CN118812930B - Wear-resistant tire tread rubber and preparation method thereof - Google Patents
Wear-resistant tire tread rubber and preparation method thereof Download PDFInfo
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- CN118812930B CN118812930B CN202411297542.XA CN202411297542A CN118812930B CN 118812930 B CN118812930 B CN 118812930B CN 202411297542 A CN202411297542 A CN 202411297542A CN 118812930 B CN118812930 B CN 118812930B
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 112
- 239000005060 rubber Substances 0.000 title claims abstract description 112
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000006229 carbon black Substances 0.000 claims abstract description 116
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000945 filler Substances 0.000 claims abstract description 39
- 239000002131 composite material Substances 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 229920003048 styrene butadiene rubber Polymers 0.000 claims abstract description 29
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 244000043261 Hevea brasiliensis Species 0.000 claims abstract description 9
- 229920003052 natural elastomer Polymers 0.000 claims abstract description 9
- 229920001194 natural rubber Polymers 0.000 claims abstract description 9
- CBXRMKZFYQISIV-UHFFFAOYSA-N 1-n,1-n,1-n',1-n',2-n,2-n,2-n',2-n'-octamethylethene-1,1,2,2-tetramine Chemical compound CN(C)C(N(C)C)=C(N(C)C)N(C)C CBXRMKZFYQISIV-UHFFFAOYSA-N 0.000 claims abstract description 8
- MHKLKWCYGIBEQF-UHFFFAOYSA-N 4-(1,3-benzothiazol-2-ylsulfanyl)morpholine Chemical compound C1COCCN1SC1=NC2=CC=CC=C2S1 MHKLKWCYGIBEQF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004642 Polyimide Substances 0.000 claims abstract description 8
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 8
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000292 calcium oxide Substances 0.000 claims abstract description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920003049 isoprene rubber Polymers 0.000 claims abstract description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920001721 polyimide Polymers 0.000 claims abstract description 8
- 239000008117 stearic acid Substances 0.000 claims abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 8
- 239000011593 sulfur Substances 0.000 claims abstract description 8
- 239000011787 zinc oxide Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 80
- 239000000243 solution Substances 0.000 claims description 78
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 27
- 239000005543 nano-size silicon particle Substances 0.000 claims description 26
- 238000007599 discharging Methods 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 230000004048 modification Effects 0.000 claims description 19
- 238000012986 modification Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 13
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 13
- 238000000265 homogenisation Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 230000003712 anti-aging effect Effects 0.000 claims description 7
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 3
- DTRIDVOOPAQEEL-UHFFFAOYSA-N 4-sulfanylbutanoic acid Chemical compound OC(=O)CCCS DTRIDVOOPAQEEL-UHFFFAOYSA-N 0.000 claims description 3
- GCIZMJUHGHGRNW-UHFFFAOYSA-N 5-sulfanylpentanoic acid Chemical compound OC(=O)CCCCS GCIZMJUHGHGRNW-UHFFFAOYSA-N 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 238000009423 ventilation Methods 0.000 claims 1
- 238000005096 rolling process Methods 0.000 abstract description 9
- 239000010692 aromatic oil Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 239000006087 Silane Coupling Agent Substances 0.000 description 11
- 239000012065 filter cake Substances 0.000 description 7
- 238000004073 vulcanization Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 229940093429 polyethylene glycol 6000 Drugs 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000010074 rubber mixing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Tires In General (AREA)
Abstract
The invention discloses wear-resistant tire tread rubber and a preparation method thereof, which belong to the technical field of compositions of high molecular compounds, and the wear-resistant tire tread rubber comprises, by weight, 40-60 parts of natural rubber, 25-35 parts of styrene-butadiene rubber, 15-25 parts of isoprene rubber, 25-30 parts of modified white carbon black, 20-25 parts of composite filler, 15-20 parts of N330 carbon black, 2-3 parts of stearic acid, 1-2 parts of calcium oxide, 1-2 parts of zinc oxide, 2.5-3.5 parts of age resister 4020.5, 8-12 parts of environment-friendly aromatic oil TDAE, 0.1-0.5 part of polyimide, 1.2-2 parts of sulfur, 1-2 parts of accelerator TM1, 0.5-1 part of accelerator NOBS and 1-3 parts of anti-reversion agent HTS. The wear-resistant tire tread rubber prepared by the invention can improve the wet skid resistance of the tire applying the tread rubber, reduce the rolling resistance of the tire, and ensure that the tread rubber has higher wear resistance, tensile strength and elongation at break.
Description
Technical Field
The invention belongs to the technical field of compositions of high molecular compounds, and particularly relates to wear-resistant tire tread rubber and a preparation method thereof.
Background
The base material of tread rubber is rubber, but the rubber material has large free volume, small intermolecular force, low glass transition temperature and amorphous high-elastic state, so most of rubber cannot be applied without filler reinforcement. The white carbon black is used as a reinforcing filler, so that the wet skid resistance of the tire can be improved, the rolling resistance of the tire can be effectively reduced, but the white carbon black is extremely easy to agglomerate, the interface effect between the white carbon black and a rubber matrix is weak, and the reinforcing effect is not ideal.
In the prior art, in order to improve the dispersibility of the white carbon black and improve the compatibility of the white carbon black and a matrix material, the added white carbon black is often modified by a silane coupling agent or a surfactant, or the silane coupling agent and the white carbon black dispersing agent are added while the white carbon black is added in the rubber mixing process.
CN113929978B discloses a tread rubber under solid aviation tire and its preparation method, its raw materials include natural rubber, white carbon black, silane coupling agent, white carbon black dispersant, N660 carbon black, etc., the invention adds white carbon black, silane coupling agent, white carbon black dispersant directly in the banburying step, silane coupling agent and white carbon black dispersant can improve the dispersibility of white carbon black in the rubber matrix, but the silane coupling agent added directly disperses the effect poorly, cause the white carbon black to disperse the poor stability and is apt to agglomerate again, can not raise the wet skid resistance of the tire to which this tread rubber is applied effectively, can not reduce its rolling resistance effectively.
CN113502135B discloses a self-repairing rubber composition for tires and a preparation method thereof, which are matched with a plurality of materials such as a reverse vulcanized rubber prepolymer, liquid isoprene, modified white carbon black, tackifying resin and the like for use, wherein the modified white carbon black is a group formed by modifying and grafting hydrated silicon dioxide on the surface, and the group comprises vinyl-triethoxysilane, dimethyl dichlorosilane and polyethylene glycol-6000. According to the invention, the silane coupling agent or the surfactant is adopted to modify the white carbon black, and although the method improves the compatibility of the white carbon black and a rubber matrix, the vulcanization of the rubber material is delayed, so that the tensile strength, the breaking elongation and the wear resistance of the tread rubber are reduced.
In conclusion, the direct addition of the silane coupling agent has an unsatisfactory dispersing effect, the white carbon black is easy to agglomerate again, the wet skid resistance of the tire cannot be effectively improved, the rolling resistance of the tire cannot be effectively reduced, and the white carbon black modified by the silane coupling agent or the surfactant can delay the vulcanization of rubber materials and influence the tensile strength, the stretch-break elongation and the wear resistance of tread rubber.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the wear-resistant tire tread rubber and the preparation method thereof, which can improve the wet skid resistance of the tire prepared by applying the tread rubber, reduce the rolling resistance of the tire, and ensure that the tread rubber has higher wear resistance, tensile strength and stretch-break elongation.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
The wear-resistant tire tread rubber comprises, by weight, 40-60 parts of natural rubber, 25-35 parts of styrene-butadiene rubber, 15-25 parts of isoprene rubber, 25-30 parts of modified white carbon black, 20-25 parts of composite filler, 15-20 parts of N330 carbon black, 2-3 parts of stearic acid, 1-2 parts of calcium oxide, 1-2 parts of zinc oxide, 2.5-3.5 parts of anti-aging agent 4020.5, 8-12 parts of environment-friendly aromatic hydrocarbon oil TDAE, 0.1-0.5 part of polyimide, 1.2-2 parts of sulfur, 1-2 parts of accelerator TMTD, 0.5-1 part of accelerator NOBS and 1-3 parts of anti-reversion agent HTS.
The preparation method of the modified white carbon black comprises primary modification and secondary modification;
Blending mercaptoalkanoic acid and ethanol to prepare a blend solution A, blending white carbon black and ethanol to prepare a blend solution B, adding the blend solution B into the blend solution A with the same volume, stirring and reacting for 4-6 hours at 600-800rpm, controlling the reaction temperature to be 70-85 ℃, standing for 10-12 hours after stirring and reacting, and carrying out suction filtration, washing and drying to obtain the primary modified white carbon black;
The mercaptoalkanoic acid is one of 3-mercaptopropionic acid, 4-mercaptobutyric acid and 5-mercaptopentanoic acid;
The mass ratio of the mercaptoalkanoic acid to the ethanol in the blend solution A is (2-4) (10-40);
the mass ratio of the white carbon black to the ethanol in the blend liquid B is (10-15) to (70-100);
in the primary modification step, the washing liquid used for washing is ethanol, and the drying temperature is 50-70 ℃.
The secondary modification, namely adding tert-butyl peroxybenzoate and primary modified white carbon black into solution polymerized styrene-butadiene rubber toluene solution, controlling the temperature to be 85-100 ℃, ensuring that the reaction is carried out under nitrogen atmosphere, stirring at 300-400rpm for reaction for 6-10h, and obtaining the modified white carbon black through suction filtration, washing and drying;
The mass ratio of the tert-butyl peroxybenzoate to the primary modified white carbon black to the solution polymerized styrene-butadiene rubber is (0.2-0.3) (12-16) (50-60);
The mass ratio of the solution polymerized styrene-butadiene rubber to toluene in the solution polymerized styrene-butadiene rubber toluene solution is (50-60) (400-600);
In the secondary modification step, the washing liquid used for washing is ethanol, and the drying temperature is 40-50 ℃.
The preparation method of the composite filler comprises the steps of preparing mixed liquid, preparing wet composite filler and drying;
mixing nano silicon carbide, nano silicon nitride and graphite, loading into a ball milling tank, adding ethanol-water mixed solution for ball milling, controlling the ball-to-material ratio to be (25-35): 1, the rotating speed to be 200-320rpm, the time to be 4-6h, performing ultrasonic treatment for 10-20min after ball milling, and controlling the ultrasonic frequency to be 30-40kHz to obtain mixed material liquid;
The volume fraction of the ethanol in the ethanol-water mixed solution is 60-80%;
The mass ratio of the nano silicon carbide to the nano silicon nitride to the graphite to the ethanol-water mixed solution is (0.3-0.5), (0.1-0.2), (3-5) and (70-90).
Dispersing N660 carbon black in an ethanol solution, carrying out high-speed homogenization treatment for 10-20min at a rotating speed of 8000-12000rpm to obtain a carbon black solution, adding a mixed solution into the carbon black solution, carrying out high-speed homogenization treatment for 12-18min at a rotating speed of 8000-12000rpm, and then filtering to remove a solvent to obtain the wet composite filler;
The mass ratio of N660 carbon black to ethanol in the carbon black solution is (5-9) 100;
The mass ratio of the mixed solution to the carbon black solution is (15-25) 100.
And (3) drying, namely drying the wet composite filler for 12-18 hours, and controlling the temperature of the drying process to be 55-70 ℃ to obtain the composite filler.
The preparation method of the wear-resistant tire tread rubber comprises the following steps of plasticating, banburying, discharging sheets and vulcanizing;
Plasticating, namely plasticating the natural rubber, the styrene-butadiene rubber and the isoprene rubber in an open mill at 56-62 ℃ for 14-16 minutes, and then carrying out thin pass through for 3-5 times to obtain plasticated rubber.
Banburying, namely setting the initial temperature of an internal mixer to 65-75 ℃, setting the initial rotating speed to 25-30rpm, adding plasticated rubber into the internal mixer, adjusting the rotating speed to 45-60rpm after the plasticated rubber is added, mixing for 1-2min, adding stearic acid, calcium oxide, zinc oxide, an anti-aging agent 4020, environment-friendly aromatic hydrocarbon oil TDAE and polyimide, mixing for 1-2min, sequentially adding modified white carbon black, composite filler and N330 carbon black, mixing for 12-14min, discharging, standing and cooling for 10-12h after discharging, and obtaining the banburying.
And (3) discharging the sheet, namely transferring the banburying glue to an open mill, adding sulfur, an accelerator TMTD, an accelerator NOBS and an anti-reversion agent HTS, carrying out thin pass for 4-6 times, controlling the processing temperature at 55-65 ℃, discharging the sheet, standing and cooling for 14-18h, and obtaining the glue mixture.
Vulcanizing the mixed rubber at 150-160 ℃ for 20-25min to obtain the tread rubber.
Compared with the prior art, the invention has the beneficial effects that:
(1) The wear-resistant tire tread rubber prepared by the invention has excellent dynamic performance, and the tire prepared by the tread rubber has excellent wet skid resistance and low rolling resistance, wherein 0 degree Ctan delta of the tread rubber is 0.268-0.278,60 degrees Ctan delta of the tread rubber is 0.091-0.095.
(2) The wear-resistant tire tread rubber prepared by the invention has good wear resistance and strength performance, the attorney abrasion volume of the tread rubber is 0.095-0.102cm 3, the tensile strength is 28.6-29.4MPa, and the elongation at break is 658-670%.
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
The wear-resistant tire tread rubber comprises the following raw materials in parts by weight in table 1;
the preparation method of the wear-resistant tire tread rubber comprises the following steps of plasticating, banburying, discharging sheets and vulcanizing;
(1) Plasticating
The natural rubber, the styrene-butadiene rubber and the isoprene rubber are plasticated in an open mill at 56 ℃ for 16 minutes, and then the rubber is thinned and passed through for 3 times to obtain plasticated rubber.
(2) Banburying
The initial temperature of the internal mixer is set to 65 ℃, the initial rotating speed is set to 25rpm, then the plasticated rubber is added into the internal mixer, the rotating speed is adjusted to 45rpm after the plasticated rubber is added, stearic acid, calcium oxide, zinc oxide, an anti-aging agent 4020, environment-friendly aromatic hydrocarbon oil TDAE and polyimide are added after mixing for 2min, modified white carbon black, composite filler and N330 carbon black are sequentially added after mixing for 1min, mixing is carried out for 12min, discharging is carried out, and standing and cooling are carried out for 10h after discharging, thus obtaining the banbury mixer.
The preparation of the modified white carbon black comprises the following steps:
A. One-time modification
Blending 3-mercaptopropionic acid and ethanol (the mass ratio is 2:10) to prepare a blend solution A, blending white carbon black and ethanol (the mass ratio is 10:70) to prepare a blend solution B, adding the blend solution B into the blend solution A with the same volume, stirring at 600rpm for reaction for 6h, controlling the reaction temperature to be 70 ℃, standing for 10h after stirring, filtering to obtain a filter cake, washing 3 times with ethanol, and drying at 50 ℃ to obtain the primary modified white carbon black.
B. Secondary modification
Adding tert-butyl peroxybenzoate and primary modified white carbon black into solution polymerized styrene-butadiene rubber toluene solution under the stirring condition, controlling the temperature to be 85 ℃, ensuring that the reaction is carried out under the nitrogen atmosphere, stirring at 300rpm for reaction for 10 hours, carrying out suction filtration to obtain a filter cake, washing with ethanol for 3 times, and drying at 40 ℃ to obtain modified white carbon black;
the mass ratio of the tert-butyl peroxybenzoate to the primary modified white carbon black to the solution polymerized styrene-butadiene rubber is 0.2:12:50;
the mass ratio of the solution polymerized styrene-butadiene rubber to toluene in the solution polymerized styrene-butadiene rubber toluene solution is 50:400.
The preparation of the composite filler comprises the following steps:
A. Preparation of the Mixed liquor
Mixing nano silicon carbide, nano silicon nitride and graphite, then filling the mixture into a ball milling tank, adding ethanol-water mixed solution for ball milling, controlling the ball-material ratio during ball milling to be 25:1, the rotating speed to be 200rpm, and the time to be 6 hours, performing ultrasonic treatment for 10 minutes after ball milling, and controlling the ultrasonic frequency to be 40kHz to obtain mixed solution;
The mass ratio of the nano silicon carbide to the nano silicon nitride to the graphite to the ethanol-water mixed solution is 0.3:0.1:3:70;
The volume fraction of ethanol in the ethanol-water mixed solution is 60%.
B. preparation of wet composite filler
Dispersing N660 carbon black in an ethanol solution, carrying out high-speed homogenization treatment at 8000rpm for 20min to obtain a carbon black solution, adding the mixed solution into the carbon black solution, carrying out high-speed homogenization treatment at 8000rpm for 18min, and then filtering to remove a solvent to obtain a wet composite filler;
the mass ratio of the mixed solution to the carbon black solution is 15:100;
the mass ratio of the N660 carbon black to the ethanol in the carbon black solution is 5:100.
C. Drying
And drying the wet composite filler for 12 hours, and controlling the temperature of the drying process to be 70 ℃ to obtain the composite filler.
(3) Sheet discharging
Transferring the rubber compound to an open mill, adding sulfur, an accelerator TMTD, an accelerator NOBS and an anti-reversion agent HTS, carrying out thin pass through for 4 times, controlling the processing temperature at 65 ℃, taking out the rubber compound, standing and cooling for 18 hours, and obtaining the rubber compound.
(4) Vulcanization
The compound was vulcanized for 25min at 150 ℃ to give a tread band.
Example 2
The wear-resistant tire tread rubber comprises the following raw materials in parts by weight in table 1;
the preparation method of the wear-resistant tire tread rubber comprises the following steps of plasticating, banburying, discharging sheets and vulcanizing;
(1) Plasticating
The natural rubber, the styrene-butadiene rubber and the isoprene rubber are plasticated in an open mill at 60 ℃ for 15 minutes, and then the rubber is thinned and passed for 4 times to obtain plasticated rubber.
(2) Banburying
The initial temperature of the internal mixer is set to 70 ℃, the initial rotating speed is set to 27rpm, then plasticated rubber is added into the internal mixer, the rotating speed is adjusted to 50rpm after the plasticated rubber is added, stearic acid, calcium oxide, zinc oxide, an anti-aging agent 4020, environment-friendly aromatic hydrocarbon oil TDAE and polyimide are added after mixing for 1.5min, modified white carbon black, composite filler and N330 carbon black are sequentially added after mixing for 1.5min, mixing is carried out for 13min, discharging is carried out, and standing cooling is carried out for 11h after discharging, thus obtaining the banburying rubber.
The preparation of the modified white carbon black comprises the following steps:
A. One-time modification
Blending 4-mercaptobutyric acid and ethanol (the mass ratio is 3:20) to prepare a blend solution A, blending white carbon black and ethanol (the mass ratio is 12:80) to prepare a blend solution B, adding the blend solution B into the blend solution A with the same volume, stirring and reacting for 5 hours at 700rpm, controlling the reaction temperature to be 75 ℃, standing for 11 hours after stirring and reacting, filtering to obtain a filter cake, washing 3 times by ethanol, and drying at 60 ℃ to obtain the primary modified white carbon black.
B. Secondary modification
Adding tert-butyl peroxybenzoate and primary modified white carbon black into solution polymerized styrene-butadiene rubber toluene solution under the stirring condition, controlling the temperature to 90 ℃, ensuring that the reaction is carried out under the nitrogen atmosphere, stirring at 350rpm for reaction for 8 hours, carrying out suction filtration to obtain a filter cake, washing with ethanol for 3 times, and drying at 45 ℃ to obtain modified white carbon black;
the mass ratio of the tert-butyl peroxybenzoate to the primary modified white carbon black to the solution polymerized styrene-butadiene rubber is 0.25:14:55;
The mass ratio of the solution polymerized styrene-butadiene rubber to toluene in the solution polymerized styrene-butadiene rubber toluene solution is 55:500.
The preparation of the composite filler comprises the following steps:
A. Preparation of the Mixed liquor
Mixing nano silicon carbide, nano silicon nitride and graphite, then filling the mixture into a ball milling tank, adding ethanol-water mixed solution for ball milling, controlling the ball-material ratio during ball milling to be 30:1, the rotating speed to be 260rpm, the time to be 5 hours, performing ultrasonic treatment for 15 minutes after ball milling, and controlling the ultrasonic frequency to be 35kHz to obtain mixed solution;
The volume fraction of ethanol in the ethanol-water mixed solution is 70%;
The mass ratio of the nano silicon carbide to the nano silicon nitride to the graphite to the ethanol-water mixed solution is 0.4:0.15:4:80.
B. preparation of wet composite filler
Dispersing N660 carbon black in an ethanol solution, carrying out high-speed homogenization treatment at 10000rpm for 15min to obtain a carbon black solution, adding the mixed solution into the carbon black solution, carrying out high-speed homogenization treatment at 10000rpm for 15min, and then filtering to remove a solvent to obtain a wet composite filler;
the mass ratio of the N660 carbon black to the ethanol in the carbon black solution is 7:100;
the mass ratio of the mixed solution to the carbon black solution is 20:100.
C. Drying
And (3) drying the wet composite filler for 15 hours, and controlling the temperature of the drying process to be 60 ℃ to obtain the composite filler.
(3) Sheet discharging
Transferring the rubber compound to an open mill, adding sulfur, an accelerator TMTD, an accelerator NOBS and an anti-reversion agent HTS, carrying out thin pass through for 5 times, controlling the processing temperature at 60 ℃, taking out the rubber compound, standing and cooling for 16 hours, and obtaining the rubber compound.
(4) Vulcanization
And vulcanizing the rubber material of the mixed rubber at 155 ℃ for 22min to obtain the tread rubber.
Example 3
The wear-resistant tire tread rubber comprises the following raw materials in parts by weight in table 1;
the preparation method of the wear-resistant tire tread rubber comprises the following steps of plasticating, banburying, discharging sheets and vulcanizing;
(1) Plasticating
The natural rubber, the styrene-butadiene rubber and the isoprene rubber are plasticated in an open mill at 62 ℃ for 14 minutes, and then the rubber is thinned and passed through for 5 times to obtain plasticated rubber.
(2) Banburying
The initial temperature of the internal mixer is set to 75 ℃, the initial rotating speed is set to 30rpm, then the plasticated rubber is added into the internal mixer, the rotating speed is adjusted to 60rpm after the plasticated rubber is added, stearic acid, calcium oxide, zinc oxide, an anti-aging agent 4020, environment-friendly aromatic hydrocarbon oil TDAE and polyimide are added after mixing for 1min, modified white carbon black, composite filler and N330 carbon black are sequentially added after mixing for 2min, mixing is carried out for 14min, discharging is carried out, and standing cooling is carried out for 12h after discharging, thus obtaining the banbury mixer.
The preparation method of the modified white carbon black comprises the following steps:
A. One-time modification
Blending 5-mercaptopentanoic acid and ethanol (the mass ratio is 4:40) to prepare a blend solution A, blending white carbon black and ethanol (the mass ratio is 15:100) to prepare a blend solution B, adding the blend solution B into the blend solution A with the same volume, stirring at 800rpm for reaction for 4 hours, controlling the reaction temperature to be 85 ℃, standing for 12 hours after stirring, filtering to obtain a filter cake, washing with ethanol for 4 times, and drying at 70 ℃ to obtain the primary modified white carbon black.
B. Secondary modification
Adding tert-butyl peroxybenzoate and primary modified white carbon black into solution polymerized styrene-butadiene rubber toluene solution under the stirring condition, controlling the temperature to be 100 ℃, ensuring that the reaction is carried out under the nitrogen atmosphere, stirring at 400rpm for 6 hours, carrying out suction filtration to obtain a filter cake, washing with ethanol for 4 times, and drying at 50 ℃ to obtain modified white carbon black;
the mass ratio of the tert-butyl peroxybenzoate to the primary modified white carbon black to the solution polymerized styrene-butadiene rubber is 0.3:16:60;
the mass ratio of the solution polymerized styrene-butadiene rubber to toluene in the solution polymerized styrene-butadiene rubber toluene solution is 60:600.
The preparation of the composite filler comprises the following steps:
A. Preparation of the Mixed liquor
Mixing nano silicon carbide, nano silicon nitride and graphite, then filling the mixture into a ball milling tank, adding ethanol-water mixed solution for ball milling, controlling the ball-material ratio during ball milling to be 35:1, the rotating speed to be 320rpm, and the time to be 4 hours, performing ultrasonic treatment for 20 minutes after ball milling, and controlling the ultrasonic frequency to be 30kHz to obtain mixed solution;
The volume fraction of ethanol in the ethanol-water mixed solution is 80%;
the mass ratio of the nano silicon carbide to the nano silicon nitride to the graphite to the ethanol-water mixed solution is 0.5:0.2:5:90.
B. preparation of wet composite filler
Dispersing N660 carbon black in an ethanol solution, carrying out high-speed homogenization treatment at 12000rpm for 10min to obtain a carbon black solution, adding the mixed solution into the carbon black solution, carrying out high-speed homogenization treatment at 12000rpm for 12min, and then filtering to remove the solvent to obtain a wet composite filler;
The mass ratio of the N660 carbon black to the ethanol in the carbon black solution is 9:100;
the mass ratio of the mixed solution to the carbon black solution is 25:100.
C. Drying
And drying the wet composite filler for 18 hours, and controlling the temperature of the drying process to be 55 ℃ to obtain the composite filler.
(3) Sheet discharging
Transferring the rubber compound to an open mill, adding sulfur, an accelerator TMTD, an accelerator NOBS and an anti-reversion agent HTS, carrying out thin pass through for 6 times, controlling the processing temperature at 55 ℃, taking out the rubber compound, standing and cooling for 14 hours, and obtaining the rubber compound.
(4) Vulcanization
The compound was vulcanized at 160 ℃ for 20min to obtain a tread rubber.
Comparative example 1
Comparative example 1 the method for preparing a tread rubber for a wear-resistant tire described in example 2 was used, and the components were added according to the weight parts shown in table 1, except that in the banburying step, the preparation of the modified white carbon black was changed to:
Blending silane coupling agent gamma-methacryloxypropyl trimethoxy silane (KH 570) and ethanol (mass ratio is 3:20) to prepare blending liquid A, blending white carbon black and ethanol (mass ratio is 12:80) to prepare blending liquid B, adding the blending liquid B into the blending liquid A with equal volume, stirring at 700rpm for reaction for 5h, controlling the reaction temperature to 75 ℃, standing for 11h after stirring, filtering to obtain a filter cake, washing 3 times with ethanol, and drying at 60 ℃ to obtain the modified white carbon black.
Comparative example 2
Comparative example 2 the method for preparing a tread rubber for a wear-resistant tire described in example 2 was used, and the components were added according to the weight parts shown in table 1, except that in the banburying step, the preparation of the composite filler was changed to:
adding nano silicon carbide, nano silicon nitride, graphite and N660 carbon black (the mass ratio is 0.4:0.15:4:80) into a mixer, mixing for 30min at 300rpm, and discharging to obtain the composite filler.
Comparative example 3
Comparative example 3 the method for preparing a tread rubber for a wear-resistant tire described in example 2 was used, and the component formulation was added according to the weight parts of table 1, except that in the banburying step, white carbon black was used instead of modified white carbon black.
Table 1 tread stock formulation:
The tread rubber prepared in comparative examples 1-3 and examples 1-3 was subjected to performance test, the mechanical properties of the tread rubber were tested according to GB/T528-2009, the test samples were cut into specific dumbbell shapes, the thickness of the samples was 2mm, the fixture distance was 75mm, the punctuation distance was 25mm, the stretching speed was 500mm/min, the dynamic mechanical properties of the tread rubber were subjected to temperature scan test using Dynamic Mechanical Thermal Analysis (DMTA), the temperature test scan range was-10 ℃ to 70 ℃, the temperature rise rate was set to 5 ℃/min, the frequency was 10Hz, the strain was 0.20%, the wear resistance of the tread rubber was tested according to GBT1689-2014, and the test results are shown in Table 2.
Table 2 tread band performance:
The dynamic mechanical properties of the tread rubber are represented by testing the loss factors of the tread rubber at different temperatures, wherein the loss factor tan delta at 0 ℃ is generally related to the wet skid resistance of the tread rubber to a certain extent, the higher the loss factor tan delta is, the better the wet skid resistance of the tread rubber is, the lower the loss factor tan delta is related to the hysteresis loss of the tread rubber at 60 ℃, and the smaller the hysteresis heat generation of the tread rubber is, the smaller the rolling resistance is. As can be seen from Table 2, the tread rubber of comparative example 1 and comparative example 3 has 0 DEG Ctan delta lower than that of example 2 and 60 DEG Ctan delta higher than that of example 2, and the tensile strength, elongation at break and wear resistance of the tread rubber of comparative example 1 and comparative example 3 are slightly reduced as compared with those of example 2, which shows that the modified white carbon black prepared by the method of the invention effectively improves the dynamics performance of the tread rubber, effectively improves the wet skid resistance and reduces the rolling resistance, and simultaneously improves the tensile strength, elongation at break and wear resistance of the tread rubber.
According to the invention, after the white carbon black is subjected to primary modification by the mercapto-alkanoic acid, the white carbon black is reacted with the solution polymerized styrene-butadiene rubber, and the white carbon black is bonded with a rubber molecular chain to prepare the modified white carbon black, so that the dispersibility of the modified white carbon black is greatly improved, the modified white carbon black can be tightly combined with a rubber matrix, and the energy dissipation under dynamic load is reduced. Compared with the traditional white carbon black modified by a silane coupling agent, the modified white carbon black prepared by the two-step method avoids the problems of aggregation of the white carbon black and vulcanization delay of rubber materials caused by unstable dispersibility, effectively improves the dynamic performance of tread rubber, improves the wet skid resistance, reduces the rolling resistance, and simultaneously improves the tensile strength and the stretch-break elongation of the tread rubber.
As can be seen from table 2, the acle abrasion volume of the tread rubber of comparative example 2 is obviously higher than that of example 2, the tensile strength and the elongation at break are obviously lower than those of example 2, and compared with the simple mixed composite filler, the composite filler prepared by ball milling and high-speed homogenization treatment can obviously improve the abrasion resistance, the tensile strength and the elongation at break of the tread rubber;
the invention adopts the nano silicon nitride, the nano silicon carbide and the graphite to perform ball milling pre-compounding, and then forms the composite filler through high-speed homogenization, thereby being beneficial to dispersing the nano silicon nitride, the nano silicon carbide and the graphite pre-compound in rubber, leading the composite filler to generate stronger interface interaction with the rubber, and improving the wear resistance, the tensile strength and the stretch-break elongation of the tread.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto, but may be modified or substituted for some of the technical features thereof by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The wear-resistant tire tread rubber is characterized by comprising, by weight, 40-60 parts of natural rubber, 25-35 parts of styrene-butadiene rubber, 15-25 parts of isoprene rubber, 25-30 parts of modified white carbon black, 20-25 parts of composite filler, 15-20 parts of N330 carbon black, 2-3 parts of stearic acid, 1-2 parts of calcium oxide, 1-2 parts of zinc oxide, 2.5-3.5 parts of anti-aging agent 4020, 8-12 parts of environment-friendly aromatic hydrocarbon oil TDAE, 0.1-0.5 part of polyimide, 1.2-2 parts of sulfur, 1-2 parts of accelerator TMTD, 0.5-1 part of accelerator NOBS and 1-3 parts of anti-reversion agent HTS;
The preparation method of the modified white carbon black comprises primary modification and secondary modification;
Blending mercaptoalkanoic acid and ethanol to prepare a blend solution A, blending white carbon black and ethanol to prepare a blend solution B, adding the blend solution B into the blend solution A with the same volume, stirring and reacting for 4-6 hours at 70-85 ℃, standing for 10-12 hours after the reaction is finished, and carrying out suction filtration, washing and drying to obtain the primary modified white carbon black;
The secondary modification, namely adding tert-butyl peroxybenzoate and primary modified white carbon black into solution polymerized styrene-butadiene rubber toluene solution, controlling the temperature to be 85-100 ℃, ensuring that the reaction is carried out under nitrogen atmosphere, stirring at 300-400rpm for reaction for 6-10h, and obtaining the modified white carbon black through suction filtration, washing and drying;
the preparation method of the composite filler comprises the steps of preparing mixed liquid, preparing wet composite filler and drying;
Mixing nano silicon carbide, nano silicon nitride and graphite, adding ethanol-water mixed solution for ball milling, and performing ultrasonic treatment after ball milling to obtain mixed solution;
Dispersing N660 carbon black in an ethanol solution, carrying out high-speed homogenization treatment for 10-20min at a rotating speed of 8000-12000rpm to obtain a carbon black solution, adding a mixed solution into the carbon black solution, carrying out high-speed homogenization treatment for 12-18min at a rotating speed of 8000-12000rpm, and then filtering to remove a solvent to obtain the wet composite filler.
2. The wear-resistant tire tread rubber according to claim 1, wherein in the primary modification step, the stirring rate is 600 to 800rpm.
3. The wear-resistant tire tread rubber according to claim 1, wherein in the primary modification step, the mercaptoalkanoic acid is one of 3-mercaptopropionic acid, 4-mercaptobutyric acid, and 5-mercaptovaleric acid;
The mass ratio of the mercaptoalkanoic acid to the ethanol in the blend solution A is (2-4) (10-40);
the mass ratio of the white carbon black to the ethanol in the blend liquid B is (10-15) to (70-100).
4. The wear-resistant tire tread rubber according to claim 1, wherein in the secondary modification step, the mass ratio of the tert-butyl peroxybenzoate to the primary modified white carbon black to the solution polymerized styrene-butadiene rubber is (0.2-0.3): 12-16): 50-60;
The mass ratio of the solution polymerized styrene-butadiene rubber to toluene in the solution polymerized styrene-butadiene rubber toluene solution is (50-60) (400-600).
5. The wear-resistant tire tread rubber according to claim 1, wherein in the step of preparing the mixed solution, the ball-milling process has a ball-to-material ratio of (25-35) 1, a rotating speed of 200-320rpm and a time of 4-6h;
In the step of preparing the mixed solution, the ultrasonic treatment time is 10-20min, and the ultrasonic frequency is 30-40kHz.
6. The wear-resistant tire tread rubber according to claim 1, wherein in the step of preparing the mixed solution, the volume fraction of ethanol in the ethanol-water mixed solution is 60-80%;
The mass ratio of the nano silicon carbide to the nano silicon nitride to the graphite to the ethanol-water mixed solution is (0.3-0.5), (0.1-0.2), (3-5) and (70-90).
7. The wear-resistant tire tread rubber according to claim 1, wherein in the step of preparing the wet composite filler, the mass ratio of the N660 carbon black to the ethanol in the carbon black solution is (5-9) 100;
The mass ratio of the mixed solution to the carbon black solution is (15-25) 100.
8. The method for preparing the tread rubber for the wear-resistant tire according to any one of claims 1 to 7, wherein the preparation method comprises the steps of plasticating, banburying, sheet discharging and vulcanizing;
Plasticating natural rubber, styrene-butadiene rubber and isoprene rubber at 56-62 ℃ for 14-16 minutes, and then carrying out thin pass through for 3-5 times to obtain plasticated rubber;
The banburying is carried out, plasticated rubber is added into banburying equipment with the initial temperature of 65-75 ℃ and the initial rotating speed of 25-30rpm, the rotating speed is adjusted to 45-60rpm after the plasticated rubber is added, the banburying is carried out for 1-2min, then stearic acid, calcium oxide, zinc oxide, an anti-aging agent 4020, environment-friendly aromatic hydrocarbon oil TDAE and polyimide are added, after mixing for 1-2min, modified white carbon black, composite filler and N330 carbon black are added, mixing is carried out for 12-14min, discharging is carried out, and standing cooling is carried out for 10-12h after discharging, thus obtaining banburying;
Adding sulfur, an accelerator TMTD, an accelerator NOBS and an anti-reversion agent HTS into the rubber compound, carrying out thin ventilation for 4-6 times, controlling the processing temperature at 55-65 ℃, standing and cooling the rubber compound for 14-18h to obtain rubber compound;
And vulcanizing the mixed rubber at 150-160 ℃ for 20-25min to obtain the tread rubber.
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| CN109181038A (en) * | 2018-07-25 | 2019-01-11 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of modified white carbon black tread rubber |
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| US7019084B2 (en) * | 2002-12-11 | 2006-03-28 | The Goodyear Tire & Rubber Company | Tire with rubber composition |
| JP2004263041A (en) * | 2003-02-28 | 2004-09-24 | Yokohama Rubber Co Ltd:The | Decomposition method of vulcanized rubber, decomposed rubber recovered by it, and decomposed rubber composition containing the decomposed rubber |
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| CN109181038A (en) * | 2018-07-25 | 2019-01-11 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of modified white carbon black tread rubber |
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