CN111454484A - Solid-phase regenerated rubber and preparation method thereof - Google Patents
Solid-phase regenerated rubber and preparation method thereof Download PDFInfo
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- CN111454484A CN111454484A CN202010273119.1A CN202010273119A CN111454484A CN 111454484 A CN111454484 A CN 111454484A CN 202010273119 A CN202010273119 A CN 202010273119A CN 111454484 A CN111454484 A CN 111454484A
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- rubber
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- solid
- phase
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 201
- 239000005060 rubber Substances 0.000 title claims abstract description 201
- 239000007790 solid phase Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title abstract description 27
- 239000002699 waste material Substances 0.000 claims abstract description 82
- 239000000843 powder Substances 0.000 claims abstract description 71
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims description 35
- -1 tris (3-mercaptopropionic acid) trimethylolpropane ester Chemical class 0.000 claims description 29
- 239000005077 polysulfide Substances 0.000 claims description 17
- 229920001021 polysulfide Polymers 0.000 claims description 17
- 150000008117 polysulfides Polymers 0.000 claims description 17
- SGUVLZREKBPKCE-UHFFFAOYSA-N 1,5-diazabicyclo[4.3.0]-non-5-ene Chemical compound C1CCN=C2CCCN21 SGUVLZREKBPKCE-UHFFFAOYSA-N 0.000 claims description 14
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 12
- 229920000459 Nitrile rubber Polymers 0.000 claims description 11
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 11
- 229920001084 poly(chloroprene) Polymers 0.000 claims description 11
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 10
- 229920005556 chlorobutyl Polymers 0.000 claims description 10
- 239000010920 waste tyre Substances 0.000 claims description 10
- 229920005549 butyl rubber Polymers 0.000 claims description 9
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- WZRRRFSJFQTGGB-UHFFFAOYSA-N 1,3,5-triazinane-2,4,6-trithione Chemical compound S=C1NC(=S)NC(=S)N1 WZRRRFSJFQTGGB-UHFFFAOYSA-N 0.000 claims description 7
- 229920005555 halobutyl Polymers 0.000 claims description 7
- FVKFHMNJTHKMRX-UHFFFAOYSA-N 3,4,6,7,8,9-hexahydro-2H-pyrimido[1,2-a]pyrimidine Chemical compound C1CCN2CCCNC2=N1 FVKFHMNJTHKMRX-UHFFFAOYSA-N 0.000 claims description 6
- 244000043261 Hevea brasiliensis Species 0.000 claims description 6
- 229920005557 bromobutyl Polymers 0.000 claims description 6
- 239000011256 inorganic filler Substances 0.000 claims description 6
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 6
- 229920003052 natural elastomer Polymers 0.000 claims description 6
- 229920001194 natural rubber Polymers 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 6
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 4
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 2
- 229920003049 isoprene rubber Polymers 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- ACTRVOBWPAIOHC-UHFFFAOYSA-N succimer Chemical compound OC(=O)C(S)C(S)C(O)=O ACTRVOBWPAIOHC-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 4
- 238000007259 addition reaction Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 18
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 15
- 238000003756 stirring Methods 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 10
- MDWVSAYEQPLWMX-UHFFFAOYSA-N 4,4'-Methylenebis(2,6-di-tert-butylphenol) Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 MDWVSAYEQPLWMX-UHFFFAOYSA-N 0.000 description 8
- 239000003963 antioxidant agent Substances 0.000 description 8
- 230000003078 antioxidant effect Effects 0.000 description 8
- JOBBTVPTPXRUBP-UHFFFAOYSA-N [3-(3-sulfanylpropanoyloxy)-2,2-bis(3-sulfanylpropanoyloxymethyl)propyl] 3-sulfanylpropanoate Chemical compound SCCC(=O)OCC(COC(=O)CCS)(COC(=O)CCS)COC(=O)CCS JOBBTVPTPXRUBP-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- QSRJVOOOWGXUDY-UHFFFAOYSA-N 2-[2-[2-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]ethoxy]ethoxy]ethyl 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCCOCCOCCOC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 QSRJVOOOWGXUDY-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 description 5
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 5
- 239000010445 mica Substances 0.000 description 5
- 229910052618 mica group Inorganic materials 0.000 description 5
- 229910052901 montmorillonite Inorganic materials 0.000 description 5
- VFBJXXJYHWLXRM-UHFFFAOYSA-N 2-[2-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]ethylsulfanyl]ethyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCCSCCOC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 VFBJXXJYHWLXRM-UHFFFAOYSA-N 0.000 description 4
- 238000013016 damping Methods 0.000 description 4
- IUNMPGNGSSIWFP-UHFFFAOYSA-N dimethylaminopropylamine Chemical compound CN(C)CCCN IUNMPGNGSSIWFP-UHFFFAOYSA-N 0.000 description 4
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- AIAMDEVDYXNNEU-UHFFFAOYSA-N 6-methylheptyl propanoate Chemical compound CCC(=O)OCCCCCC(C)C AIAMDEVDYXNNEU-UHFFFAOYSA-N 0.000 description 3
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- CFXCGWWYIDZIMU-UHFFFAOYSA-N Octyl-3,5-di-tert-butyl-4-hydroxy-hydrocinnamate Chemical compound CCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 CFXCGWWYIDZIMU-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000003396 thiol group Chemical class [H]S* 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- VSTXCZGEEVFJES-UHFFFAOYSA-N 1-cycloundecyl-1,5-diazacycloundec-5-ene Chemical compound C1CCCCCC(CCCC1)N1CCCCCC=NCCC1 VSTXCZGEEVFJES-UHFFFAOYSA-N 0.000 description 1
- HCILJBJJZALOAL-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n'-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyl]propanehydrazide Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 HCILJBJJZALOAL-UHFFFAOYSA-N 0.000 description 1
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 1
- VSAWBBYYMBQKIK-UHFFFAOYSA-N 4-[[3,5-bis[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-2,4,6-trimethylphenyl]methyl]-2,6-ditert-butylphenol Chemical compound CC1=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C1CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VSAWBBYYMBQKIK-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 125000001501 propionyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- HERSKCAGZCXYMC-UHFFFAOYSA-N thiophen-3-ol Chemical compound OC=1C=CSC=1 HERSKCAGZCXYMC-UHFFFAOYSA-N 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 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
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
- C08K5/375—Thiols containing six-membered aromatic rings
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L17/00—Compositions of reclaimed rubber
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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
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/02—Copolymers with acrylonitrile
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/06—Copolymers with styrene
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- C08J2311/00—Characterised by the use of homopolymers or copolymers of chloroprene
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- C08J2321/00—Characterised by the use of unspecified rubbers
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- 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
- C08J2323/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08J2323/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
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- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
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- 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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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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Abstract
The invention discloses a solid-phase regenerated rubber and a preparation method thereof, wherein the solid-phase regenerated rubber is prepared from the following raw materials in parts by mass: 80-120 parts of waste rubber, 5-50 parts of multi-mercapto compound and 0.5-10 parts of alkaline catalyst. The invention utilizes residual unreacted double bonds in the waste rubber to generate mercapto-alkene addition reaction with mercapto in a multi-mercapto compound under the action of an alkaline catalyst, thereby realizing the re-bonding of waste rubber powder to form a rubber sheet to prepare solid phase regenerated rubber, and the solid phase regenerated rubber with better performance is obtained by matching with an auxiliary agent. The process of recycling the waste rubber does not need to use a solvent, and has mild reaction conditions and simple process.
Description
Technical Field
The invention relates to the technical field of waste rubber recycling, and particularly relates to solid-phase recycled rubber and a preparation method thereof.
Background
With the rapid development of society and economy, the demand of rubber is increasing. In daily life, rubber gains a very large market share by virtue of its excellent physicochemical properties. The rubber has wide application fields in various rubber gaskets and soles commonly used in life, rubber gloves and guide pipes in medical experimental articles, tires, conveyor belts and the like widely used in the transportation industry. However, the covalent network structure formed by vulcanization and crosslinking of rubber is insoluble and infusible, so that the rubber is difficult to recycle, which not only causes a great deal of rubber resource waste, but also brings about serious black pollution and influences the living environment of human beings. Therefore, the effective recycling of the waste rubber has great significance. At present, the waste rubber is recycled mainly by means of desulfurization treatment by physical, chemical or biological technologies and then is formed into regenerated rubber. However, these desulfurization processes not only require a large amount of energy consumption, but also generate a large amount of wastewater and exhaust gas, which causes secondary pollution to the environment, and do not conform to the principle of green chemistry. In recent years, different dynamic chemistries are introduced into a vulcanized rubber system to realize solid phase recycling of vulcanized rubber, for example, chinese patent CN105086326A discloses a hydrogen bond-ionic bond interpenetrating thermoreversible crosslinked rubber, which is subjected to hydrogen bond-ionic bond breakage at high temperature, and the opened hydrogen bond-ionic bond can be reformed again at low temperature, so that the vulcanized rubber exhibits thermoplastic processability, but the method needs to perform grafting modification of maleic anhydride, and uses alkylamine as a crosslinking agent for vulcanization; the grafting modification needs additional investment, and alkylamine has certain biological toxicity; the whole preparation method is too complicated and is not beneficial to industrial production.
Disclosure of Invention
The invention aims to solve the technical problems of complex recovery method of the existing waste rubber and the defect and deficiency of adding toxic substances, provides solid-phase regenerated rubber, utilizes waste rubber and multi-sulfhydryl compound in a certain proportion to perform sulfhydryl-alkene addition reaction under the action of an alkaline catalyst to prepare rubber which can be recycled, avoids adding substances with biological toxicity, has simple process and is non-toxic and harmless, and the preparation method can be directly used for recovering a large amount of waste rubber formed in industrial production.
The invention also aims to provide a preparation method of the solid-phase reclaimed rubber.
The above purpose of the invention is realized by the following technical scheme:
the solid-phase regenerated rubber is prepared from the following raw materials in parts by mass:
80-120 parts of waste rubber, 5-50 parts of multi-mercapto compound and 0.5-10 parts of alkaline catalyst.
The invention directly takes waste rubber produced in industry as raw material, and generates mercapto-alkene addition reaction with mercapto in multi-mercapto compound under the action of alkaline catalyst by means of residual unreacted double bond in the waste rubber, thereby realizing the re-bonding of waste rubber powder to form rubber sheet. The recovery process does not need solvent, the reaction condition is mild, and the process is simple.
Preferably, the feed additive is prepared from the following raw materials in parts by mass: 100-120 parts of waste rubber, 20-30 parts of multi-mercapto compound and 3-10 parts of alkaline catalyst.
More preferably, the raw material also comprises one or more of inorganic filler, halogenated butyl rubber and hindered phenol.
Further preferably, the feed additive is prepared from the following raw materials in parts by mass: 100-120 parts of waste rubber, 5-20 parts of inorganic filler, 20-30 parts of halogenated butyl rubber, 20-30 parts of multi-mercapto compound, 30-50 parts of hindered phenol and 3-10 parts of alkaline catalyst.
Preferably, the particle size of the waste rubber is 30-200 meshes.
Preferably, the waste rubber is one or a mixture of more than two of waste natural rubber, waste butyl rubber, waste polybutadiene rubber, waste ethylene propylene rubber, waste nitrile rubber, waste styrene butadiene rubber, waste chloroprene rubber, waste isoprene rubber and waste tire rubber.
Preferably, the multi-mercapto compound is one or a mixture of more than two of polysulfide rubber, 2, 3-dimercapto-1-propanol, tris (3-mercaptopropionic acid) trimethylolpropane ester, 2,4, 6-trimercapto-1, 3, 5-triazine and tetra (3-mercaptopropionic acid) pentaerythritol ester.
More preferably, the multi-mercapto compound is one or a mixture of more than two of polysulfide rubber, 2, 3-dimercapto-1-propanol, tris (3-mercaptopropionic acid) trimethylolpropane ester, 2,4, 6-trimercapto-1, 3, 5-triazine and tetra (3-mercaptopropionic acid) pentaerythritol ester.
Preferably, the basic catalyst comprises one or a mixture of more than two of triethylamine, pyridine, quinoline, diisopropylethylamine, triethylenediamine, 1, 8-diazabicycloundec-7-ene, 1, 5-diazabicyclo [4.3.0] non-5-ene, 1,5, 7-triazabicyclo [4.4.0] dec-5-ene, N-dimethyl-1, 3-propanediamine, N-dimethylaniline and 4-dimethylaminopyridine.
Preferably, the hindered phenol includes pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1010), N-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (antioxidant 1076), hexamethylenediamine N, N '-bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylene diamine (antioxidant 1098), isooctyl N, N' -bis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine (antioxidant 1024), 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene (antioxidant 1330), isooctyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (1135), triethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 245), 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 3115), bis [3, 5-di-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant), bis [3, 5-di-tert-butyl-4-hydroxy-5-methyl phenyl ] propionate ] (antioxidant), bis [3, 5-butyl-4-methyl ] phenol) ] (3, bis (3, 5-butyl-4-hydroxy-methyl) isocyanurate (3, 6-2, 6-bis (3, 5-bis-butyl-4-butyl-methyl) isocyanurate, 6-methyl) phenol, 5-bis (3, 5-bis (4-butyl-methyl) isocyanurate), bis (3, 6-butyl-hydroxy-phenyl) phenol), bis (4-thiophenol) isocyanurate, 5-thiobis (3, 5-4-methyl) phenol.
Preferably, the inorganic filler is one or a mixture of more than two of silica, carbon black, wollastonite, montmorillonite, calcium carbonate, mica powder and alumina.
Preferably, the halogenated butyl rubber is chlorinated butyl rubber and/or brominated butyl rubber.
The invention also protects the preparation method of the solid-phase regenerated rubber, which comprises the following steps:
s1, uniformly mixing waste rubber, adding other raw materials, and banburying for 5-20 min to prepare banburying rubber powder;
s2, vulcanizing the banburying rubber powder prepared in the step S1 for 10-150 min at the pressure of 5-20 MPa and the temperature of 60-130 ℃ to prepare the solid phase regenerated rubber.
Compared with the prior art, the invention has the beneficial effects that:
the solid phase regenerated rubber prepared by the invention directly takes waste rubber produced in industry as raw material, and generates mercapto-alkene addition reaction with mercapto group in a certain proportion of multi-mercapto compound under the action of alkaline catalyst by means of residual unreacted double bond in the waste rubber, thereby realizing the re-bonding of waste rubber powder particles to form rubber sheets, obtaining the solid phase regenerated rubber, and then adding auxiliary agents such as inorganic filler, halogenated butyl rubber, hindered phenol and the like to further improve the performance of the solid phase regenerated rubber. The mechanical property of the solid-phase regenerated rubber prepared by the method is improved to a certain extent compared with that of the waste rubber, the regenerated rubber treated by the preparation method disclosed by the invention can be applied to the fields of damping, shock absorption, shock insulation, noise reduction, sound insulation, sealing and the like, the industrial mass production is facilitated, the regeneration utilization rate of the waste rubber is improved, and the process for recycling the waste rubber does not need a solvent, so that the reaction condition is mild, and the process is simple. The used raw materials are very easy to obtain, and have market competitiveness and production value.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A solid-phase regenerated rubber is prepared from (by mass parts) waste natural rubber (200 meshes) (produced by Danyang Ruibang renewable resources Co., Ltd.) 100 parts, mica powder 5 parts, polysulfide rubber J L Y-12115 parts, and 1, 8-diazabicycloundecen-7-ene 3 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste natural rubber (100 meshes) into an internal mixer, uniformly mixing at a stirring speed of 50r/min, sequentially adding 5 parts of mica powder, J L Y-12115 parts of polysulfide rubber and 3 parts of 1, 8-diazabicycloundecene-7-ene, and internally mixing for 15min to obtain internal mixing rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 10MPa and at the temperature of 100 ℃ for 120min to prepare the solid-phase regenerated rubber.
Example 2
A solid-phase regenerated rubber is prepared from (by mass parts) waste natural rubber (200 meshes) (produced by Danyang Ruibang renewable resources Co., Ltd.) 100 parts, mica powder 5 parts, polysulfide rubber J L Y-12130 parts, and 1, 8-diazabicycloundecen-7-ene 3 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste natural rubber (100 meshes) into an internal mixer, uniformly mixing at a stirring speed of 50r/min, sequentially adding 5 parts of mica powder, J L Y-12130 parts of polysulfide rubber and 3 parts of 1, 8-diazabicycloundecene-7-ene, and internally mixing for 15min to obtain internal mixing rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 10MPa and at the temperature of 100 ℃ for 120min to prepare the solid-phase regenerated rubber.
Example 3
A solid-phase regenerated rubber is prepared from (by mass parts) waste nitrile-butadiene rubber powder (60 meshes) (produced by Danyang Ribang regenerated resources Co., Ltd.) 100 parts, polysulfide rubber J L Y-21520 parts, thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1035)20 parts, and 1, 5-diazabicyclo [4.3.0] non-5-ene 2 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste nitrile rubber powder (200 meshes) into an internal mixer, uniformly mixing at a stirring speed of 100r/min, sequentially adding 20 parts of polysulfide rubber J L Y-21520 parts, 20 parts of thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1035) and 2 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene, and internally mixing for 10min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 110 ℃ for 60min to prepare the solid-phase regenerated rubber.
Example 4
A solid-phase regenerated rubber is prepared from (by mass parts) waste nitrile-butadiene rubber powder (60 meshes) (produced by Danyang Ribang regenerated resources Co., Ltd.) 100 parts, polysulfide rubber J L Y-21520 parts, thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1035)40 parts, and 1, 5-diazabicyclo [4.3.0] non-5-ene 2 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste nitrile rubber powder (100 meshes) into an internal mixer, uniformly mixing at a stirring speed of 100r/min, sequentially adding 40 parts of polysulfide rubber J L Y-21520 parts, 40 parts of thiodiethylene bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1035) and 2 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene, and internally mixing for 10min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 110 ℃ for 60min to prepare the solid-phase regenerated rubber.
Example 5
A solid-phase regenerated rubber is prepared from (by mass parts) waste butyl rubber powder (60 meshes) (produced by Danyang Ruibang renewable resources Co., Ltd.) 100 parts, chlorinated butyl rubber 20 parts, pentaerythritol tetrakis (3-mercaptopropionate) 10 parts, diethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 245)30 parts, and N, N-dimethyl-1, 3-propanediamine 3 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste butyl rubber powder (100 meshes) into an internal mixer, uniformly mixing at the stirring speed of 100r/min, sequentially adding 20 parts of chlorinated butyl rubber, 10 parts of pentaerythritol tetrakis (3-mercaptopropionate) and 30 parts of diethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 245) and 3 parts of N, N-dimethyl-1, 3-propane diamine, and internally mixing for 15min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 10MPa and the temperature of 80 ℃ for 150min to prepare the solid-phase regenerated rubber.
Example 6
A solid-phase regenerated rubber is prepared from (by mass parts) waste butyl rubber powder (30 meshes) (produced by Danyang Ruibang renewable resources Co., Ltd.) 100 parts, chlorinated butyl rubber 20 parts, pentaerythritol tetrakis (3-mercaptopropionate) 10 parts, diethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 245)30 parts, and N, N-dimethyl-1, 3-propanediamine 3 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste butyl rubber powder (60 meshes) into an internal mixer, uniformly mixing at the stirring speed of 100r/min, sequentially adding 20 parts of chlorinated butyl rubber, 10 parts of pentaerythritol tetrakis (3-mercaptopropionate) and 30 parts of diethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 245) and 3 parts of N, N-dimethyl-1, 3-propane diamine, and internally mixing for 15min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 10MPa and the temperature of 80 ℃ for 150min to prepare the solid-phase regenerated rubber.
Example 7
The solid-phase regenerated rubber is prepared from the following raw materials in parts by mass: 100 parts of waste chloroprene rubber powder (100 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.), 10 parts of calcium carbonate, 20 parts of brominated butyl rubber, 20 parts of 2,4, 6-trimercapto-1, 3, 5-triazine, 40 parts of 4, 4' -methylenebis (2, 6-di-tert-butylphenol) (antioxidant 702) and 1 part of 1,5, 7-triazabicyclo [4.4.0] dec-5-ene.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste chloroprene rubber powder (200 meshes) into an internal mixer, uniformly mixing at a stirring speed of 100r/min, sequentially adding 10 parts of calcium carbonate, 20 parts of brominated butyl rubber, 20 parts of 2,4, 6-trimercapto-1, 3, 5-triazine, 40 parts of 4, 4' -methylenebis (2, 6-di-tert-butylphenol) (antioxidant 702) and 1 part of 1,5, 7-triazabicyclo [4.4.0] dec-5-ene, and internally mixing for 20min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 15MPa and at the temperature of 110 ℃ for 50min to prepare the solid-phase regenerated rubber.
Example 8
The solid-phase regenerated rubber is prepared from the following raw materials in parts by mass: 100 parts of waste chloroprene rubber powder (100 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.), 10 parts of calcium carbonate, 20 parts of brominated butyl rubber, 20 parts of 2,4, 6-trimercapto-1, 3, 5-triazine, 40 parts of 4, 4' -methylenebis (2, 6-di-tert-butylphenol) (antioxidant 702) and 3 parts of 1,5, 7-triazabicyclo [4.4.0] dec-5-ene.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste chloroprene rubber powder (200 meshes) into an internal mixer, uniformly mixing at a stirring speed of 70r/min, sequentially adding 10 parts of calcium carbonate, 20 parts of brominated butyl rubber, 20 parts of 2,4, 6-trimercapto-1, 3, 5-triazine, 40 parts of 4, 4' -methylenebis (2, 6-di-tert-butylphenol) (antioxidant 702) and 3 parts of 1,5, 7-triazabicyclo [4.4.0] dec-5-ene, and internally mixing for 20min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 15MPa and at the temperature of 110 ℃ for 50min to prepare the solid-phase regenerated rubber.
Example 9
A solid-phase regenerated rubber is prepared from (by mass parts) waste styrene-butadiene rubber (100 meshes) (produced by Wuhan Heilli rubber powder Co., Ltd.) 100 parts, montmorillonite 5 parts, 2, 3-dimercapto-1-propanol 30 parts, pentaerythrityl tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] 1010 parts, and triethylenediamine 3 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste styrene-butadiene rubber (100 meshes) into an internal mixer, uniformly mixing at a stirring speed of 100r/min, sequentially adding 5 parts of montmorillonite, 30 parts of 2, 3-dimercapto-1-propanol, 30 parts of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010) and 3 parts of triethylenediamine, and internally mixing for 10min to obtain internal mixing rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 10MPa and at the temperature of 130 ℃ for 120min to prepare the solid-phase regenerated rubber.
Example 10
A solid-phase regenerated rubber is prepared from (by mass parts) waste styrene-butadiene rubber (100 meshes) (produced by Wuhan Heilli rubber powder Co., Ltd.) 50 parts, waste butyl rubber powder (60 meshes) 50 parts, montmorillonite 5 parts, 2, 3-dimercapto-1-propanol 30 parts, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate 30 parts, and triethylenediamine 3 parts.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 50 parts of waste styrene-butadiene rubber (100 meshes) and 50 parts of waste butyl rubber powder (60 meshes) into an internal mixer, stirring at the speed of 100r/min, uniformly mixing, sequentially adding 5 parts of montmorillonite, 30 parts of 2, 3-dimercapto-1-propanol, 30 parts of β - (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate and 3 parts of triethylenediamine, and internally mixing for 10min to obtain internal mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 10MPa and at the temperature of 130 ℃ for 120min to prepare the solid-phase regenerated rubber.
Example 11
A solid-phase regenerated rubber is prepared from 50 parts by mass of waste chloroprene rubber (100 meshes) (produced by Danyang Ribang regenerated resource Co., Ltd.), 50 parts by mass of waste nitrile rubber (100 meshes), 10 parts by mass of silicon dioxide, 4 parts by mass of aluminum oxide, 10 parts by mass of tris (3-mercaptopropionic acid) trimethylolpropane ester, 5 parts by mass of 4' 4-dimercaptodiphenyl sulfide, 10 parts by mass of β - (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl propionate (antioxidant 1135) and 5 parts by mass of triethylamine.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 50 parts of waste chloroprene rubber (100 meshes) and 50 parts of waste nitrile rubber (100 meshes) into an internal mixer, stirring at the speed of 70r/min, uniformly mixing, sequentially adding 10 parts of silicon dioxide, 4 parts of aluminum oxide, 10 parts of tris (3-mercaptopropionic acid) trimethylolpropane ester, 5 parts of 4', 4-dimercaptodiphenyl sulfide, 10 parts of β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid isooctyl ester (antioxidant 1135) and 5 parts of triethylamine, and internally mixing for 20min to obtain internally mixed rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 120 ℃ for 100min to prepare the solid-phase regenerated rubber.
Example 12
The solid-phase regenerated rubber is prepared from 50 parts by mass of waste chloroprene rubber (100 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.), 50 parts by mass of waste nitrile rubber (100 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.), 10 parts by mass of silica, 4 parts by mass of alumina, 15 parts by mass of chlorinated butyl rubber, 15 parts by mass of polysulfide rubber J L Y-15520 parts by mass of tris (3-mercaptopropionic acid) trimethylolpropane ester and 10 parts by mass of 4-dimethylaminopyridine.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 50 parts of waste chloroprene rubber (100 meshes) and 50 parts of waste nitrile rubber (100 meshes) into an internal mixer, stirring at the speed of 100r/min, uniformly mixing, sequentially adding 10 parts of silicon dioxide, 4 parts of aluminum oxide, 15 parts of chlorinated butyl rubber, J L Y-15520 parts of polysulfide rubber, 5 parts of tris (3-mercaptopropionic acid) trimethylolpropane ester and 10 parts of 4-dimethylaminopyridine, and internally mixing for 15min to obtain internal mixing rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 15MPa and at the temperature of 100 ℃ for 150min to prepare the solid-phase regenerated rubber.
Example 13
A solid-phase regenerated rubber is prepared from (by mass parts) 100 parts of waste tyre rubber powder (200 meshes) (produced by Danyang Ruibang regenerated resources Co., Ltd.), 100 parts of polysulfide rubber J L Y-15530 parts, and 5 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste tire rubber powder (200 meshes) and 5 parts of polysulfide rubber J L Y-15530 and 1, 5-diazabicyclo [4.3.0] non-5-ene in sequence, and banburying for 15min to prepare banburying rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 100 ℃ for 100min to prepare the solid-phase regenerated rubber.
Example 14
A solid-phase regenerated rubber is prepared from (by mass parts) 100 parts of waste tyre rubber powder (200 meshes) (produced by Danyang Ruibang regenerated resources Co., Ltd.), 100 parts of polysulfide rubber J L Y-15520 parts, and 5 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste tire rubber powder (200 meshes) into 5 parts of polysulfide rubber J L Y-15520 parts and 1, 5-diazabicyclo [4.3.0] non-5-ene in sequence, and banburying for 15min to prepare banburying rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 100 ℃ for 100min to prepare the solid-phase regenerated rubber.
Example 15
The solid-phase regenerated rubber is prepared from the following raw materials in parts by mass: 100 parts of waste tire rubber powder (200 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.), 20 parts of pentaerythritol tetrakis (3-mercaptopropionate) and 5 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste tire rubber powder (200 meshes) and 20 parts of pentaerythritol tetra (3-mercaptopropionate) and 5 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene in sequence, and banburying for 10min to prepare banburying rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 100 ℃ for 100min to prepare the solid-phase regenerated rubber.
Example 16
The solid-phase regenerated rubber is prepared from the following raw materials in parts by mass: 100 parts of waste tire rubber powder (200 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.), 20 parts of 2, 3-dimercapto-1-propanol and 5 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene.
The preparation method of the solid-phase regenerated rubber comprises the following steps:
s1, adding 100 parts of waste tire rubber powder (200 meshes) and 20 parts of 2, 3-dimercapto-1-propanol and 5 parts of 1, 5-diazabicyclo [4.3.0] non-5-ene in sequence, and banburying for 10min to obtain banburying rubber powder;
s2, heating and vulcanizing the banburying rubber powder prepared in the step S1 in a flat vulcanizing machine under the pressure of 20MPa and at the temperature of 100 ℃ for 100min to prepare the solid-phase regenerated rubber.
Comparative example 1
The preparation method of this comparative example was:
s1, adding 50 parts of waste chloroprene rubber (100 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.) and 50 parts of waste nitrile rubber (100 meshes) into an internal mixer, stirring at a speed of 100r/min, uniformly mixing, sequentially adding 10 parts of silicon dioxide, 4 parts of aluminum oxide, 15 parts of chlorinated butyl rubber and 10 parts of 4-dimethylaminopyridine, and internally mixing for 15min to prepare internal mixing rubber powder;
step S2A solid-phase reclaimed rubber was obtained in the same manner as in example 1.
Comparative example 2
The preparation method of this comparative example was:
s1, adding 100 parts of waste butyl rubber powder (30 meshes) (produced by Danyang Ribang renewable resources Co., Ltd.) into an internal mixer, stirring at a speed of 100r/min, uniformly mixing, sequentially adding 20 parts of chlorinated butyl rubber, 10 parts of pentaerythritol tetrakis (3-mercaptopropionate) and 30 parts of diethylene glycol bis [ β - (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] (antioxidant 245), and internally mixing for 15min to obtain internal mixed rubber powder;
step S2A solid-phase reclaimed rubber was obtained in the same manner as in example 1.
Performance testing
1. Test method
A dumbbell plate sample is prepared by adopting a CMT4204 type microcomputer control electronic universal testing machine of Meitess Industrial System (China) Limited company, tested according to GB13022-1991 and the tensile rate of 50mm/min, and tested by adopting Metravib DMA-50N and the tensile mode is selected and the displacement is 1 × 10-5m, frequency 10Hz, heating the sample from-60 deg.C to 60 deg.C, taking the tan > 0.3 part as shown in Table 1, and heating rate 3 deg.C/min.
2. Test results
TABLE 1 dynamic mechanical Properties and mechanical Properties of solid-phase reclaimed rubbers obtained in examples of the present invention and comparative examples
As can be seen from the above table 1, in general, the regenerated rubber material prepared by the method of the present invention has certain mechanical strength and damping performance, and as the particle size of the rubber powder is reduced, the larger the specific surface area is, the stronger the interaction between the particles is, and the higher the mechanical property (tensile strength) of the regenerated rubber is; the damping performance of the regenerated rubber is higher along with the increase of the use amount of the hindered phenol; the mechanical strength of the regenerated rubber can be increased by increasing the consumption of the multi-sulfhydryl compound in a proper amount; the functionality of the multi-mercapto compound is increased, and the mechanical strength of the reclaimed rubber can be improved. The samples in the comparative example 1 lack the basic catalyst, while the samples in the comparative example 2 lack the multi-sulfhydryl compound, which causes the sulfhydryl-alkene reaction to be difficult to be rapidly and effectively carried out, thereby causing the interface of rubber powder particles to lack the covalent crosslinking effect, and the prepared regenerated rubber has weak mechanical strength, so that the damping temperature is difficult to detect, and the tensile strength and the elongation at break are not as good as those of the solid-phase regenerated rubber materials prepared in the examples. Therefore, the invention has certain application value and can realize solid phase recycling of the waste rubber.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The solid-phase regenerated rubber is characterized by comprising the following raw materials in parts by mass: 80-120 parts of waste rubber, 5-50 parts of multi-mercapto compound and 0.5-10 parts of alkaline catalyst.
2. The solid-phase reclaimed rubber according to claim 1, which is prepared from the following raw materials in parts by mass: 100-120 parts of waste rubber, 20-30 parts of multi-mercapto compound and 3-10 parts of alkaline catalyst.
3. The solid-phase reclaimed rubber according to claim 1, wherein the raw material further comprises one or more of inorganic filler, halogenated butyl rubber and hindered phenol.
4. The solid-phase reclaimed rubber according to claim 3, which is prepared from the following raw materials in parts by mass: 100-120 parts of waste rubber, 5-20 parts of inorganic filler, 20-30 parts of halogenated butyl rubber, 20-30 parts of multi-mercapto compound, 30-50 parts of hindered phenol and 3-10 parts of alkaline catalyst.
5. The solid-phase reclaimed rubber according to claim 1, wherein the particle size of the waste rubber is 30-200 meshes.
6. The solid-phase reclaimed rubber according to claim 1, wherein the waste rubber is one or a mixture of more than two of waste natural rubber, waste butyl rubber, waste polybutadiene rubber, waste ethylene propylene rubber, waste nitrile rubber, waste styrene butadiene rubber, waste chloroprene rubber, waste isoprene rubber and waste tire rubber.
7. The solid-phase reclaimed rubber according to claim 1, wherein the multi-mercapto compound is one or a mixture of two or more of polysulfide rubber, 4' 4-dimercaptodiphenylsulfide, 2, 3-dimercapto-1-propanol, 2, 3-dimercaptosuccinic acid, tris (3-mercaptopropionic acid) trimethylolpropane ester, 2,4, 6-trimercapto-1, 3, 5-triazine, and tetrakis (3-mercaptopropionic acid) pentaerythritol ester.
8. The solid-phase reclaimed rubber according to claim 1, wherein the basic catalyst comprises one or a mixture of two or more of triethylamine, pyridine, quinoline, diisopropylethylamine, triethylenediamine, 1, 8-diazabicycloundecen-7-ene, 1, 5-diazabicyclo [4.3.0] non-5-ene, 1,5, 7-triazabicyclo [4.4.0] dec-5-ene, N-dimethyl-1, 3-propanediamine, N-dimethylaniline and 4-dimethylaminopyridine.
9. The solid-phase reclaimed rubber according to claim 3 or 4, wherein the halogenated butyl rubber is chlorinated butyl rubber and/or brominated butyl rubber.
10. The method for preparing solid-phase reclaimed rubber according to any one of claims 1 to 9, comprising the steps of:
s1, uniformly mixing waste rubber, adding other raw materials, and banburying for 5-20 min to prepare banburying rubber powder;
s2, vulcanizing the banburying rubber powder prepared in the step S1 for 10-150 min at the pressure of 5-20 MPa and the temperature of 60-130 ℃ to prepare the solid phase regenerated rubber.
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