CN116376129B - Ultra-high performance tire tread rubber and preparation method thereof - Google Patents
Ultra-high performance tire tread rubber and preparation method thereof Download PDFInfo
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- CN116376129B CN116376129B CN202310061033.6A CN202310061033A CN116376129B CN 116376129 B CN116376129 B CN 116376129B CN 202310061033 A CN202310061033 A CN 202310061033A CN 116376129 B CN116376129 B CN 116376129B
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 99
- 239000005060 rubber Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001195 polyisoprene Polymers 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 229920003049 isoprene rubber Polymers 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 25
- 239000006229 carbon black Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 7
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008117 stearic acid Substances 0.000 claims abstract description 7
- 238000004073 vulcanization Methods 0.000 claims abstract description 7
- 239000011787 zinc oxide Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 48
- 238000003825 pressing Methods 0.000 claims description 30
- 238000004513 sizing Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000003921 oil Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000005062 Polybutadiene Substances 0.000 claims description 7
- 229920005555 halobutyl Polymers 0.000 claims description 7
- -1 naphthene hydrocarbon Chemical class 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 244000043261 Hevea brasiliensis Species 0.000 claims description 6
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 6
- 229920003052 natural elastomer Polymers 0.000 claims description 6
- 229920001194 natural rubber Polymers 0.000 claims description 6
- 229920002857 polybutadiene Polymers 0.000 claims description 6
- 238000010074 rubber mixing Methods 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 5
- 239000012188 paraffin wax Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000010734 process oil Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical class C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 239000012990 dithiocarbamate Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical compound [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 2
- 229960002447 thiram Drugs 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims 1
- 235000019809 paraffin wax Nutrition 0.000 claims 1
- 235000019271 petrolatum Nutrition 0.000 claims 1
- 238000005096 rolling process Methods 0.000 abstract description 18
- 239000006185 dispersion Substances 0.000 abstract description 8
- 239000004636 vulcanized rubber Substances 0.000 abstract description 5
- 239000006087 Silane Coupling Agent Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 28
- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical compound CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- 238000007306 functionalization reaction Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229920006978 SSBR Polymers 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0016—Compositions of the tread
-
- 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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Tires In General (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to an ultra-high performance tire tread rubber and a preparation method thereof, wherein the ultra-high performance tire tread rubber comprises the following components in parts by weight: 100 parts of rubber, 2-20 parts of functionalized polyisoprene rubber, 1-3 parts of zinc oxide, 1-2 parts of stearic acid, 2-6 parts of vulcanizing agent, 3-6 parts of anti-aging agent, 40-170 parts of filler, 10-60 parts of operating oil, 10-50 parts of resin, 2-20 parts of silane coupling agent TESPT and 10-25 parts of other components; the functionalized polyisoprene rubber is a double-ended functionalized liquid isoprene rubber. According to the invention, through reasonable proportioning of the tread rubber formula and application of the double-end functionalized liquid isoprene rubber which can be in reactive bonding with the surface active groups of the white carbon black in the mixing and vulcanization processes, filler dispersion is promoted, the number of free ends of polyisoprene is reduced, a crosslinked network of a vulcanization system is reinforced, the mechanical property of the vulcanized rubber is improved, rolling resistance is reduced, and the braking and control performances of the tire under dry and wet road surfaces are improved.
Description
Technical Field
The invention belongs to the technical field of tire rubber materials, and particularly relates to ultra-high performance tire tread rubber and a preparation method thereof.
Background
Under the background of continuous development of social economy, the living standard of people is continuously rising, and automobiles are ubiquitous and have gradually improved performance. In order to accommodate the high performance of automobiles, the demand for ultra-high performance tires is also continuously increasing. The ultra-high performance tires are attached to the market of high-end automobiles and are beginning to develop, and the continuous introduction of high-end automobile models enables the cognition of consumers on the high-end tires to be improved, and the attention to the ultra-high performance tires with excellent performance is continuously increased. In recent years, although sales of cars have been reduced, consumer demand for sport-type vehicles has been continuously increasing, and demand for ultra-high performance tires has been continuously increasing.
A number of factors to be considered in the manufacture of ultra-high performance tires include tire structure, material stock, tread design, size and weight, while the high performance of a tire depends largely on the raw materials or compounds used in its production. With the continued development of the ultra-high performance tire market, tire manufacturers and designers are also constantly changing in factors that are considered in developing ultra-high performance tires. The continuous development of new energy automobiles also brings new problems for the development of ultra-high performance tires, such as light weight and the like. In addition, with increasing importance of environmental protection performance of tires in various countries, more and more countries around the world have implemented the tire labeling method, so that there is also strict requirement on rolling resistance, wet road gripping performance and the like of tires, so as to achieve the purposes of safe, energy-saving and environmental protection production and use of tires.
The ultra-high performance tread formula needs more filler to meet the requirement of service performance, the filling of the white carbon black is beneficial to the improvement of the braking and controlling performance of the tire on a wet road surface, the filling of the carbon black in the formula is beneficial to the improvement of the braking and controlling performance of the tire on a dry road surface, but with the increase of the filler, the heat generation of the rubber material is increased, and the rolling resistance of the tire is also increased. In order to reduce the heat generation of the rubber material, the functionalized solution polymerized styrene-butadiene rubber is widely used, but most of the functionalized solution polymerized styrene-butadiene rubber belongs to customization and has poor replaceability, and as the functionalization degree of the solution polymerized styrene-butadiene rubber is higher and higher, the processability of the rubber material is also deteriorated, and the problems of chipping, chipping and the like of the tire on a complex road surface are easily caused. In addition, when the filler consumption reaches a certain degree, the hardness of the operation oil matched with the sizing material needs to be increased, more operation oil needs to be added in the formula, but the effective dispersion of the filler is not facilitated when the addition amount is more, the strength of the sizing material is reduced, and the processing technology performance is reduced; the process oil is a small molecular substance, and is likely to be precipitated from the tire when the amount of the process oil added is large. Therefore, in the development process of the formula, balance is still required to be found among different material components, and the ultra-high performance tread rubber with excellent braking and control performances on dry and wet road surfaces is developed.
Currently, there is no tread formulation in the art that has excellent overall performance in all respects. Patent application CN113072750A discloses a high-strength rubber composite material with excellent processability and a preparation method thereof, and the mechanical property and fatigue resistance of vulcanized rubber can be improved by using siloxane end-capped modified low-molecular-weight polyisoprene; CN113072751a discloses a wet skid resistant and high stretching rubber composite material and a preparation method thereof, wherein low molecular weight polyisoprene with specific microstructure content is adopted to replace plasticizer in the traditional formula system, so that the processability is improved, the wet skid resistant performance is improved, and higher stretching stress and tearing strength are ensured; CN114773514a discloses a macromolecular coupling agent for improving the vulcanized rubber performance of rubber materials and application thereof, and in a formula system of white carbon black filled rubber, the macromolecular coupling agent is a low molecular polyisoprene grafted and modified by a sulfhydryl silane coupling agent, so that the processability of the rubber composite material is improved, and the mechanical property and fatigue resistance of the composite material are improved. The above patents are used instead of silane or traditional low molecular weight isoprene, with a focus on improving mechanical properties and with little application in tires.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides an ultra-high performance tire tread rubber and a preparation method thereof, wherein the ultra-high performance tire tread rubber is prepared from double-end functionalized liquid isoprene rubber, is applied to a tire tread formula of high filling filler, improves the dispersion of the filler, has better mixing process performance through reasonable proportioning of materials, reduces rolling resistance of the tire while ensuring mechanical properties of the rubber, and improves braking and control performance under dry and wet road conditions.
The technical scheme of the invention is as follows:
the ultra-high performance tire tread rubber comprises the following components in parts by weight:
100 parts of rubber, 2-20 parts of functionalized polyisoprene rubber, 1-3 parts of zinc oxide, 1-2 parts of stearic acid, 2-6 parts of vulcanizing agent, 2.9-6 parts of anti-aging agent, 40-170 parts of filler, 10-60 parts of operating oil, 10-50 parts of resin, 2-20 parts of silane coupling agent TESPT and 6.5-25 parts of other components;
Wherein the functionalized polyisoprene rubber is double-end functionalized liquid isoprene rubber, one end of the functionalized polyisoprene rubber is blocked by alkoxy silicon, and the other end of the functionalized polyisoprene rubber is coupled by tin;
The rubber is one or more selected from natural rubber, butadiene rubber, styrene-butadiene rubber and halogenated butyl rubber; further, the rubber comprises the following components in parts by weight: 0-25 parts of natural rubber, 0-60 parts of butadiene rubber, 15-90 parts of styrene-butadiene rubber and 0-23 parts of halogenated butyl rubber; namely, the rubber comprises 15-90 parts of styrene-butadiene rubber, and also comprises any one or two or three of natural rubber, butadiene rubber and halogenated butyl rubber in the rest parts.
The tread rubber formula provided by the invention is applied with the double-end functionalized liquid isoprene rubber, one end of the double-end functionalized liquid isoprene rubber is blocked by alkoxy silicon, and an alkoxy silicon modified group of the double-end functionalized liquid isoprene rubber can react with hydroxyl groups on the surface of white carbon black in the mixing process, so that the dispersion degree of filler is increased, the heat generation of rubber materials is reduced, the rolling resistance of the tire is reduced, and meanwhile, the double-end functionalized liquid isoprene rubber is applied to a high-filled tire tread formula, and the other end of the double-end functionalized liquid isoprene rubber is tin coupled, so that the free end of a molecular chain end is reduced, the dispersion of the filler is further improved, the processing technological performance is improved, the rolling resistance of the tire is reduced while the mechanical performance of the rubber materials is ensured, and the dry and wet land braking and operating performance of the tire are improved, so that the purposes of energy conservation and safety are achieved.
Further, the ultra-high performance tire tread rubber comprises the following components in parts by weight:
100 parts of rubber, 5-15 parts of double-end functionalized liquid isoprene rubber, 1-2 parts of zinc oxide, 1-1.5 parts of stearic acid, 3-5 parts of vulcanizing agent, 4-5 parts of anti-aging agent, 80-130 parts of filler, 20-50 parts of operating oil, 20-40 parts of resin, 5-15 parts of silane coupling agent TESPT and 15-20 parts of other components;
Wherein the rubber is composed of 15-90 parts of styrene-butadiene rubber and any one or two or three of natural rubber, butadiene rubber and halogenated butyl rubber in the rest parts.
Further, the molecular weight of the double-ended functionalized liquid isoprene rubber is 1X 10 4～1×105 g/mol.
Further, the double-ended functionalized liquid isoprene rubber comprises one or more of 1, 4-polyisoprene, 3, 4-polyisoprene, 1, 2-polyisoprene; wherein, the content of 1, 4-polyisoprene is 15% -96%, the content of 3, 4-polyisoprene is 0% -35%, and the content of 1, 2-polyisoprene is 0% -20%;
Preferably, the content of the 1, 4-polyisoprene is 15% -96%, the content of the 3, 4-polyisoprene is 2% -35%, and the content of the 1, 2-polyisoprene is 2% -20%.
The tread rubber component is a commercially available product except for the double-end functional liquid isoprene rubber. The preparation method of the double-end functional liquid isoprene rubber comprises the following steps:
Synthesizing a low molecular weight polyisoprene precursor by an anionic solution polymerization method, adding a functional modified group under the protection of nitrogen, continuing to react, and finally adding an ethanol solution containing a small amount of hydrochloric acid to terminate the reaction, condensing the polymer, and drying at a constant temperature of 40-50 ℃ to obtain the double-end modified liquid isoprene.
Specifically, the preparation steps of the double-end functionalized liquid isoprene rubber are as follows:
Pumping out 3 times by using high-purity nitrogen in a polymerization kettle, adding a certain amount of isoprene monomer, linear alkane or naphthene hydrocarbon solvent and a small amount of structure regulator, heating to 40-50 ℃, adding a certain amount of tert-butyl dimethyl siloxypropyl lithium initiator for reaction, reacting at 60-80 ℃ for 30-60 min under 0.2-0.5 MPa, adding tin tetrachloride coupling agent for coupling reaction after the polymerization reaction reaches 100% of conversion rate, and removing the solvent by using a thin film evaporator after the reaction is completed to obtain the liquid isoprene rubber.
Wherein, the straight-chain alkane or naphthenic hydrocarbon solvent used in the preparation process comprises hexane, pentane, cyclohexane, cyclopentane and carbon hexaraffinate oil, and the dosage is 200-600% (wt) of the dosage of the monomer;
The structure regulator used in the preparation process is any one or more of ethers and amine polar substances, preferably tetrahydrofuran, diethylene glycol dimethyl ether and pentamethyl divinyl benzene triamine, and is used for improving the reaction rate and regulating the 3, 4-structure content of isoprene, and the dosage is 0.05-0.2% (wt) of the dosage of the monomer;
the initiator used in the preparation process is a lithium initiator containing a silicon oxygen group, preferably tertiary butyl dimethyl silicon oxygen propyl lithium, and the dosage is 0.01-00.1% (wt) of the dosage of the monomer.
Further, the styrene-butadiene rubber is solution polymerized styrene-butadiene rubber.
Further, the vulcanizing agent consists of a sulfur vulcanizing agent and a vulcanizing accelerator, a common vulcanizing system or an effective and semi-effective sulfur vulcanizing system is adopted, the sulfur vulcanizing agent is sulfur or a sulfur carrier, and the vulcanizing accelerator is one or more of a piperidine, a sulfenamide, a thiuram and a dithiocarbamate.
Further, the filler is carbon black and white carbon black, the carbon black is fine particle size, and the white carbon black is high-dispersion white carbon black by a precipitation method;
The operation oil is environment-friendly aromatic hydrocarbon oil or naphthenic oil, and the resin is hydrogenated DCPD resin.
Further, the other components comprise a filler dispersing agent and paraffin wax, wherein the filler dispersing agent is white carbon black dispersing agent zinc soap salt.
The invention also provides a preparation method of the ultra-high performance tire tread rubber, which comprises the following steps:
(1) And (3) mixing: the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm for speed regulation;
Adding rubber, functionalized polyisoprene rubber, 2/3 white carbon black, si69, paraffin, stearic acid, 2/3 resin, filler dispersant and accelerator DPG into an internal mixer, and pressing a top plug for 30s;
lifting the top bolt, adding all carbon black, pressing the top bolt, and heating the sizing material to 118 ℃;
raising the top bolt, adding operating oil, pressing the top bolt, raising the temperature of the sizing material to 135 ℃,
Lifting the top bolt, cleaning, pressing the top bolt, heating the rubber material to 146 ℃, keeping the constant temperature rubber mixing for 40s, and discharging rubber;
(2) Two-stage mixing: the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm for speed regulation;
Adding a section of master batch, residual white carbon black, residual resin and an anti-aging agent into an internal mixer, and pressing a top bolt for 30s;
lifting the top bolt, cleaning, pressing the top bolt, and heating the sizing material to 140 ℃;
Lifting the top bolt, cleaning, pressing the top bolt, heating the rubber material to 146 ℃, keeping the constant temperature rubber mixing for 40s, and discharging rubber;
(3) Three-stage mixing: the method is characterized in that a series internal mixer is used and consists of two internal mixers and an open mill unit, wherein the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm according to the setting of a program, and the open mill can adjust the mixing temperature according to the requirement so as to ensure the smooth passing of a mixing process;
adding the two-stage masterbatch and zinc oxide into an internal mixer, and pressing a top bolt for 30s;
lifting the top bolt, cleaning, pressing the top bolt, and heating the sizing material to 135 ℃;
lifting the top bolt, keeping for 5s, pressing the top bolt, and mixing for 90s at the constant temperature of 148 ℃;
opening a discharge door to discharge rubber to a second internal mixer, regulating the rotating speed of the second internal mixer from 40 rpm to 5 rpm, keeping the temperature at 146 ℃, then keeping the temperature at 146 ℃ for 180 seconds, and opening the discharge door to discharge rubber;
The temperature of the roller of the open mill is raised to 70 ℃, the sizing material discharged from the internal mixer is conveyed to one of the lower open mill groups, the sizing material turning, the addition of sulfur and accelerator and the mixing work are completed, the roller spacing of the open mill in different steps is accurately changed between 3.0 and 6.0, the total mixing time of the open mill is about 1000 seconds, and then the sizing material enters the lower open mill for cooling and stacking.
The invention has the beneficial effects that:
(1) According to the invention, through reasonable proportioning of the tread rubber formula and application of the double-end functionalized liquid isoprene rubber, the molecular chain terminal of the rubber can be in reaction bonding with active groups on the surface of white carbon black in the mixing and vulcanization processes, so that the filler dispersion is promoted, the number of free terminals of polyisoprene is effectively reduced, the crosslinking network of a vulcanization system is reinforced, the mechanical property and dynamic property of the vulcanized rubber are greatly improved, the rolling resistance of the tire is reduced, and the braking and control performances of the tire under the dry and wet road surface conditions are improved.
(2) The tread rubber prepared by the double-end functionalized liquid isoprene rubber can also provide better rolling resistance, meets the performance requirement of an ultra-high performance tire, can reduce the oil consumption of an automobile by reducing the rolling resistance, and can improve the safety performance of the automobile by shortening the braking distance and the control performance of a dry road surface and a wet road surface.
According to the rolling resistance of the tire is reduced by 20%, the fuel is saved by 3%, the fuel consumption can be saved by 30W liter/W vehicles (the annual driving mileage is 2WKm,10L fuel is calculated per 100 Km), the double-end functional liquid isoprene rubber is applied, the rolling resistance is reduced by 5%, and the fuel consumption can be saved by 7.5W liter/W vehicles each year; when the braking distance under the wet road surface is reduced by 1 meter, the safety coefficient of driving is improved by several times; meanwhile, the fuel consumption is saved, the emission of carbon dioxide is reduced, and the economic benefit is immeasurable.
Detailed Description
For a further understanding of the present invention, the technical aspects of the present invention will be clearly and fully described in connection with the following embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, 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 ultra-high performance tire tread rubber has the formula components shown in table 1, and the preparation method comprises the following steps:
(1) One-stage mixing, wherein the rotating speed of the internal mixer can be changed from 50 rpm to 5 rpm:
adding rubber, double-end functionalized liquid isoprene rubber, white carbon black of (2/3), si69, paraffin wax, stearic acid, resin of (2/3), filler dispersant and accelerator DPG into an internal mixer, and pressing a top plug for 30s;
Lifting the top bolt, adding all carbon black, pressing the top bolt, and heating the sizing material to 118 ℃;
raising the top bolt, adding operating oil, pressing the top bolt, raising the temperature of the sizing material to 135 ℃,
Lifting the top bolt, cleaning, pressing the top bolt, heating the rubber material to 146 ℃, keeping the constant temperature rubber mixing for 40s, and discharging rubber;
(2) The two-stage mixing can realize the speed change from 50 rpm to 5 rpm:
adding the 1-section masterbatch, the residual white carbon black, the residual resin and the anti-aging agent into an internal mixer, and pressing a top bolt for 30s;
lifting the top bolt, cleaning, pressing the top bolt, and heating the sizing material to 140 ℃;
Lifting the top bolt, cleaning, pressing the top bolt, heating the rubber material to 146 ℃, keeping the constant temperature rubber mixing for 40s, and discharging rubber;
(3) Three-stage mixing: the method is characterized in that a series internal mixer is used and consists of two internal mixers and an open mill unit, wherein the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm according to the setting of a program, and the open mill can adjust the mixing temperature according to the requirement so as to ensure the smooth passing of a mixing process;
adding the two-stage masterbatch and zinc oxide into an internal mixer, and pressing a top bolt for 30s;
lifting the top bolt, cleaning, pressing the top bolt, and heating the sizing material to 135 ℃;
lifting the top bolt, keeping for 5s, pressing the top bolt, and mixing for 90s at the constant temperature of 148 ℃;
Opening a discharge door to discharge rubber to a second internal mixer (the rotating speed of the second internal mixer can be adjusted from 40 rpm to 5 rpm), the temperature reaches 146 ℃, then the temperature is kept constant for 180 seconds at 146 ℃, and the discharge door is opened to discharge rubber;
The temperature of the roller of the open mill is raised to 70 ℃, the sizing material discharged from the internal mixer is conveyed to one of the lower open mill groups, the sizing material turning, the addition of sulfur and accelerator and the mixing work are completed, the roller spacing of the open mill in different steps is accurately changed between 3.0 and 6.0, the total mixing time of the open mill is about 1000 seconds, and then the sizing material enters the lower open mill for cooling and stacking.
Example 2
The components of the formula of the ultra-high performance tire tread rubber are shown in table 1, and the preparation method is the same as that of example 1.
Example 3
The components of the formula of the ultra-high performance tire tread rubber are shown in table 1, and the preparation method is the same as that of example 1.
Example 4
The components of the formula of the ultra-high performance tire tread rubber are shown in table 1, and the preparation method is the same as that of example 1.
Comparative example 1
The formulation components of comparative example 1 are shown in table 1;
in the first-stage mixing of comparative example 1, the temperature of the sizing material is 150 ℃, the sizing material is kept for 45 seconds, and the sizing material is discharged; the other steps were the same as in example 1;
in the two-stage mixing of the comparative example 1, the rubber discharging temperature is 148 ℃, and the rubber discharging is carried out for 45 seconds; the other steps were the same as in example 1,
The three-stage kneading of comparative example 1 was the same as in example 1.
Comparative examples 2 to 7
The formulation components of comparative examples 2-7 are shown in Table 1 and were prepared in the same manner as in comparative example 1.
By adopting the mixing process, each example has better mixing processing performance, more oil exists in the formula of the comparative example 1, the rubber material is softer during rubber discharge, the phenomenon that the rubber material sticks to the open mill roller and is easy to break occurs, compared with the comparative example 1, the processing performance of the comparative example 3 is easier to break, the processing performance of the comparative examples 4 and 5 is close to that of the comparative example 1, the rubber is easier to break due to the use of solution polymerized butylbenzene with higher functionalization degree in the comparative example 6, and the state of the rubber material is rough; although the kneading processability of comparative example 2 was not as good as that of the other comparative examples; comparative example 7 the compounding process performance was similar to comparative example 1.
Table 1 formulation components of examples 1-4 and comparative examples 1-7
Note that: solution-polymerized butylbenzene 1 is solution-polymerized butylbenzene with low functionalization degree, and solution-polymerized butylbenzene 2 is solution-polymerized butylbenzene with high functionalization degree and double end functionalization.
Test example 1
The tread rubber compounds prepared in the examples 1-4 and the comparative examples 1-7 are subjected to performance test, mainly comprising physical properties and dynamic viscoelastic properties, and the dynamic mechanical properties of the vulcanized rubber are represented by dynamic viscoelastic data, which are important means for researching the tread rubber of a tire, such as rolling resistance, wet skid resistance, handling performance and the like, and can be effectively represented in the data. The tan delta value at 0 ℃ is related to the wet skid resistance of the rubber material, and the higher the tan delta value at 0 ℃, the better the wet skid resistance of the tread rubber material; the hysteresis loss factor tan delta at 20 ℃ characterizes the dry grip performance of the compound, the larger the value of which indicates the better the dry grip performance of the compound; the elastic modulus E' at 20 ℃ represents the handling property of the rubber compound, and the larger the numerical value is, the better the handling property of the rubber composition is; the tan delta value at 60 ℃ correlates with the rolling resistance properties of the compound, the lower the tan delta value at 60 ℃, the lower the rolling resistance of the tread compound. The test results are shown in the following table.
TABLE 2 results of Performance test of examples 1-4 and comparative examples 1-7
Note that: the above vulcanization conditions: 168 ℃ C. (t90+2 mine)
From the compound properties of table 2 above, it can be seen that:
Examples 1-4 showed increasing trends in 0℃tan delta, 20℃tan delta, 20℃E' of the compounds with increasing amounts of functionalized liquid isoprene rubber, 60℃tan delta decreasing, demonstrating improved dry and wet braking and handling properties and lower rolling resistance;
Comparative examples 1 and 2 are lower in the rubber compounds at 0℃tan delta, 20℃tan delta and 20℃E';
Comparative example 3 increased filler amount, comparative example 4 increased resin amount, comparative example 5 increased SSBR amount, reduced BR amount, slightly increased tan delta at 0 ℃, tan delta at 20 ℃, and E' at 20 ℃, but increased tan delta at 60 ℃, i.e., increased rolling resistance of the tire; comparative example 7 using halogenated butyl rubber, tan delta at 0℃and tan delta at 20℃were slightly decreased and tan delta at 60℃was increased.
The comparative example 6 uses the solution-polymerized butadiene-styrene 2, the elongation at break of the sizing material is lower, the risk of falling blocks occurs when the tire runs on a complex road surface, the tan delta at 0 ℃ is slightly improved, the tan delta at 60 ℃ is still higher than that of the example, and when the functionalization degree of the solution-polymerized butadiene-styrene is higher, the dispersion of the filler is promoted, and the rolling resistance of the tire is reduced, but the comparison of the example and the comparative example 6 shows that the effect of the application of the functionalized liquid isoprene rubber is better than that of the solution-polymerized butadiene-styrene 2.
The tread rubber provided by the invention provides excellent dry and wet braking and control performances and excellent rolling resistance, and can meet the performance requirements of ultra-high performance tires.
The foregoing description is only a preferred embodiment of the present invention and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or that equivalents may be substituted for part of the technical features thereof. Any modification, equivalent replacement, variation, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The ultra-high performance tire tread rubber is characterized by comprising the following components in parts by weight:
100 parts of rubber, 2-20 parts of functionalized polyisoprene rubber, 1-3 parts of zinc oxide, 1-2 parts of stearic acid, 2-6 parts of vulcanizing agent, 2.9-6 parts of anti-aging agent, 40-170 parts of filler, 10-60 parts of operating oil, 10-50 parts of resin, si 692-20 parts and 6.5-25 parts of other components;
Wherein the functionalized polyisoprene rubber is double-end functionalized liquid isoprene rubber, one end of the functionalized polyisoprene rubber is blocked by alkoxy silicon, and the other end of the functionalized polyisoprene rubber is coupled by tin; the preparation method of the double-end functional liquid isoprene rubber comprises the following steps:
Pumping out 3 times by using high-purity nitrogen in a polymerization kettle, adding a certain amount of isoprene monomer, linear alkane or naphthene hydrocarbon solvent and a small amount of structure regulator, heating to 40-50 ℃, adding a certain amount of tert-butyl dimethyl siloxypropyl lithium initiator for reaction, reacting at 60-80 ℃ for 30-60 min under 0.2-0.5 MPa, adding tin tetrachloride coupling agent for coupling reaction after the polymerization reaction reaches 100% of conversion rate, reacting at 70-90 ℃ for 20-40 min, and removing the solvent by using a thin film evaporator after the reaction is completed to obtain double-end functionalized liquid isoprene rubber;
the rubber is one or more of natural rubber, butadiene rubber, styrene-butadiene rubber and halogenated butyl rubber;
the other components include filler dispersants and paraffin waxes.
2. The ultra-high performance tire tread rubber according to claim 1, wherein the rubber comprises the following components in parts by weight:
0 to 25 parts of natural rubber, 0 to 60 parts of butadiene rubber, 15 to 90 parts of styrene-butadiene rubber and 0 to 23 parts of halogenated butyl rubber.
3. The ultra-high performance tire tread band of claim 1, wherein the double-ended functionalized liquid isoprene rubber has a molecular weight of 1 x 10 4～1×105 g/mol.
4. The ultra-high performance tire tread band of claim 3, wherein the double-ended functionalized liquid isoprene rubber comprises one or more of 1, 4-polyisoprene, 3, 4-polyisoprene, 1, 2-polyisoprene; wherein, the content of 1, 4-polyisoprene is 15% -96%, the content of 3, 4-polyisoprene is 0% -35%, and the content of 1, 2-polyisoprene is 0% -20%.
5. The ultra-high performance tire tread rubber according to claim 1, wherein the styrene-butadiene rubber is solution polymerized styrene-butadiene rubber.
6. The ultra-high performance tire tread rubber according to claim 1, wherein the vulcanizing agent comprises a sulfur vulcanizing agent and a vulcanization accelerator, wherein the sulfur vulcanizing agent is sulfur or a sulfur carrier, and the vulcanization accelerator is one or more selected from the group consisting of a piperidine, a sulfenamide, a thiuram and a dithiocarbamate.
7. The ultra-high performance tire tread rubber according to claim 1, wherein the filler is carbon black and white carbon black, the process oil is an environment-friendly aromatic or naphthenic oil, and the resin is a hydrogenated DCPD resin.
8. The ultra-high performance tire tread rubber of claim 1, wherein the filler dispersant is a white carbon black dispersant zinc soap salt.
9. The method for preparing the ultra-high performance tire tread rubber according to any one of claims 1 to 8, comprising the steps of:
(1) And (3) mixing: the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm for speed regulation;
Adding rubber, functionalized polyisoprene rubber, 2/3 white carbon black, si69, paraffin, stearic acid, 2/3 resin, filler dispersant and accelerator DPG into an internal mixer, and pressing a top plug for 30s; lifting the top bolt, adding all carbon black, pressing the top bolt, and heating the sizing material to 118 ℃; raising the top bolt, adding operating oil, pressing the top bolt, raising the temperature of the rubber material to 135 ℃, raising the top bolt, cleaning, pressing the top bolt, raising the temperature of the rubber material to 146 ℃, keeping constant temperature rubber mixing for 40s, and discharging rubber;
(2) Two-stage mixing: the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm for speed regulation;
Adding a section of master batch, residual white carbon black, residual resin and an anti-aging agent into an internal mixer, and pressing a top bolt for 30s; lifting the top bolt, cleaning, pressing the top bolt, and heating the sizing material to 140 ℃; lifting the top bolt, cleaning, pressing the top bolt, heating the rubber material to 146 ℃, keeping the constant temperature rubber mixing for 40s, and discharging rubber;
(3) Three-stage mixing: the method is characterized in that a series internal mixer is used and consists of two internal mixers and an open mill unit, wherein the rotating speed of the internal mixer is changed from 50 rpm to 5 rpm according to the setting of a program, and the open mill can adjust the mixing temperature according to the requirement so as to ensure the smooth passing of a mixing process;
Adding the two-stage masterbatch and zinc oxide into an internal mixer, and pressing a top bolt for 30s; lifting the top bolt, cleaning, pressing the top bolt, and heating the sizing material to 135 ℃; lifting the top bolt, keeping for 5s, pressing the top bolt, and mixing for 90s at the constant temperature of 148 ℃; opening a discharge door to discharge rubber to a second internal mixer, regulating the rotating speed of the second internal mixer from 40 rpm to 5 rpm, keeping the temperature at 146 ℃, then keeping the temperature at 146 ℃ for 180 seconds, and opening the discharge door to discharge rubber;
The temperature of the roller of the open mill is raised to 70 ℃, the sizing material discharged from the internal mixer is conveyed to one of the lower open mill groups, the sizing material turning, the addition of sulfur and accelerator and the mixing work are completed, the distance between the rollers of the open mill in different steps is accurately changed from 3.0 to 6.0, the total mixing time of the open mill is 1000s, and then the sizing material enters the lower open mill for cooling and stacking.
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