CN113025056A - Conductive silicone rubber and preparation method thereof - Google Patents
Conductive silicone rubber and preparation method thereof Download PDFInfo
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- CN113025056A CN113025056A CN202110208065.5A CN202110208065A CN113025056A CN 113025056 A CN113025056 A CN 113025056A CN 202110208065 A CN202110208065 A CN 202110208065A CN 113025056 A CN113025056 A CN 113025056A
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- conductive
- silicone rubber
- rubber
- polyphenol
- carbon
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 117
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229920001971 elastomer Polymers 0.000 claims abstract description 79
- 239000000463 material Substances 0.000 claims abstract description 79
- 239000005060 rubber Substances 0.000 claims abstract description 79
- 239000011246 composite particle Substances 0.000 claims abstract description 50
- 239000006229 carbon black Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008117 stearic acid Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 49
- 235000013824 polyphenols Nutrition 0.000 claims description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 36
- 239000000945 filler Substances 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 30
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 25
- 239000002184 metal Substances 0.000 claims description 25
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 23
- 239000001263 FEMA 3042 Substances 0.000 claims description 23
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 23
- 235000015523 tannic acid Nutrition 0.000 claims description 23
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 23
- 229940033123 tannic acid Drugs 0.000 claims description 23
- 229920002258 tannic acid Polymers 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000011231 conductive filler Substances 0.000 claims description 16
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 12
- 238000004513 sizing Methods 0.000 claims description 12
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 12
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000004898 kneading Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 238000004073 vulcanization Methods 0.000 claims description 10
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 4
- 235000019359 magnesium stearate Nutrition 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 229920005560 fluorosilicone rubber Polymers 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims description 2
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 claims description 2
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- AFSDNFLWKVMVRB-UHFFFAOYSA-N Ellagic acid Chemical compound OC1=C(O)C(OC2=O)=C3C4=C2C=C(O)C(O)=C4OC(=O)C3=C1 AFSDNFLWKVMVRB-UHFFFAOYSA-N 0.000 claims description 2
- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 claims description 2
- 229920002079 Ellagic acid Polymers 0.000 claims description 2
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229930014669 anthocyanidin Natural products 0.000 claims description 2
- 150000001452 anthocyanidin derivatives Chemical class 0.000 claims description 2
- 235000008758 anthocyanidins Nutrition 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000005487 catechin Nutrition 0.000 claims description 2
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 claims description 2
- 229940074393 chlorogenic acid Drugs 0.000 claims description 2
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 claims description 2
- 235000001368 chlorogenic acid Nutrition 0.000 claims description 2
- 229950001002 cianidanol Drugs 0.000 claims description 2
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 235000004132 ellagic acid Nutrition 0.000 claims description 2
- 229960002852 ellagic acid Drugs 0.000 claims description 2
- 235000004515 gallic acid Nutrition 0.000 claims description 2
- 229940074391 gallic acid Drugs 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- -1 methyl phenyl vinyl Chemical group 0.000 claims description 2
- FAARLWTXUUQFSN-UHFFFAOYSA-N methylellagic acid Natural products O1C(=O)C2=CC(O)=C(O)C3=C2C2=C1C(OC)=C(O)C=C2C(=O)O3 FAARLWTXUUQFSN-UHFFFAOYSA-N 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 claims description 2
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 12
- 241000872198 Serjania polyphylla Species 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000002905 metal composite material Substances 0.000 description 5
- 239000004342 Benzoyl peroxide Substances 0.000 description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 description 4
- 150000001721 carbon Chemical class 0.000 description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000002482 conductive additive Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 239000002096 quantum dot Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention relates to the technical field of rubber, in particular to conductive silicone rubber and a preparation method thereof, wherein the conductive silicone rubber comprises the following raw materials in parts by weight: 60-80 parts of raw silicon rubber, 8-20 parts of conductive composite particles, 5-20 parts of white carbon black, 0.2-1.4 parts of hydroxyl-terminated silicone oil, 0.2-2 parts of stearic acid material and 0.5-2 parts of vulcanizing agent. The invention takes the silicon rubber as the body, can better disperse the conductive particles by utilizing the characteristics of good flexibility, weather resistance, formability and the like, ensures that the conductive particles have good and uniform conductivity, and ensures that the conductive particles are applied to various life application scenes.
Description
Technical Field
The invention relates to the technical field of rubber, in particular to conductive silicone rubber and a preparation method thereof.
Background
With the rapid development of the electronic industry and information technology, electromagnetic waves are applied in large scale in the fields of electronic communication, satellite positioning, large data transmission, radar detection, medical diagnosis and the like, but the electromagnetic waves bring convenience to people, and meanwhile, the problem of electromagnetic radiation pollution is increasingly serious.
The key of the electromagnetic shielding composite material mainly depends on the performance of the conductive filler, and the current conductive filler mainly comprises two types of metal and carbon: the metal filler has high conductivity and good electromagnetic shielding effect, but in actual use, a large amount of metal is often required to be added to achieve the ideal shielding effect, so that the cost is increased, and excessive metal addition can cause the problems of poor compatibility between metal and a matrix, poor dispersibility of the metal filler and the like, so that the difficulty of a material processing process is increased, and the mechanical property of the whole material is reduced; the carbon-based filler has the advantages of low cost, low density and relatively good compatibility with a matrix, but the electromagnetic shielding effect is not ideal due to the low conductivity. At present, the preparation and exploration of the composite conductive filler are also carried out, mainly by an electrochemical method and a chemical method, and the defects of complex preparation process, large environmental pollution and the like exist.
In the electromagnetic shielding composite material substrate, silicone rubber has become one of the most favored electromagnetic shielding material substrates in recent years due to its many advantages of good flexibility, heat resistance, low temperature resistance, ozone resistance, weather resistance, oil resistance, chemical resistance, good biocompatibility and the like, and conductive silicone rubber also becomes one of the development directions of high-end electromagnetic shielding materials at present.
Patent CN106589966A discloses a conductive silicone rubber, in the patent technology, the conductive filler is mainly carbon series filler acetylene black, which has the characteristics of large addition amount, large specific surface area, weak conductivity and the like, and the production process thereof has the disadvantages of easy aggregation, difficult dispersion, difficult processing and the like, and is limited by the low conductivity of the acetylene black, and the prepared conductive silicone rubber has limited conductivity. Patent CN 110724382A discloses a conductive silicone rubber and a preparation process thereof, in the patent technology, conductive fillers mainly comprise conductive additives and polyaniline/metal quantum dots, wherein the conductive additives comprise conductive carbon black and indium tin oxide, and the conductivity of the conductive additives is improved by coating two coating layers with different indium tin ratios with the conductive carbon black. However, the whole preparation process of the technology comprises preparation of the conductive auxiliary agent and preparation of the polyaniline/metal quantum dot, the process flow is very complicated, and pollutants such as hydrochloric acid, stannic chloride, indium trichloride and the like are involved in the preparation process, so that the technology is not beneficial to large-scale industrial production.
Based on the above, there is a need for a conductive silicone rubber and a preparation process thereof, which solve the problems of the prior art.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the conductive silicone rubber, which takes silicone rubber as a body, can better disperse conductive particles by utilizing the characteristics of good flexibility, weather resistance, formability and the like, ensures that the conductive silicone rubber has good and uniform conductivity, and ensures that the conductive silicone rubber is applied to various life application scenes.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
the conductive silicone rubber comprises the following raw materials in parts by weight: 60-80 parts of raw silicon rubber, 8-20 parts of conductive composite particles, 5-20 parts of white carbon black, 0.2-1.4 parts of hydroxyl-terminated silicone oil, 0.2-2 parts of stearic acid material and 0.5-2 parts of vulcanizing agent.
The raw silicone rubber is one or a mixture of more of methyl vinyl silicone rubber, dimethyl silicone rubber, methyl phenyl vinyl silicone rubber, fluorosilicone rubber, nitrile silicone rubber, phenylene silicone rubber or silicon-nitrogen rubber
The conductive composite particles are composite particles of carbon-based conductive filler/metal/polyphenol, wherein the carbon-based conductive filler is any one or a mixture of carbon-based fillers such as carbon black, graphite, carbon fibers, carbon nanotubes and graphene. The metal is any one or a mixture of more of gold, silver, copper, aluminum, iron, nickel, zinc, zirconium and titanium. The polyphenol is plant polyphenol, and is one or more of tannic acid, chlorogenic acid, ellagic acid, anthocyanidin, catechin, gallic acid, catechol, and benzenetriol.
The preparation steps of the conductive composite particles are as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the carbon-series filler and polyphenol into deionized water, and uniformly stirring to obtain a dispersion liquid A of the carbon-series filler with the surface compounded with the polyphenol; the molar ratio of the carbon-based filler to the polyphenol is 1:5-6: 1;
step b: preparing a modified solution: dissolving a metal salt solution and polyphenol in pure water to prepare a modified solution B; the molar ratio of the metal salt solution to the polyphenol is 1:4-3: 1;
step c: slowly adding the modified solution B into the carbon-series filler dispersion liquid A after the polyphenol pretreatment, continuously stirring for reaction, and then filtering to obtain carbon-series conductive filler/metal/polyphenol composite particles; the volume ratio of the modified solution to the carbon filler dispersion liquid after polyphenol pretreatment is 0.05:1-0.8: 1.
The stearic acid material is one or more of stearic acid, zinc stearate and magnesium stearate
A preparation process of conductive silicone rubber comprises the following steps:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll, and premixing at the temperature of 140-160 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles wrapped by the silicone rubber into the first sizing material, and mixing at the temperature of 140-;
step 3, adding hydroxyl-terminated silicone oil and stearic acid materials into the rubber material prepared in the step 2, mixing for 10-30 minutes, controlling the banburying temperature within the range of 80-90 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 5-15 minutes, pressing and vulcanizing at high temperature for molding, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention takes the silicon rubber as the body, can better disperse the conductive particles by utilizing the characteristics of good flexibility, weather resistance, formability and the like, ensures that the conductive particles have good and uniform conductivity, and ensures that the conductive particles are applied to various life application scenes.
2. The invention takes the carbon series/metal composite material as the conductive composite particles, organically combines the advantages of high conductivity of the metal filler, light weight and low price of the carbon series filler, good compatibility with the matrix and the like, and reduces the cost of raw materials and the processing difficulty while obtaining the silicon rubber with excellent conductivity.
3. Compared with other conventional chemical methods, the preparation method of the carbon-series/metal composite particles is simpler, quicker and more universal in process, less in energy consumption, more green in preparation process, wide in polyphenol source, low in cost and more economic and effective in technological process; meanwhile, the polyphenol layer has good adhesion, so that the bonding performance of the filler and the matrix is improved, and the mechanical performance of the silicone rubber is improved.
Detailed Description
A specific embodiment of the present invention will be described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 70g of methyl vinyl silicone rubber crude rubber, 12g of conductive composite particles, 15g of white carbon black, 0.5g of hydroxyl-terminated silicone oil, 1.5g of zinc stearate and 1g of vulcanizing agent benzoyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive carbon black and the tannic acid into deionized water according to the molar ratio of 1:2, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with a certain polyphenol compounded on the surface.
Step b: preparing a modified solution: dissolving ferric chloride and tannic acid in pure water at a molar ratio of 1:3 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A of the conductive carbon black pretreated by the tannic acid (the volume ratio is 0.1:1), continuously stirring for reaction, and filtering to obtain the carbon-series conductive composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding methyl vinyl silicone rubber raw rubber and white carbon black into a mixing roll according to the formula, and premixing at 140 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first sizing material, and mixing at 140 ℃ to obtain a second sizing material;
step 3, adding hydroxyl-terminated silicone oil and zinc stearate into the rubber material prepared in the step 2, mixing for 20 minutes, controlling the banburying temperature to be 80 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 10 minutes, pressing and vulcanizing at high temperature for 5 minutes under the vulcanizing condition of 180 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 2
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 70g of methyl vinyl silicone rubber crude rubber, 10g of conductive composite particles, 17g of white carbon black, 0.5g of hydroxyl-terminated silicone oil, 1.5g of zinc stearate and 1g of vulcanizing agent benzoyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive carbon black and the tannic acid into deionized water according to the molar ratio of 1:2, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the surface compounded with polyphenol.
Step b: preparing a modified solution: dissolving ferric chloride and tannic acid in pure water at a molar ratio of 1:3 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A (volume ratio is 0.1:1) of the conductive carbon black pretreated by the tannic acid, continuously stirring for reaction, and filtering to obtain the carbon-series conductive composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding methyl vinyl silicone rubber raw rubber and white carbon black into a mixing roll according to the formula, and premixing at the temperature of 150 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first sizing material, and mixing at the temperature of 150 ℃ to obtain a second sizing material;
step 3, adding hydroxyl-terminated silicone oil and zinc stearate into the rubber material prepared in the step 2, mixing for 30 minutes, controlling the banburying temperature at 90 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 15 minutes, pressing and vulcanizing at high temperature for 3 minutes under the vulcanizing condition of 190 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 3
The conductive silicone rubber is prepared by weighing: 80g of methyl vinyl silicone rubber crude rubber, 10g of conductive composite particles, 5.1g of white carbon black, 1.4g of hydroxyl-terminated silicone oil, 2g of stearic acid and 1.5g of dicumyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive carbon black and the tannic acid into deionized water according to the molar ratio of 2:1, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the surface compounded with polyphenol.
Step b: preparing a modified solution: copper chloride and tannic acid were dissolved in pure water at a molar ratio of 1:2 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A (volume ratio of 0.2:1) of the conductive carbon black pretreated by the tannic acid, continuously stirring for reaction, and filtering to obtain the carbon-series conductive composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll according to the formula, and premixing at the temperature of 160 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first rubber material, and mixing at the temperature of 160 ℃ to obtain a second rubber material;
step 3, adding hydroxyl-terminated silicone oil and stearic acid into the rubber material prepared in the step 2, mixing for 10 minutes, controlling the banburying temperature at 90 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 15 minutes, pressing and vulcanizing at high temperature for 6 minutes under the vulcanizing condition of 150 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 4
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 50g of methyl vinyl silicone rubber crude rubber, 25g of nitrile silicone rubber crude rubber, 8g of conductive composite particles, 14g of white carbon black, 1g of hydroxyl-terminated silicone oil, 1.4g of zinc stearate and 1g of vulcanizing agent benzoyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the carbon nano tube and the tannic acid into deionized water according to the molar ratio of 1:5, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the surface compounded with the polyphenol.
Step b: preparing a modified solution: silver nitrate and tannic acid were dissolved in pure water at a molar ratio of 2:1 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A (volume ratio is 0.05:1) of the conductive carbon black pretreated by the tannic acid, continuously stirring for reaction, and filtering to obtain the carbon-series conductive filler/metal/polyphenol composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll according to the formula, and premixing at the temperature of 145 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first sizing material, and mixing at the temperature of 145 ℃ to obtain a second sizing material;
step 3, adding hydroxyl-terminated silicone oil and zinc stearate into the rubber material prepared in the step 2, mixing for 15 minutes, controlling the banburying temperature at 85 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 10 minutes, pressing and vulcanizing at a high temperature for 5 minutes under the vulcanizing condition of 165 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 5
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 55g of methyl vinyl silicone rubber crude rubber, 10g of fluorosilicone rubber, 13g of conductive composite particles, 20g of white carbon black, 0.2g of hydroxyl-terminated silicone oil, 1.3g of zinc stearate and 0.5g of vulcanizing agent benzoyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive carbon black and catechol into deionized water in a molar ratio of 1:5, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the polyphenol compounded on the surface.
Step b: preparing a modified solution: dissolving zinc chloride and catechol in pure water according to a molar ratio of 1:4 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A of the conductive carbon black pretreated by catechol (the volume ratio is 0.8:1), continuously stirring for reaction, and filtering to obtain the carbon series conductive filler/metal/polyphenol composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll according to the formula, and premixing at the temperature of 155 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first sizing material, and mixing at the temperature of 155 ℃ to obtain a second sizing material;
step 3, adding hydroxyl-terminated silicone oil and zinc stearate into the rubber material prepared in the step 2, mixing for 20 minutes, controlling the banburying temperature at 85 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 8 minutes, pressing and vulcanizing at a high temperature for 4 minutes under the condition that the vulcanizing temperature is 180 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 6
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 50g of methyl vinyl silicone rubber crude rubber, 10g of dimethyl silicon rubber crude rubber, 20g of conductive composite particles, 16.9g of white carbon black, 0.9g of hydroxyl-terminated silicone oil, 0.2g of zinc stearate and 2g of vulcanizing agent di-tert-butyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive graphite and the tannic acid into deionized water according to the molar ratio of 6:1, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the polyphenol compounded on the surface.
Step b: preparing a modified solution: ferric chloride and tannic acid were dissolved in pure water at a molar ratio of 1:1 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A of the conductive carbon black pretreated by the tannic acid (the volume ratio is 0.5:1), continuously stirring for reaction, and filtering to obtain the carbon-series conductive filler/metal/polyphenol composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll according to the formula, and premixing at the temperature of 155 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first sizing material, and mixing at the temperature of 155 ℃ to obtain a second sizing material;
step 3, adding hydroxyl-terminated silicone oil and zinc stearate into the rubber material prepared in the step 2, mixing for 20 minutes, controlling the banburying temperature to be 80 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 8 minutes, pressing and vulcanizing at high temperature for 4 minutes under the vulcanizing condition of 180 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 7
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 68g of raw methyl vinyl silicone rubber, 16.4g of conductive composite particles, 12.7g of white carbon black, 0.8g of hydroxyl-terminated silicone oil, 0.9g of magnesium stearate and 1.2g of vulcanizing agent dicumyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive carbon black and the tannic acid into deionized water according to the molar ratio of 3:1, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the surface compounded with polyphenol.
Step b: preparing a modified solution: the nickel sulfate and the tannic acid were dissolved in pure water at a molar ratio of 3:1 to prepare a modified solution B.
Step c: slowly adding the modified solution B into the dispersion liquid A of the conductive carbon black pretreated by the tannic acid (the volume ratio is 0.08:1), continuously stirring for reaction, and filtering to obtain the carbon-series conductive filler/metal/polyphenol composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll according to the formula, and premixing at 157 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first rubber material, and mixing at 157 ℃ to obtain a second rubber material;
step 3, adding hydroxyl-terminated silicone oil and magnesium stearate into the rubber material prepared in the step 2, mixing for 14 minutes, controlling the banburying temperature to be 80 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 9 minutes, pressing and vulcanizing at high temperature for 4 minutes under the vulcanizing condition of 185 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Example 8
The conductive silicone rubber is prepared by weighing the following components in parts by weight: 78g of methyl vinyl silicone rubber crude rubber, 9.8g of conductive composite particles, 9g of white carbon black, 0.7g of hydroxyl-terminated silicone oil, 0.7g of stearic acid and 1.8g of vulcanizing agent dicumyl peroxide.
The preparation process of the conductive composite particle is as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the conductive carbon black and the tannic acid into deionized water according to the molar ratio of 1:2, and uniformly stirring to obtain a dispersion liquid A of the conductive carbon black with the surface compounded with polyphenol.
Step b: preparing a modified solution: dissolving ferric chloride and tannic acid in pure water at a molar ratio of 1:3 to prepare a modified solution B.
Step c: and slowly adding the modified solution B into the dispersion liquid A of the conductive carbon black pretreated by the tannic acid, continuously stirring for reaction, and filtering to obtain the carbon-series conductive filler/metal/polyphenol composite particles.
The preparation process of the silicone rubber is as follows:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll according to the formula, and premixing at the temperature of 160 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles coated by the silicon rubber into the first rubber material, and mixing at the temperature of 160 ℃ to obtain a second rubber material;
step 3, adding hydroxyl-terminated silicone oil and stearic acid into the rubber material prepared in the step 2, mixing for 25 minutes, controlling the banburying temperature at 85 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 10 minutes, pressing and vulcanizing at a high temperature for 5 minutes under the vulcanizing condition of 165 ℃, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
Comparative example 1
An electrically conductive silicone rubber is prepared by the first embodiment of the Chinese patent with the publication number of CN 106589966A.
Comparative example 2
An electrically conductive silicone rubber is prepared from embodiment I of the Chinese patent with publication number CN 110724382A.
Comparative example 3
The conductive silicone rubber has the conductive composite particles replaced by the same amount of conductive carbon black, and the content of the other raw materials is the same as that of the conductive silicone rubber in example 1.
Comparative example 4
The conductive silicone rubber has the conductive composite particles replaced by equal amount of iron powder and the rest raw material content is the same as that of the example 1.
Comparative example 5
A conductive silicone rubber, the conductive composite particles were replaced with the same amount of the mixture of conductive carbon black and iron powder as in example 1, and the remaining raw material contents were the same as in example 1.
Evaluation:
the volume resistivity and tensile strength of the conductive silicone rubbers obtained in examples 1 to 8 of the present invention and comparative examples 1 to 5 were evaluated, respectively.
Evaluation index and test method:
the evaluation criteria were tensile strength: GB/T528-2009;
volume resistivity GB/T2349-2001
The results of comparing the properties of the conductive silicone rubbers obtained in examples 1 to 8 and comparative example are shown in Table 1.
TABLE 1 results of the Performance test of the conductive silicone rubbers obtained in examples 1 to 8 and comparative example
As can be seen from table 1, the conductive properties of the silicone rubber in the examples of the present invention are greatly improved compared to the conductive silicone rubber of the ordinary carbon-based filler (comparative example 1), and are close to or better than the conductive silicone rubber obtained in comparative example 2. However, the chemical modification method used in comparative example 2 involves various pollutants and has complicated preparation process and high application limitation.
The conductive performance and tensile strength of the embodiment 1-8 of the invention are better than those of the comparative example 3-5, and the obtained carbon series/metal composite particle filler has good conductive performance and good compatibility with a silicon rubber matrix.
In summary, the invention has the following advantages:
1. the invention takes the silicon rubber as the body, can better disperse the conductive particles by utilizing the characteristics of good flexibility, weather resistance, formability and the like, ensures that the conductive particles have good and uniform conductivity, and ensures that the conductive particles are applied to various life application scenes.
2. The invention takes the carbon series/metal composite material as the conductive composite particles, organically combines the advantages of high conductivity of the metal filler, light weight and low price of the carbon series filler, good compatibility with the matrix and the like, and reduces the cost of raw materials and the processing difficulty while obtaining the silicon rubber with excellent conductivity.
3. Compared with other conventional chemical methods, the preparation method of the carbon-series/metal composite particles is simpler, quicker and more universal in process, less in energy consumption, more green in preparation process, wide in polyphenol source, low in cost and more economic and effective in technological process; meanwhile, the polyphenol layer has good adhesion, so that the bonding performance of the filler and the matrix is improved, and the mechanical performance of the silicone rubber is improved.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. An electrically conductive silicone rubber characterized by: the raw materials comprise the following components in parts by weight: 60-80 parts of raw silicon rubber, 8-20 parts of conductive composite particles, 5-20 parts of white carbon black, 0.2-1.4 parts of hydroxyl-terminated silicone oil, 0.2-2 parts of stearic acid material and 0.5-2 parts of vulcanizing agent.
2. The conductive silicone rubber according to claim 1, wherein: the raw silicone rubber is any one or a mixture of more of methyl vinyl silicone rubber, dimethyl silicone rubber, methyl phenyl vinyl silicone rubber, fluorosilicone rubber, nitrile silicone rubber, phenylene silicone rubber or silicon nitrogen rubber.
3. The conductive silicone rubber according to claim 1, wherein: the conductive composite particles are carbon-based conductive filler/metal/polyphenol composite particles.
4. The conductive silicone rubber according to claim 3, wherein: the carbon-based conductive filler is any one or a mixture of carbon-based fillers such as carbon black, graphite, carbon fibers, carbon nanotubes and graphene.
5. The conductive silicone rubber according to claim 3, wherein: the metal is any one or a mixture of more of gold, silver, copper, aluminum, iron, nickel, zinc, zirconium and titanium.
6. The conductive silicone rubber according to claim 3, wherein: the polyphenol is plant polyphenol, and is one or more of tannic acid, chlorogenic acid, ellagic acid, anthocyanidin, catechin, gallic acid, catechol, and benzenetriol.
7. The conductive silicone rubber according to claim 3, wherein: the preparation steps of the conductive composite particles are as follows:
step a: pretreatment of carbon filler particle polyphenol: adding the carbon-series filler and polyphenol into deionized water, and uniformly stirring to obtain a dispersion liquid A of the carbon-series filler with the surface compounded with the polyphenol; the molar ratio of the carbon-based filler to the polyphenol is 1:5-6: 1;
step b: preparing a modified solution: dissolving a metal salt solution and polyphenol in pure water to prepare a modified solution B; the molar ratio of the metal salt solution to the polyphenol is 1:4-3: 1;
step c: slowly adding the modified solution B into the carbon-series filler dispersion liquid A after the polyphenol pretreatment, continuously stirring for reaction, and then filtering to obtain carbon-series conductive filler/metal/polyphenol composite particles; the volume ratio of the modified solution to the carbon filler dispersion liquid after polyphenol pretreatment is 0.05:1-0.8: 1.
8. The conductive silicone rubber according to claim 1, wherein: the stearic acid material is any one or a mixture of stearic acid, zinc stearate and magnesium stearate.
9. A preparation process of conductive silicone rubber comprises the following steps:
step 1, adding silicone rubber crude rubber containing vinyl end groups and white carbon black into a mixing roll, and premixing at the temperature of 140-160 ℃ to obtain a first rubber material;
step 2, adding the conductive composite particles wrapped by the silicone rubber into the first sizing material, and mixing at the temperature of 140-;
step 3, adding hydroxyl-terminated silicone oil and stearic acid materials into the rubber material prepared in the step 2, mixing for 10-30 minutes, controlling the banburying temperature within the range of 80-90 ℃ in the process, and vacuumizing to ensure that the pressure difference between the rubber material and the atmosphere is more than or equal to 0.07 MPa; and preparing a third rubber material.
And 4, adding a vulcanizing agent into the third rubber material, kneading for 5-15 minutes, pressing and vulcanizing at high temperature for molding, and finally carrying out secondary vulcanization to obtain the conductive silicone rubber.
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