CN117903685A - Environment-friendly polyimide insulating paint and preparation method and application thereof - Google Patents
Environment-friendly polyimide insulating paint and preparation method and application thereof Download PDFInfo
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- CN117903685A CN117903685A CN202410035837.3A CN202410035837A CN117903685A CN 117903685 A CN117903685 A CN 117903685A CN 202410035837 A CN202410035837 A CN 202410035837A CN 117903685 A CN117903685 A CN 117903685A
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- CN
- China
- Prior art keywords
- dianhydride
- polyimide insulating
- polyimide
- diamine
- insulating paint
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Links
- 229920001721 polyimide Polymers 0.000 title claims abstract description 80
- 239000004642 Polyimide Substances 0.000 title claims abstract description 76
- 239000003973 paint Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 38
- 150000004985 diamines Chemical class 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 15
- 239000002966 varnish Substances 0.000 claims description 15
- -1 biphenyl tetracarboxylic anhydride Chemical class 0.000 claims description 13
- 239000000945 filler Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 5
- 150000005690 diesters Chemical class 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 125000005591 trimellitate group Chemical group 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 claims description 4
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 3
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 3
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 3
- CFTXGNJIXHFHTH-UHFFFAOYSA-N bis(4-aminophenyl) benzene-1,4-dicarboxylate Chemical compound C1=CC(N)=CC=C1OC(=O)C1=CC=C(C(=O)OC=2C=CC(N)=CC=2)C=C1 CFTXGNJIXHFHTH-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 claims description 3
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 3
- FCGXLCNBWYIEAA-UHFFFAOYSA-N 1,3-benzothiazol-6-ylmethanamine Chemical compound NCC1=CC=C2N=CSC2=C1 FCGXLCNBWYIEAA-UHFFFAOYSA-N 0.000 claims description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 2
- STCBUTTVBMCYJL-UHFFFAOYSA-N 3-[2-carboxyethyl(methyl)phosphoryl]propanoic acid Chemical compound OC(=O)CCP(=O)(C)CCC(O)=O STCBUTTVBMCYJL-UHFFFAOYSA-N 0.000 claims description 2
- DKKYOQYISDAQER-UHFFFAOYSA-N 3-[3-(3-aminophenoxy)phenoxy]aniline Chemical compound NC1=CC=CC(OC=2C=C(OC=3C=C(N)C=CC=3)C=CC=2)=C1 DKKYOQYISDAQER-UHFFFAOYSA-N 0.000 claims description 2
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 2
- WUPRYUDHUFLKFL-UHFFFAOYSA-N 4-[3-(4-aminophenoxy)phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC1=CC=CC(OC=2C=CC(N)=CC=2)=C1 WUPRYUDHUFLKFL-UHFFFAOYSA-N 0.000 claims description 2
- JCRRFJIVUPSNTA-UHFFFAOYSA-N 4-[4-(4-aminophenoxy)phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC(C=C1)=CC=C1OC1=CC=C(N)C=C1 JCRRFJIVUPSNTA-UHFFFAOYSA-N 0.000 claims description 2
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 2
- 229910052580 B4C Inorganic materials 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 claims description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- 239000003085 diluting agent Substances 0.000 claims description 2
- HPGJOUYGWKFYQW-UHFFFAOYSA-N diphenyl benzene-1,4-dicarboxylate Chemical compound C=1C=C(C(=O)OC=2C=CC=CC=2)C=CC=1C(=O)OC1=CC=CC=C1 HPGJOUYGWKFYQW-UHFFFAOYSA-N 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 125000006158 tetracarboxylic acid group Chemical group 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 230000007774 longterm Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002028 Biomass Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 210000003298 dental enamel Anatomy 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- MEJYDZQQVZJMPP-ULAWRXDQSA-N (3s,3ar,6r,6ar)-3,6-dimethoxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan Chemical compound CO[C@H]1CO[C@@H]2[C@H](OC)CO[C@@H]21 MEJYDZQQVZJMPP-ULAWRXDQSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 125000006159 dianhydride group Chemical group 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- JBFHTYHTHYHCDJ-UHFFFAOYSA-N gamma-caprolactone Chemical compound CCC1CCC(=O)O1 JBFHTYHTHYHCDJ-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- XUSNPFGLKGCWGN-UHFFFAOYSA-N 3-[4-(3-aminopropyl)piperazin-1-yl]propan-1-amine Chemical compound NCCCN1CCN(CCCN)CC1 XUSNPFGLKGCWGN-UHFFFAOYSA-N 0.000 description 1
- QQGYZOYWNCKGEK-UHFFFAOYSA-N 5-[(1,3-dioxo-2-benzofuran-5-yl)oxy]-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(OC=2C=C3C(=O)OC(C3=CC=2)=O)=C1 QQGYZOYWNCKGEK-UHFFFAOYSA-N 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- CXISKMDTEFIGTG-UHFFFAOYSA-N [4-(1,3-dioxo-2-benzofuran-5-carbonyl)oxyphenyl] 1,3-dioxo-2-benzofuran-5-carboxylate Chemical compound C1=C2C(=O)OC(=O)C2=CC(C(OC=2C=CC(OC(=O)C=3C=C4C(=O)OC(=O)C4=CC=3)=CC=2)=O)=C1 CXISKMDTEFIGTG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000004984 aromatic diamines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000003880 polar aprotic solvent Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The invention provides an environment-friendly polyimide insulating paint, a preparation method and application thereof, and relates to the field of insulating paint; the raw materials of the polyimide insulating paint adopt dianhydride and diamine with specific components, and simultaneously, the polyimide insulating paint is matched with a green biomass solvent, so that the polyimide insulating paint has excellent performance, can effectively improve the long-term exposure risk of operators in the preparation process of the polyimide insulating paint, and meets the environmental protection requirement.
Description
Technical Field
The invention relates to the field of insulating paint, in particular to an environment-friendly polyimide insulating paint and a preparation method and application thereof.
Background
Polyimide (PI) is a preferred insulating material for preparing high-performance flat wire enamelled wires, has the advantages of molecular structure and high process dispatching capability, and can improve the R angle coating uniformity of flat wires by preparing high-solid-content high-viscosity high-performance PI insulating paint.
PI insulating paints are typically prepared by reacting diamines with dianhydrides in polar aprotic solvents, the most commonly used solvents including N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), N-methylpyrrolidone (NMP), dimethylsulfoxide (DMSO), and the like, for example: the patent CN116162407A discloses a high-voltage and corona-resistant polyimide insulating paint material and a preparation method thereof, wherein the polyimide insulating paint material comprises resin and nano inorganic particles, the resin contains polyimide and/or polyamide acid structures, the resin is prepared from dianhydride and diamine, the diamine comprises silane and/or siloxane containing a diamino structure and aromatic diamine, and the mass ratio of the resin to solid in the nano inorganic particles is 99:1-50:50. The solvent is selected from one or more of DMF, DMAc, NMP, gamma-caprolactone, toluene and xylene. The polyimide insulating paint material has the advantages of excellent heat resistance, mechanical toughness, high pressure resistance and corona resistance, simple processing, excellent storage stability, high solid content and low viscosity.
As further disclosed in patent CN106336795a, the raw materials of the aromatic polyimide wire enamel include a component a and a component B, wherein the weight ratio of the component a to the component B is 1:10.5 to 17.5, wherein the component A comprises the following components: the nanometer filler, the silane coupling agent, the organic solvent and the component B comprise the following components: polyimide wire enamel, an anti-settling agent and sodium silicate, wherein the organic solvent is one or a combination of more of DMF, DMAc, NMP, DMSO, toluene and xylene. The heat level of the aromatic polyimide wire enamel provided by the invention can reach more than 260 levels, and the aromatic polyimide wire enamel can adapt to a working environment with higher temperature; other performance indexes also meet the standard requirements.
The proportion of solvents in PI insulating paint products exceeds 60%, however DMAc, DMF, NMP, DMSO solvents are toxic and are not beneficial to human health, and waste liquid generated in the production process can further cause harm to nature and environment, so that a large amount of protection and treatment resources must be input in the process of processing and using the PI insulating paint containing the solvents to reduce and avoid harm to human bodies and the environment. Therefore, it is necessary to develop a polyimide insulating varnish which is environmentally friendly, is green and economical, and has excellent properties.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides the environment-friendly polyimide insulating paint, and the preparation method and application thereof, which can effectively improve the long-term exposure risk of operators in the preparation process of the polyimide insulating paint and meet the environmental protection requirement.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The invention provides a polyimide insulating paint, which comprises dianhydride, diamine and a solvent;
The dianhydride includes one or more of p-phenyl bis (trimellitate) dianhydride (TAHQ), bisphenol a-type diether dianhydride (BPDAD), pyromellitic anhydride (PMDA), biphenyl tetracarboxylic anhydride (BPDA), diphenyl ether tetracarboxylic dianhydride (ODPA), 3', 4' -Benzophenone Tetracarboxylic Dianhydride (BTDA), bisphenol AF diester dianhydride, p-biphenylene-bis-trimellitate dianhydride, and bisphenol S diester dianhydride;
The diamine may include one or more of 4,4' -diaminodiphenyl ether (ODA), 2' -bis [4- (4-aminophenoxyphenyl) ] propane (BAPP), p-phenylene diamine (p-PDA), M-phenylene diamine (M-PDA), 1, 3-bis (3-aminophenoxy) benzene (133 APB), 1, 3-bis (4-aminophenoxy) benzene (134 APB), 1, 4-bis (4-aminophenoxy) benzene (144 APB), 4' -diamino-2, 2' -dimethylbiphenyl (M-Tolidine), 3,4' -diaminoanilide, bisphenol a diester diamine, bisphenol S diester diamine, and bis (4-aminophenyl) terephthalate.
Preferably, the dianhydride and/or diamine contains ester bonds, the proportion of the dianhydride containing ester bonds in the total dianhydride content is not less than 10mol% and/or the proportion of the diamine containing ester bonds in the total diamine content is not less than 10mol%. Here, 10mol% or more of all the dianhydrides containing an ester bond, that is, 100mol of all the dianhydrides, and/or 10mol or more of all the diamines containing an ester bond, that is, 100mol of all the diamines.
Further, the dianhydride containing an ester bond includes one or more of p-phenyl bis (trimellitate) dianhydride, bisphenol AF dianhydride, p-biphenylene-bis (trimellitate) dianhydride and bisphenol S dianhydride, and the diamine containing an ester bond includes one or more of bisphenol A diamine, bisphenol S diamine and bis (4-aminophenyl) terephthalate.
Further, the solvent includes one or more of gamma-butyrolactone (GBL), gamma-valerolactone (GVL), tamiSolve (NxG), dimethyl isosorbide (DMI), dihydro-l-glucosone (CyreneTM), water, methanol, ethanol, and isobutanol. The solvent has the characteristics of low volatility, low flammability, low toxicity, biodegradability and recycling.
Further, the polyimide insulating varnish also comprises a filler, wherein the filler comprises one or more of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon carbide, boron carbide, graphite, silicon dioxide and titanium dioxide.
Further, the polyimide insulating paint further comprises an auxiliary agent, wherein the auxiliary agent comprises one or more of a flame retardant, a plasticizer, a defoaming agent, a leveling agent, a coupling agent and a diluent. The above-mentioned auxiliary agent is preferably a bio-based auxiliary agent or a green auxiliary agent which is less harmful to the environment.
Preferably, the auxiliary agent comprises one or more of triphenylphosphine, ammonium polyphosphate, aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane, diphenyl terephthalate, bis (2-carboxyethyl) methylphosphine oxide, tricresyl phosphate, dibutyl sebacate and triphenyl phosphate.
Further, the weight average molecular weight of the polyimide insulating paint is 30000-200000g/mol, the prepolymer solid content of the polyimide insulating paint is 5-50wt% and the solvent content is 50-95wt%. The solid content of the prepolymer is specifically polyimide prepolymer mass/polyimide insulating paint mass.
Further, the molar ratio of diamine to dianhydride is 1 (0.95-1.05). Preferably 1:1.
Further, the polyimide insulating paint comprises, by weight, 5-50% of polyimide prepolymer and the balance of solvent.
Preferably, the polyimide insulating paint comprises, by weight, 5-50% of polyimide prepolymer, 40-80% of solvent, 1-10% of filler and 1-10% of auxiliary agent.
Preferably, the polyimide insulating paint comprises, by weight, 10-25% of polyimide prepolymer, 5-10% of auxiliary agent and the balance of solvent.
Further preferably, the polyimide insulating paint comprises, by weight, 10-25% of polyimide prepolymer, 1-5% of filler, 5-10% of auxiliary agent and the balance of solvent.
Further, the invention also provides a preparation method of the polyimide insulating paint, which comprises the following steps: in a solvent, diamine and dianhydride are polycondensed to obtain polyimide prepolymer, and polyimide insulating paint obtained by heating imidization is obtained.
In some specific embodiments, the preparation method of the polyimide insulating paint comprises the following steps: and (3) in a solvent, carrying out polycondensation on diamine and dianhydride to obtain polyimide prepolymer, heating and stirring, and continuously adding a filler and an auxiliary agent to obtain the polyimide insulating paint.
Further, the heating temperature is 45 ℃, and the stirring time is 12 hours.
Furthermore, the polyimide insulating paint provided by the invention or the polyimide insulating paint prepared by the preparation method can be applied to new energy automobiles.
The invention has the technical effects that:
The solvent used in the invention has the characteristics of low volatility, low flammability, low toxicity, biodegradability and cyclic utilization, and can be used together with dianhydride and diamine with specific components, so that the long-term exposure risk of operators in the preparation process of the polyimide insulating paint can be effectively improved, the environment protection requirement can be met, and the polyimide insulating paint still has excellent performance under the conditions of high temperature and high humidity.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Before the embodiments of the invention are explained in further detail, it is to be understood that the invention is not limited in its scope to the particular embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is worth noting that TamiSolve (NxG) used in the present invention is purchased from eastman, isosorbide dimethyl ether (DMI) is purchased from kandeli biotechnology limited of marchann, dihydro l-glucosone (CyreneTM) is purchased from sigma aldrich (Shanghai) trade limited, and the other raw materials are all common commercial products, so the sources thereof are not particularly limited.
Examples 1 to 8, comparative examples 1 to 4
Example 1: the preparation method of the environment-friendly polyimide insulating paint comprises the following steps:
A500 ml three-necked flask with nitrogen, stirring paddle and condenser was charged with 256.12g NxG solvent and 0.1mol of p-PDA diamine monomer, after sufficiently stirring at 45℃for dissolution, 16.01g of nano alumina was added, then 0.07mol of bisphenol AF diester dianhydride monomer and 0.03mol of BPDA dianhydride were added, after stirring for 12 hours, the viscosity was stabilized, and then 3% triphenyl phosphate, 2% aminopropyl triethoxysilane was added to prepare the insulating paint of example 1. Insulating varnishes were prepared for analytical comparison according to the synthetic method of example 1, with the formulations of examples 2 to 8 and comparative examples 1 to 4.
The performance of the prepared insulating material is evaluated, and the specific method is as follows:
(1) Viscosity of insulating paint
A small amount of insulating paint material was used to cover the test rotor and the average was taken three times using a Bruker DVPlus cone-plate viscometer.
(2) GPC test
Waters-1515-2414 gel chromatograph, test speed 1ml/min, mobile phase DMF, column temperature 35 ℃, detector 40 ℃.
(3) Method for manufacturing insulated wire
The insulating varnish of each example in the present invention was applied 3 times to a copper wire having a circular cross-sectional area (d=1 mm), baked at 350℃for 30 minutes and at 450℃for 20 minutes to obtain an insulating layer having a thickness of 15. Mu.m.
Copper wires having a flat cross-sectional area (a=2.5 mm, b=4 mm, r-angle radius 0.8 mm) were coated 10 times, and baked at 350 ℃ for 30 minutes at high temperature and at 450 ℃ for 20 minutes to obtain an insulating layer having a thickness of 80 μm. The adhesive is used for 85RH% and the adhesive is used for 30 days after being stored at 85 ℃.
(4) PI film preparation
On glass, uniformly scraping and coating polyimide prepolymer resin into a certain thickness, pre-baking for 1 hour at 80 ℃, then heating to 400 ℃ for 2 hours, performing imidization, cooling, taking out, and stripping from a glass substrate to obtain a polyimide film with uniform thickness of 20 mu m for dielectric constant test, 85RH% and elongation, insulating strength and flame retardance test after 30 days of storage at 85 ℃.
(5) Adhesion property
With reference to GBT7095.6-2008, round and flat samples were tensile tested for elongation, respectively. And respectively stretching and testing the round sample and the flat sample by 20%, wherein the distance of losing the adhesive insulating layer is less than 1b, and the adhesion is qualified. Universal electronic testing machine: shimadzu XG-Plus.
(6) Dielectric constant
Agilent network analyzer E5063A-2H5, frequency 10GHz.
(7) Vertical burn test
The polyimide film is tested after being stored for 30 days at 85 ℃ and is referenced to the standards of a horizontal method and a vertical method for measuring the burning performance of GB T2408-2021 plastics.
(8) Elongation test
After the polyimide film is stored for 30 days at 85 ℃ for testing, the Shimadzu AG-Xplus tensile machine, the extensometer TRViewX, the sample width of 10cm, the gauge length of 50mm and the testing speed of 100mm/min are adopted.
(9) Breakdown strength test
Reference is made to part 6 of the film for electrical insulation of GB-T13542.6-2006: electrical insulation was tested using polyimide film standards.
The raw material compositions, properties, etc. of the polyimide insulating paints in examples 1 to 8 and comparative examples 1 to 4 are shown in tables 1 to 2 in detail.
TABLE 1 composition of polyimide insulating varnishes in examples 1 to 8 and comparative examples 1 to 4
( And (3) injection: the percentages in the table are weight percentage, the solid content=polyimide prepolymer mass/polyimide insulating paint mass, the polyimide prepolymer, filler and auxiliary agent are removed, and the rest is solvent content; wherein the molar ratio of dianhydride to diamine is 1:1. )
TABLE 2 Properties of polyimide insulating enamels in examples 1 to 8 and comparative examples 1 to 4
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1.A polyimide insulating paint is characterized in that: the raw materials comprise dianhydride, diamine and solvent;
The dianhydride comprises one or more of p-phenyl bis (trimellitate) dianhydride, bisphenol A type diether dianhydride, pyromellitic anhydride, biphenyl tetracarboxylic anhydride, diphenyl ether tetracarboxylic dianhydride, 3', 4' -benzophenone tetracarboxylic dianhydride, bisphenol AF diester dianhydride, p-biphenylene-bisphenol trimellitate dianhydride and bisphenol S diester dianhydride;
The diamine may include one or more of 4,4' -diaminodiphenyl ether, 2' -bis [4- (4-aminophenoxyphenyl) ] propane, p-phenylenediamine, m-phenylenediamine, 1, 3-bis (3-aminophenoxy) benzene, 1, 3-bis (4-aminophenoxy) benzene, 1, 4-bis (4-aminophenoxy) benzene, 4' -diamino-2, 2' -dimethylbiphenyl, 3,4' -diaminoanilide, bisphenol A diester diamine, bisphenol S diester diamine, and bis (4-aminophenyl) terephthalate.
2. An insulating varnish according to claim 1, wherein: the solvent comprises one or more of gamma-butyrolactone, gamma-valerolactone, tamiSolve, isosorbide dimethyl ether, dihydro-l-glucosone, water, methanol, ethanol and isobutanol.
3. The polyimide insulating varnish according to claim 1, wherein: the polyimide insulating paint is characterized by further comprising a filler, wherein the filler comprises one or more of aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon carbide, boron carbide, graphite, silicon dioxide and titanium dioxide.
4. The polyimide insulating varnish according to claim 1, wherein: the polyimide insulating paint is characterized by further comprising an auxiliary agent, wherein the auxiliary agent comprises one or more of a flame retardant, a plasticizer, a defoaming agent, a leveling agent, a coupling agent and a diluent; preferably, the auxiliary agent comprises one or more of triphenylphosphine, ammonium polyphosphate, aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane, diphenyl terephthalate, bis (2-carboxyethyl) methylphosphine oxide, tricresyl phosphate, dibutyl sebacate and triphenyl phosphate.
5. The polyimide insulating varnish according to claim 1, wherein: the dianhydride and/or diamine contains ester bonds, the content of the dianhydride containing the ester bonds in the total dianhydride content is more than or equal to 10mol percent, and/or the content of the diamine containing the ester bonds in the total diamine content is more than or equal to 10mol percent.
6. The polyimide insulating varnish according to claim 1, wherein: the weight average molecular weight of the polyimide insulating paint is 30000-200000g/mol, the solid content of the prepolymer of the polyimide insulating paint is 5-50wt% and the solvent content is 50-95wt%.
7. The polyimide insulating varnish according to claim 1, wherein: the molar ratio of the diamine to the dianhydride is 1 (0.95-1.05).
8. The polyimide insulating varnish according to claim 1, wherein: comprises polyimide prepolymer 5-50wt%, solvent 40-80wt%, filler 1-10wt% and auxiliary agent 1-10wt%.
9. A method for producing a polyimide insulating varnish according to any one of claims 1 to 8, wherein: the method comprises the following steps: in a solvent, diamine and dianhydride are polycondensed to obtain polyimide prepolymer, and polyimide insulating paint obtained by heating imidization is obtained.
10. Use of the polyimide insulating varnish according to any one of claims 1 to 8 or the polyimide insulating varnish prepared by the preparation method according to claim 9 in new energy automobiles.
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