CN116854990A - Waste tire reclaimed rubber treatment process - Google Patents
Waste tire reclaimed rubber treatment process Download PDFInfo
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- CN116854990A CN116854990A CN202310775793.3A CN202310775793A CN116854990A CN 116854990 A CN116854990 A CN 116854990A CN 202310775793 A CN202310775793 A CN 202310775793A CN 116854990 A CN116854990 A CN 116854990A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000010920 waste tyre Substances 0.000 title claims abstract description 36
- 230000008569 process Effects 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 40
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 35
- 244000005700 microbiome Species 0.000 claims abstract description 35
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 claims abstract description 34
- 241000894006 Bacteria Species 0.000 claims abstract description 32
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000000813 microbial effect Effects 0.000 claims abstract description 26
- 241000605222 Acidithiobacillus ferrooxidans Species 0.000 claims abstract description 22
- 230000000593 degrading effect Effects 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 230000003009 desulfurizing effect Effects 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 238000002347 injection Methods 0.000 claims abstract description 8
- 239000007924 injection Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 48
- 239000001963 growth medium Substances 0.000 claims description 28
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 22
- 230000001580 bacterial effect Effects 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000010298 pulverizing process Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 230000001954 sterilising effect Effects 0.000 claims description 8
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical group CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000001110 calcium chloride Substances 0.000 claims description 7
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 7
- 235000011148 calcium chloride Nutrition 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 7
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 5
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004327 boric acid Substances 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 4
- 238000012258 culturing Methods 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- 235000011147 magnesium chloride Nutrition 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- 235000002867 manganese chloride Nutrition 0.000 claims description 4
- 229940099607 manganese chloride Drugs 0.000 claims description 4
- 239000011684 sodium molybdate Substances 0.000 claims description 4
- 235000015393 sodium molybdate Nutrition 0.000 claims description 4
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 4
- 239000010902 straw Substances 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000001540 sodium lactate Substances 0.000 claims description 2
- 235000011088 sodium lactate Nutrition 0.000 claims description 2
- 229940005581 sodium lactate Drugs 0.000 claims description 2
- 229940111688 monobasic potassium phosphate Drugs 0.000 claims 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims 1
- 238000006477 desulfuration reaction Methods 0.000 abstract description 27
- 230000023556 desulfurization Effects 0.000 abstract description 27
- 239000002699 waste material Substances 0.000 abstract description 26
- 229910052717 sulfur Inorganic materials 0.000 abstract description 19
- 239000011593 sulfur Substances 0.000 abstract description 19
- 239000003575 carbonaceous material Substances 0.000 abstract description 5
- 102000004190 Enzymes Human genes 0.000 abstract description 3
- 108090000790 Enzymes Proteins 0.000 abstract description 3
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 24
- 239000000463 material Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000007792 addition Methods 0.000 description 4
- 230000002779 inactivation Effects 0.000 description 3
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 3
- 235000013923 monosodium glutamate Nutrition 0.000 description 3
- 239000004223 monosodium glutamate Substances 0.000 description 3
- 235000016709 nutrition Nutrition 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 241001441571 Hiodontidae Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005906 dihydroxylation reaction Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009456 molecular mechanism Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- NGSFWBMYFKHRBD-DKWTVANSSA-M sodium;(2s)-2-hydroxypropanoate Chemical compound [Na+].C[C@H](O)C([O-])=O NGSFWBMYFKHRBD-DKWTVANSSA-M 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 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
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/105—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with enzymes
-
- 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
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/16—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with inorganic material
-
- 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
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/28—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic compounds containing nitrogen, sulfur or 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
- C08J2317/00—Characterised by the use of reclaimed rubber
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
The invention relates to a waste tire reclaimed rubber treatment process, which belongs to the technical field of waste tire desulfurization and regeneration and comprises the following steps: mixing polycyclic aromatic hydrocarbon degrading bacteria with thiobacillus ferrooxidans liquid to obtain compound microbial liquid; adsorbing the composite microbial liquid by adopting porous carbon to obtain porous carbon loaded with the composite microbial liquid; crushing the waste tires by adopting a supercritical carbon dioxide injection method, adding a desulfurizing agent to obtain solid particles, adding the solid particles into an organic solvent, stirring, adding porous carbon loaded with a composite microbial liquid, stirring, and filtering to obtain the regenerated rubber. The supercritical carbon dioxide injection can damage the cross-linked network structure in the waste rubber, and has good plasticity; the porous carbon material can adsorb more microorganisms, can improve the removal of microorganisms in rubber desulfurization, and the enzyme contained in the thiobacillus ferrooxidans can absorb sulfur elements in rubber molecular chains.
Description
Technical Field
The invention belongs to the technical field of desulfurization and regeneration of junked tires, and particularly relates to a junked tire regenerated rubber treatment process.
Background
The waste tires belong to waste rubber, the rubber is used as raw materials of the tires, in the process of preparing the tires by using the rubber, the waste tires cannot be naturally degraded for a long time in order to meet the requirements of high strength, wear resistance, stability and ageing resistance of the tires, a large number of waste tires cause black pollution which is more difficult to treat than plastic pollution, precious rubber resources are wasted, the number of waste rubber materials is only inferior to that of waste plastics in waste polymer materials, the waste tires are used as raw materials for recycling the rubber, the environment is protected, the energy is saved, the recycling is a sustainable action, the raw materials and energy sources are saved, and the sustainable development of social economy is facilitated.
The physical desulfurization (namely decomposition and crushing) and chemical desulfurization (softening and activation under high temperature and high pressure) are carried out on the waste tires, and a macromolecular network crosslinking structure in the waste rubber is broken into a single-chain small molecular mechanism, so that the flowability of the rubber is recovered, and the rubber is changed into a processable viscoelastic from an elastomer, thereby achieving the purpose of utilization; desulfurization techniques include physical and chemical methods such as mechanical, mechanochemical, thermomechanical, and thermochemical; desulfurizing agent can be introduced to destroy the bond energy of S-S bond and S-C bond of waste tyre.
The unconsumed free sulfur element can participate in chemical reaction in the organic desulfurization process, new carbon-sulfur bonds are generated in rubber, incomplete vulcanization is caused, the sulfur content is relatively high, the energy consumption is high, and the oil production is limited to a certain extent; the sulfur element in the waste rubber can be effectively removed by adopting the microorganism to carry out desulfurization treatment on the waste rubber, but the polycyclic aromatic hydrocarbon compound released by the waste rubber can inhibit the growth of the microorganism, so that the microorganism desulfurization efficiency is lower.
Disclosure of Invention
The invention aims to provide a waste tire reclaimed rubber treatment process which comprises the following steps: preparing polycyclic aromatic hydrocarbon degrading bacteria, mixing the polycyclic aromatic hydrocarbon degrading bacteria with thiobacillus ferrooxidans solution, wherein enzymes contained in the thiobacillus ferrooxidans can absorb sulfur elements in rubber molecular chains, and the polycyclic aromatic hydrocarbon degrading bacteria effectively remove polycyclic aromatic hydrocarbon compounds released by rubber; the composite microorganism bacterial liquid is adsorbed in the porous carbon, and the porous carbon material has a larger specific surface area and a pore structure, so that more microorganisms can be adsorbed, and the effect of the microorganisms in rubber desulfurization is improved; the waste tires are crushed by adopting a supercritical carbon dioxide injection method, the desulfurizing agent is added in the crushing process, the supercritical carbon dioxide injection enables the waste tires to be small-size particles, the cross-linked network structure in the waste rubber can be damaged, the desulfurizing agent can be promoted to be uniformly immersed into the cross-linked network, and the desulfurizing reaction of the desulfurizing agent on the rubber is realized.
The invention aims to solve the technical problems: the unconsumed free sulfur element can participate in chemical reaction in the organic desulfurization process, new carbon-sulfur bonds are generated in rubber, incomplete vulcanization is caused, the sulfur content is relatively high, the energy consumption is high, and secondary pollution is caused; the sulfur element in the waste rubber can be effectively removed by adopting the microorganism to carry out desulfurization treatment on the waste rubber, but the polycyclic aromatic hydrocarbon compound released by the waste rubber can inhibit the growth of the microorganism, so that the microorganism desulfurization efficiency is lower.
The aim of the invention can be achieved by the following technical scheme:
a process for treating reclaimed rubber of junked tires comprises the following steps:
s1, mixing polycyclic aromatic hydrocarbon degrading bacteria with thiobacillus ferrooxidans liquid to obtain compound microbial liquid;
s2, adsorbing the composite microbial liquid by adopting porous carbon to obtain porous carbon loaded with the composite microbial liquid;
s3, crushing the waste tires by adopting a supercritical carbon dioxide injection method, and adding a desulfurizing agent in the crushing process to obtain solid particles;
s4, adding the solid particles into an organic solvent, stirring, adding porous carbon loaded with the composite microorganism bacterial liquid, stirring, filtering, and sequentially passing through an open mill and a refiner, and cooling and storing to obtain the regenerated rubber.
Further, the compound microorganism bacterial liquid specifically comprises the following steps:
A1. adding sodium hydroxide into a culture medium, regulating pH to be neutral, purging the culture medium with nitrogen to realize anaerobic conditions, facilitating growth of yeast monosodium glutamate, adding 10mL of polycyclic aromatic hydrocarbon solution into the culture medium, sterilizing the culture medium in an autoclave for 20min, centrifuging at 4000rpm for 10min, placing the culture medium in an anaerobic bottle, performing microorganism enrichment culture at 22 ℃ to obtain polycyclic aromatic hydrocarbon degrading bacteria, and preserving the polycyclic aromatic hydrocarbon degrading bacteria at-80 ℃;
A2. placing a ferrous oxide culture medium in a shaking incubator, culturing at a speed of 882rpm at 30 ℃, adding a sulfuric acid solution with a mass fraction of 98% to adjust the pH to 2.12 so as to enable ferrous oxide to grow, adding 10g/L of elemental sulfur, sterilizing the elemental sulfur at 121 ℃ for 15min, adding a sulfuric acid solution with a mass fraction of 98% to supplement culture medium nutrition, and incubating at 30 ℃ and a speed of 115rpm for 24h to obtain a thiobacillus ferrooxidans solution;
A3. preparing a clean and sterilized culture dish, placing the thiobacillus ferrooxidans liquid in the culture dish, adding polycyclic aromatic hydrocarbon degrading bacteria, covering a cover, slightly vibrating the culture dish for 5min to uniformly mix, and obtaining the compound microorganism bacterial liquid.
Further, in the step A1, the culture medium is formed by mixing the concentration ratio of (0.5-1.5): (0.3-0.7): (0.004-0.009): (0.04-0.07): (0.04-0.07): (0.1-0.3): (2.6-3): (1.5-1.9): (0.01-0.03) of ammonium chloride, monopotassium phosphate, ferrous sulfate, calcium chloride, magnesium sulfate, yeast monosodium glutamate, sodium sulfate, sodium nitrate and sodium lactate.
Further, in the step A2, the ferrous oxide culture medium is formed by mixing the concentration ratio of (0.2-0.8): (1.3-1.7): (0.04-0.09): (0.01-0.05): (3-4): (0.81-0.83): (2.6-2.9): (1.2-1.4): (0.2-0.5): (0.03-0.05) of ammonium sulfate, magnesium chloride, monopotassium phosphate, calcium chloride, ferrous sulfate, manganese chloride, cobalt chloride, boric acid, sodium molybdate and cupric chloride.
Further, the porous carbon loaded with the composite microbial liquid specifically comprises the following steps:
soaking straw in zinc chloride solution to form a porous structure, drying at 110 ℃ for 12 hours, taking out, placing in a stainless steel tube type reactor, heating to 600 ℃ at a speed of 20 ℃/min, keeping at the temperature for 36 hours, cooling, placing in hydrochloric acid solution, placing at 50 ℃ for 30 minutes, washing with deionized water until washing solution is neutral, drying in an oven at 80 ℃ for 2 hours to obtain porous carbon, adding 3g of porous carbon into 100mL of composite microorganism bacteria solution, placing in constant-temperature oscillation for 20 minutes, taking out, and drying at room temperature to obtain the porous carbon loaded with the composite microorganism bacteria solution.
In the operation process, in the zinc chloride solution serving as an activating agent, the straw is subjected to catalytic dehydroxylation and dehydration, hydrogen and oxygen are released in the form of water vapor to form a porous structure, and after high-temperature carbonization, metal ions and ash content in the porous carbon material are removed in the hydrochloric acid solution, so that the porous carbon contains a larger cavity structure, and bacterial liquid is adsorbed conveniently.
Further, the solid particles specifically comprise the steps of:
100g of junked tires are placed in a supercritical carbon dioxide jet pulverizer, then 10g of desulfurizing agent is placed in the pulverizing chamber, the supercritical carbon dioxide jet pulverizer is started after the pulverizing chamber is sealed, after 60min, the junked tires are pulverized under the impact of the jet pulverizer in the pulverizing chamber, and solid particles are collected at an outlet.
In the operation process, the supercritical carbon dioxide jet pulverizer pulverizes the waste tires into small-size particles, and the waste rubber expands to uniformly impregnate the desulfurated bis (3-triethoxysilylpropyl) tetrasulfide into the waste rubber crosslinking network; in the crushing process, sulfur-sulfur bonds in the bis (3-triethoxysilylpropyl) tetrasulfide are broken to generate free radicals, and the free radicals can react with sulfur-sulfur bonds and carbon-sulfur bonds in waste rubber molecules to complete desulfurization.
Further, the reclaimed rubber specifically comprises the following steps:
adding solid particles into an organic solvent, mixing and stirring for 10min at the speed of 300rpm and the temperature of 40 ℃ to obtain a rubber solution, immersing porous carbon loaded with composite microorganism bacteria liquid into the rubber solution, stirring uniformly, filtering to obtain a desulfurized rubber solution, placing the desulfurized rubber solution into a water bath, heating to 138 ℃ to remove the organic solvent, washing with deionized water for 3 times, drying in a 60 ℃ oven for 10min, sequentially passing through an open mill and a refiner, wherein the roller distance of the open mill roller is 0.8mm, the roller temperature of the refiner is 35 ℃, the roller distance of the refiner is 0.2mm, the roller temperature is 110 ℃, and discharging to obtain regenerated rubber.
It should be noted that: the solid particles are dissolved in the xylene which is an organic solvent, and the xylene is treated in a dissolving way, so that the inactivation of bacteria in the composite microbial liquid can not be caused like high-temperature melting, the xylene has no sterilization effect, and the bacterial liquid in the porous carbon loaded with the composite microbial liquid can survive in the rubber solution.
In addition, it is also to be stated that: the composite microorganism bacteria are immersed in the porous carbon material, the thiobacillus ferrooxidans can absorb sulfur elements in rubber molecular chains, and the polycyclic aromatic hydrocarbon compounds released by the rubber are attached to the surface of the porous carbon, so that the polycyclic aromatic hydrocarbon degradation bacteria in the porous carbon loaded with the composite microorganism bacteria liquid can be effectively removed, the inactivation of the thiobacillus ferrooxidans caused by the contact of the polycyclic aromatic hydrocarbon compounds and the thiobacillus ferrooxidans is avoided, and the purpose of desulfurization is achieved.
Further, the usage ratio of the junked tire to the desulfurizing agent is 10:1.
further, the desulfurizing agent is bis (3-triethoxysilylpropyl) tetrasulfide.
Further, the organic solvent is xylene.
The invention has the beneficial effects that:
(1) In the technical scheme of the invention, the bis (3-triethoxysilylpropyl) tetrasulfide is used as the desulfurizing agent, so that carbon-sulfur bonds and sulfur-sulfur bonds in the waste rubber can be destroyed, the waste tire is made into small-size particles by supercritical carbon dioxide injection, the cross-linked network structure in the waste rubber can be destroyed, the mechanical properties of the external and internal structures are reduced, the good plasticity is realized, and the waste rubber expansion can promote the desulfurizing agent to be uniformly immersed into the cross-linked network, so that the desulfurizing reaction of the desulfurizing agent on the rubber is realized.
(2) According to the technical scheme, the porous carbon material has a larger specific surface area and a pore structure, can adsorb more microorganisms, improves the desorption of microorganisms in rubber desulfurization, enables enzymes contained in the thiobacillus ferrooxidans loaded in the porous carbon loaded with the composite microorganism bacterial liquid to absorb sulfur elements in rubber molecular chains, achieves the purpose of desulfurization, avoids secondary pollution caused by the existence of sulfur elements in the processing process of regenerated rubber, and enables polycyclic aromatic hydrocarbon compounds released by the rubber to be attached to the surface of the porous carbon, so that polycyclic aromatic hydrocarbon compounds can be effectively removed by polycyclic aromatic hydrocarbon degrading bacteria in the porous carbon loaded with the composite microorganism bacterial liquid, and further avoids inactivation of the thiobacillus ferrooxidans caused by contact of the polycyclic aromatic hydrocarbon compounds and the thiobacillus ferrooxidans, thereby improving the efficiency of microbial desulfurization.
(3) According to the technical scheme, organic desulfurization and microbial desulfurization are carried out on the waste rubber, so that sulfur components in the waste rubber are effectively removed, the defect of incomplete desulfurization caused by new carbon-sulfur bonds generated in the organic desulfurization process is overcome, and the quality of the regenerated rubber is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the compound microorganism bacterial liquid specifically comprises the following steps:
A1. placing 1g/L ammonium chloride, 0.5g/L monopotassium phosphate, 0.007g/L ferrous sulfate, 0.05g/L calcium chloride, 0.05g/L magnesium sulfate, 0.2g/L yeast monosodium glutamate, 2.8g/L sodium sulfate, 1.7g/L sodium nitrate and 0.02g/L sodium lactate in a culture medium, adding sodium hydroxide into the culture medium, adjusting pH to be neutral, purging the culture medium with nitrogen to realize anaerobic condition, adding 10mL of polycyclic aromatic hydrocarbon solution into the culture medium, placing the culture medium in an autoclave, sterilizing at 120 ℃ for 20min, centrifuging at 4000rpm for 10min, placing in an anaerobic bottle, performing microorganism enrichment culture at 22 ℃ to obtain polycyclic aromatic hydrocarbon degrading bacteria, and storing the polycyclic aromatic hydrocarbon degrading bacteria at-80 ℃;
A2. placing a ferrous oxide culture medium into a shaking incubator, culturing at a speed of 882rpm at 30 ℃, wherein the ferrous oxide culture medium comprises 0.6g/L ammonium sulfate, 1.5g/L magnesium chloride, 0.07g/L monopotassium phosphate, 0.04g/L calcium chloride, 3.5g/L ferrous sulfate, 0.82g/L manganese chloride, 2.7g/L cobalt chloride, 1.3g/L boric acid, 0.3g/L sodium molybdate and 0.04g/L copper chloride, adding a sulfuric acid solution with a mass fraction of 98% to adjust the pH to 2.12, so that ferrous oxide grows, adding 10g/L elemental sulfur, sterilizing the elemental sulfur at 121 ℃ for 15min, adding a sulfuric acid solution with a mass fraction of 98% to supplement culture medium nutrition, and incubating for 24 hours at 30 ℃ and a speed of 115rpm to obtain a thiobacillus ferrooxidans solution;
A3. preparing a clean and sterilized culture dish, placing the thiobacillus ferrooxidans liquid in the culture dish, adding polycyclic aromatic hydrocarbon degrading bacteria, covering a cover, slightly vibrating the culture dish for 5min to uniformly mix, and obtaining the compound microorganism bacterial liquid.
Comparative example 1
This comparative example differs from example 1 in that no polycyclic aromatic hydrocarbon degrading bacteria were added.
Placing a ferrous oxide culture medium into a shaking incubator, culturing at a speed of 882rpm at 30 ℃, wherein the ferrous oxide culture medium comprises 0.6g/L ammonium sulfate, 1.5g/L magnesium chloride, 0.07g/L monopotassium phosphate, 0.04g/L calcium chloride, 3.5g/L ferrous sulfate, 0.82g/L manganese chloride, 2.7g/L cobalt chloride, 1.3g/L boric acid, 0.3g/L sodium molybdate and 0.04g/L copper chloride, adding a sulfuric acid solution with a mass fraction of 98% to adjust the pH to 2.12, so that ferrous oxide grows, adding 10g/L elemental sulfur, sterilizing the elemental sulfur at 121 ℃ for 15min, adding a sulfuric acid solution with a mass fraction of 98% to supplement culture medium nutrition, and incubating for 24 hours at 30 ℃ and a speed of 115rpm to obtain a thiobacillus ferrooxidans solution.
Example 2:
the porous carbon loaded with the composite microbial liquid is prepared by the following steps:
soaking straw in zinc chloride solution, drying at 110 ℃ for 12 hours, taking out, placing in a stainless steel tube reactor, heating to 600 ℃ at a speed of 20 ℃/min, keeping at the temperature for 36 hours, cooling, placing in hydrochloric acid solution, placing at 50 ℃ for 30 minutes, washing with deionized water until the washing solution is neutral, drying in an oven at 80 ℃ for 2 hours to obtain porous carbon, adding 10g of porous carbon into 100mL of composite microorganism bacterial solution, placing in constant temperature for 20 minutes, taking out, and drying at room temperature to obtain the porous carbon loaded with the composite microorganism bacterial solution.
Comparative example 2
The present comparative example is different from example 2 in that the complex microbial liquid was replaced with the material prepared in comparative example 1.
Example 3:
a process for treating reclaimed rubber of junked tires comprises the following steps:
s1, placing 100g of waste tires into a supercritical carbon dioxide jet pulverizer, then placing 10g of bis (3-triethoxysilylpropyl) tetrasulfide into a pulverizing chamber, sealing the pulverizing chamber, starting the supercritical carbon dioxide jet pulverizer, pulverizing the waste tires under the impact of the jet pulverizer in the pulverizing chamber after 60min, and collecting solid particles at an outlet.
S2, adding solid particles into dimethylbenzene, mixing and stirring for 10min at the speed of 300rpm and the temperature of 40 ℃ to obtain a rubber solution, immersing porous carbon loaded with composite microorganism bacteria liquid into the rubber solution, stirring uniformly, filtering to obtain a desulfurized rubber solution, placing the desulfurized rubber solution into a water bath, heating to 138 ℃, washing for 3 times by deionized water, drying in a 60 ℃ oven for 10min, sequentially passing through an open mill and a refiner, wherein the roller distance of the open mill roller is 0.8mm, the roller temperature of the refiner is 35 ℃, the roller distance of the refiner is 0.2mm, the roller temperature is 110 ℃, and discharging to obtain the regenerated rubber.
Comparative example 3
The comparative example differs from example 3 in that the junked tires were not subjected to supercritical carbon dioxide jet pulverization treatment.
Comparative example 4
This comparative example differs from example 3 in that bis (3-triethoxysilylpropyl) tetrasulfide is not added.
Comparative example 5
The comparative example differs from example 3 in that the porous carbon carrying the composite microbial liquid was replaced with the material prepared in comparative example 2.
Comparative example 6
The comparative example differs from example 3 in that the porous carbon carrying the composite microbial liquid was replaced with a material prepared from the composite microbial liquid.
The regenerated rubber prepared by the waste tire regenerated rubber treatment process of example 3 and comparative examples 3-6 was subjected to performance test, the regenerated rubber was ground and then polished with diamond slurry to obtain a cross section of particles, and the sulfur content of the regenerated rubber was analyzed with a scanning electron microscope; the mechanical property detection is carried out on the regenerated rubber by adopting the national standard GB/T13460-2016 to determine the desulfurization effect of the regenerated rubber;
according to the GB1232 standard, the Mooney viscosity of the prepared regenerated rubber is measured by a Mooney viscometer, and the lower the Mooney viscosity is, the better the plasticity of the regenerated rubber is; the test results are shown in table 1 below:
TABLE 1
| Project | Sulfur content/% | Elongation at break/% | Tensile Strength/MPa | Mooney viscosity/Pa second |
| Example 3 | 1.09 | 450 | 25 | 62 |
| Comparative example 3 | 8.61 | 425 | 20 | 90 |
| Comparative example 4 | 11.23 | 350 | 15 | 65 |
| Comparative example 5 | 6.5 | 380 | 17 | 62 |
| Comparative example 6 | 4.6 | 320 | 10 | 67 |
As can be seen from the data in table 1, in comparative example 3, the waste tires were not subjected to the supercritical carbon dioxide jet pulverization treatment, and the plasticity and sulfur content of the prepared reclaimed rubber were reduced, which is probably because the supercritical carbon dioxide jet pulverization treatment of the waste tires can destroy the crosslinked network structure in the waste rubber, improve the plasticity of the reclaimed rubber, and promote the desulfurization reaction of the waste rubber by the desulfurizing agent; comparative example 4 the sulfur content and mechanical properties of the reclaimed rubber prepared without the addition of bis (3-triethoxysilylpropyl) tetrasulfide are reduced, probably because the addition of the devulcanizing agent can effectively break the sulfur-sulfur bond and the carbon-sulfur bond in the used rubber to complete devulcanization and reduce the sulfur content; comparative example 5 the sulfur content of the prepared reclaimed rubber was reduced by adsorbing the composite bacterial liquid prepared without the addition of the polycyclic aromatic hydrocarbon degrading bacteria in the porous carbon and then adding the same to the rubber solution, probably because the polycyclic aromatic hydrocarbon degrading bacteria can effectively remove the polycyclic aromatic hydrocarbon compounds released from the waste rubber, avoid damaging the thiobacillus ferrooxidans liquid and improve the desulfurization efficiency of the waste rubber by the microorganisms; comparative example 6 is a regenerated rubber prepared by the fact that the composite bacterial liquid is not adsorbed in the porous carbon, and the sulfur content and mechanical properties of the regenerated rubber are reduced, probably because the composite bacterial liquid is adsorbed in the porous carbon, the microbial load can be increased, and the desulfurization effect on waste rubber is increased.
The regenerated rubber prepared in the example 4 has a good desulfurization effect on the junked tires, and the prepared regenerated rubber has good plasticity. The method comprises the steps of preparing polycyclic aromatic hydrocarbon degrading bacteria, mixing the polycyclic aromatic hydrocarbon degrading bacteria with thiobacillus ferrooxidans liquid, adsorbing the polycyclic aromatic hydrocarbon degrading bacteria and the thiobacillus ferrooxidans liquid in porous carbon to obtain porous carbon loaded with compound microbial bacterial liquid, crushing waste tires by adopting a supercritical carbon dioxide injection method, adding a desulfurizing agent in the crushing process, adding the porous carbon loaded with compound microbial bacterial liquid into the solution, stirring, filtering, sequentially passing through an open mill and a refiner, cooling and storing to obtain regenerated rubber which meets the requirement of test performance, and the regenerated rubber prepared in comparative examples 3-6 does not meet the standard of performance requirement, so that the regenerated rubber prepared by the method has better desulfurizing effect and better plasticity.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (10)
1. The process for treating the reclaimed rubber of the junked tire is characterized by comprising the following steps of:
s1, mixing polycyclic aromatic hydrocarbon degrading bacteria with thiobacillus ferrooxidans liquid to obtain compound microbial liquid;
s2, adsorbing the composite microbial liquid by adopting porous carbon to obtain porous carbon loaded with the composite microbial liquid;
s3, crushing the waste tires by adopting a supercritical carbon dioxide injection method, and adding a desulfurizing agent in the crushing process to obtain solid particles;
s4, adding the solid particles into an organic solvent, stirring, adding porous carbon loaded with the composite microorganism bacterial liquid, stirring, filtering, and sequentially passing through an open mill and a refiner, and cooling and storing to obtain the regenerated rubber.
2. The process for treating reclaimed rubber of waste tires according to claim 1, wherein the composite microbial liquid comprises the following steps:
A1. adding sodium hydroxide into a culture medium, regulating pH to be neutral, purging the culture medium with nitrogen to realize anaerobic conditions, adding a polycyclic aromatic hydrocarbon solution into the culture medium, placing the culture medium into an autoclave, sterilizing for 20min, centrifuging at 4000rpm for 10min, placing the culture medium into an anaerobic bottle, and culturing at 22 ℃ for 20h to obtain polycyclic aromatic hydrocarbon degrading bacteria;
A2. placing a ferrous oxide culture medium in a shaking incubator, shaking at a speed of 882rpm for 10min at 30 ℃, adding sulfuric acid solution with a mass fraction of 98% to adjust pH to 2.12, adding elemental sulfur, sterilizing the elemental sulfur for 15min, and incubating at a speed of 115rpm at 30 ℃ for 24h to obtain a thiobacillus ferrooxidans solution;
A3. preparing a clean and sterilized culture dish, placing the thiobacillus ferrooxidans liquid in the culture dish, adding polycyclic aromatic hydrocarbon degrading bacteria, covering a cover, slightly vibrating the culture dish for 5min to uniformly mix, and obtaining the compound microorganism bacterial liquid.
3. The process for treating waste tire reclaimed rubber according to claim 2, wherein in the step A1, the deionized water culture medium is formed by mixing the concentration ratio of (0.5-1.5): (0.3-0.7): (0.004-0.009): (0.04-0.07): (0.1-0.3): (2.6-3): (1.5-1.9): (0.01-0.03) of ammonium chloride, monobasic potassium phosphate, ferrous sulfate, calcium chloride, magnesium sulfate, yeast monosodium sulfate, sodium nitrate and sodium lactate.
4. The process for treating waste tire reclaimed rubber according to claim 2, wherein in the step A2, the ferrous oxide culture medium is formed by mixing ammonium sulfate, magnesium chloride, monopotassium phosphate, calcium chloride, ferrous sulfate, manganese chloride, cobalt chloride, boric acid, sodium molybdate and cupric chloride according to a concentration ratio of (0.2-0.8): (1.3-1.7): (0.04-0.09): (0.01-0.05): (0.04-0.07): (0.81-0.83): (2.6-2.9): (1.2-1.4): (0.2-0.5).
5. The process for treating waste tire reclaimed rubber according to claim 1, wherein the porous carbon loaded with the composite microorganism bacterial liquid comprises the following steps:
soaking straw in zinc chloride solution, drying at 110 ℃ for 12 hours, taking out, placing in a stainless steel tube reactor, heating to 600 ℃ at a speed of 20 ℃/min, keeping at the temperature for 36 hours, cooling, placing in hydrochloric acid solution, placing at 50 ℃ for 30 minutes, washing with deionized water until washing solution is neutral, drying in an oven at 80 ℃ for 2 hours to obtain porous carbon, adding the porous carbon into composite microbial bacteria solution, placing in constant-temperature oscillation for 20 minutes, taking out, and drying at room temperature to obtain the porous carbon loaded with the composite microbial bacteria solution.
6. The process for treating reclaimed rubber of waste tires according to claim 1, wherein the devulcanizer is bis (3-triethoxysilylpropyl) tetrasulfide.
7. The process for treating reclaimed rubber of waste tires according to claim 1, wherein the organic solvent is xylene.
8. The process for treating reclaimed rubber of waste tires according to claim 1, wherein the solid particles comprise the steps of:
placing the waste tires into a supercritical carbon dioxide jet pulverizer, placing a desulfurizing agent into the pulverizing chamber, sealing the pulverizing chamber, starting the supercritical carbon dioxide jet pulverizer, pulverizing the waste tires under the impact of the jet pulverizer in the pulverizing chamber after 60min, and collecting solid particles at an outlet.
9. The process for treating reclaimed rubber of waste tires according to claim 8, wherein the ratio of the amount of the waste tires to the amount of the devulcanizing agent is 10:1.
10. the process for treating waste tire reclaimed rubber according to claim 1, wherein the reclaimed rubber comprises the following steps:
adding solid particles into an organic solvent, mixing and stirring for 10min at the speed of 300rpm and the temperature of 40 ℃ to obtain a rubber solution, immersing porous carbon loaded with composite microorganism bacteria liquid into the rubber solution, stirring uniformly, filtering to obtain a desulfurized rubber solution, placing the desulfurized rubber solution into a water bath kettle, heating to 138 ℃, washing for 3 times by deionized water, drying in a 60 ℃ oven for 10min, sequentially passing through an open mill and a refiner, wherein the roller distance of the open mill roller is 0.8mm, the roller temperature of the refiner is 35 ℃, the roller distance of the refiner is 0.2mm, the roller temperature is 110 ℃, and discharging to obtain the regenerated rubber.
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| CN114031811A (en) * | 2021-12-07 | 2022-02-11 | 北京工业大学 | Method for desulfurizing waste tires by using supercritical carbon dioxide |
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