CN116478409A - Application of alkenyl heptapolyphenyl POSS in preparation of ceramic organic silicon heat insulation material - Google Patents
Application of alkenyl heptapolyphenyl POSS in preparation of ceramic organic silicon heat insulation material Download PDFInfo
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- CN116478409A CN116478409A CN202310199795.2A CN202310199795A CN116478409A CN 116478409 A CN116478409 A CN 116478409A CN 202310199795 A CN202310199795 A CN 202310199795A CN 116478409 A CN116478409 A CN 116478409A
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- CN
- China
- Prior art keywords
- alkenyl
- poss
- heptapolyphenyl
- component
- heat insulation
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- 125000003342 alkenyl group Chemical group 0.000 title claims abstract description 107
- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 53
- 239000012774 insulation material Substances 0.000 title claims abstract description 39
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 36
- 239000010703 silicon Substances 0.000 title claims abstract description 36
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims abstract description 40
- HSSJULAPNNGXFW-UHFFFAOYSA-N [Co].[Zn] Chemical compound [Co].[Zn] HSSJULAPNNGXFW-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000001746 injection moulding Methods 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 81
- 238000006243 chemical reaction Methods 0.000 claims description 61
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 53
- 238000001723 curing Methods 0.000 claims description 49
- 229920002050 silicone resin Polymers 0.000 claims description 41
- 239000004964 aerogel Substances 0.000 claims description 33
- 239000000377 silicon dioxide Substances 0.000 claims description 33
- 235000012239 silicon dioxide Nutrition 0.000 claims description 33
- 239000003054 catalyst Substances 0.000 claims description 28
- 239000006185 dispersion Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 25
- 239000001257 hydrogen Substances 0.000 claims description 25
- 229910052739 hydrogen Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 22
- 229920002545 silicone oil Polymers 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000004005 microsphere Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- -1 alkenyl trichlorosilane Chemical compound 0.000 claims description 11
- 239000004965 Silica aerogel Substances 0.000 claims description 10
- 229920001296 polysiloxane Polymers 0.000 claims description 10
- JIUFUEGXYSZGJV-UHFFFAOYSA-N [O-2].[Fe+2].[Zn+2].[Co+2].[O-2].[O-2] Chemical compound [O-2].[Fe+2].[Zn+2].[Co+2].[O-2].[O-2] JIUFUEGXYSZGJV-UHFFFAOYSA-N 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 239000011810 insulating material Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000005052 trichlorosilane Substances 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 18
- 238000009413 insulation Methods 0.000 abstract description 16
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052802 copper Inorganic materials 0.000 abstract description 6
- 239000010949 copper Substances 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract 1
- XJWOWXZSFTXJEX-UHFFFAOYSA-N phenylsilicon Chemical compound [Si]C1=CC=CC=C1 XJWOWXZSFTXJEX-UHFFFAOYSA-N 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 230000000694 effects Effects 0.000 description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229920002554 vinyl polymer Polymers 0.000 description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000011261 inert gas Substances 0.000 description 9
- 229920002379 silicone rubber Polymers 0.000 description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 9
- 230000008569 process Effects 0.000 description 7
- NSJAWXMCLJVBPM-UHFFFAOYSA-N 3-butyloxolane-2,5-dione Chemical compound CCCCC1CC(=O)OC1=O NSJAWXMCLJVBPM-UHFFFAOYSA-N 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000006459 hydrosilylation reaction Methods 0.000 description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- GNEPOXWQWFSSOU-UHFFFAOYSA-N dichloro-methyl-phenylsilane Chemical compound C[Si](Cl)(Cl)C1=CC=CC=C1 GNEPOXWQWFSSOU-UHFFFAOYSA-N 0.000 description 5
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 5
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 239000004945 silicone rubber Substances 0.000 description 5
- 239000005051 trimethylchlorosilane Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 125000005065 undecenyl group Chemical group C(=CCCCCCCCCC)* 0.000 description 4
- 239000005046 Chlorosilane Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000007259 addition reaction Methods 0.000 description 3
- 239000002956 ash Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 238000009396 hybridization Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- NOKUWSXLHXMAOM-UHFFFAOYSA-N hydroxy(phenyl)silicon Chemical compound O[Si]C1=CC=CC=C1 NOKUWSXLHXMAOM-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000006855 networking Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000000051 modifying effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000006798 ring closing metathesis reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- YVRYYVDHGQKMMU-BQYQJAHWSA-N trichloro-[(e)-oct-1-enyl]silane Chemical compound CCCCCC\C=C\[Si](Cl)(Cl)Cl YVRYYVDHGQKMMU-BQYQJAHWSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- 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
Abstract
The invention relates to the field of composite materials, and discloses application of alkenyl heptapolyphenyl POSS in preparation of ceramic organic silicon heat insulation materials. Firstly, the invention takes the alkenyl heptapolyphenyl POSS as the raw material to prepare the ceramic organic silicon heat insulation material capable of injection molding, which can effectively reduce the raw material viscosity of the ceramic organic silicon heat insulation material, thereby being prepared by injection molding. Secondly, the raw materials of the ceramic organic silicon heat insulation material of the terminal alkenyl heptapolyphenyl POSS contain phenyl silicon resin with low molecular weight and side chain hanging alkenyl, cobalt zinc ferrite complex and terminal alkenyl heptapolyphenyl POSS, and the ceramic organic silicon heat insulation material has high heat insulation performance and high heat resistance and is suitable for injection molding technology. The material obtained by the injection molding process can be used for coating the soft copper bar insulated wire, so that the space utilization rate of the battery pack can be improved, and the energy density of the power battery can be improved.
Description
Technical Field
The invention relates to the field of composite materials, in particular to an alkenyl heptapolyphenyl POSS and application thereof in preparing ceramic organic silicon heat insulation materials.
Background
The sales of new energy automobiles are increased, but the problem of overheat and fire is still a shade which is not kept by manufacturers and consumers. The heat insulation treatment of the copper bar connecting wire for transmitting electric energy is one of methods for effectively avoiding the ignition of the electric automobile. The existing copper bar connecting wire treatment scheme is mainly concentrated on heat shrinkage tubes and insulating resin spraying. The heat shrinkage tube and the insulating resin have the defects of limited temperature resistance, and the battery is easy to decompose to form ash when being exposed to high temperature or flame during thermal runaway, so that the insulating fireproof capability is lost, and the fireproof requirement of a host factory cannot be met. Even if a layer of high-temperature resistant glass fiber adhesive tape is bound on the outer surface of the insulating resin or the heat-shrinkable tube, the problem that the protective layer is easy to peel off under the impact of high-temperature flame to cause insulation failure still cannot be solved.
Ceramic silicon rubber is an ideal high-temperature resistant insulating material at present. The ceramic silicon rubber is intrinsically heat-resistant and insulating, and silicon oxide structural units are converted into continuous, oxidation-resistant and insulating network-shaped silicon oxide ashes which are covered on the surface during combustion, so that further ablation can be prevented, eutectic reaction can be carried out between the silicon oxide ashes and refractory fillers, a compact high-temperature-resistant ceramic layer with certain strength is generated, and the purposes of flame retardance, fire resistance and insulation are achieved.
The current molding process commonly used for ceramic silicone rubber is a compression molding process. For example, chinese patent No. CN202111273551.1 discloses a ceramic silicone rubber for heat insulation of a power battery and a preparation method thereof, the ceramic silicone rubber comprises the following raw materials in parts by weight: 100 parts of silica gel, 5-20 parts of zinc borate, 6-15 parts of aluminum oxide, 5-10 parts of mica powder, 3-5 parts of kaolin, 10-25 parts of glass powder, 0.1-0.4 part of a silane coupling agent, 5-20 parts of silicone oil, 20-30 parts of white carbon black, 4-10 parts of magnesium oxide and 10-20 parts of ceramic fiber. The preparation method comprises the steps of weighing raw materials, mixing into powder, banburying, stirring, cooling, aging, vulcanizing, open milling, tabletting and finally heating, vulcanizing and forming to obtain the ceramic silicone rubber. Chinese patent No. CN202110350619.5 discloses a heat conductive ceramic silicone rubber material and its preparation method. The material is prepared by adding a composite porcelain filler, a flame retardant and a vulcanizing agent into a silicon rubber matrix and vulcanizing the mixture through high-temperature mould pressing. The molding process has the defects of low efficiency, great amount of glue loss in the production process, flash removal of the product after demolding and limited productivity. Moreover, the molding process is not suitable for soft copper bars which have a positive effect on improving the energy density of the power battery pack, but the technical problems can be solved if the outside of the soft copper bars is coated with an organosilicon heat-insulating material by adopting an injection molding process. However, the existing injection molding resins require lower viscosities, whereas the viscosities of conventional phenyl silicone resins for making ceramic silicone rubbers are generally higher. Therefore, the direct injection molding has a problem of difficult processing.
In view of the above, development of a ceramic silicone heat insulating material which has excellent heat insulating properties and heat resistance and can be suitably used for injection molding has positive significance.
Disclosure of Invention
Firstly, in order to solve the technical problem that the traditional phenyl silicone resin cannot prepare the ceramic organic silicon heat insulation material through an injection molding process, the invention provides application of the terminal alkenyl heptapolyphenyl POSS in preparing the ceramic organic silicon heat insulation material, and the terminal alkenyl heptapolyphenyl POSS can effectively reduce the viscosity of raw materials of the ceramic organic silicon heat insulation material, so that the ceramic organic silicon heat insulation material can be prepared through injection molding. In order to solve the technical problems that the existing ceramic organic silicon heat insulation material is difficult to have high heat insulation property and high heat resistance and is applicable to injection molding, the invention provides the ceramic organic silicon heat insulation material of the terminal alkenyl heptapolyphenyl POSS.
The specific technical scheme of the invention is as follows:
in a first aspect, the invention provides an application of alkenyl heptapolyphenyl POSS in preparing an injection-moldable ceramic organic silicon heat insulation material and an application in improving injection molding processing adaptability of the ceramic organic silicon heat insulation material. The structural formula of the alkenyl heptapolyphenyl POSS is shown as follows:
wherein n=0 to 9, more preferably 3 to 6.
According to the invention, the alkenyl heptapolyphenyl POSS is introduced into the ceramic organic silicon heat insulation material by utilizing hydrosilylation, so that after the phenyl POSS with huge volume is grafted on the main chain of the polymer, the acting force among molecules can be reduced, the viscosity of a resin reaction system can be obviously reduced, the high-viscosity condition of the traditional phenyl silicone resin is changed, and the ceramic organic silicon heat insulation material is prepared by an injection molding process.
In addition, the invention adjusts the crosslinking density of the ceramic organic silicon heat insulation material by controlling the introduction amount and the type of the terminal alkenyl heptapolyphenyl POSS, and can obviously improve the heat resistance of the material by enhancing the heat insulation and heat resistance effects through inorganic/organic hybridization.
Further, it is preferred in the present invention that the alkenyl-terminated carbon chain length of the alkenyl-terminated heptapolyphenyl POSS is from 5 to 8 (alkenyl-containing). The reason is that we find that: because of the huge volume of phenyl POSS, if the carbon chain length is too short, the terminal alkenyl is easily shielded by the phenyl POSS, and the grafting efficiency is low because of the steric hindrance effect and the increase of the molecular weight of the superposed main chain in the reaction process, which can not fully participate in the addition reaction. Conversely, if the carbon chain length is too long, the viscosity of the compound is easily too high due to the reduction of the inorganic-organic synergistic effect, so that the viscosity reduction effect of the terminal alkenyl heptapolyphenyl POSS is reduced, and the terminal alkenyl can be fully extended to avoid the interference of the phenyl POSS by properly increasing the carbon chain arm length.
Preferably, the preparation route of the alkenyl heptapolyphenyl POSS is as follows:
preferably, the preparation method of the alkenyl heptapolyphenyl POSS comprises the following steps: adding an organic solvent, sodium hydroxide and water into a reactor, uniformly stirring, dropwise adding phenyltriethoxysilane, heating to reflux after the dripping is finished, and reacting; cooling, vacuum removing organic solvent, adding another organic solvent for dissolving, cooling to-5-0 ℃, adding pyridine, dropwise adding alkenyl trichlorosilane with carbon chain length of 2-11 for reaction, heating for continuous reaction, and obtaining the alkenyl heptapolyphenyl POSS.
The invention prepares phenyl T7 trisiloxane by phenyl siloxane, and then prepares terminal alkenyl heptapolyphenyl POSS by a unfilled-corner ring closure method. Wherein, the pyridine is used for absorbing HC1 in the reaction process, so that the synthesis of the alkenyl heptapolyphenyl POSS is more complete.
In a second aspect, the invention provides an injection-moldable ceramic organic silicon heat-insulating material of an alkenyl heptapolyphenyl POSS, which is prepared by uniformly mixing components including a component A and a component B and then heating and curing; wherein:
the component A comprises the following raw materials: hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microspheres and a reaction rate regulator.
In the component A, hydrogen-containing silicone oil is used as one of the cross-linking agent components; the combination of the silicon dioxide aerogel, the cobalt zinc ferrite complex and the hollow glass microspheres can synergistically play a heat insulation effect; in addition, the silica aerogel also has the function of reinforcing resin. The reaction rate modifier is used to control the reaction time.
The component B comprises the following raw materials: phenyl silicone resin with low molecular weight side chain hanging alkenyl, terminal alkenyl heptapolyphenyl POSS, silicon dioxide aerogel, spherical alumina, cobalt zinc ferrite complex, a dispersion promoter and a catalyst.
In the component B, phenyl silicone resin with low molecular weight side chain hanging alkenyl and terminal alkenyl heptapolyphenyl POSS are used as main cross-linking agents; the combination of the silica aerogel, the spherical alumina and the cobalt zinc ferrite composite can synergistically play a heat insulation effect; the catalyst is used to promote the reaction.
The component A and the component B are uniformly mixed and heated and cured through injection molding, so that the ceramic organic silicon heat insulation material of the alkenyl-terminated heptapolyphenyl POSS can be obtained, and the curing mechanism is as follows:
in the curing reaction process, under the action of a catalyst, the hydrogen-containing silicone oil, the phenyl silicone resin with low molecular weight side chain hanging alkenyl and the alkenyl-terminated heptapolyphenyl POSS undergo hydrosilylation reaction, and the formed organic silicon heat insulation material has a three-dimensional cross-linked network structure on microcosmic scale, wherein inorganic particles such as silica aerogel, cobalt zinc ferrite complex, hollow glass microspheres, spherical alumina and the like and POSS with cage-shaped structures are dispersedly embedded in grid pores of the three-dimensional network structure, so that the excellent heat insulation effect of the material is provided. The reaction rate regulator is used for controlling the reaction time of the formation of the three-dimensional crosslinked network structure, so that the problem that the heat insulation effect of the material is affected because inorganic materials are not uniformly distributed in the three-dimensional network structure due to the too high crosslinking reaction rate is avoided.
The raw materials of the ceramic organic silicon heat insulation material simultaneously contain phenyl silicone resin with low molecular weight and side chain hanging alkenyl, cobalt zinc ferrite complex and terminal alkenyl heptapolyphenyl POSS, and the technical effects are as follows: 1) The inorganic/organic hybridization is fully utilized to enhance the heat insulation and heat resistance effect. The terminal alkenyl heptapolyphenyl POSS is connected into a reaction system by utilizing hydrosilylation, and is optimized to a proper crosslinking density by controlling the introduction amount and the type, so that the heat insulation property and the heat resistance of the organosilicon material are obviously improved under the condition of not obviously increasing the viscosity of the raw material. 2) Uses the viscosity reducing effect of the macromolecular side chain large group. The phenyl POSS with huge volume is grafted on the main chain of the polymer, so that the acting force among molecules is reduced, the high-viscosity condition of the traditional phenyl silicone resin is changed, the viscosity of a resin reaction system is reduced, and the quick molding of the organosilicon heat insulation material by injection is facilitated. 3) The inorganic-inorganic synergetic porcelain effect is utilized. The cobalt zinc ferrite complex with spinel structure is introduced, and is cooperatively embedded into the three-dimensional cross-linked network structure of the material together with the silicon dioxide aerogel, so that a compact continuous structure is formed in a rivet networking mode, and the material is easier to quickly form porcelain in the combustion process of the material when meeting fire. In addition, the cobalt zinc ferrite complex and the silicon dioxide aerogel have excellent heat resistance, and are more excellent than the heat resistance of a single system.
Preferably, the component A comprises the following raw materials in percentage by mass: 20-50% of hydrogen-containing silicone oil, 5-25% of silicon dioxide aerogel, 5-25% of cobalt zinc ferrite complex, 5-20% of hollow glass microsphere and 0-1% of reaction rate regulator.
Preferably, the component B comprises the following raw materials in percentage by mass: 20-45% of phenyl silicone resin with low molecular weight side chain hanging alkenyl, 5-15% of alkenyl heptapolyphenyl POSS, 5-25% of silica aerogel, 5-25% of spherical alumina, 15-25% of cobalt zinc ferrite complex, 1-5% of dispersion promoter and 0.1-0.3% of catalyst.
It should be noted that the present invention finds that the amount of alkenyl heptapolyphenyl POSS incorporated can have a significant impact on the properties of the material. If the content is too low, the modifying effect is poor, whereas if it is too high, the resin tends to crack after curing. For this reason, the present invention preferably found that the control of the content of alkenyl heptapolyphenyl POSS at 5 to 15% solves the above technical problems.
Preferably, the mass ratio of the component A to the component B is 1.5-2.5:1.
Preferably, the phenyl silicone resin with low molecular weight side chain hanging alkenyl has the following structural formula:
wherein X is 4-10.
The invention discovers that the molecular weight of phenyl silicone resin with side chain hanging alkenyl is also important to whether the final material is suitable for injection molding processing, and if the molecular chain is too long and the molecular weight is too large, the intermolecular acting force is strong, the viscosity of the resin is high, and the injection molding processing is not facilitated. Finally we found that in the range x=4-10, good injectability can be imparted to the material.
Preferably, the preparation method of the phenyl silicone resin with the low molecular weight side chain hanging alkenyl comprises the following synthetic route:
wherein X is 4-10.
Preferably, the preparation method of the phenyl silicone resin with the low molecular weight side chain hanging alkenyl comprises the following steps: uniformly mixing methyl phenyl dichlorosilane, methyl alkenyl dichlorosilane and diphenyl diethoxysilane in an inert gas atmosphere with the water content of 0.05-0.1wt%, dropwise adding the mixture into a reaction system with an ice salt bath, continuously reacting for 4-8 hours after dropwise adding, separating out generated HCl, removing inert gas protection, heating to room temperature, continuously reacting for 4-8 hours, dropwise adding trimethyl chlorosilane for end-capping reaction, heating to 70-90 ℃ after dropwise adding, continuously reacting for 10-15 hours, distilling under reduced pressure to remove low-boiling substances, and then heating to 140-160 ℃ for structural reforming for 20-30 hours to obtain phenyl silicone resin with low molecular weight side chain hanging alkenyl.
In the preparation process of the invention, chlorosilane is very active, and water vapor meeting air is decomposed to generate silanol and hydrogen chloride gas. Under acidic conditions, silanol further undergoes condensation reaction with alkoxysilane to produce a small molecule silicone polymer and release ethanol. In order to control the hydrolysis speed of the chlorosilane, the method is carried out under the protection of an inert gas (preferably nitrogen), and the water content of the inert gas is important, so that the chlorosilane can be slowly hydrolyzed by the proper water content, and if the water content is too low, the hydrolysis cannot be smoothly carried out; conversely, if the water content is too high, the hydrolysis rate tends to be too high, resulting in gelation of the product. Meanwhile, the continuously circulated inert gas can bring out the generated hydrogen chloride gas, so that the reaction is promoted to be continuously and stably carried out. Under the condition of rising to room temperature and in the subsequent steps, the inert gas protection needs to be withdrawn in time, otherwise, the subsequent reaction is affected.
Preferably, the molar ratio of the methyl phenyl dichlorosilane to the methyl alkenyl dichlorosilane to the diphenyl diethoxy silane to the trimethyl chlorosilane is (0.7-0.9) to (0.1-0.3) to (0.8-1.2) to (0.1-0.3).
Preferably, the cobalt zinc ferrite complex is CoZnFe 4 O 8 。
Preferably, the cobalt zinc ferrite complex is prepared according to the following reaction formula: 4Fe (NO) 3 ) 3 +Co(NO 3 ) 2 +7O 2 +Zn(NO 3 ) 2 +6C 6 H 8 O 7 →CoZnFe 4 O 8 +8N 2 +36CO 2 +24H 2 O。
As a further preferred aspect, the method for preparing the cobalt zinc ferrite complex specifically includes: fully dissolving ferric nitrate, cobalt nitrate, zinc nitrate and citric acid into water, heating to 85-95 ℃, continuously supplementing water under the bubbling action of continuous air flow, reacting, filtering and drying to obtain the cobalt-zinc-iron-oxygen complex.
The invention prepares the cobalt zinc ferrite complex in one step by utilizing a sol-gel precipitation method, the process is simple, the product stability is good, and the prepared complex has a spinel structure.
Preferably, the reaction rate regulator is formed by mixing butyl succinic anhydride and 3, 5-propyl-1-butyn-3-ol in an alcohol excess.
In the hydrosilation reaction at the injection molding curing stage of the invention, a platinum catalyst such as Karster is very active, and the reaction is intense and easy to gel. In order to reduce the reaction rate, it is generally necessary to add reagents capable of slowing down the reaction rate, but the addition of these reagents reduces the reaction rate and is disadvantageous for injection molding. Thus, one of the key points in injection mouldability is how to trigger the catalytic rapid curing reaction. And after the trigger temperature is reached, the silicone resin is rapidly molded to form the ceramic organic silicon heat insulation material. The solution provided by the invention is as follows: the concentration of 3, 5-propyl-1-butyn-3-ol in a reaction system is controlled by utilizing the reaction of butyl succinic anhydride with temperature responsiveness (the phase transition temperature is 46 ℃) and 3, 5-propyl-1-butyn-3-ol which can slow down the reaction (the butyl succinic anhydride is open to form acid), when the temperature is higher than 50 ℃, the butyl succinic anhydride is changed from solid state to liquid state, the reaction rate with the 3, 5-propyl-1-butyn-3-ol is improved, the 3, 5-propyl-1-butyn-3-ol is rapidly consumed, the efficiency of the catalyst is released, and the organic acid generated by the reaction can further improve the efficiency of the catalyst, so that the rapid solidification of the temperature responsiveness trigger catalysis is realized.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.1 to 2.0wt%; the dispersion promoter is isopropyl tri (p-aminophenoxy) titanate; the catalyst is a platinum catalyst.
In a third aspect, the invention provides a method for preparing the injection-moldable ceramic organic silicon heat insulation material of the alkenyl-terminated heptapolyphenyl POSS, which comprises the following steps:
s1: preparation of a component A: uniformly mixing hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microspheres and a reaction rate regulator to obtain a component A;
s2: and (3) preparation of a component B: uniformly mixing phenyl silicone resin with low molecular weight and side chain hanging alkenyl, terminal alkenyl heptapolyphenyl POSS, silicon dioxide aerogel, spherical alumina, cobalt zinc ferrite complex, a dispersion promoter and a catalyst to obtain a component B;
s3: and uniformly mixing the component A and the component B, and heating and curing.
Preferably, in S1, hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microspheres and reaction rate regulator are mixed and stirred uniformly for 1-3h under the conditions that the temperature is lower than 40 ℃ and the vacuum degree is-0.01 to-0.1 Mpa, so as to obtain the component A.
Preferably, in S2, phenyl silicone resin with low molecular weight side chain hanging alkenyl, terminal alkenyl heptapolyphenyl POSS, silicon dioxide aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion accelerator and catalyst are mixed and stirred uniformly for 1-3h under the condition that the temperature is lower than 60 ℃ and the vacuum degree is-0.01 to-0.1 Mpa, so as to obtain the component B.
Preferably, in S3, the component A and the component B are uniformly mixed, heated to 50-90 ℃ for curing, and the curing is completed within 3 min.
Compared with the prior art, the invention has the following technical effects:
(1) According to the invention, the alkenyl heptapolyphenyl POSS is introduced into the ceramic organic silicon heat insulation material by utilizing hydrosilylation, so that after the phenyl POSS with huge volume is grafted on the main chain of the polymer, the intermolecular acting force can be reduced, the viscosity of a resin reaction system can be obviously reduced, and the ceramic organic silicon heat insulation material is prepared by an injection molding process.
(2) The invention prepares phenyl T7 trisiloxane by using phenyl siloxane, then prepares terminal alkenyl heptapolyphenyl POSS by using a unfilled corner closed loop method, and then accesses the terminal alkenyl heptapolyphenyl POSS into a reaction system by using hydrosilylation, adjusts the crosslinking density by controlling the introducing amount and the type, fully utilizes inorganic/organic hybridization to enhance the heat-insulating and heat-resisting effect, thereby obviously improving the heat resistance of the heat-insulating material.
(3) The invention is limited by the carbon chain length of the terminal alkenyl in the terminal alkenyl heptapolyphenyl POSS, so that the terminal alkenyl is not interfered by the phenyl POSS in the addition reaction, and the terminal alkenyl heptapolyphenyl POSS and the polymer viscosity after polymerization thereof are prevented from being too high.
(4) The invention prepares the cobalt zinc iron oxide complex in one step by utilizing a sol-gel precipitation method, and has simple process and good product stability. The prepared composite has a spinel structure, can be cooperatively embedded into a three-dimensional cross-linked network structure of a material with silicon dioxide aerogel, forms a compact continuous structure in a rivet networking mode, utilizes an inorganic-inorganic cooperative ceramic forming effect, and is easier to quickly form ceramic under a high-temperature condition. In addition, the cobalt zinc ferrite complex and the silicon dioxide aerogel have excellent heat resistance, and are more excellent than the heat resistance of a single system.
(5) The injection liquid of the raw materials of the ceramic heat insulation material has low viscosity, and can be suitable for injection molding process, so that the product has high precision and less flash, and the production efficiency is improved. In addition, the material can be used for coating the soft copper bar insulated wire, so that the space utilization rate of the battery pack can be improved, and the energy density of the power battery can be improved.
Detailed Description
The invention is further described below with reference to examples.
General examples
An application of alkenyl heptapolyphenyl POSS in preparing injection-moldable ceramic organic silicon heat-insulating material. The structural formula of the alkenyl heptapolyphenyl POSS is shown as follows:
wherein n=0 to 9, more preferably 3 to 6.
The application of the alkenyl heptapolyphenyl POSS in improving the injection molding processing adaptability of the ceramic organic silicon heat insulation material.
Preferably, the preparation route of the alkenyl heptapolyphenyl POSS is as follows:
the preparation method comprises the following steps: adding an organic solvent, sodium hydroxide and water into a reactor, uniformly stirring, dropwise adding phenyltriethoxysilane, heating to reflux after the dripping is finished, and reacting; cooling, vacuum removing organic solvent, adding another organic solvent for dissolving, cooling to-5-0 ℃, adding pyridine, dropwise adding alkenyl trichlorosilane with carbon chain length of 2-11 for reaction, heating for continuous reaction, and obtaining alkenyl heptapolyphenyl POSS.
An injection-moldable ceramic organic silicon heat-insulating material of an alkenyl heptapolyphenyl POSS is prepared by uniformly mixing a component A and a component B in a mass ratio of 1.5-2.5:1 and then heating and curing; wherein:
the component A comprises the following raw materials in percentage by mass: the hydrogen-containing silicone oil (the hydrogen content is 0.1-2.0 wt%) 20-50%, the silicon dioxide aerogel 5-25%, the cobalt zinc ferrite complex 5-25%, the hollow glass microsphere 5-20%, the reaction rate regulator (preferably formed by mixing butyl succinic anhydride and 3, 5-propyl-1-butine-3-alcohol in an excessive amount, and more preferably 1:1.05-1.2) 0-1%.
The component B comprises the following raw materials in percentage by mass: 20-45% of phenyl silicone resin with low molecular weight side chain hanging alkenyl, 5-15% of terminal alkenyl heptapolyphenyl POSS, 5-25% of silica aerogel, 5-25% of spherical alumina, 15-25% of cobalt zinc ferrite complex, 1-5% of dispersion promoter (preferably isopropoxy tris (p-aminophenoxy) titanate) and 0.1-0.3% of catalyst (preferably platinum catalyst).
Preferably, the phenyl silicone resin with low molecular weight side chain hanging alkenyl has the following structural formula:
wherein X is 4-10.
The synthetic route of the phenyl silicone resin with the low molecular weight side chain hanging alkenyl is as follows:
the preparation method comprises the following steps: uniformly mixing methyl phenyl dichlorosilane, methyl alkenyl dichlorosilane and diphenyl diethoxysilane in an inert gas atmosphere with the water content of 0.05-0.1wt%, dripping the mixture into a reaction system with an ice salt bath, controlling the temperature to be-25-15 ℃, continuously reacting for 4-8 hours after dripping, separating out generated HCl during the dripping, removing inert gas, heating to room temperature, continuously reacting for 4-8 hours, dripping trimethyl chlorosilane for end-capping reaction, heating to 70-90 ℃ after dripping, continuously reacting for 10-15 hours, distilling under reduced pressure to remove low-boiling substances, and then heating to 140-160 ℃ for structural reforming for 20-30 hours to obtain the phenyl silicone resin with low molecular weight side chain hanging alkenyl. Wherein the molar ratio of the methyl phenyl dichlorosilane to the methyl alkenyl dichlorosilane to the diphenyl diethoxy silane to the trimethyl chlorosilane is (0.7-0.9) to (0.1-0.3) to (0.8-1.2) to (0.1-0.3).
Preferably, the cobalt zinc ferrite complex is CoZnFe 4 O 8 The preparation reaction formula is as follows: 4Fe (NO) 3 ) 3 +Co(NO 3 ) 2 +7O 2 +Zn(NO 3 ) 2 +6C 6 H 8 O 7 →COZnFe 4 O 8 +8N 2 +36CO 2 +24H 2 O. The preparation method specifically comprises the following steps: fully dissolving ferric nitrate, cobalt nitrate, zinc nitrate and citric acid into water, heating to 85-95 ℃, continuously supplementing water under the bubbling action of continuous air flow, reacting, filtering and drying to obtain the cobalt-zinc-iron-oxygen complex.
The preparation method of the injection-moldable ceramic organic silicon heat insulation material of the alkenyl-terminated heptapolyphenyl POSS comprises the following steps:
s1: preparation of a component A: mixing and stirring hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microsphere and reaction rate regulator for 1-3h under the conditions that the temperature is lower than 40 ℃ and the vacuum degree is-0.01 to-0.1 Mpa, thus obtaining the component A.
S2: and (3) preparation of a component B: phenyl silicone resin with low molecular weight and side chain hanging alkenyl, terminal alkenyl heptapolyphenyl POSS, silicon dioxide aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter and catalyst are mixed and stirred uniformly for 1-3h under the conditions that the temperature is lower than 60 ℃ and the vacuum degree is-0.01 to-0.1 Mpa, so that the component B is obtained.
S3: and uniformly mixing the component A and the component B, heating to 50-90 ℃ for curing, and finishing curing within 3 min.
Raw material preparation example 1: preparation of vinyl heptapolyphenyl POSS
200mL of tetrahydrofuran, 2.8g (0.07 mol) of sodium hydroxide and 3.34g of redistilled water were charged in a 500mL three-necked flask equipped with a condenser and a stirrer. After stirring uniformly, 30.66g (0.13 mol) of phenyltriethoxysilane was slowly added dropwise, and after the completion of the dropwise addition, the mixture was heated to reflux and reacted for 5 hours. After cooling to room temperature, tetrahydrofuran was removed in vacuo, and 100mL of methanol was added for dissolution. After sufficient dissolution, cooling to 0 ℃, adding 4.4g of pyridine, dropwise adding 3.0g (0.0186 mol) of vinyl trichlorosilane, reacting for 12 hours, heating to room temperature, continuing to react for 12 hours, filtering, washing with methanol, and removing the solvent to obtain 18.2g of vinyl heptapolyphenyl polyhedral silsesquioxane (vinyl heptapolyphenyl POSS). The preparation route is as follows:
where n=0.
Raw material preparation example 2: preparation of octenyl heptapolyphenyl POSS
200mL of tetrahydrofuran, 2.8g (0.07 mol) of sodium hydroxide and 3.34g of redistilled water were charged in a 500mL three-necked flask equipped with a condenser and a stirrer. After stirring uniformly, 30.66g (0.13 mol) of phenyltriethoxysilane was slowly added dropwise, and after the completion of the dropwise addition, the mixture was heated to reflux and reacted for 5 hours. After cooling to room temperature, tetrahydrofuran was removed in vacuo, and 100mL of methanol was added for dissolution. After sufficient dissolution, cooling to 0 ℃, adding 4.4g of pyridine, dropwise adding 4.57g (0.0186 mol) of octenyl trichlorosilane, reacting for 12 hours, heating to room temperature, continuing to react for 12 hours, filtering, washing with methanol, and removing the solvent to obtain 19.6g of octenyl heptapolyphenyl polyhedral silsesquioxane (octenyl heptapolyphenyl POSS). The preparation route is as follows:
where n=6.
Raw material preparation example 3: preparation of undecenyl heptapolyphenyl POSS
200mL of tetrahydrofuran, 2.8g (0.07 mol) of sodium hydroxide and 3.34g of redistilled water were charged in a 500mL three-necked flask equipped with a condenser and a stirrer. After stirring uniformly, 30.66g (0.13 mol) of phenyltriethoxysilane was slowly added dropwise, and after the completion of the dropwise addition, the mixture was heated to reflux and reacted for 5 hours. After cooling to room temperature, tetrahydrofuran was removed in vacuo, and 100mL of methanol was added for dissolution. After sufficient dissolution, cooling to 0 ℃, adding 4.4g of pyridine, dropwise adding 5.35g (0.0186 mol) of undecenyl trichlorosilane, reacting for 12 hours, heating to room temperature, continuing to react for 12 hours, filtering, washing with methanol, and removing the solvent to obtain 20.2g of n-octenyl heptapolyphenyl polyhedral silsesquioxane (undecenyl heptapolyphenyl POSS). The preparation route is as follows:
where n=9.
Raw material preparation example 4: preparation of cobalt zinc ferrite complex
Ferric nitrate (96.7 g,0.4 mol), cobalt nitrate (18.3 g,0.1 mol), zinc nitrate (18.9 g,0.1 mol), citric acid (115.3 g,0.6 mol) are fully dissolved in secondary distilled water, the mixture is heated to 90 ℃, the secondary distilled water is continuously supplemented under the bubbling action of continuous air flow, the reaction is carried out for 24 hours, and the cobalt-zinc-iron-oxygen complex is obtained after filtration and vacuum drying, and the yield is 99.8%. The reaction formula is as follows: 4Fe (NO) 3 ) 3 +Co(NO 3 ) 2 +7O 2 +Zn(NO 3 ) 2 +6C 6 H 8 O 7 →CoZnFe 4 O 8 +8N 2 +36CO 2 +24H 2 O
Raw material preparation example 5: preparation of phenyl silicone resin with low molecular weight side chain hanging alkenyl
Under the protection of nitrogen with the water content of 0.1wt%, methyl phenyl dichlorosilane (152.8 g,0.8 mol), methyl alkenyl dichlorosilane (28.2 g,0.2 mol) and diphenyl diethoxy silane (272.4 g,1 mol) are uniformly mixed, dropwise added into a reaction system with ice salt bath, the temperature is controlled at-18 ℃, HCl generated is filtered out through vacuum equipment after dropwise addition, continuous reaction is carried out for 6 hours, the suction filtration equipment is removed, inert gas is removed, the temperature is raised to room temperature, after continuous reaction for 6 hours, trimethyl chlorosilane (21.8 g,0.2 mol) is slowly dropwise added for carrying out end-capping reaction, after dropwise addition is completed, the temperature is raised to 80 ℃, after continuous reaction for 12 hours, low-boiling substances are removed through reduced pressure distillation, then the temperature is raised to 150 ℃, and the structure is reformed for 24 hours, so as to obtain phenyl silicone resin with low molecular weight side chain hanging alkenyl.
The product passes GPC testing, mn is 3654, mw is 6943, and dispersity is 1.90. The viscosity of the system was 1.54 Pa.S as measured by a rotational viscometer. The preparation route is as follows:
preparation examples of silicone insulation:
the component A and the component B are uniformly mixed according to the weight ratio of 2:1, and are obtained after heating and curing.
The formula of the component A is specifically as follows: 20-50wt% of hydrogen-containing silicone oil, 5-25wt% of silica aerogel, 5-25wt% of cobalt-zinc-iron oxide complex, 5-20wt% of hollow glass microspheres and 0-1wt% of reaction rate regulator.
Wherein, the hydrogen-containing silicone oil is provided by Guangdong silicon new material science and technology Co., ltd, the silicon dioxide aerogel is provided by the consolidated general Shanzhong bright bright composite material Co., ltd, the cobalt zinc ferrite composite is prepared by raw material preparation example 4, the hollow glass microsphere is provided by Shanxi He Nuo technology Co., ltd, and the reaction rate regulator is formed by mixing butyl succinic anhydride and 3, 5-propyl-1-butyn-3-ol according to a mol ratio of 1:1.1.
Preparation of component A (A1): 45.5 parts of hydrogen-containing silicone oil (hydrogen content is 0.18%), 19 parts of silicon dioxide aerogel, 20 parts of cobalt zinc iron oxide complex, 15 parts of hollow glass microspheres and 0.5 part of reaction rate regulator are added into a high-speed dispersion planetary stirrer, the temperature is controlled below 40 ℃ to be mixed and stirred for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component A (A1) is obtained.
Preparation of component A (A2): 40.5 parts of hydrogen-containing silicone oil (hydrogen content is 0.8%) is added into a high-speed dispersion planetary mixer, the temperature is controlled below 40 ℃ for mixing and stirring for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component A (A2) is obtained.
Preparation of component A (A3): 35 parts of hydrogen-containing silicone oil (hydrogen content is 1.5%), 19 parts of silicon dioxide aerogel, 25 parts of cobalt zinc iron oxide complex, 20 parts of hollow glass microspheres and 1 part of reaction rate regulator are added into a high-speed dispersion planetary stirrer, the temperature is controlled below 40 ℃, the mixture is mixed and stirred for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component A (A3) is obtained.
The formula of the component B is specifically as follows: 20-45wt% of phenyl silicone resin with low molecular weight side chain hanging alkenyl, 5-15wt% of alkenyl heptapolyphenyl POSS, 5-25wt% of silica aerogel, 5-25wt% of spherical alumina, 15-25wt% of cobalt zinc ferrite complex, 1-5wt% of dispersion promoter and 0.1-0.3wt% of platinum catalyst.
Wherein, the phenyl silicone resin with low molecular weight side chain hanging alkenyl is prepared by raw material preparation example 5, the terminal alkenyl heptapolyphenyl POSS is prepared by raw material preparation examples 1-3, the silicon dioxide aerogel is provided by the composite material Co., ltd. Of the general sharp bright, the spherical alumina is provided by the composite material Co., ltd. Of the Zibo-starter, the cobalt zinc iron oxide composite is prepared by raw material preparation example 4, the dispersion promoter is isopropyl tris (p-aminophenoxy) titanate, and the platinum catalyst is KARSTEDT catalyst.
Preparation of component B (B1): 40 parts of phenyl silicone resin with alkenyl hanging on a low molecular weight side chain, 15 parts of vinyl heptapolyphenyl POSS (example 1), 18 parts of silicon dioxide aerogel, 5 parts of spherical alumina, 17 parts of cobalt zinc ferrite complex, 4.9 parts of dispersion accelerator and 0.1 part of KARSTEDT catalyst are added into a high-speed dispersion planetary mixer, the temperature is controlled below 60 ℃ for mixing and stirring for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component B (B1) is obtained.
Preparation of component B (B2): 35 parts of phenyl silicone resin with alkenyl hanging on a low molecular weight side chain, 10 parts of vinyl heptapolyphenyl POSS (example 1), 13 parts of silicon dioxide aerogel, 21 parts of spherical alumina, 16 parts of cobalt zinc ferrite complex, 4.9 parts of dispersion promoter and 0.1 part of KARSTEDT catalyst are added into a high-speed dispersion planetary mixer, the temperature is controlled below 60 ℃ for mixing and stirring for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component B (B2) is obtained.
Preparation of component B (B3): 30 parts of phenyl silicone resin with alkenyl hanging side chains with low molecular weight, 5 parts of vinyl heptapolyphenyl POSS (example 1), 13 parts of silicon dioxide aerogel, 25 parts of spherical alumina, 22 parts of cobalt zinc ferrite complex, 4.9 parts of dispersion accelerator and 0.1 part of KARSTEDT catalyst are added into a high-speed dispersion planetary mixer, the temperature is controlled below 60 ℃ for mixing and stirring for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component B (B3) is obtained.
Preparation of component B (B4): 30 parts of phenyl silicone resin with low molecular weight side chain hanging alkenyl, 5 parts of octenyl heptapolyphenyl POSS (example 2), 13 parts of silicon dioxide aerogel, 25 parts of spherical alumina, 22 parts of cobalt zinc iron oxide complex, 4.9 parts of dispersion accelerator and 0.1 part of KARSTEDT catalyst are added into a high-speed dispersion planetary mixer, the temperature is controlled below 60 ℃ for mixing and stirring for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component B (B4) is obtained.
Preparation of component B (B5): 30 parts of phenyl silicone resin with low molecular weight side chain hanging alkenyl, 5 parts of undecenyl heptapolyphenyl POSS (example 3), 13 parts of silicon dioxide aerogel, 25 parts of spherical alumina, 22 parts of cobalt zinc iron oxide complex, 4.9 parts of dispersion accelerator and 0.1 part of KARSTEDT catalyst are added into a high-speed dispersion planetary mixer, the temperature is controlled below 60 ℃ for mixing and stirring for 2 hours, the vacuum degree is-0.1 Mpa, and the mixture is discharged after being uniformly stirred, so that the component B (B5) is obtained.
The component A and the component B are uniformly mixed according to the ratio of 2:1, and the viscosity is lower, so that the injection molding composition is suitable for injection molding. Heating to 80 ℃, and curing within 3 min.
Curing example
Curing example 1: a1+E1;
curing example 2: me2+ethyl2;
curing example 3: a3+E3;
curing example 4: a3+E4;
curing example 5: me3+ethyl5.
Comparative example
Comparative example 1: the difference compared to curing example 3 is that the B component does not contain terminal alkenyl heptapolyphenyl POSS and is replaced by phenyl silicone resin with equal mass and low molecular weight side chain hanging alkenyl.
The formula of the component B (B6) is as follows: 35 parts of phenyl silicone resin with alkenyl hanging side chains with low molecular weight, 13 parts of silicon dioxide aerogel, 25 parts of spherical alumina, 22 parts of cobalt zinc ferrite complex, 4.9 parts of dispersion promoter and 0.1 part of KARSTEDT catalyst.
Comparative example 2: the difference compared with curing example 3 is that the component B (B7) is a phenyl silicone resin having an equal mass of a high molecular weight side chain pendant alkenyl group, and the phenyl silicone resin having a high molecular weight side chain pendant alkenyl group has an average molecular weight Mn of 10w.
Comparative example 3: the difference compared with curing example 3 is that the component A and the component B do not contain cobalt zinc iron oxide complex and are replaced by silicon dioxide aerogel, hollow glass microspheres and spherical alumina.
The formula of the component A (A4) is as follows: 35 parts of hydrogen-containing silicone oil (hydrogen content 1.5%), 29 parts of silica aerogel, 35 parts of hollow glass microspheres and 1 part of reaction rate regulator.
The formula of the component B (B8) is as follows: 30 parts of phenyl silicone resin with alkenyl hanging side chains with low molecular weight, 5 parts of vinyl heptapolyphenyl POSS (example 1), 20 parts of silicon dioxide aerogel, 40 parts of spherical alumina, 4.9 parts of a dispersion promoter and 0.1 part of KARSTEDT catalyst.
Performance testing
The organosilicon heat insulation materials obtained by mixing, heating and curing different components A and B are subjected to performance test, and the data are shown in the following table:
*1 the back surface temperature of the coating is measured by continuously spraying the high-temperature flame for 30min on the front surface of the coating with the thickness of 0.3 mm. The viscosity before curing is measured by sampling after the components A and B are uniformly mixed.
*2 The commercial comparative example is a silicone thermal insulation coating (supplied by Ningbo Convergence) prepared by a commercial molding technique.
The comparison of the data in the table above shows that:
the viscosities of the inventive cure examples 1-5 are lower in terms of the viscosity of the mixture prior to curing than comparative examples 1 and 2 and are therefore well suited for injection molding processes. The reason is that comparative example 1 differs from curing example 3 in that the b component is replaced with phenyl silicone resin having an equal mass of low molecular weight side chain pendant alkenyl groups, resulting in an increase in material viscosity due to the lack of viscosity reduction of phenyl POSS; whereas comparative example 2 differs from curing example 3 in that the phenyl silicone of low molecular weight side chain pendant alkenyl groups is replaced with phenyl silicone of equal mass of high molecular weight side chain pendant alkenyl groups in component b, too high a molecular weight leads to an increase in the viscosity of the system. Comparing curing examples 3-5, it can be seen that the viscosity of curing example 4 is slightly higher than that of curing example 3, because octenyl heptapolyphenyl POSS is added in curing example 4, the viscosity is slightly increased compared with that of the vinyl heptapolyphenyl POSS added in curing example 3, but the vinyl carbon chain length of the vinyl heptapolyphenyl POSS is shorter, the participation rate of the addition reaction is lower due to steric hindrance, the crosslinking density is reduced, and the tensile strength of the material after curing is obviously inferior to that of curing example 4; it was also found that the viscosity of curing example 5 was significantly higher than that of curing example 3, because the addition of undecenyl heptapolyphenyl POSS in curing example 5 had a longer alkenyl carbon chain length, which increased the viscosity of the system to some extent. In addition, compared to curing examples 1-5, the commercial products of the commercial comparative examples cannot be injection molded, only a molding process can be used, and the curing time is more than 20 minutes. And curing examples 1-5 only need less than or equal to 5min, and the curing time is short.
In addition, curing examples 1 to 5 were also found to be significantly superior to each comparative example in terms of tensile strength, heat insulation and heat resistance.
The raw materials and equipment used in the invention are common raw materials and equipment in the field unless specified otherwise; the methods used in the present invention are conventional in the art unless otherwise specified.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent transformation of the above embodiment according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. The application of the alkenyl heptapolyphenyl POSS in preparing the injection-moldable ceramic organic silicon heat insulation material is characterized in that: the structural formula of the alkenyl heptapolyphenyl POSS is shown as follows:
wherein n=0-9.
2. The application of the alkenyl heptapolyphenyl POSS in improving the injection molding processing adaptability of the ceramic organic silicon heat insulation material is characterized in that: the structural formula of the alkenyl heptapolyphenyl POSS is shown as follows:
wherein n=0-9.
3. Use according to claim 1 or 2, characterized in that: the preparation route of the alkenyl heptapolyphenyl POSS comprises the following steps:
4. a use according to claim 3, wherein: the preparation method of the alkenyl-terminated heptapolyphenyl POSS comprises the following steps: adding an organic solvent, sodium hydroxide and water into a reactor, uniformly stirring, dropwise adding phenyltriethoxysilane, heating to reflux after the dripping is finished, and reacting; cooling, vacuum removing organic solvent, adding another organic solvent for dissolving, cooling to-5-0 ℃, adding pyridine, dropwise adding alkenyl trichlorosilane with carbon chain length of 2-11 for reaction, heating for continuous reaction, and obtaining alkenyl heptapolyphenyl POSS.
5. An injection-moldable ceramic organic silicon heat-insulating material of an alkenyl-terminated heptapolyphenyl POSS is characterized in that: the adhesive is prepared by uniformly mixing the components including the component A and the component B and then heating and curing; wherein: the component A comprises the following raw materials: hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microspheres and a reaction rate regulator;
the component B comprises the following raw materials: phenyl silicone with low molecular weight side chain hanging alkenyl, alkenyl-terminated heptapolyphenyl POSS, silica aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter and catalyst for the application according to any one of claims 1 to 4.
6. The injection moldable ceramic silicone insulation material of an alkenyl heptapolyphenyl POSS of claim 5, wherein:
the component A comprises the following raw materials in percentage by mass: 20-50% of hydrogen-containing silicone oil, 5-25% of silicon dioxide aerogel, 5-25% of cobalt zinc ferrite complex, 5-20% of hollow glass microsphere and 0-1% of reaction rate regulator;
the component B comprises the following raw materials in percentage by mass: 20-45% of phenyl silicone resin with low molecular weight side chain hanging alkenyl, 5-15% of alkenyl heptapolyphenyl POSS, 5-25% of silica aerogel, 5-25% of spherical alumina, 15-25% of cobalt zinc ferrite complex, 1-5% of dispersion promoter and 0.1-0.3% of catalyst.
7. The injection moldable ceramic silicone insulation material of an alkenyl heptapolyphenyl POSS of claim 5 or 6, wherein:
the structural formula of the phenyl silicone resin with the low molecular weight side chain hanging alkenyl is as follows:
wherein X is 4-10; and/or
The cobalt zinc iron oxide complex is CoZnFe 4 O 8 。
8. A method for preparing an injection-moldable ceramic organosilicon thermal insulation material of an alkenyl-terminated heptapolyphenyl POSS according to any one of claims 5-7, comprising the steps of:
s1: preparation of a component A: uniformly mixing hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microspheres and a reaction rate regulator to obtain a component A;
s2: and (3) preparation of a component B: uniformly mixing phenyl silicone resin with low molecular weight and side chain hanging alkenyl, terminal alkenyl heptapolyphenyl POSS, silicon dioxide aerogel, spherical alumina, cobalt zinc ferrite complex, a dispersion promoter and a catalyst to obtain a component B;
s3: and uniformly mixing the component A and the component B, and heating and curing.
9. The method of preparing as claimed in claim 8, wherein:
in S1, mixing and stirring hydrogen-containing silicone oil, silicon dioxide aerogel, cobalt zinc ferrite complex, hollow glass microspheres and a reaction rate regulator uniformly under the conditions that the temperature is lower than 40 ℃ and the vacuum degree is between-0.01 and-0.1 Mpa to obtain a component A;
s2, mixing and stirring phenyl silicone resin with low molecular weight side chain hanging alkenyl, alkenyl heptapolyphenyl POSS, silicon dioxide aerogel, spherical alumina, cobalt zinc ferrite complex, dispersion promoter and catalyst uniformly under the conditions that the temperature is lower than 60 ℃ and the vacuum degree is between-0.01 and-0.1 Mpa to obtain a component B;
and S3, uniformly mixing the component A and the component B, and heating to 50-90 ℃ for curing.
10. An injection moldable ceramic silicone insulation material of an alkenyl-terminated heptapolyphenyl-based POSS according to any one of claims 5-7 or an injection moldable ceramic silicone insulation material of an alkenyl-terminated heptapolyphenyl-based POSS obtained by the preparation method of claim 8 or 9, characterized in that: the viscosity of the injection-moldable ceramic organic silicon heat insulation material before curing is less than or equal to 25 Pa.S, the curing time is less than or equal to 5min, and the tensile strength after curing and molding is more than or equal to 1.7MPa.
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