure cannot be formed; when the molecular weight is too large, the compatibility is poor, even precipitation occurs, the system is unstable, and film formation is impossible. In a preferred embodiment, the fluoropolymer has a weight average molecular weight of 8000 to 500000, and thus has good film forming properties.
The present invention is not limited to a specific kind of the volatile solvent, as long as it can sufficiently dissolve the fluoropolymer without affecting film formation requirements, and in a specific embodiment, the volatile solvent is a hydrofluoroether solvent, preferably one or more of HFE-7200, HFE-7100, HFE-347, HFE-458, HFE-374 and HFE-356 mec. The volatile solvent is more preferably one or two or more of HFE-7200, HFE-7100 and HFE-347 from the viewpoint of the annual increase in VOC demand and the influence on the atmosphere.
In a preferred embodiment, the unsaturated non-fluorine monomer is one or more selected from the group consisting of methyl acrylate, methyl methacrylate, n-butyl acrylate, n-butyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, vinyl acetate, and styrene. By adding the unsaturated non-fluorine monomer, on one hand, the industrialization cost can be reduced, and on the other hand, the film forming property, the flow thixotropy and the adhesiveness of the fluoropolymer to a substrate are improved.
When the unsaturated non-fluorine monomer is excessive, the hydrophobic and oleophobic performance of the electronic protective agent is affected, and the crystallinity of a polymer side chain is also affected, so that the surface layer is not compact enough and the performance is reduced; if the unsaturated non-fluorine monomer is too little, the effect of reducing the cost and enhancing the efficiency cannot be achieved. In a preferred embodiment, the unsaturated non-fluorine monomer is contained in an amount of 1 to 30% by weight based on the total weight of the unsaturated fluorine monomer and the unsaturated non-fluorine monomer, in view of the combination of the barrier property and the cost. That is, the content of the unsaturated non-fluorine monomer in the fluoropolymer is 1 to 30wt%, more preferably 10 to 15wt%, so that the electron protecting agent is low in cost and excellent in protecting performance.
In a preferred embodiment, the electronic grade protectant further comprises an adjunct. The present invention is not limited to the specific kind of the auxiliary agent, and may be added according to actual needs, as long as the auxiliary agent used is sufficiently compatible with the mixed liquid formed by the fluoropolymer and the volatile solvent. In a specific embodiment, the auxiliary agent is selected from one or more of a leveling agent, an antifoaming agent and a fluorescence indicator.
In one embodiment, the preparation method of the electronic protective agent comprises the following steps: the fluoropolymer solution, volatile solvent and optionally auxiliary agent are mixed to obtain the electronic protective agent.
The electronic-grade protective agent provided by the invention has excellent water and oil repellency, corrosion resistance, good adhesive force and high mechanical damage resistance, and can effectively prevent the protected product from being damaged in severe environments, water vapor infection, chemical corrosion and other environments, thereby prolonging the service life of the protected product.
In addition, the protective layer formed on the product by the existing protective agent is difficult to remove, so that when part of the protective layer is damaged, the protective layer can hardly be repaired, and the use cost is high; the electronic protective agent provided by the invention can realize repair repainting and repair, and reduces the use cost.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto. The experimental materials used in the examples described below were purchased from biochemical reagent stores unless otherwise specified.
In the following examples, the preparation method of the electron protecting agent comprises the following steps:
and adding a volatile solvent into the fluoropolymer solution, and uniformly mixing to obtain the electronic grade protective agent.
The compositions of the perfluoropolyether-based monomer 1 and the fluoroalkyl monomer 2 in examples and comparative examples are shown in tables 1 and 2.
TABLE 1 composition of perfluoropolyether monomer 1
TABLE 2 composition of fluoroalkyl monomers 2
| Fluoroalkyl monomer 2 | Number of C atoms of Rf | R 3 | R 4 |
| F-1 | 1 | Cl | CH3 |
| F-2 | 6 | CH 3 | CH 2 CH 3 |
| F-3 | 4 | CH 3 | CH 3 |
| F-4 | 3 | CH 2 CH 3 | CH 3 |
The compositions of the electron protecting agent and the fluoropolymer in the examples and comparative examples are shown in Table 3, and the contents and proportions in Table 3 are by weight.
TABLE 3 Table 3
Test example 1 physicochemical Property test
1. Preparing a physical and chemical property test sample:
(1) The electron protecting agents of examples 1 to 9 and comparative examples 1 to 3 were prepared according to the above-described methods and compositions and components described in tables 1 to 3 for use;
(2) The ICP-B-24 type circuit board (figure 2) is cleaned by acetone, cleaned and dried by HFE-7100, and then the circuit board is immersed in the electronic protective agent and dried at room temperature to prepare a sample for standby.
2. The testing method comprises the following steps:
(1) Hydrophobicity: a dynamic contact angle measuring instrument of JC2000D1 in the Shanghai, which measures the static contact angle of water with respect to a droplet volume of 2 μl;
(2) Oleophobic: a dynamic contact angle measuring instrument of Shanghai morning JC2000D1, which measures the static contact angle of n-hexadecane with respect to the liquid drop volume of 2 mu L;
(3) Resistance to brine corrosion: simulating the durability of an offshore environment according to a neutral brine spray test GB/T2423.17-2008 standard; the appearance of the swatches was evaluated according to the following criteria: almost no change of the sample wafer is 'none', 1 to 10 percent of the corrosion point or surface of the sample wafer reaches the whole sample plate area is "+", and more than 10 percent is "++";
(4) Chemical resistance: simulating the corrosion process of accelerating outdoor acid rain by using 5% HCl solution, immersing a test sample into a closed glass container filled with 5% HCl solution for 4 hours, cleaning with clear water, drying at room temperature for 4 hours, taking the cleaned sample as a cycle, and repeating the cycle for 50 times; the appearance of the swatches was evaluated according to the following criteria: the sample piece corrosion points or surfaces reach more than 10% of the whole sample plate area and do not pass through, and less than 10% pass through;
3. the prepared sample was subjected to the above performance test, and the test results are shown in table 4.
TABLE 4 Table 4
As can be seen from Table 4, the electron protectants prepared in examples 1-9 of the invention have excellent hydrophobicity, oleophobicity and corrosion resistance.
In contrast, in comparative example 1, compared with example 2, the electron protectant prepared without adding perfluoropolyether monomer 1 has significantly reduced water contact angle and oil contact angle, and reduced salt spray resistance and chemical resistance.
Comparative example 2 the electronic protective agent produced without addition of fluoroalkyl monomer 2 has reduced salt spray resistance and chemical resistance compared with example 2.
Comparative example 3 was inferior to example 2 in salt spray resistance and chemical resistance of the electron protecting agent prepared without adding a non-fluorine monomer.
Test example 2 running Performance test
1. Preparation of a running performance test template:
(1) The electron protecting agents of examples 1 to 9 and comparative examples 1 to 3 were prepared according to the above-described methods and compositions and components described in tables 1 to 3 for use;
(2) Taking an alarm control system (figure 3) of a certain domestic electric bicycle as an electrified operation test article, cleaning a circuit board of a connector by acetone, cleaning and drying by HFE-7100, immersing the circuit board 6 in the prepared electronic protective agent, airing at room temperature, and communicating the circuit to prepare a test template for later use;
2. the testing method comprises the following steps:
immersing the test sample plate of the communication circuit into 5% saline water for 24 hours, pressing a remote controller switch, and taking the alarm lamp to light and make a sound as test passing, wherein the alarm lamp is not light or does not make a sound and is regarded as not passing.
3. The test results are shown in Table 5.
TABLE 5
| Project | Run for 24h results |
| Example 1 | By passing through |
| Example 2 | By passing through |
| Example 3 | By passing through |
| Example 4 | By passing through |
| Example 5 | By passing through |
| Example 6 | By passing through |
| Example 7 | By passing through |
| Example 8 | By passing through |
| Example 9 | By passing through |
| Comparative example 1 | Not pass through |
| Comparative example 2 | Not pass through |
| Comparative example 3 | Not pass through |
As can be seen from the results of Table 5, the electronic protectants prepared in examples 1-9 exhibited better performance than those prepared in comparative examples 1-3, indicating that the electronic protectants provided by the invention are capable of protecting the protected product from adverse environmental effects or damage.
In conclusion, the electronic protective agent provided by the invention has excellent water and oil repellency and corrosion resistance, and can prevent the protected product from being damaged by severe environment; furthermore, the components in the electron protecting agent have necessary synergism, and the lack of any one of the components can lead to a great reduction in performance.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (7)
1. An electronic grade protective agent, which is characterized in that the protective agent contains a fluorine polymer and a volatile solvent, wherein the raw material of the fluorine polymer contains an unsaturated fluorine monomer and an unsaturated non-fluorine monomer,
the unsaturated fluorine monomer contains a perfluoropolyether-based monomer 1 and a fluoroalkyl monomer 2;
the perfluoropolyether monomer 1 has a structure shown in a structural formula (I):
（Ⅰ）
in the formula (I), PFPE is a perfluoropolyether group, n is 1 or 2, m is not less than 1 and not more than 3, k is not less than 1 and not more than 12, m and k are integers, R 1 Selected from H, CH 3 Or CH (CH) 2 CH 3 ，R 2 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 ；
The fluoroalkyl monomer 2 has a structure as shown in a structural formula (II):
（Ⅱ）
in the formula (II), rf is a linear perfluoroalkyl group having not more than 6 carbon atoms, R 3 Selected from H, cl, F, CH 3 Or CH (CH) 2 CH 3 ，R 4 Is CH 3 Or CH (CH) 2 CH 3 ；
Wherein, the content of the fluorine polymer is 2-15wt% based on the total weight of the electronic grade protective agent;
the content of the unsaturated non-fluorine monomer is 1-30wt% based on the total weight of the unsaturated fluorine monomer and the unsaturated non-fluorine monomer;
the weight average molecular weight of the fluoropolymer is 8000-500000.
2. The electronic grade protectant of claim 1, wherein the perfluoropolyether group of formula (i) is in the Z-, Y-, K-, or D-form.
3. The electronic grade protectant of claim 1, wherein the perfluoropolyether group of formula (i) has a number average molecular weight of 500 to 2500.
4. The electronic grade protective agent according to claim 1, wherein the weight ratio of the perfluoropolyether-based monomer 1 to the fluoroalkyl-based monomer 2 is 0.5 to 4:1.
5. the electronic grade protectant of claim 1, wherein said unsaturated non-fluorinated monomer is selected from one or more of methyl acrylate, methyl methacrylate, n-butyl acrylate, n-butyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, vinyl acetate, and styrene.
6. The electronic grade protectant of claim 1, wherein said volatile solvent is selected from one or more of HFE-7200, HFE-7100, HFE-347, HFE-458, HFE-374, and HFE-356 mec.
7. The electronic grade protectant of claim 1, further comprising an auxiliary agent selected from one or more of a leveling agent, an antifoaming agent, and a fluorescent indicator.
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