CN117567865A - Mica part with good surface compatibility for new energy vehicle battery and preparation method thereof - Google Patents
Mica part with good surface compatibility for new energy vehicle battery and preparation method thereof Download PDFInfo
- Publication number
- CN117567865A CN117567865A CN202311500900.8A CN202311500900A CN117567865A CN 117567865 A CN117567865 A CN 117567865A CN 202311500900 A CN202311500900 A CN 202311500900A CN 117567865 A CN117567865 A CN 117567865A
- Authority
- CN
- China
- Prior art keywords
- mica
- organic silicon
- silicon resin
- component
- silicone oil
- Prior art date
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- Pending
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- 239000010445 mica Substances 0.000 title claims abstract description 189
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 189
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 100
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 100
- 239000010703 silicon Substances 0.000 claims abstract description 100
- 229920005989 resin Polymers 0.000 claims abstract description 98
- 239000011347 resin Substances 0.000 claims abstract description 98
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229920002635 polyurethane Polymers 0.000 claims abstract description 65
- 239000004814 polyurethane Substances 0.000 claims abstract description 65
- 229920002545 silicone oil Polymers 0.000 claims abstract description 58
- 239000011159 matrix material Substances 0.000 claims abstract description 54
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 49
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 45
- 239000003960 organic solvent Substances 0.000 claims abstract description 39
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 38
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000012948 isocyanate Substances 0.000 claims abstract description 32
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 32
- 229920005906 polyester polyol Polymers 0.000 claims abstract description 32
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 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 abstract description 15
- 239000003063 flame retardant Substances 0.000 claims abstract description 15
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 15
- 239000004417 polycarbonate Substances 0.000 claims abstract description 15
- 230000003139 buffering effect Effects 0.000 claims abstract description 12
- 239000004970 Chain extender Substances 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 10
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 8
- 229920000570 polyether Polymers 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 46
- 239000002002 slurry Substances 0.000 claims description 44
- 238000004512 die casting Methods 0.000 claims description 43
- -1 dihydroxyvinyl Chemical group 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000007731 hot pressing Methods 0.000 claims description 28
- 229920002050 silicone resin Polymers 0.000 claims description 27
- 238000005187 foaming Methods 0.000 claims description 26
- 238000007723 die pressing method Methods 0.000 claims description 23
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 22
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 21
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 21
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 20
- 150000004985 diamines Chemical class 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 20
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 19
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 239000003431 cross linking reagent Substances 0.000 claims description 16
- 238000005259 measurement Methods 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- UUWPVKAWLRJGKD-UHFFFAOYSA-N 1,3,5-tris[3-(isocyanatomethyl)phenyl]-1,3,5-triazinane-2,4,6-trione Chemical compound O=C=NCC1=CC=CC(N2C(N(C=3C=C(CN=C=O)C=CC=3)C(=O)N(C=3C=C(CN=C=O)C=CC=3)C2=O)=O)=C1 UUWPVKAWLRJGKD-UHFFFAOYSA-N 0.000 claims description 15
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 15
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 15
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 15
- 239000005543 nano-size silicon particle Substances 0.000 claims description 15
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 15
- 150000001993 dienes Chemical group 0.000 claims description 14
- 150000002009 diols Chemical class 0.000 claims description 14
- 229920005749 polyurethane resin Polymers 0.000 claims description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000000465 moulding Methods 0.000 claims description 13
- SXFJDZNJHVPHPH-UHFFFAOYSA-N 3-methylpentane-1,5-diol Chemical compound OCCC(C)CCO SXFJDZNJHVPHPH-UHFFFAOYSA-N 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 12
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 11
- 239000001361 adipic acid Substances 0.000 claims description 10
- 235000011037 adipic acid Nutrition 0.000 claims description 10
- 150000008065 acid anhydrides Chemical class 0.000 claims description 9
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 239000012745 toughening agent Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 230000003712 anti-aging effect Effects 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004760 aramid Substances 0.000 claims description 3
- 229920003235 aromatic polyamide Polymers 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000002135 nanosheet Substances 0.000 claims description 3
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical group [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 abstract description 13
- 238000009413 insulation Methods 0.000 abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052744 lithium Inorganic materials 0.000 abstract description 6
- 229920001971 elastomer Polymers 0.000 abstract description 4
- 239000000741 silica gel Substances 0.000 abstract description 4
- 229910002027 silica gel Inorganic materials 0.000 abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 23
- 238000004519 manufacturing process Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 15
- 239000003292 glue Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 229910052797 bismuth Inorganic materials 0.000 description 8
- 229920000909 polytetrahydrofuran Polymers 0.000 description 8
- 239000010410 layer Substances 0.000 description 5
- 229920005862 polyol Polymers 0.000 description 5
- 150000003077 polyols Chemical class 0.000 description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 125000005442 diisocyanate group Chemical group 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- OZCRKDNRAAKDAN-UHFFFAOYSA-N but-1-ene-1,4-diol Chemical compound O[CH][CH]CCO OZCRKDNRAAKDAN-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000010292 electrical insulation Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 229910052628 phlogopite Inorganic materials 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- OEMSKMUAMXLNKL-UHFFFAOYSA-N 5-methyl-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C(C)=CCC2C(=O)OC(=O)C12 OEMSKMUAMXLNKL-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000002952 polymeric resin Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- 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
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2101/00—Manufacture of cellular products
-
- 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
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
-
- 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
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/08—Polyurethanes from polyethers
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application relates to the technical field of mica composite materials for automobile battery modules, in particular to a mica part with good surface compatibility for a new energy automobile battery and a preparation method thereof. A mica part with good surface compatibility for a new energy vehicle battery is mainly prepared from a mica powder composition, a matrix organic silicon resin and a polyurethane modified organic silicon resin; the polyurethane modified organic silicon resin comprises a component A and a component B, wherein the component A comprises polyalcohol, a chain extender, isocyanate, an organic solvent, a catalyst, a functional auxiliary agent and vinyl silicone oil, and the polyalcohol comprises polyether glycol, anhydride modified polyester polyol and polycarbonate glycol; the component B comprises hydrogen-containing silicone oil with the hydrogen content of 0.03-1.60 percent. The flexible mica composite material with good surface compatibility and good buffering and heat insulation can be obtained by integrally forming the flexible mica composite material with the foamed silica gel, the foamed polyurethane and the foamed rubber, and the flexible mica composite material is used for improving the flame-retardant, fireproof safety and stability of the lithium battery cell module between automobile cells.
Description
Technical Field
The application relates to the technical field of mica composite materials for automobile battery modules, in particular to a mica part with good surface compatibility for a new energy automobile battery and a preparation method thereof.
Background
The flexible mica paper has excellent flame retardant and fireproof performance and insulating and puncture resistance, and is widely applied to the fields of cables, electronic and electric appliances, chemical production, new energy automobiles and the like. In the field of thermal runaway protection of new energy automobiles, the flexible mica paper plays a key role in protecting the lithium battery cell, so that the safety performance of the battery of the new energy automobile can be effectively improved, and the safety of automobile drivers is ensured.
At present, the flexible mica paper in the prior art is mainly prepared by uniformly mixing organic silicon resin and mica powder to prepare slurry with the solid content of 30-55% and then adopting a mould pressing process, wherein the larger the organic silicon content is, the overall flexibility is relatively good, but the electric insulation performance and the protective flame retardant performance of the flexible mica paper are reduced, so that the organic silicon content in the current flexible mica paper is preferably controlled to be 10-20%. Because of the influence of organic silicon resin in the flexible mica paper, the surface compatibility of the flexible mica paper and a high polymer resin material is poor, and if the high polymer resin material is directly prepared by integral compounding on the flexible mica paper, the prepared flexible mica composite material has poor interlayer bonding stability and peeling strength, is easy to rub and has the problems of interlayer separation and breakage, and has no practical industrial use value, so that the production and the manufacture of the flexible mica composite material are restricted.
For example, in the field of thermal runaway protection of new energy automobiles, the flexible mica product is required to have good fireproof flame retardant property and insulating breakdown resistance, and also is required to have certain buffering and damping properties and heat insulating properties. The ideal flexible mica composite material needs to be compounded by flexible mica paper and a foaming material, and the current compounding mode of the flexible mica paper and the foaming material adopts commercially available conventional glue (such as hot melt adhesive, acrylic acid adhesive and the like) to bond and compound the flexible mica paper and the foaming material to form the flexible mica composite material. However, the heat-resistant use performance and the ageing-resistant performance of the prepared flexible mica composite material are relatively poor, and the use requirement of the lithium battery cell module of the new energy automobile cannot be met.
The key point of the technical problem is that the flexible mica accords with the extremely high requirements of the material on the heat resistance and ageing resistance of the adhesive glue, and the special glue which accords with the use requirement has extremely high cost. Therefore, in order to solve the problems of the prior art, the applicant provides a mica part with good surface compatibility for new energy vehicle batteries and a preparation method thereof, wherein the mica part is suitable for mass production.
Disclosure of Invention
In order to solve the problems of high production cost, poor interlayer bonding stability and poor peeling strength of the flexible mica material in the prior art, the application provides a mica part with good surface compatibility for a new energy vehicle battery and a preparation method thereof.
The application provides a new energy vehicle battery is with mica finished piece that has good surface compatibility, is realized through following scheme:
a mica part with good surface compatibility for a new energy vehicle battery comprises a flexible mica matrix, wherein the flexible mica matrix is formed by integrating a mica powder composition, matrix organic silicon resin and polyurethane modified organic silicon resin through a compression molding process; the polyurethane modified organic silicon resin comprises a component A and a component B, wherein the component A comprises polyol, a chain extender, isocyanate, an organic solvent, a catalyst, a functional auxiliary agent and vinyl silicone oil, the polyol consists of polyether glycol, anhydride modified polyester polyol and polycarbonate glycol, and the anhydride modified polyester polyol accounts for 65-90% of the total molar weight of the polyol; the vinyl content of the vinyl silicone oil is controlled to be 0.5-12wt%; the isocyanate comprises MDI and IPDI; the chain extender is dihydroxyvinyl silicone oil, and alkene diol with unsaturated bond is matched with saturated diol and/or saturated diamine and/or saturated alcohol amine; the saturated diol is at least one of 1, 4-butanediol, 3-methyl-1, 5-pentanediol and 1, 6-hexanediol; the saturated diamine is at least one of 1, 4-butanediamine and 1, 6-hexanediamine; the saturated alcohol amine is at least one of diethanolamine and triethanolamine; the vinyl silicone oil accounts for 80-90wt% of the total mass of the component A; the component B comprises hydrogen-containing silicone oil with hydrogen content of 0.03-1.60%; the molar ratio of vinyl in the component A to active hydrogen in the hydrogen-containing silicone oil of the component B is 1 (1.08-1.32).
The flexible mica substrate in this application has good surface compatibility with foaming silica gel, foaming polyurethane, foaming rubber, satisfies the prerequisite that both integrated into one piece preparation have good thermal-insulated flexible mica combined material of buffering, can effectively reduce the manufacturing cost of flexible mica finished piece, promotes the production efficiency of flexible mica finished piece. In addition, the flexible mica part prepared in the application can play good roles in flame retardance, heat insulation, buffering and shock absorption when being used between the battery cells of the automobile, is favorable for improving the flame retardance, fire prevention, safety and stability of the battery cell module of the lithium battery, meets the requirements of the safety development trend of new energy automobiles, and has excellent market prospect and potential.
Preferably, the molar ratio of vinyl in the component A to active hydrogen in the hydrogen-containing silicone oil of the component B is 1 (1.18-1.24); the chain extender consists of dihydroxyvinyl silicone oil, 1, 4-butylene glycol and 3-methyl-1, 5-pentanediol in a molar ratio of (0.5-2) to (4-6).
Preferably, the isocyanate consists of MDI, IPDI, 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, the content of 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione accounting for 5-10wt% of the total mass of the isocyanate; the content of IPDI is 10-20wt% of the total mass of isocyanate.
By adopting the technical scheme, the heat-resistant stability and weather resistance of the flexible mica part can be improved.
Preferably, the anhydride modified polyester polyol is prepared from unsaturated double bond-containing anhydride, adipic acid, 2, 5-dimethyl-1, 4-benzene glycol, 1, 6-hexanediol, antioxidant 1010 and tetrabutyl titanate; the molar quantity of carboxyl contained in the unsaturated double bond-containing anhydride and adipic acid is 0.98-1.00 times of that of hydroxyl contained in 2, 5-dimethyl-1, 4-benzene glycol and 1, 6-hexanediol; the molar ratio of the 2, 5-dimethyl-1, 4-benzene glycol to the 1, 6-hexanediol is 1 (3-4); the preparation method of the anhydride modified polyester polyol comprises the following steps: adding accurately measured acid anhydride containing unsaturated double bonds, adipic acid, 2, 5-dimethyl-1, 4-benzene glycol, 1, 6-hexanediol and antioxidant 1010 into a reaction kettle, heating to 130-135 ℃ under magnetic stirring at 300-600rpm, preserving heat for at least 3 hours, heating to 225-232 ℃ at a constant speed of 1-1.2 ℃/min, preserving heat for 2-4 hours, controlling the temperature at the top of a distillation tower to 102+/-0.5 ℃, sampling to measure the acid value, adding tetrabutyl titanate after the acid value reaches 28-32mgKOH/g, vacuumizing, pumping the pressure in the kettle to about 20-25torr relatively vacuum within 4 hours, sampling and detecting until the hydroxyl value of the product reaches 35.4-56.0mgKOH/g, breaking vacuum with nitrogen, and cooling to 110+/-2 ℃, thus obtaining the acid anhydride modified polyester polyol with the molecular weight of 2000-3000.
Preferably, the preparation method of the polyurethane modified organic silicon resin comprises the following steps:
s1, preparing anhydride modified polyester polyol;
s2, heating the anhydride modified polyester polyol, polyether glycol, polycarbonate glycol, dihydroxyvinyl silicone oil, 1, 4-butylene glycol, 1, 6-hexanediol, an organic solvent, a catalyst and a functional auxiliary agent which are accurately metered in the S1 to 40-45 ℃, stirring for 20-25min, adding the accurately metered IPDI and MDI, adjusting the kettle temperature to be controlled at 75-78 ℃ for reacting for 60-80min, adding the catalyst for continuous reaction, and obtaining the viscosity of 3000-6000 mPa.s/25 ℃; adding 1,3, 5-tri (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione and an organic solvent, reacting for 30-40min at 75-78 ℃, and discharging to obtain anhydride modified polyurethane resin with the solid content of 30-50%;
s3, uniformly mixing the anhydride modified polyurethane resin and vinyl silicone oil prepared in the S2 with accurate metering to prepare a component A;
and S4, when the polyurethane modified organic silicon resin is used, the component A prepared in the step S3 is magnetically stirred, the platinum catalyst and the component B, namely hydrogen-containing silicone oil, are added at 300-360rpm, and the stirring speed is continuously and uniformly mixed at 300-360rpm to obtain the polyurethane modified organic silicon resin.
The preparation method of the polyurethane modified organic silicon resin is relatively simple, low in implementation operation difficulty, convenient for realizing industrialized mass production, beneficial to controlling the cost of the polyurethane modified organic silicon resin, and further beneficial to improving the production competitiveness of the flexible mica part.
Preferably, the matrix organic silicon resin is mainly prepared from 100 parts of methyl phenyl silicone resin, 25-60 parts of organic solvent, 0.3-0.6 part of diethylenetriamine, 40-60 parts of polysiloxane cross-linking agent and 1-3 parts of nano-scale vitreous ceramic powder; the polysiloxane crosslinking agent is at least one of FM-3321 type double-terminal diamine type reactive silicone, FM-3325 type double-terminal diamine type reactive silicone, FM-7721 type double-terminal diene type reactive silicone and FM-7725 type double-terminal diene type reactive silicone of JNC company; the preparation method of the matrix organic silicon resin comprises the following steps: adding polysiloxane cross-linking agent, methyl phenyl silicone resin and diethylenetriamine accounting for 40-60% of the total mass of the diethylenetriamine into a reaction kettle, heating to 60-65 ℃ under the magnetic stirring rotation speed of 60-120rpm, preserving heat for 100-160s, cooling to 0-4 ℃ by using an ice salt bath, adding an organic solvent, stirring for 5-10min at 80-160rpm, adding the rest of the diethylenetriamine, stirring for 100-160s at 40-60rpm, and obtaining the matrix organic silicone resin, wherein the storage temperature of the obtained matrix organic silicone resin is preferably controlled to 0-4 ℃.
Preferably, the polysiloxane crosslinking agent consists of FM-3325 type double-terminal diamine type reactive silicone and FM-7721 type double-terminal diene type reactive silicone of JNC company in a molar ratio of (3-4): 1; the mass ratio of the matrix organic silicon resin to the polyurethane modified organic silicon resin is controlled to be (3-7) 1; the surface of the flexible mica substrate is integrally formed with a buffering heat-insulating foaming layer.
By adopting the technical scheme, the fireproof flame-retardant performance of the flexible mica substrate is ensured, and meanwhile, the flexible mica substrate is endowed with good flexibility.
Preferably, the functional auxiliary agent comprises a flame retardant, an anti-aging agent and a toughening agent; the flame retardant is at least one of aluminum hydroxide, magnesium hydroxide, nano magnesium oxide, nano silicon dioxide powder and nano silicon nitride micro powder with granularity of more than 800 meshes; the anti-aging agent is at least one of antioxidant 1010, antioxidant 1098 and antioxidant 168; the toughening agent is at least one of nano alumina powder, titanium nitride whisker, boron nitride nanosheet and aramid staple fiber which are subjected to surface modification by siloxane, and the siloxane used for surface modification of the toughening agent is phenylsilane and/or vinylsilane.
By adopting the technical scheme, the weather resistance and the wear resistance of the prepared polyurethane modified organic silicon resin can be ensured.
The preparation method of the mica part with good surface compatibility for the new energy vehicle battery is realized through the following technical scheme:
a preparation method of a mica part with good surface compatibility for a new energy vehicle battery comprises the following steps:
step one, respectively preparing a mica powder composition, a matrix organic silicon resin and a polyurethane modified organic silicon resin; uniformly mixing the mica powder composition, the matrix organic silicon resin and the polyurethane modified organic silicon resin with accurate measurement at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 75-78 ℃ to remove an organic solvent in the die casting mica slurry, and then carrying out die pressing leveling treatment on the die casting mica slurry to obtain a prefabricated member;
Step three, spraying polyurethane modified organic silicon resin on the surface of the prefabricated part, wherein the spraying amount of the polyurethane modified organic silicon resin is 3-4g/m 2 Vacuumizing at 75-78deg.C for 5-10min, and hot-press molding to obtain flexible mica matrix;
and step four, adding the polymer foaming resin into a forming die for compression molding foaming treatment, and obtaining the finished flexible mica product.
The preparation method provided by the application is relatively simple, low in operation difficulty and convenient for realizing industrial production and manufacturing.
Preferably, the hot press molding method in the third step is specifically as follows: the first step, hot pressing conditions in hot press molding are that the temperature of a pressing plate is 80+/-0.5 ℃, the pressure is 0.20-0.25Mpa, and the duration is 60-80s; the second step, the hot pressing condition in the hot pressing forming is that the temperature of the pressing plate is 130-135 ℃, the pressure is 0.50-0.60Mpa, the duration is 100-120s, the third step, the hot pressing condition in the hot pressing forming is that the temperature of the pressing plate is 180+/-0.5 ℃, the pressure is 0.8-0.85Mpa, and the duration is 140-160s; and fourthly, the hot pressing condition in hot pressing forming is that the temperature of the pressing plate is 120-125 ℃, the pressure is 0.5-0.6Mpa, and the duration is 60+/-5 s.
By adopting the technical scheme, the flame retardance and the flexibility of the prepared flexible mica substrate can be effectively ensured.
In summary, the present application has the following advantages:
1. the flexible mica substrate in this application has good surface compatibility with foaming silica gel, foaming polyurethane, foaming rubber, satisfies the prerequisite that both integrated into one piece preparation have good thermal-insulated flexible mica combined material of buffering, can effectively reduce the manufacturing cost of flexible mica finished piece, promotes the production efficiency of flexible mica finished piece.
2. The flexible mica part prepared in the application can play good roles of flame retardance, heat insulation, buffering and shock absorption when being used between the automobile battery cells, is favorable for improving the flame retardance, fire prevention, safety and stability performance of the lithium battery cell module, meets the requirements of the safety development trend of new energy automobiles, and has excellent market prospect and potential.
3. The preparation method provided by the application is relatively simple, low in operation difficulty and convenient for realizing industrial production and manufacturing.
Description of the embodiments
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention and are not limiting of the invention claims. Those skilled in the art can, with the benefit of this disclosure, suitably modify the process parameters to achieve this. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included within the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that variations and modifications can be made in the methods and applications described herein, and in the practice and application of the techniques of this invention, without departing from the spirit or scope of the invention. While the following terms are believed to be well understood by those of ordinary skill in the art, the following definitions are set forth to aid in the description of the presently disclosed subject matter.
As used herein, the term "comprising" is synonymous with "including," "containing," or "characterized by," and is inclusive or open-ended and does not exclude additional unrecited elements or method steps. "comprising" is a technical term used in claim language to mean that the recited element is present, but other elements may be added and still form a construct or method within the scope of the recited claims.
Examples
The application discloses a new energy vehicle battery is with mica finished piece that has good surface compatibility includes flexible mica base member and integrated into one piece in the thermal-insulated foaming layer of buffering of flexible mica base member surface, and the gluey content of flexible mica base member is 10-15wt%.
The flexible mica matrix is mainly formed by integrally molding a mica powder composition, matrix organic silicon resin and polyurethane modified organic silicon resin through a compression molding process. The mass ratio of the matrix organic silicon resin to the polyurethane modified organic silicon resin is controlled to be (3-7): 1.
The matrix organic silicon resin is mainly prepared from 100 parts of methyl phenyl silicon resin, 25-60 parts of organic solvent,
0.3-0.6 part of diethylenetriamine, 40-60 parts of polysiloxane cross-linking agent and 1-3 parts of nano-grade vitreous ceramic powder.
The polysiloxane crosslinking agent is at least one of FM-3321 type double-terminal diamine type reactive silicone, FM-3325 type double-terminal diamine type reactive silicone, FM-7721 type double-terminal diene type reactive silicone and FM-7725 type double-terminal diene type reactive silicone of JNC company. Preferably, the polysiloxane crosslinker is composed of FM-3325 type of di-terminal diamine type reactive silicone from JNC corporation, FM-7721 type of di-terminal diene type reactive silicone in a molar ratio of (3-4): 1.
The preparation method of the matrix organic silicon resin comprises the following steps: adding polysiloxane cross-linking agent, methyl phenyl silicone resin and diethylenetriamine accounting for 40-60% of the total mass of the diethylenetriamine into a reaction kettle, heating to 60-65 ℃ under the magnetic stirring rotation speed of 60-120rpm, preserving heat for 100-160s, cooling to 0-4 ℃ by using an ice salt bath, adding an organic solvent, stirring for 5-10min at 80-160rpm, adding the rest of the diethylenetriamine, stirring for 100-160s at 40-60rpm, and obtaining the matrix organic silicone resin, wherein the storage temperature of the obtained matrix organic silicone resin is controlled to be 0-4 ℃ so that the polyurethane modified organic silicone resin comprises a component A and a component B, and the component A comprises polyalcohol, chain extender, isocyanate, organic solvent, catalyst, functional auxiliary agent and vinyl silicone oil with the vinyl content controlled to be 0.5-12 wt%. The vinyl silicone oil accounts for 80-90wt% of the total mass of the component A
The polyol consists of polyether glycol, anhydride modified polyester polyol and polycarbonate glycol, wherein the anhydride modified polyester polyol accounts for 65-90% of the total molar weight of the polyol. The anhydride modified polyester polyol is prepared from unsaturated double bond-containing anhydride, adipic acid, 2, 5-dimethyl-1, 4-benzene glycol, 1, 6-hexanediol, antioxidant 1010 and tetrabutyl titanate. The molar amount of carboxyl contained in the acid anhydride containing unsaturated double bond and adipic acid is 0.98-1.00 times of that of hydroxyl contained in 2, 5-dimethyl-1, 4-benzene glycol and 1, 6-hexanediol. The molar ratio of the 2, 5-dimethyl-1, 4-benzene glycol to the 1, 6-hexanediol is 1 (3-4).
The preparation method of the anhydride modified polyester polyol comprises the following steps: adding accurately measured acid anhydride containing unsaturated double bonds, adipic acid, 2, 5-dimethyl-1, 4-benzene glycol, 1, 6-hexanediol and antioxidant 1010 into a reaction kettle, heating to 130-135 ℃ under magnetic stirring at 300-600rpm, preserving heat for at least 3 hours, heating to 225-232 ℃ at a constant speed of 1-1.2 ℃/min, preserving heat for 2-4 hours, controlling the temperature at the top of a distillation tower to 102+/-0.5 ℃, sampling to measure the acid value, adding tetrabutyl titanate after the acid value reaches 28-32mgKOH/g, vacuumizing, pumping the pressure in the kettle to about 20-25torr relatively vacuum within 4 hours, sampling and detecting until the hydroxyl value of the product reaches 35.4-56.0mgKOH/g, breaking vacuum with nitrogen, and cooling to 110+/-2 ℃, thus obtaining the acid anhydride modified polyester polyol with the molecular weight of 2000-3000.
The isocyanate comprises MDI and IPDI, and preferably further comprises 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, wherein the content of the 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione accounts for 5-10wt% of the total mass of the isocyanate; the content of IPDI is 10-20wt% of the total mass of isocyanate.
The chain extender is dihydroxyvinyl silicone oil, and alkene diol with unsaturated bond is matched with saturated diol and/or saturated diamine and/or saturated alcohol amine. The saturated diol is at least one of 1, 4-butanediol, 3-methyl-1, 5-pentanediol and 1, 6-hexanediol. The saturated diamine is at least one of 1, 4-butanediamine and 1, 6-hexanediamine. The saturated alcohol amine is at least one of diethanolamine and triethanolamine. Preferably, the chain extender consists of dihydroxyvinyl silicone oil, 1, 4-butylene glycol and 3-methyl-1, 5-pentanediol in a molar ratio of (0.5-2): (0.5-2): (4-6).
The functional auxiliary agent comprises a flame retardant, an anti-aging agent and a toughening agent. Wherein the flame retardant is at least one of aluminum hydroxide, magnesium hydroxide, nano magnesium oxide, nano silicon dioxide powder and nano silicon nitride micro powder with granularity of more than 800 meshes. The anti-aging agent is at least one of antioxidant 1010, antioxidant 1098 and antioxidant 168. The toughening agent is at least one of nano alumina powder, titanium nitride whisker, boron nitride nanosheet and aramid staple fiber which are subjected to surface modification by siloxane, and the siloxane used for surface modification of the toughening agent is phenylsilane and/or vinylsilane.
The preparation method of the polyurethane modified organic silicon resin comprises the following steps:
s1, preparing anhydride modified polyester polyol;
s2, heating the anhydride modified polyester polyol, polyether glycol, polycarbonate glycol, dihydroxyvinyl silicone oil, 1, 4-butylene glycol, 1, 6-hexanediol, an organic solvent, a catalyst and a functional auxiliary agent which are accurately metered in the S1 to 40-45 ℃, stirring for 20-25min, adding the accurately metered IPDI and MDI, adjusting the kettle temperature to be controlled at 75-78 ℃ for reacting for 60-80min, adding the catalyst for continuous reaction, and obtaining the viscosity of 3000-6000 mPa.s/25 ℃; adding 1,3, 5-tri (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione and an organic solvent, reacting for 30-40min at 75-78 ℃, and discharging to obtain anhydride modified polyurethane resin with the solid content of 30-50%;
s3, uniformly mixing the anhydride modified polyurethane resin and vinyl silicone oil prepared in the S2 with accurate metering to prepare a component A;
and S4, when the polyurethane modified organic silicon resin is used, the component A prepared in the step S3 is magnetically stirred, the platinum catalyst and the component B, namely hydrogen-containing silicone oil, are added at 300-360rpm, and the stirring speed is continuously and uniformly mixed at 300-360rpm to obtain the polyurethane modified organic silicon resin.
The component B comprises hydrogen-containing silicone oil with the hydrogen content of 0.03-1.60 percent. The molar ratio of vinyl groups in the component A to active hydrogen in the hydrogen-containing silicone oil of the component B is 1 (1.08-1.32), preferably 1 (1.18-1.24).
A preparation method of a mica part with good surface compatibility for a new energy vehicle battery comprises the following steps:
step one, respectively preparing a mica powder composition, a matrix organic silicon resin and a polyurethane modified organic silicon resin; uniformly mixing the mica powder composition, the matrix organic silicon resin and the polyurethane modified organic silicon resin with accurate measurement at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 75-78 ℃ to remove an organic solvent in the die casting mica slurry, and then carrying out die pressing leveling treatment on the die casting mica slurry to obtain a prefabricated member;
step three, spraying polyurethane modified organic silicon resin on the surface of the prefabricated part, wherein the spraying amount of the polyurethane modified organic silicon resin is 3-4g/m 2 Vacuumizing at 75-78deg.C for 5-10min, and hot-press molding to obtain flexible mica matrix;
the hot press molding method in the third step is specifically as follows: the first step, hot pressing conditions in hot press molding are that the temperature of a pressing plate is 80+/-0.5 ℃, the pressure is 0.20-0.25Mpa, and the duration is 60-80s; the second step, the hot pressing condition in the hot pressing forming is that the temperature of the pressing plate is 130-135 ℃, the pressure is 0.50-0.60Mpa, the duration is 100-120s, the third step, the hot pressing condition in the hot pressing forming is that the temperature of the pressing plate is 180+/-0.5 ℃, the pressure is 0.8-0.85Mpa, and the duration is 140-160s; fourthly, the hot pressing condition in hot pressing forming is that the temperature of the pressing plate is 120-125 ℃, the pressure is 0.5-0.6Mpa, and the duration is 60+/-5 s;
And step four, adding the polymer foaming resin into a forming die for compression molding foaming treatment, and obtaining the finished flexible mica product.
Example 1A mica part with good surface compatibility for a new energy vehicle battery comprises a flexible mica substrate and a buffer heat insulation foaming layer integrally formed on the surface of the flexible mica substrate. The flexible mica matrix is formed by integrating a mica powder composition (phlogopite powder with the granularity of 30-50 microns), matrix organic silicon resin-KR-242A organic silicon resin of Japanese Xinyue and self-made polyurethane modified organic silicon resin through a mould pressing process, and the thickness of the prepared flexible mica matrix is controlled to be 0.3+/-0.02 mm, and the glue content is 12+/-0.05%.
The polyurethane modified organic silicon resin is prepared from an A component and a B component.
The component A comprises 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 12g of ethanolamine, 8g of dihydroxyvinyl silicone oil, 2g of 1, 4-butylene glycol, 2g of 1, 4-butanediol, 138.96g of isocyanate MDI, 30.87g of isocyanate IPDI, 400g of toluene as an organic solvent, 0.005g of bismuth octopamoate as a catalyst, 0.1g of antioxidant 1010, 0.1g of antioxidant 1098, 0.4g of nano silicon nitride micropowder, 0.2g of titanium nitride whisker modified with KH621, and 100g of vinyl silicone oil with a vinyl content of 10-12% (MY 273 vinyl silicone oil molecular weight 500 in Anhui Ming silicon).
The component B is hydrogen-containing silicone oil (SHIN-ETSU KF99, CAS: 7223-15) with hydrogen content of 1.6%.
The molar ratio of vinyl in the component A to active hydrogen in the hydrogen-containing silicone oil in the component B is about 1:1.16.
The preparation method of the mica part with good surface compatibility for the new energy vehicle battery comprises the following steps:
step one, respectively preparing a mica powder composition, a matrix organic silicon resin and a polyurethane modified organic silicon resin; the mica powder composition is phlogopite powder with 30-50 microns of granularity treated by KH151 vinyl triethoxysilane;
the matrix silicone resin is KR-242A silicone resin (solid content 50%) of Japanese Kogyo;
the preparation method of the polyurethane modified organic silicon resin comprises the following steps:
s1.1, preparation of anhydride modified polyester polyol: putting 24.74g of 4-methyl-4-cyclohexene-1, 2-dicarboxylic anhydride (CAS number: 3425-89-6), 146g of adipic acid, 138.2g of 2, 5-dimethyl-1, 4-benzene glycol, 42.96g of 1, 6-hexanediol and 0.4g of antioxidant 1010 into a reaction kettle, heating to react, keeping the temperature of the kettle at 135 ℃ for 3.0h at the first stage, keeping the temperature at 230 ℃ for 3.0h at a constant speed within 4.0h, controlling the temperature at the top of a distillation tower to be 102+/-0.5 ℃, sampling and measuring the acid value, adding 0.025g of tetrabutyl titanate after the acid value reaches 30mgKOH/g, vacuumizing, pumping the kettle to about 25torr relatively vacuum within 4 h, sampling and detecting until the hydroxyl value of the product reaches 56.0mgKOH/g, breaking the vacuum by nitrogen and cooling to 110 ℃ to obtain the anhydride modified polyester polyol with the molecular weight of 2000
S1.2, mixing 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 12g of ethanolamine, 8g of dihydroxyvinyl silicone oil, 2g of 1, 4-butylene glycol, 2g of 1, 4-butanediol, 400g of toluene as an organic solvent, 0.005g of catalyst-octozornide bismuth, 0.1g of antioxidant 1010 and 0.1g of antioxidant 1098, heating to 45 ℃ and mechanically stirring for 20min, adding 58.96g of MDI and 30.87g of IPDI, adjusting the temperature to 78 ℃ and reacting for 1h for viscosity test, and obtaining the viscosity of the reactant of 5 x 10 3 ～2.0×10 4 Adding 80g of diisocyanate MDI at the temperature of mPas/25 ℃, uniformly mixing, preserving heat for 100s, testing the NCO content of a system, regulating the NCO content to 4.2% by adding the diisocyanate MDI, ending the reaction to obtain modified polyurethane resin, and mixing 15g of the obtained modified polyurethane resin with 84.4g of vinyl silicone oil and 0.4g of nano silicon nitride microUniformly mixing the powder and 0.2g of titanium nitride whisker modified by KH621 to obtain a first component, mixing the prepared first component and second component according to the mol ratio of vinyl to active hydrogen of 1:1.16, adding 0.05g of platinum catalyst, and uniformly mixing to obtain the finished polyurethane modified organic silicon resin.
Uniformly mixing 880g of mica powder composition with accurate measurement, 200g of KR-242A organic silicon resin (solid content is 50%) with 20g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120s to obtain a prefabricated member;
step three, spraying polyurethane modified organic silicon resin on the surface of the prefabricated part, wherein the spraying amount of the polyurethane modified organic silicon resin is 4g/m 2 Vacuumizing at 78 ℃ for 5min, and preparing a finished flexible mica substrate by hot press molding;
the hot press molding method comprises the following specific steps: the first step, hot pressing conditions in hot press molding are that the temperature of a pressing plate is 80+/-0.5 ℃, the pressure is 0.25Mpa, and the duration is 60s; the second step, the hot pressing condition in hot pressing forming is that the temperature of the pressing plate is 135 ℃, the pressure is 0.60Mpa, the duration is 120s, and the third step, the hot pressing condition in hot pressing forming is that the temperature of the pressing plate is 180+/-0.5 ℃, the pressure is 0.8Mpa, and the duration is 150s; fourthly, the hot pressing condition in hot pressing forming is that the temperature of a pressing plate is 120 ℃, the pressure is 0.6Mpa, the duration is 60s, and the finished flexible mica substrate is prepared after natural cooling to room temperature;
And step four, mixing polyurethane isocyanate combined polyether high-grade composite materials (gallery high-grade heat-insulating materials Co., ltd., milky white time 25s, gas generation rate 25ml/g, viscosity (25 ℃ mPa.s) 150-250) according to a required weight ratio (A material: B material=1:1), adopting mechanical stirring time of 16s, rotating speed 1400 r/min, stirring uniformly, and immediately pouring into a mould for mould pressing foaming treatment (curing), wherein the mould temperature is 35 ℃, and the environment temperature is 25 ℃ to obtain the finished flexible mica product.
Example 2 differs from example 1 in that: uniformly mixing 880g of mica powder composition with accurate measurement, 180g of KR-242A organic silicon resin (solid content is 50%) with 30g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member.
Example 3 differs from example 1 in that: uniformly mixing 880g of mica powder composition with accurate measurement, 210g of KR-242A organic silicon resin (solid content is 50%) with 15g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120s to obtain the prefabricated member.
Example 4 differs from example 1 in that: uniformly mixing 880g of mica powder composition with accurate measurement, 180g of KR-242A organic silicon resin (solid content is 50%) with 30g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member.
Example 5 differs from example 1 in that: step two, uniformly mixing 900g of mica powder composition with accurate measurement, 160g of KR-242A organic silicon resin (solid content is 50%) with 20g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member. The content of the prepared finished flexible mica matrix glue is 10.0-10.2wt%.
Example 6 differs from example 1 in that: uniformly mixing 850g of mica powder composition with accurate measurement, 240g of KR-242A organic silicon resin (solid content is 50%) with 30g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120s to obtain the prefabricated member. The content of the prepared finished flexible mica matrix glue is 14.8-15wt%.
Example 7 differs from example 1 in that: 10g of the obtained modified polyurethane resin is uniformly mixed with 89.4g of vinyl silicone oil, 0.4g of nano silicon nitride micro powder and 0.2g of titanium nitride whisker modified by KH621 to obtain a first component, the prepared first component and a second component are mixed according to the molar ratio of vinyl to active hydrogen of 1:1.16, and then 0.05g of platinum catalyst is added, and the mixture is uniformly mixed to obtain the finished polyurethane modified organic silicon resin.
Example 8 differs from example 1 in that: the obtained modified polyurethane resin 20g is uniformly mixed with vinyl silicone oil 79.4g, nano silicon nitride micropowder 0.4g and titanium nitride whisker modified by KH621 0.2g to obtain a first component, the prepared first component and a second component are mixed according to the molar ratio of vinyl to active hydrogen of 1:1.16, and then 0.05g of platinum catalyst is added, and the mixture is uniformly mixed to obtain the finished polyurethane modified organic silicon resin.
Example 9 differs from example 1 in that: the A component comprises 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 26.2g of 3-methyl-1, 5-pentanediol, 8g of dihydroxyvinyl silicone oil, 4g of 1, 4-butylene glycol, 138.96g of isocyanate MDI, 30.87g of isocyanate IPDI, 400g of toluene as an organic solvent, 0.005g of bismuth octo-canthazole, 0.1g of antioxidant 1010, 0.1g of antioxidant 1098, 0.4g of nano silicon nitride micropowder, 0.2g of titanium nitride whisker modified with KH621, and 100g of vinyl silicone oil with a vinyl content of 10-12% (MY 273 vinyl silicone oil molecular weight 500 of Anhui Ming silicon industry Co., ltd.).
Example 10 differs from example 1 in that: the component A comprises 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 26.2g of 3 methyl-1, 5-pentanediol, 8g of dihydroxyvinyl silicone oil, 4g of 1, 4-butenediol, 147.65g of isocyanate MDI, 15.43g of isocyanate IPDI, 12.1g of 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, 400g of toluene as an organic solvent, 0.005g of catalyst-bismuth octo-gibbose, 0.1g of antioxidant 1010, 0.1g of antioxidant 1098, 0.4g of nano silicon nitride micropowder, 0.2g of titanium nitride 621 modified by KH, and 100g of vinyl silicone oil whisker with a vinyl content of 10-12%.
S1.2, mixing 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 26.2g of 3-methyl-1, 5-pentanediol, 8g of dihydroxyvinyl silicone oil, 4g of 1, 4-butylene glycol, 400g of organic solvent toluene, 0.005g of catalyst-bismuth octo-zornide, 0.1g of antioxidant 1010 and 0.1g of antioxidant 1098, heating to 45 ℃ and mechanically stirring for 20min, adding 67.65g of MDI, 15.43g of isocyanate IPDI and 12.1g of 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, adjusting the temperature to 78 ℃ and reacting for 1h to perform viscosity test when the reactant viscosity reaches 5 x 10 3 ～2.0×10 4 And (3) adding 80g of diisocyanate MDI at the temperature of mPa.s/25 ℃, uniformly mixing, preserving heat for 100s, testing the NCO content of a system, regulating the NCO content to 4.2% by adding the diisocyanate MDI, finishing the reaction to obtain modified polyurethane resin, uniformly mixing 15g of the obtained modified polyurethane resin with 84.4g of vinyl silicone oil, 0.4g of nano silicon nitride micro powder and 0.2g of titanium nitride whisker modified by KH621 to obtain a first component, mixing the prepared first component and second component according to the molar ratio of vinyl to active hydrogen of 1:1.16, adding 0.05g of platinum catalyst, and uniformly mixing to obtain the finished polyurethane modified organic silicon resin.
Example 11 differs from example 10 in that: the component A comprises 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 26.2g of 3 methyl-1, 5-pentanediol, 8g of dihydroxyvinyl silicone oil, 4g of 1, 4-butenediol, 138.96g of isocyanate MDI, 20.06g of isocyanate IPDI, 16.95g of 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, 400g of toluene as an organic solvent, 0.005g of catalyst-bismuth octo-gibbose, 0.1g of antioxidant 1010, 0.1g of antioxidant 1098, 0.4g of nano silicon nitride micropowder, 0.2g of titanium nitride 621 modified by KH, and 100g of vinyl silicone oil whisker with a vinyl content of 10-12%.
Example 12 differs from example 10 in that: the component A comprises 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 26.2g of 3 methyl-1, 5-pentanediol, 8g of dihydroxyvinyl silicone oil, 4g of 1, 4-butenediol, 130.28g of isocyanate MDI, 23.15g of isocyanate IPDI, 24.23g of 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, 400g of toluene as an organic solvent, 0.005g of catalyst-bismuth octo-gibbose, 0.1g of antioxidant 1010, 0.1g of antioxidant 1098, 0.4g of nano silicon nitride micropowder, 0.2g of titanium nitride 621 modified by KH, and 100g of vinyl silicone oil whisker with a vinyl content of 10-12%.
Example 13 differs from example 1 in that: the matrix organic silicon resin is mainly prepared from 100 parts of methyl phenyl silicone resin, 30 parts of organic solvent-methanol, 0.38 part of diethylenetriamine, 40 parts of polysiloxane cross-linking agent and 1.12 parts of nano-scale vitreous ceramic powder. The polysiloxane crosslinking agent is FM-3325 type double-end diamine type reactive silicone and FM-7721 type double-end diene type reactive silicone of JNC company, and the molar ratio is 3:1.
The preparation method of the matrix organic silicon resin comprises the following steps: 45g of FM-3325 type double-end diamine type reactive silicone, 15g of FM-7721 type double-end diene type reactive silicone and 100g of methylphenyl silicone resin (with the solid content of 50 percent) are added into a reaction kettle, the temperature is raised to 65 ℃ at 80rpm by magnetic stirring speed, the temperature is kept for 120 seconds, an organic solvent is added after the temperature is reduced to 0-4 ℃ by ice salt bath, the stirring is carried out for 5 minutes at 80rpm, then the rest of diethylenetriamine is added, the stirring is carried out for 120 seconds at 60rpm, and the storage temperature of the obtained matrix silicone resin is controlled to be 0-4 ℃ preferably.
Example 14 differs from example 1 in that: the polysiloxane crosslinking agent is FM-3325 type double-end diamine type reactive silicone and FM-7721 type double-end diene type reactive silicone of JNC company, and the molar ratio is 4:1.
Example 15 differs from example 11 in that: the matrix silicone resin prepared in example 13 was used.
Comparative example 1 differs from example 1 in that: the flexible mica matrix is formed by integrating a mica powder composition (phlogopite powder with the granularity of 30-50 microns) and a matrix organic silicon resin-KR-242A organic silicon resin of Japanese Xinyue through a compression molding process, and the thickness of the prepared flexible mica matrix is controlled to be 0.3+/-0.02 mm, and the glue content is 12+/-0.05%.
Comparative example 2 differs from example 1 in that: uniformly mixing 880g of mica powder composition with accurate measurement, 230g of KR-242A organic silicon resin (solid content is 50%) with 5g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member.
Comparative example 3 differs from example 1 in that: uniformly mixing 880g of mica powder composition with accurate measurement, 160g of KR-242A organic silicon resin (solid content is 50%) with 40g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member.
Comparative example 4 differs from example 1 in that: step two, uniformly mixing 920g of mica powder composition with accurate measurement, 130g of KR-242A organic silicon resin (solid content is 50%) with 15g of self-made polyurethane modified organic silicon resin at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment, and carrying out die pressing leveling at normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member. The content of the prepared finished flexible mica matrix glue is 8.0-8.2wt%.
Comparative example 5 differs from example 1 in that: step two, uniformly mixing 800g of mica powder composition, 320g of KR-242A organic silicon resin (solid content is 50%) of Japanese Xingyue and 40g of self-made polyurethane modified organic silicon resin at the temperature of 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to the temperature of 78 ℃ to remove organic solvent in the die casting mica slurry, then carrying out die pressing leveling treatment on the die casting mica slurry, and carrying out die pressing leveling at the normal temperature under the pressure of 1kg for 120 seconds to obtain the prefabricated member. The content of the prepared finished flexible mica matrix glue is 20.0-20.2wt%. .
Comparative example 6 differs from example 1 in that: the A component comprises 60g of polytetrahydrofuran glycol with a molecular weight of 3000, 100g of anhydride modified polyester polyol with a molecular weight of 2000, 20g of polycarbonate diol with a molecular weight of 2000, 16.75g of 3-methyl-1, 5-pentanediol, 4.32g of 1, 4-butanediol, 8.4g of diethanolamine, 138.96g of isocyanate MDI, 30.87g of isocyanate IPDI, 400g of toluene as an organic solvent, 0.005g of bismuth octoate as a catalyst, 0.1g of antioxidant 1010, 0.1g of antioxidant 1098, 0.4g of nano silicon nitride micropowder, 0.2g of titanium nitride whisker modified with KH621, and 100g of vinyl silicone oil with a vinyl content of 10-12% (MY 273 vinyl silicone oil molecular weight 500 of Anhui Ming silicon industry Co., ltd.).
Comparative example 7 differs from example 1 in that: 5g of the obtained modified polyurethane resin is uniformly mixed with 94.4g of vinyl silicone oil, 0.4g of nano silicon nitride micro powder and 0.2g of titanium nitride whisker modified by KH621 to obtain a first component, the prepared first component and a second component are mixed according to the molar ratio of vinyl to active hydrogen of 1:1.16, and then 0.05g of platinum catalyst is added, and the mixture is uniformly mixed to obtain the finished polyurethane modified organic silicon resin.
Comparative example 8 differs from example 1 in that: 25g of the obtained modified polyurethane resin is uniformly mixed with 74.4g of vinyl silicone oil, 0.4g of nano silicon nitride micro powder and 0.2g of titanium nitride whisker modified by KH621 to obtain a first component, the prepared first component and second component are mixed according to the molar ratio of vinyl to active hydrogen of 1:1.16, and then 0.05g of platinum catalyst is added, and the mixture is uniformly mixed to obtain the finished polyurethane modified organic silicon resin.
The heat conductivity testing method comprises the following steps: the measurement was carried out according to the GB/T10295-2008 test method. Peel strength test method: the measurement is carried out according to the GB/T2792-2014 test method. And (3) ageing resistance test: the flexible mica composites of examples 1-12 and comparative examples 1-4 were cut to a size of length x width = 24cm x 18cm, placed in an aging test box, treated at 85 ℃/80% (humidity) for 1200 hours, and tested for peel strength. The flame retardant performance test method comprises the following steps: the measurement was carried out in accordance with the UL94 v-0 flame retardant test standard. The breakdown voltage testing method comprises the following steps: the measurement was carried out according to the test method of ASTMD 149-09.
It can be seen from the combination of examples 1 to 15 and comparative examples 1 to 8 that the composition and proportion of the matrix silicone resin-KR-242A silicone resin of Japanese Kogyo, the self-made polyurethane modified silicone resin have an influence on the electrical insulation performance of the prepared flexible mica substrate, and have little influence on flame retardance and fire prevention.
It can be seen from the combination of examples 1 to 15 and comparative examples 1 to 8 that the flexible mica substrate of comparative example 4 is relatively good in electrical insulation property and fire resistance but poor in bending property, and cannot satisfy the production of three-dimensional shaped pieces. Thus, the gum content of the flexible mica matrix is controlled in this application to 10-15wt%, preferably 12.0wt%. In order to further improve the flexibility of the flexible mica substrate and ensure the flame retardant and fireproof performance and the electrical insulation performance of the flexible mica substrate and meet the production requirements of three-dimensional special-shaped pieces, the substrate organic silicon resin is mainly prepared from 100 parts of methyl phenyl silicone resin, 25-60 parts of organic solvent, 0.3-0.6 part of diethylenetriamine, 40-60 parts of polysiloxane cross-linking agent and 1-3 parts of nanoscale vitreous ceramic powder; the polysiloxane crosslinking agent is at least one of FM-3321 type double-terminal diamine type reactive silicone, FM-3325 type double-terminal diamine type reactive silicone, FM-7721 type double-terminal diene type reactive silicone and FM-7725 type double-terminal diene type reactive silicone of JNC company.
As can be seen from the combination of examples 1 to 15 and comparative examples 1 to 8, the comparison of example 1 with comparative example 1 shows that the flexible mica products prepared by using the matrix silicone resin and the polyurethane modified silicone resin as the binding resin of the mica powder composition have good fireproof flame retardant property and insulation breakdown resistance, and also have good shock absorption and heat insulation effects.
As can be seen from a combination of examples 1 to 15 and comparative examples 1 to 8, the mass ratio of the matrix silicone resin to the polyurethane-modified silicone resin is preferably controlled to be (3-7): 1, and preferably to be (4-5): 1, as can be seen from a comparison of examples 1 to 4 with comparative examples 2 to 3.
As can be seen from the combination of examples 1-15 and comparative examples 1-8, the comparison of examples 1, 5-6 and comparative examples 2-3 shows that the glue content of the prepared flexible mica products is preferably controlled to be 10-15wt%, and the too low glue content can affect the bonding stability of the flexible mica substrate and the foaming material layer, and the flexible mica substrate with the too low glue content can not meet the production of the three-dimensional special-shaped products.
As can be seen from the combination of examples 1-15 and comparative examples 1-8, the combination of examples 1, 7-8 and comparative examples 7-8 shows that the vinyl silicone oil accounts for 80-90wt% of the total mass of the A component, and the prepared flexible mica matrix has excellent comprehensive properties.
As can be seen from a comparison of examples 1 to 15 and comparative examples 1 to 8, examples 1 and examples 9 to 12 and comparative example 6, the isocyanate consisted of MDI, IPDI, 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, the content of 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione being 5 to 10% by weight based on the total mass of the isocyanate; the content of IPDI accounts for 10-20wt% of the total mass of isocyanate, so that the bonding strength and bonding stability of the prepared flexible mica substrate can be ensured, and better heat-resistant stability is provided.
As can be seen from the combination of examples 1 to 15 and comparative examples 1 to 8, the comparison of examples 1 and examples 13 to 15 shows that the flexible mica product produced by using the matrix silicone resin in examples 13 to 14 and the self-made polyurethane modified silicone resin has better flexibility and bending resistance, is suitable for producing three-dimensional profiled mica products, has better bonding strength and bonding stability between the prepared flexible mica substrate and the foaming material layer, and improves the market competitiveness of the product.
In summary, the flexible mica substrate in the application has good surface compatibility with foaming materials such as foaming silica gel, foaming polyurethane, foaming rubber and the like with buffering and damping effects, meets the precondition that the flexible mica composite material with good buffering and heat insulation is prepared by integrally forming the two materials, can effectively reduce the production cost of the flexible mica part, and improves the production efficiency of the flexible mica part. The flexible mica part prepared in the application can play good roles of flame retardance, heat insulation, buffering and shock absorption when being used between the automobile battery cells, is favorable for improving the flame retardance, fire prevention, safety and stability performance of the lithium battery cell module, meets the requirements of the safety development trend of new energy automobiles, and has excellent market prospect and potential.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (10)
1. A mica part with good surface compatibility for a new energy vehicle battery is characterized in that: the flexible mica matrix is formed by integrating a mica powder composition, matrix organic silicon resin and polyurethane modified organic silicon resin through a mould pressing process; the polyurethane modified organic silicon resin comprises a component A and a component B, wherein the component A comprises polyalcohol, a chain extender, isocyanate, an organic solvent, a catalyst, a functional auxiliary agent and vinyl silicone oil, the polyalcohol consists of polyether glycol, acid anhydride modified polyester polyol and polycarbonate glycol, and the acid anhydride modified polyester polyol accounts for 65-90% of the total mole amount of the polyalcohol; the vinyl content of the vinyl silicone oil is controlled to be 0.5-12wt%; the isocyanate comprises MDI and IPDI; the chain extender is dihydroxyvinyl silicone oil, and alkene diol with unsaturated bond is matched with saturated diol and/or saturated diamine and/or saturated alcohol amine; the saturated diol is at least one of 1, 4-butanediol, 3-methyl-1, 5-pentanediol and 1, 6-hexanediol; the saturated diamine is at least one of 1, 4-butanediamine and 1, 6-hexanediamine; the saturated alcohol amine is at least one of diethanolamine and triethanolamine; the vinyl silicone oil accounts for 80-90wt% of the total mass of the component A; the component B comprises hydrogen-containing silicone oil with hydrogen content of 0.03-1.60%; the molar ratio of vinyl in the component A to active hydrogen in the hydrogen-containing silicone oil of the component B is 1 (1.08-1.32).
2. The mica product with good surface compatibility for a new energy vehicle battery according to claim 1, wherein the mica product is characterized in that: the molar ratio of vinyl in the component A to active hydrogen in the hydrogen-containing silicone oil of the component B is 1 (1.18-1.24); the chain extender consists of dihydroxyvinyl silicone oil, 1, 4-butylene glycol and 3-methyl-1, 5-pentanediol in a molar ratio of (0.5-2) to (4-6).
3. The mica product with good surface compatibility for a new energy vehicle battery according to claim 2, wherein the mica product is characterized in that: the isocyanate consists of MDI, IPDI, 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione, wherein the content of the 1,3, 5-tris (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione accounts for 5-10wt% of the total mass of the isocyanate; the content of IPDI is 10-20wt% of the total mass of isocyanate.
4. The mica product with good surface compatibility for a new energy vehicle battery according to claim 2, wherein the mica product is characterized in that: the anhydride modified polyester polyol is prepared from unsaturated double bond-containing anhydride, adipic acid, 2, 5-dimethyl-1, 4-benzene glycol, 1, 6-hexanediol, antioxidant 1010 and tetrabutyl titanate; the molar quantity of carboxyl contained in the unsaturated double bond-containing anhydride and adipic acid is 0.98-1.00 times of that of hydroxyl contained in 2, 5-dimethyl-1, 4-benzene glycol and 1, 6-hexanediol; the molar ratio of the 2, 5-dimethyl-1, 4-benzene glycol to the 1, 6-hexanediol is 1 (3-4);
The preparation method of the anhydride modified polyester polyol comprises the following steps: adding accurately measured acid anhydride containing unsaturated double bonds, adipic acid, 2, 5-dimethyl-1, 4-benzene glycol, 1, 6-hexanediol and antioxidant 1010 into a reaction kettle, heating to 130-135 ℃ under magnetic stirring at 300-600rpm, preserving heat for at least 3 hours, heating to 225-232 ℃ at a constant speed of 1-1.2 ℃/min, preserving heat for 2-4 hours, controlling the temperature at the top of a distillation tower to 102+/-0.5 ℃, sampling to measure the acid value, adding tetrabutyl titanate after the acid value reaches 28-32mgKOH/g, vacuumizing, pumping the pressure in the kettle to about 20-25torr relatively vacuum within 4 hours, sampling and detecting until the hydroxyl value of the product reaches 35.4-56.0mgKOH/g, breaking vacuum with nitrogen, and cooling to 110+/-2 ℃, thus obtaining the acid anhydride modified polyester polyol with the molecular weight of 2000-3000.
5. The mica product with good surface compatibility for a new energy vehicle battery according to claim 4, wherein the mica product is characterized in that: the preparation method of the polyurethane modified organic silicon resin comprises the following steps:
s1, preparing anhydride modified polyester polyol;
s2, heating the anhydride modified polyester polyol, polyether glycol, polycarbonate glycol, dihydroxyvinyl silicone oil, 1, 4-butylene glycol, 1, 6-hexanediol, an organic solvent, a catalyst and a functional auxiliary agent which are accurately metered in the S1 to 40-45 ℃, stirring for 20-25min, adding the accurately metered IPDI and MDI, adjusting the kettle temperature to be controlled at 75-78 ℃ for reacting for 60-80min, adding the catalyst for continuous reaction, and obtaining the viscosity of 3000-6000 mPa.s/25 ℃; adding 1,3, 5-tri (3-isocyanatomethylphenyl) -1,3, 5-triazine-2, 4,6 (1H, 2H, 5H) -trione and an organic solvent, reacting for 30-40min at 75-78 ℃, and discharging to obtain anhydride modified polyurethane resin with the solid content of 30-50%;
S3, uniformly mixing the anhydride modified polyurethane resin and vinyl silicone oil prepared in the S2 with accurate metering to prepare a component A;
and S4, when the polyurethane modified organic silicon resin is used, the component A prepared in the step S3 is magnetically stirred, the platinum catalyst and the component B, namely hydrogen-containing silicone oil, are added at 300-360rpm, and the stirring speed is continuously and uniformly mixed at 300-360rpm to obtain the polyurethane modified organic silicon resin.
6. The mica product with good surface compatibility for a new energy vehicle battery according to claim 5, wherein the mica product is characterized in that: the matrix organic silicon resin is mainly prepared from 100 parts of methyl phenyl silicone resin, 25-60 parts of organic solvent, 0.3-0.6 part of diethylenetriamine, 40-60 parts of polysiloxane cross-linking agent and 1-3 parts of nano-scale vitreous ceramic powder; the polysiloxane crosslinking agent is at least one of FM-3321 type double-terminal diamine type reactive silicone, FM-3325 type double-terminal diamine type reactive silicone, FM-7721 type double-terminal diene type reactive silicone and FM-7725 type double-terminal diene type reactive silicone of JNC company; the preparation method of the matrix organic silicon resin comprises the following steps: adding polysiloxane cross-linking agent, methyl phenyl silicone resin and diethylenetriamine accounting for 40-60% of the total mass of the diethylenetriamine into a reaction kettle, heating to 60-65 ℃ under the magnetic stirring rotation speed of 60-120rpm, preserving heat for 100-160s, cooling to 0-4 ℃ by using an ice salt bath, adding an organic solvent, stirring for 5-10min at 80-160rpm, adding the rest of the diethylenetriamine, stirring for 100-160s at 40-60rpm, and obtaining the matrix organic silicone resin, wherein the storage temperature of the obtained matrix organic silicone resin is preferably controlled to 0-4 ℃.
7. The mica product with good surface compatibility for a new energy vehicle battery according to claim 6, wherein the mica product is characterized in that: the polysiloxane crosslinking agent consists of FM-3325 type double-end diamine reactive silicone and FM-7721 type double-end diene type reactive silicone of JNC company according to a molar ratio of (3-4): 1; the mass ratio of the matrix organic silicon resin to the polyurethane modified organic silicon resin is controlled to be (3-7) 1; the surface of the flexible mica substrate is integrally formed with a buffering heat-insulating foaming layer.
8. The mica product with good surface compatibility for a new energy vehicle battery according to claim 1, wherein the mica product is characterized in that: the functional auxiliary agent comprises a flame retardant, an anti-aging agent and a toughening agent; the flame retardant is at least one of aluminum hydroxide, magnesium hydroxide, nano magnesium oxide, nano silicon dioxide powder and nano silicon nitride micro powder with granularity of more than 800 meshes; the anti-aging agent is at least one of antioxidant 1010, antioxidant 1098 and antioxidant 168; the toughening agent is at least one of nano alumina powder, titanium nitride whisker, boron nitride nanosheet and aramid staple fiber which are subjected to surface modification by siloxane, and the siloxane used for surface modification of the toughening agent is phenylsilane and/or vinylsilane.
9. A method for preparing a mica part with good surface compatibility for a new energy vehicle battery according to any one of claims 1-8, which is characterized in that: the method comprises the following steps:
step one, respectively preparing a mica powder composition, a matrix organic silicon resin and a polyurethane modified organic silicon resin;
uniformly mixing the mica powder composition, the matrix organic silicon resin and the polyurethane modified organic silicon resin with accurate measurement at 0-4 ℃ to obtain die casting mica slurry, conveying the prepared die casting mica slurry into a forming die, heating to 75-78 ℃ to remove an organic solvent in the die casting mica slurry, and then carrying out die pressing leveling treatment on the die casting mica slurry to obtain a prefabricated member;
step three, spraying polyurethane modified organic silicon resin on the surface of the prefabricated part, wherein the spraying amount of the polyurethane modified organic silicon resin is 3-4g/m 2 Vacuumizing at 75-78deg.C for 5-10min, and hot-press molding to obtain flexible mica matrix;
and step four, adding the polymer foaming resin into a forming die for compression molding foaming treatment, and obtaining the finished flexible mica product.
10. The method for preparing the mica part with good surface compatibility for the new energy vehicle battery, which is characterized in that: the hot press molding method in the third step specifically comprises the following steps: the first step, hot pressing conditions in hot press molding are that the temperature of a pressing plate is 80+/-0.5 ℃, the pressure is 0.20-0.25Mpa, and the duration is 60-80s; the second step, the hot pressing condition in the hot pressing forming is that the temperature of the pressing plate is 130-135 ℃, the pressure is 0.50-0.60Mpa, the duration is 100-120s, the third step, the hot pressing condition in the hot pressing forming is that the temperature of the pressing plate is 180+/-0.5 ℃, the pressure is 0.8-0.85Mpa, and the duration is 140-160s; and fourthly, the hot pressing condition in hot pressing forming is that the temperature of the pressing plate is 120-125 ℃, the pressure is 0.5-0.6Mpa, and the duration is 60+/-5 s.
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