CN112795106A - Modified ethylene propylene diene monomer composite material and preparation method thereof - Google Patents
Modified ethylene propylene diene monomer composite material and preparation method thereof Download PDFInfo
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- CN112795106A CN112795106A CN202011629027.9A CN202011629027A CN112795106A CN 112795106 A CN112795106 A CN 112795106A CN 202011629027 A CN202011629027 A CN 202011629027A CN 112795106 A CN112795106 A CN 112795106A
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- Prior art keywords
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- ethylene propylene
- propylene diene
- diene monomer
- foaming
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- 239000002131 composite material Substances 0.000 title claims abstract description 78
- 229920002943 EPDM rubber Polymers 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000005187 foaming Methods 0.000 claims abstract description 70
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 claims abstract description 39
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000003063 flame retardant Substances 0.000 claims abstract description 29
- 229920001971 elastomer Polymers 0.000 claims abstract description 27
- 239000005060 rubber Substances 0.000 claims abstract description 27
- 239000006229 carbon black Substances 0.000 claims abstract description 21
- 239000004088 foaming agent Substances 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 229920005549 butyl rubber Polymers 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims description 47
- 238000004898 kneading Methods 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 23
- 238000004073 vulcanization Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 22
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 12
- 239000004925 Acrylic resin Substances 0.000 claims description 11
- 229920000178 Acrylic resin Polymers 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 10
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 10
- 238000003801 milling Methods 0.000 claims description 10
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 9
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 9
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 9
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 7
- 239000000347 magnesium hydroxide Substances 0.000 claims description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 7
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 7
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000009966 trimming Methods 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 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 claims description 4
- ICGLPKIVTVWCFT-UHFFFAOYSA-N 4-methylbenzenesulfonohydrazide Chemical compound CC1=CC=C(S(=O)(=O)NN)C=C1 ICGLPKIVTVWCFT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004156 Azodicarbonamide Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 4
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 4
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 230000035939 shock Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 15
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 10
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 7
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 6
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 6
- -1 ethylene, propylene Chemical group 0.000 description 6
- XZTOTRSSGPPNTB-UHFFFAOYSA-N phosphono dihydrogen phosphate;1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N)=N1.OP(O)(=O)OP(O)(O)=O XZTOTRSSGPPNTB-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910052684 Cerium Inorganic materials 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 5
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 5
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0038—Use of organic additives containing phosphorus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0085—Use of fibrous compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/38—Destruction of cell membranes
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/18—Binary blends of expanding agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/05—Open cells, i.e. more than 50% of the pores are open
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/16—Ethene-propene or ethene-propene-diene copolymers
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08J2423/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08J2423/22—Copolymers of isobutene; butyl rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2453/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2453/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
Abstract
The invention relates to the technical field of rubber, in particular to a modified ethylene propylene diene monomer composite material and a preparation method thereof. The ethylene propylene diene monomer composite material comprises the following raw materials in parts by weight: the feed comprises the following raw materials in parts by weight: 80-90 parts of ethylene propylene diene monomer, 6-10 parts of EVA resin, 8-15 parts of butyl rubber, 6-10 parts of modified SEBS, 5-9 parts of composite flame retardant, 3-6 parts of carbon black, 2-4 parts of vulcanizing agent, 3-6 parts of foaming agent, 1.5-3.5 parts of foaming promoter and 12-18 parts of functional auxiliary agent. The ethylene propylene diene monomer composite material has good mechanical property and flame retardance, good shock absorption performance, excellent slow rebound property, comfortable hand feeling, simple and convenient operation of the preparation method, easy control, good stability of the prepared ethylene propylene diene monomer composite material and contribution to industrial mass production.
Description
Technical Field
The invention relates to the technical field of rubber, in particular to a modified ethylene propylene diene monomer composite material and a preparation method thereof.
Background
Ethylene propylene diene monomer is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, is one of ethylene propylene rubbers, is represented by EPDM (ethylene propylene diene monomer), has excellent ozone resistance, heat resistance and weather resistance because the main chain of the ethylene propylene diene monomer is composed of chemically stable saturated hydrocarbon and only contains unsaturated double bonds in the side chains, and can be widely used in the fields of automobile parts, waterproof materials for buildings, wire and cable sheaths, adhesive tapes and the like. However, most of the existing ethylene propylene diene rubbers have poor shock absorption capability, cannot well realize slow rebound, and the mechanical property and the flame retardance of the ethylene propylene diene rubbers need to be improved.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the ethylene propylene diene monomer composite material which has good mechanical property and flame retardance, good shock absorption performance and excellent slow rebound property.
The invention also aims to provide a preparation method of the ethylene propylene diene monomer composite material, the preparation method is simple and convenient to operate and easy to control, and the prepared ethylene propylene diene monomer composite material has excellent comprehensive performance and good product stability and is beneficial to industrial mass production.
The purpose of the invention is realized by the following technical scheme: an ethylene propylene diene monomer composite material comprises the following raw materials in parts by weight: 80-90 parts of ethylene propylene diene monomer, 6-10 parts of EVA resin, 8-15 parts of butyl rubber, 6-10 parts of modified SEBS, 5-9 parts of composite flame retardant, 3-6 parts of carbon black, 2-4 parts of vulcanizing agent, 3-6 parts of foaming agent, 1.5-3.5 parts of foaming promoter and 12-18 parts of functional auxiliary agent.
According to the invention, the ethylene propylene diene monomer, the EVA resin, the butyl rubber and the modified SEBS are compounded and matched with the raw materials such as the composite flame retardant and the functional assistant, so that the prepared ethylene propylene diene monomer composite has good mechanical property and flame retardance, good shock absorption performance and excellent slow rebound property, and can slowly recover the original shape after being deformed by external force, has strong impact kinetic energy absorption and can be repeatedly used without permanent deformation. The ethylene propylene diene is preferably but not limited to ethylene propylene diene EPDM-K10. The EVA resin is preferably, but not limited to, Yanshan petrochemical EV A18J 3. The butyl rubber is preferably, but not limited to, Yanshan petrochemical IIR 1751.
Further, each part of the modified SEBS is prepared by the following steps:
s1, weighing 18-28 parts of SEBS and 0.5-1.5 parts of white carbon black by weight, adding into a reaction device, heating to 60-80 ℃, stirring at the speed of 200-400r/min for 20-40min, and cooling to obtain a mixture A for later use;
s2, weighing 1-3 parts of stannic chloride, 0.5-1.0 part of magnesium hydroxide and 1-3 parts of antioxidant 1010, adding the mixture A obtained in the step S1, heating to 50-70 ℃, continuing stirring for 20-40min, heating the mixed system to 150-200 ℃, sending the mixed system into a granulator, and extruding and granulating to obtain the modified SEBS.
The SEBS is modified by adopting the method and added into an ethylene propylene diene monomer system, so that the ethylene propylene diene monomer modified SEBS has the advantages of good mechanical property, air permeability, wear resistance, low-temperature flexibility, good bending resistance and the like; the addition of the white carbon black can reduce the total cost of the composite material and improve the mechanical property and the heat-resistant stability of the product; the surface of the white carbon black can be modified by the tin tetrachloride and the magnesium hydroxide, so that the white carbon black can be uniformly dispersed in the SEBS, and the modified SEBS and the ethylene terpolymer resin have good compatibility and good mechanical property, are suitable for producing high-rate foamed products, and improve the comprehensive performance of the product. The SEBS is preferably but not limited to a Yuanization 502T.
Further, each part of functional auxiliary agent comprises the following raw materials in parts by weight: 5-9 parts of acrylic resin, 2-4 parts of calcium oxide, 2-4 parts of magnesium sulfate whisker, 3-6 parts of polyethylene glycol and 3-6 parts of hydroxyethyl cellulose. According to the invention, the acrylic resin, the calcium oxide, the magnesium sulfate whisker, the polyethylene glycol and the hydroxyethyl cellulose are used, the magnesium sulfate whisker can be used as a flame retardant synergist and a reinforcing material, so that the impact resistance and the high flexural modulus of the composite material are improved, the acrylic resin and the hydroxyethyl cellulose are used as carriers of the calcium oxide and the magnesium sulfate whisker, the problems that the calcium oxide and the magnesium sulfate whisker are easy to agglomerate and disperse unevenly in a system can be effectively solved, the compatibility with ethylene propylene diene monomer, EVA resin, butyl rubber, modified SEBS and the like is improved, and the mechanical property and the aging resistance of the composite material are improved; acrylic resin, hydroxyethyl cellulose and polyethylene glycol can be matched with other resins, so that the flexibility of the composite material is improved, and the composite material has good slow rebound property. The acrylic resin is preferably, but not limited to, celluloseat 2010.
Further, the preparation method of the composite flame retardant comprises the following steps:
a1, adding 10-14 parts by weight of trimethylsilyl polyhedral oligomeric silsesquioxane, 3-5 parts by weight of vinyltrimethoxysilane, 18-24 parts by weight of 2, 2-bis (4-hydroxyphenyl) propane, 6-10 parts by weight of cyanuric chloride and 7-13 parts by weight of melamine pyrophosphate into 20-25 parts by weight of polyethylene glycol, and uniformly mixing to obtain a mixture A1;
a2, adding 1-2 parts of cerium molybdate, 4-8 parts of 2-aminopropane, 2-4 parts of aluminum hydroxide and 2-4 parts of nano titanium dioxide into the mixture A, heating to 55-65 ℃ under the condition of stirring, and preserving heat for 60-90min to obtain a mixture A2; and then washing with ionized water, drying and grinding to obtain the composite flame retardant.
According to the invention, 2-bis (4-hydroxyphenyl) propane, cyanuric chloride, cage octa (trimethylsiloxy) silsesquioxane and vinyl trimethoxy silane are adopted to coat melamine pyrophosphate, aluminum hydroxide and nano titanium dioxide to form a composite flame retardant, so that the ethylene propylene diene rubber has the characteristics of low toxicity, low smoke density and good flame retardant effect during combustion; the aluminum hydroxide adopted is an inorganic flame retardant, is environment-friendly and harmless, has stable performance in water, light and heat environments, is non-volatile, prevents fuming, does not produce drops and toxic gases, and does not pollute the environment after combustion; the surface modification of the nano titanium dioxide is carried out through the steps, so that the compatibility of the nano titanium dioxide with resin in ethylene propylene diene monomer is improved, the ultraviolet resistance, the antibacterial property and the ageing resistance of the composite material are improved, and the flame retardant property of the composite material is further improved.
Further, the foaming agent is at least one of azodimethylthiamine, azodicarbonamide and p-toluenesulfonyl hydrazide. The invention adopts the foaming agent to achieve good foaming effect in a system and high efficiency, and the prepared ethylene propylene diene monomer resin has good slow rebound property.
Further, the foaming promoter is at least one of stearic acid, zinc stearate and zinc oxide. According to the invention, the foaming promoter is matched with the foaming agent, and the auxiliary foaming agent improves the foaming effect of the ethylene propylene diene monomer composite material, so that the ethylene propylene diene monomer composite material is light and convenient, has comfortable hand feeling, has good slow rebound property, and has good shock absorption effect.
Further, the vulcanizing agent is at least one of di-tert-butyl peroxide and dicumyl peroxide. The vulcanizing agent is adopted as the vulcanizing agent, so that the crosslinking effect is good, and the ethylene propylene diene monomer rubber has excellent mechanical properties.
The invention also provides a preparation method of the ethylene propylene diene monomer composite material, which comprises the following steps:
step A, according to parts by weight, putting ethylene propylene diene monomer, EVA resin, butyl rubber, modified SEBS and carbon black into an internal mixer for first pressurization kneading, then adding a composite flame retardant, a functional auxiliary agent, a foaming agent and a foaming accelerant into the internal mixer for second pressurization kneading, then adding a vulcanizing agent for third pressurization kneading to prepare a mixture A;
step B, adding the mixture A prepared in the step A into a milling machine for hot milling, and then cooling to prepare a mixture B;
c, turning and cutting the mixture B prepared in the step B; then conveying the rubber sheets obtained by slitting into an extruder to extrude and filter rubber, and extruding the rubber sheets into rubber blanks; the outlet temperature of the extruder is 65-75 ℃.
D, conveying the rubber blank prepared in the step C into a mold of a vulcanizing machine for primary foaming; then, demolding and trimming to obtain a primary foaming material;
e, carrying out secondary foaming on the primary foaming material prepared in the step D to obtain a secondary foaming material;
and F, peeling the secondary foaming material prepared in the step E, performing hole breaking treatment, baking, and cooling to room temperature to obtain the ethylene propylene diene monomer composite material.
Further, in the step A, the temperature of the first pressure kneading is 90-110 ℃, and the pressure kneading time is 3-6 min; the second pressure kneading temperature is 90-110 deg.C, and the pressure kneading time is 8-14 min; the second pressure kneading temperature is 90-110 deg.C, and the pressure kneading time is 4-8 min.
Further, in the step D, the first foaming adopts closed-cell foaming in the membrane, the vulcanization temperature is 115-.
Further, in the step E, the second foaming is free foaming, the vulcanization temperature is 120-150 ℃, and the vulcanization time is 20-30 min.
Furthermore, in the step F, the baking temperature is 105-115 ℃, and the baking time is 90-120 min.
The preparation method of the ethylene propylene diene monomer composite material is simple and convenient to operate and easy to control, the open-cell foamed ethylene propylene diene monomer composite material is prepared by controlling the proportion of the raw materials and controlling the specific steps and process parameters, and the ethylene propylene diene monomer composite material has good mechanical property and flame retardance, good shock absorption performance, light weight, excellent slow rebound property, comfortable hand feeling, uniform pores, stable product quality and good weather resistance, and is beneficial to industrial mass production.
The invention has the beneficial effects that: the ethylene propylene diene monomer composite material has good mechanical property and flame retardance, good shock absorption performance, excellent slow rebound property and comfortable hand feeling. The preparation method of the ethylene propylene diene monomer composite material is simple and convenient to operate, easy to control and high in production efficiency, and the prepared ethylene propylene diene monomer composite material is good in stability and excellent in product performance and is beneficial to industrial mass production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
An ethylene propylene diene monomer composite material comprises the following raw materials in parts by weight: 85 parts of ethylene propylene diene monomer, 8 parts of EVA resin, 12 parts of butyl rubber, 8 parts of modified SEBS, 7 parts of composite flame retardant, 4 parts of carbon black, 3 parts of vulcanizing agent, 4 parts of foaming agent, 2.5 parts of foaming promoter and 15 parts of functional assistant. The ethylene propylene diene is ethylene propylene diene EPDM-K10. The EVA resin is Yanshan petrochemical EV A18J 3. The butyl rubber is Yanshan petrochemical IIR 1751.
Further, each part of the modified SEBS is prepared by the following steps:
s1, weighing 22 parts of SEBS and 1 part of white carbon black in parts by weight, adding into a reaction device, heating to 70 ℃, stirring at the speed of 300r/min for 30min, and cooling to obtain a mixture A for later use;
s2, weighing 2 parts by weight of tin tetrachloride, 0.8 part by weight of magnesium hydroxide and 2 parts by weight of antioxidant 1010, adding the mixture A obtained in the step S1, heating to 60 ℃, continuously stirring for 30min, heating the mixed system to 1580 ℃, sending the mixed system into a granulator, and extruding and granulating to obtain the modified SEBS. The SEBS is a Landization 502T.
Further, each part of functional auxiliary agent comprises the following raw materials in parts by weight: 7 parts of acrylic resin, 3 parts of calcium oxide, 3 parts of magnesium sulfate whisker, 5 parts of polyethylene glycol and 4 parts of hydroxyethyl cellulose. The acrylic resin is cellulous color 2010.
Further, the preparation method of the composite flame retardant comprises the following steps:
a1, adding 12 parts by weight of trimethylsilyl polyhedral oligomeric silsesquioxane, 4 parts by weight of vinyltrimethoxysilane, 21 parts by weight of 2, 2-bis (4-hydroxyphenyl) propane, 7 parts by weight of cyanuric chloride and 12 parts by weight of melamine pyrophosphate into 22 parts by weight of polyethylene glycol, and uniformly mixing to obtain a mixture A1;
a2, adding 1.5 parts of cerium molybdate, 6 parts of 2-aminopropane, 3 parts of aluminum hydroxide and 3 parts of nano titanium dioxide into the mixture A, heating to 60 ℃ under the condition of stirring, and preserving heat for 75min to obtain a mixture A2; and then washing with ionized water, drying and grinding to obtain the composite flame retardant.
Further, the foaming agent is composed of azodimethylthiamine and p-toluenesulfonyl hydrazide in a weight ratio of 1: 1.
Further, the foaming accelerant is composed of stearic acid and zinc oxide according to the weight ratio of 1: 1.
Further, the vulcanizing agent is composed of di-tert-butyl peroxide and dicumyl peroxide according to a weight ratio of 2: 1.
The preparation method of the ethylene propylene diene monomer composite material comprises the following steps:
step A, according to parts by weight, putting ethylene propylene diene monomer, EVA resin, butyl rubber, modified SEBS and carbon black into an internal mixer for first pressurization kneading, then adding a composite flame retardant, a functional auxiliary agent, a foaming agent and a foaming accelerant into the internal mixer for second pressurization kneading, then adding a vulcanizing agent for third pressurization kneading to prepare a mixture A;
step B, adding the mixture A prepared in the step A into a milling machine for hot milling, and then cooling to prepare a mixture B;
c, turning and cutting the mixture B prepared in the step B; then conveying the rubber sheets obtained by slitting into an extruder to extrude and filter rubber, and extruding the rubber sheets into rubber blanks; the exit temperature of the extruder was 70 ℃.
D, conveying the rubber blank prepared in the step C into a mold of a vulcanizing machine for primary foaming; then, demolding and trimming to obtain a primary foaming material;
e, carrying out secondary foaming on the primary foaming material prepared in the step D to obtain a secondary foaming material;
and F, peeling the secondary foaming material prepared in the step E, performing hole breaking treatment, baking, and cooling to room temperature to obtain the ethylene propylene diene monomer composite material.
Further, in the step A, the temperature of the first pressure kneading is 100 ℃, and the pressure kneading time is 4 min; the temperature of the second pressure kneading is 105 ℃, and the pressure kneading time is 12 min; the temperature of the second pressure kneading was 105 ℃ and the pressure kneading time was 6 min.
Further, in the step D, the first foaming adopts closed-cell foaming in the membrane, the vulcanization temperature is 120 ℃, the vulcanization pressure is 140MPa, and the vulcanization time is 25 min.
Further, in the step E, the second foaming adopts free foaming, the vulcanization temperature is 1350 ℃, and the vulcanization time is 25 min.
Further, in the step F, the baking temperature is 110 ℃, and the baking time is 100 min.
Example 2
An ethylene propylene diene monomer composite material comprises the following raw materials in parts by weight: 80 parts of ethylene propylene diene monomer, 6 parts of EVA resin, 85 parts of butyl rubber, 6 parts of modified SEBS, 5 parts of composite flame retardant, 3 parts of carbon black, 2 parts of vulcanizing agent, 3 parts of foaming agent, 1.5 parts of foaming promoter and 12 parts of functional assistant.
Further, each part of the modified SEBS is prepared by the following steps:
s1, weighing 18 parts of SEBS and 0.5 part of white carbon black in parts by weight, adding into a reaction device, heating to 60 ℃, stirring at the speed of 200r/min for 40min, and cooling to obtain a mixture A for later use;
s2, weighing 1 part of stannic chloride, 0.5 part of magnesium hydroxide and 1 part of antioxidant 1010, adding the weighed materials into the mixture A obtained in the step S1, heating to 50 ℃, continuously stirring for 40min, heating the mixed system to 150 ℃, feeding the heated mixed system into a granulator, and extruding and granulating to obtain the modified SEBS.
Further, each part of functional auxiliary agent comprises the following raw materials in parts by weight: 5 parts of acrylic resin, 2 parts of calcium oxide, 2 parts of magnesium sulfate whisker, 3 parts of polyethylene glycol and 3 parts of hydroxyethyl cellulose. Further, the preparation method of the composite flame retardant comprises the following steps:
a1, adding 10 parts by weight of trimethylsilyl polyhedral oligomeric silsesquioxane, 3 parts by weight of vinyltrimethoxysilane, 18 parts by weight of 2, 2-bis (4-hydroxyphenyl) propane, 6-10 parts by weight of cyanuric chloride and 7 parts by weight of melamine pyrophosphate into 20 parts by weight of polyethylene glycol, and uniformly mixing to obtain a mixture A1;
a2, adding 1 part of cerium molybdate, 4 parts of 2-aminopropane, 2 parts of aluminum hydroxide and 2 parts of nano titanium dioxide into the mixture A, heating to 55 ℃ under the stirring condition, and preserving heat for 90min to obtain a mixture A2; and then washing with ionized water, drying and grinding to obtain the composite flame retardant.
Further, the foaming agent is azodicarbonamide. The foaming accelerant is composed of zinc stearate and zinc oxide according to the weight ratio of 1.5: 1. The vulcanizing agent is di-tert-butyl peroxide.
The preparation method of the ethylene propylene diene monomer composite material comprises the following steps:
step A, according to parts by weight, putting ethylene propylene diene monomer, EVA resin, butyl rubber, modified SEBS and carbon black into an internal mixer for first pressurization kneading, then adding a composite flame retardant, a functional auxiliary agent, a foaming agent and a foaming accelerant into the internal mixer for second pressurization kneading, then adding a vulcanizing agent for third pressurization kneading to prepare a mixture A;
step B, adding the mixture A prepared in the step A into a milling machine for hot milling, and then cooling to prepare a mixture B;
c, turning and cutting the mixture B prepared in the step B; then conveying the rubber sheets obtained by slitting into an extruder to extrude and filter rubber, and extruding the rubber sheets into rubber blanks; the exit temperature of the extruder was 65 ℃.
D, conveying the rubber blank prepared in the step C into a mold of a vulcanizing machine for primary foaming; then, demolding and trimming to obtain a primary foaming material;
e, carrying out secondary foaming on the primary foaming material prepared in the step D to obtain a secondary foaming material;
and F, peeling the secondary foaming material prepared in the step E, performing hole breaking treatment, baking, and cooling to room temperature to obtain the ethylene propylene diene monomer composite material.
Further, the temperature of the first pressure kneading is 90 ℃, and the pressure kneading time is 3 min; the temperature of the second pressure kneading is 90 ℃, and the pressure kneading time is 14 min; the second pressure kneading temperature is 90-110 deg.C, and the pressure kneading time is 4 min.
Further, in the step D, the first foaming adopts closed-cell foaming in the membrane, the vulcanization temperature is 115 ℃, the vulcanization pressure is 130MPa, and the vulcanization time is 30 min.
Further, in the step E, the second foaming adopts free foaming, the vulcanization temperature is 120 ℃, and the vulcanization time is 30 min.
Further, in the step F, the baking temperature is 105 ℃, and the baking time is 120 min.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 3
An ethylene propylene diene monomer composite material comprises the following raw materials in parts by weight: 90 parts of ethylene propylene diene monomer, 10 parts of EVA resin, 15 parts of butyl rubber, 10 parts of modified SEBS, 9 parts of composite flame retardant, 6 parts of carbon black, 4 parts of vulcanizing agent, 6 parts of foaming agent, 3.5 parts of foaming promoter and 18 parts of functional assistant.
Further, each part of the modified SEBS is prepared by the following steps:
s1, weighing 28 parts of SEBS and 1.5 parts of white carbon black in parts by weight, adding into a reaction device, heating to 80 ℃, stirring at the speed of 400r/min for 20min, and cooling to obtain a mixture A for later use;
s2, weighing parts by weight of tin tetrachloride, 1.0 part by weight of magnesium hydroxide and 3 parts by weight of antioxidant 1010, adding the weighed parts into the mixture A obtained in the step S1, heating to 70 ℃, continuously stirring for 20-min, heating the mixed system to 200 ℃, feeding the heated mixed system into a granulator, and extruding and granulating to obtain the modified SEBS.
Further, each part of functional auxiliary agent comprises the following raw materials in parts by weight: 9 parts of acrylic resin, 4 parts of calcium oxide, 4 parts of magnesium sulfate whisker, 6 parts of polyethylene glycol and 6 parts of hydroxyethyl cellulose.
Further, the preparation method of the composite flame retardant comprises the following steps:
a1, adding 14 parts by weight of trimethylsilyl polyhedral oligomeric silsesquioxane, 5 parts by weight of vinyltrimethoxysilane, 24 parts by weight of 2, 2-bis (4-hydroxyphenyl) propane, 10 parts by weight of cyanuric chloride and 13 parts by weight of melamine pyrophosphate into 25 parts by weight of polyethylene glycol, and uniformly mixing to obtain a mixture A1;
a2, adding 2 parts of cerium molybdate, 8 parts of 2-aminopropane, 4 parts of aluminum hydroxide and 4 parts of nano titanium dioxide into the mixture A, heating to 65 ℃ under the stirring condition, and preserving heat for 60min to obtain a mixture A2; and then washing with ionized water, drying and grinding to obtain the composite flame retardant.
Further, the foaming agent is composed of azodicarbonamide and p-toluenesulfonyl hydrazide according to a weight ratio of 1: 2. The foaming accelerant is composed of stearic acid and zinc oxide according to the weight ratio of 1: 2. The vulcanizing agent is dicumyl peroxide.
The preparation method of the ethylene propylene diene monomer composite material comprises the following steps:
step A, according to parts by weight, putting ethylene propylene diene monomer, EVA resin, butyl rubber, modified SEBS and carbon black into an internal mixer for first pressurization kneading, then adding a composite flame retardant, a functional auxiliary agent, a foaming agent and a foaming accelerant into the internal mixer for second pressurization kneading, then adding a vulcanizing agent for third pressurization kneading to prepare a mixture A;
step B, adding the mixture A prepared in the step A into a milling machine for hot milling, and then cooling to prepare a mixture B;
c, turning and cutting the mixture B prepared in the step B; then conveying the rubber sheets obtained by slitting into an extruder to extrude and filter rubber, and extruding the rubber sheets into rubber blanks; the outlet temperature of the extruder is 65-75 ℃.
D, conveying the rubber blank prepared in the step C into a mold of a vulcanizing machine for primary foaming; then, demolding and trimming to obtain a primary foaming material;
e, carrying out secondary foaming on the primary foaming material prepared in the step D to obtain a secondary foaming material;
and F, peeling the secondary foaming material prepared in the step E, performing hole breaking treatment, baking, and cooling to room temperature to obtain the ethylene propylene diene monomer composite material.
Further, in the step A, the temperature of the first pressure kneading is 110 ℃, and the pressure kneading time is 3 min; the temperature of the second pressure kneading is 110 ℃, and the pressure kneading time is 8 min; the temperature of the second pressure kneading is 90 ℃, and the pressure kneading time is 8 min.
Further, in the step D, the first foaming adopts closed-cell foaming in the membrane, the vulcanization temperature is 145 ℃, the vulcanization pressure is 150MPa, and the vulcanization time is 20 min.
Further, in the step E, the second foaming adopts free foaming, the vulcanization temperature is 150 ℃, and the vulcanization time is 20 min.
Further, in the step F, the baking temperature is 115 ℃, and the baking time is 90 min.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Example 4
An ethylene propylene diene monomer composite material comprises the following raw materials in parts by weight: 82 parts of ethylene propylene diene monomer, 7 parts of EVA resin, 9 parts of butyl rubber, 7 parts of modified SEBS, 7 parts of composite flame retardant, 5 parts of carbon black, 3.5 parts of vulcanizing agent, 5 parts of foaming agent, 2.5 parts of foaming promoter and 15 parts of functional assistant.
Further, each part of the modified SEBS is prepared by the following steps:
s1, weighing 25 parts of SEBS and 1.2 parts of white carbon black according to parts by weight, adding into a reaction device, heating to 75 ℃, stirring at the speed of 350r/min for 35min, and cooling to obtain a mixture A for later use;
s2, weighing 2.5 parts of tin tetrachloride, 0.9 part of magnesium hydroxide and 2.5 parts of antioxidant 1010, adding the mixture A obtained in the step S1, heating to 65 ℃, continuously stirring for 35min, heating the mixed system to 180 ℃, feeding the mixed system into a granulator, and extruding and granulating to obtain the modified SEBS.
Further, each part of functional auxiliary agent comprises the following raw materials in parts by weight: 6 parts of acrylic resin, 2.5 parts of calcium oxide, 3.5 parts of magnesium sulfate whisker, 5 parts of polyethylene glycol and 4 parts of hydroxyethyl cellulose.
Further, the preparation method of the composite flame retardant comprises the following steps:
a1, adding 11 parts by weight of trimethylsilyl polyhedral oligomeric silsesquioxane, 3.5 parts by weight of vinyltrimethoxysilane, 22 parts by weight of 2, 2-bis (4-hydroxyphenyl) propane, 7 parts by weight of cyanuric chloride and 10 parts by weight of melamine pyrophosphate into 22 parts by weight of polyethylene glycol, and uniformly mixing to obtain a mixture A1;
a2, adding 1.8 parts of cerium molybdate, 5 parts of 2-aminopropane, 2.5 parts of aluminum hydroxide and 3 parts of nano titanium dioxide into the mixture A, heating to 60 ℃ under the stirring condition, and preserving heat for 75min to obtain a mixture A2; and then washing with ionized water, drying and grinding to obtain the composite flame retardant.
The rest of this embodiment is the same as embodiment 1, and is not described herein again.
Comparative example 1
This comparative example differs from example 1 above in that: the comparative example does not contain a functional aid. The remainder of this comparative example is the same as example 1 and will not be described again here.
Comparative example 2 this comparative example differs from example 1 above in that: this comparative example differs from example 3 above in that: in the comparative example, the SEBS is not modified, and the flame retardant CQFR-1010 is used for replacing the composite flame retardant in the example 1. The remainder of this comparative example is the same as example 1 and will not be described again here.
The performance of examples 1 to 4 of the present invention and comparative examples 1 to 2 was measured, and the thickness of the ethylene propylene diene monomer composite material was 100mm, and the measurement results were as follows:
detection conditions are as follows: the temperature is 23 +/-3 ℃, and the humidity is 65 +/-5%. The compression set is measured by GB/T6669-2008; the tensile strength was determined using GB/T528-2009; the tear strength was determined according to GB/T10808-2006; the slow rebound recovery time is measured by GB/T26392-2011. Examples 1-4 and comparative examples 1-2 did not show cracking, crazing and color change when subjected to ozone aging testing according to GB/T3511-2018. The combustion rating was determined according to GB/T11020-2005, examples 1-4 and comparative example 1 being grade FH-1, comparative example 2 being grade FH-2. The flame retardancy of examples 1-4 and comparative example 1 was superior to that of comparative example 2. Examples 1 to 4 had densities of 0.11 to 0.14g/cm3The Shore hardness is 12-15.
The ethylene propylene diene monomer composite material has good mechanical property and flame retardance, good shock absorption performance, excellent slow rebound property and comfortable hand feeling, the preparation method is simple and convenient to operate and easy to control, and the prepared ethylene propylene diene monomer composite material is good in stability and beneficial to industrial mass production.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A modified ethylene propylene diene monomer composite material is characterized in that: the feed comprises the following raw materials in parts by weight: 80-90 parts of ethylene propylene diene monomer, 6-10 parts of EVA resin, 8-15 parts of butyl rubber, 6-10 parts of modified SEBS, 5-9 parts of composite flame retardant, 3-6 parts of carbon black, 2-4 parts of vulcanizing agent, 3-6 parts of foaming agent, 1.5-3.5 parts of foaming promoter and 12-18 parts of functional auxiliary agent.
2. The modified ethylene propylene diene monomer composite material of claim 1, wherein: each part of the modified SEBS is prepared by the following steps:
s1, weighing 18-28 parts of SEBS and 0.5-1.5 parts of white carbon black by weight, adding into a reaction device, heating to 60-80 ℃, stirring at the speed of 200-400r/min for 20-40min, and cooling to obtain a mixture A for later use;
s2, weighing 1-3 parts of stannic chloride, 0.5-1.0 part of magnesium hydroxide and 1-3 parts of antioxidant 1010, adding the mixture A obtained in the step S1, heating to 50-70 ℃, continuing stirring for 20-40min, heating the mixed system to 150-200 ℃, sending the mixed system into a granulator, and extruding and granulating to obtain the modified SEBS.
3. The modified ethylene propylene diene monomer composite material of claim 1, wherein: each part of functional auxiliary agent comprises the following raw materials in parts by weight: 5-9 parts of acrylic resin, 2-4 parts of calcium oxide, 2-4 parts of magnesium sulfate whisker, 3-6 parts of polyethylene glycol and 3-6 parts of hydroxyethyl cellulose.
4. The modified ethylene propylene diene monomer composite material of claim 1, wherein: the foaming agent is at least one of azodimethylthiamine, azodicarbonamide and p-toluenesulfonyl hydrazide.
5. The modified ethylene propylene diene monomer composite material of claim 1, wherein: the foaming promoter is at least one of stearic acid, zinc stearate and zinc oxide.
6. The modified ethylene propylene diene monomer composite material of claim 1, wherein: the vulcanizing agent is at least one of di-tert-butyl peroxide and dicumyl peroxide.
7. A method for preparing the modified ethylene propylene diene monomer composite material of any one of claims 1 to 6, which is characterized in that: the method comprises the following steps:
step A, according to parts by weight, putting ethylene propylene diene monomer, EVA resin, butyl rubber, modified SEBS and carbon black into an internal mixer for first pressurization kneading, then adding a composite flame retardant, a functional assistant, a foaming agent and a foaming accelerant into the internal mixer for second pressurization kneading, then adding a vulcanizing agent for third pressurization kneading to prepare a mixture A;
step B, adding the mixture A prepared in the step A into a milling machine for hot milling, and then cooling to prepare a mixture B;
c, turning and cutting the mixture B prepared in the step B; then conveying the rubber sheets obtained by slitting into an extruder to extrude and filter rubber, and extruding the rubber sheets into rubber blanks;
d, conveying the rubber blank prepared in the step C into a mold of a vulcanizing machine for primary foaming; then, demolding and trimming to obtain a primary foaming material;
e, carrying out secondary foaming on the primary foaming material prepared in the step D to obtain a secondary foaming material;
and F, peeling the secondary foaming material prepared in the step E, performing hole breaking treatment, baking, and cooling to room temperature to obtain the ethylene propylene diene monomer composite material.
8. The preparation method of the modified ethylene propylene diene monomer composite material according to claim 7, wherein the preparation method comprises the following steps: in the step D, the first foaming adopts closed-cell foaming in the film, the vulcanization temperature is 115-145 ℃, the vulcanization pressure is 130-150MPa, and the vulcanization time is 20-30 min.
9. The preparation method of the modified ethylene propylene diene monomer composite material according to claim 7, wherein the preparation method comprises the following steps: in the step E, the second foaming adopts free foaming, the vulcanization temperature is 120-150 ℃, and the vulcanization time is 20-30 min.
10. The preparation method of the modified ethylene propylene diene monomer composite material according to claim 7, wherein the preparation method comprises the following steps: in the step F, the baking temperature is 105-115 ℃, and the baking time is 90-120 min.
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