CN114752123A - High-tearing-resistance cutting-resistance flexing-resistance tire tread material and preparation method thereof - Google Patents
High-tearing-resistance cutting-resistance flexing-resistance tire tread material and preparation method thereof Download PDFInfo
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- CN114752123A CN114752123A CN202210360238.XA CN202210360238A CN114752123A CN 114752123 A CN114752123 A CN 114752123A CN 202210360238 A CN202210360238 A CN 202210360238A CN 114752123 A CN114752123 A CN 114752123A
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- 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
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- 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
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- 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
Abstract
The invention discloses a high-tearing-resistance cutting-resistance flexing-resistance tire tread material and a preparation method thereof, wherein the tire tread material is prepared from the following components in parts by weight: 35-45 parts of hydrogenated nitrile rubber, 50-60 parts of butadiene rubber, 8-12 parts of polyamide thermoplastic elastomer, 5-12 parts of copolymer resin, 3-5 parts of quinolyl polyurethane based polyamide polycondensate, 1-3 parts of sulfonated poly (aryl ether ketone-benzimidazole), 1-3 parts of Luck H-518 tear-resistant assistant, 1-3 parts of anti-aging agent, 1-3 parts of stearic acid, 30-40 parts of filler, 1-2 parts of coupling agent, 2-4 parts of vulcanizing agent, 1-2 parts of accelerator, 1-2 parts of phosphorus pentoxide and 0.8-1.2 parts of polyphosphoric acid; the copolymer resin is prepared by polymerizing N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane through free radicals. The high-tearing-resistance cutting-resistance flexing-resistance tire tread material disclosed by the invention has excellent tear resistance, cutting-resistance flexing resistance, aging resistance and wear resistance.
Description
Technical Field
The invention relates to the technical field of rubber material preparation, in particular to a high-tearing-property cutting-resistant flexing-resistant tire tread material and a preparation method thereof.
Background
The tire tread is a layer on which a pattern is printed on the surface of the outermost layer of the tire in contact with the road surface, and can provide traction to the tire, absorb shocks and vibrations during running, and prevent the cutting and piercing of the cord layer. Desirable tire tread materials are required to have excellent wear resistance, aging resistance, mechanical properties, and heat resistance at the same time. The engineering tire of the mining automobile and the mountain tire of the off-road automobile are easy to be scratched by stones due to running on gravel and sharp ore pavements, and have the phenomena of cracks, chipping and falling off, and better tear resistance, cutting resistance and flexing resistance are needed.
The tire tread material of most of the existing tire plants adopts a raw rubber system which is made of natural rubber or the combination of the natural rubber and styrene-butadiene rubber, the initial cracking performance, the cutting resistance and the puncture resistance of the styrene-butadiene rubber are superior to those of the natural rubber, but the tearing strength of the styrene-butadiene rubber is poor, the butadiene rubber is easy to crack and fall into blocks, the growth speed of the cracks of the styrene-butadiene rubber is high, the cutting resistance of the tires at the middle and later stages is poor, and the service life of the tires is influenced. Other types of tire tread materials on the market also have the technical problems that the aging resistance is insufficient, the ground gripping performance is poor, and in the using process, due to the external influence, a cross-linking network in vulcanized rubber is damaged, so that the physical property of the vulcanized rubber is reduced, and the tire is scrapped.
In order to solve the problems, the Chinese invention patent CN107973950B relates to an environment-friendly engineering tire tread rubber composition for downhole use and a preparation method thereof, belonging to the technical field of tire materials. The composition comprises the following components in parts by weight: 100 parts of styrene-butadiene rubber, 30-70 parts of reinforcing carbon black, 1-10 parts of tear-resistant resin, 1-5 parts of modified aramid fiber, 0.5-2 parts of anti-vulcanization reversion agent, 1-3 parts of sulfur, 3-7 parts of anti-aging agent, 2-4 parts of accelerator, 1-4 parts of microcrystalline protective wax, 1-10 parts of zinc oxide, 1-5 parts of stearic acid and 0.05-0.5 part of anti-scorching agent. The invention adopts environment-friendly butadiene styrene rubber, and improves the cutting resistance, the anti-chipping performance, the hysteresis heating performance, the wear resistance, the fatigue resistance, the tearing resistance and the cutting resistance of the rubber material by introducing the anti-tearing resin, the modified aramid fiber and the anti-reversion agent, thereby reducing the tire burst probability and greatly prolonging the service life of the engineering tire. However, the flex resistance, grip performance, aging resistance and performance stability of the tire tread material are to be further improved.
Accordingly, there is still a need in the art for a high-tear-resistance, cut-resistant and flex-resistant tire tread material having excellent tear resistance, cut-resistant and flex-resistant properties, good grip, aging resistance and wear resistance, and long service life, and a method for preparing the same.
Disclosure of Invention
The invention mainly aims to solve the technical problems and provides a high-tearing-performance cutting-performance and flexing-performance resistant tire tread material with excellent tearing performance, excellent cutting-performance and flexing-performance resistance, excellent grip performance, excellent aging-performance and excellent wear resistance and long service life and a preparation method thereof through formula design.
In order to achieve the purpose, the invention provides a high-tearing-resistance cutting-resistance flexing-resistance tire tread material which is characterized by comprising the following components in parts by weight: 35-45 parts of hydrogenated nitrile rubber, 50-60 parts of butadiene rubber, 8-12 parts of polyamide thermoplastic elastomer, 5-12 parts of copolymer resin, 3-5 parts of quinolyl polyurethane based polyamide polycondensate, 1-3 parts of sulfonated poly (aryl ether ketone-benzimidazole), 1-3 parts of Luck H-518 tear-resistant assistant, 1-3 parts of anti-aging agent, 1-3 parts of stearic acid, 30-40 parts of filler, 1-2 parts of coupling agent, 2-4 parts of vulcanizing agent, 1-2 parts of accelerator, 1-2 parts of phosphorus pentoxide and 0.8-1.2 parts of polyphosphoric acid; the copolymer resin is prepared by polymerizing N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane through free radicals.
Preferably, the accelerator is accelerator NS.
Preferably, the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to a mass ratio of (3-5): 1.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to the mass ratio of 1 (1-3) to (3-5) to (4-6); the granularity of the filler is 800-1200 meshes; the average diameter of the nano boron fiber is 300-500nm, and the length-diameter ratio is (15-20): 1.
Preferably, the anti-aging agent is a mixture formed by mixing an anti-aging agent RD and an anti-aging agent 4020 according to the mass ratio of 1 (1-2).
Preferably, the source of the sulfonated poly (aryl ether ketone-benzimidazole) is not particularly required, and in one embodiment of the present invention, the sulfonated poly (aryl ether ketone-benzimidazole) is prepared according to the preparation method of the five-polymer 5-1 in the chinese patent CN 101230137B.
Preferably, the method for preparing the quinolyl polyurethane based polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinoline dicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, reacting at the temperature of 130 ℃ and 145 ℃ for 3-5 hours under normal pressure, heating to the temperature of 230 ℃ and 240 ℃, carrying out polycondensation reaction at the pressure of 350 ℃ and 550Pa for 10-16 hours, cooling to room temperature, adjusting to the normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and drying in a vacuum drying oven at the temperature of 85-95 ℃ to constant weight to obtain the quinolyl polyurethane based polyamide polycondensate.
Preferably, the molar ratio of the 2, 3-quinolinedicarboxylic acid to the amino-terminated polyurethane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling-point solvent is 1:1 (0.8-1.2) to (0.6-0.8) to (15-20).
Preferably, the source of the amino-terminated polyurethane has no special requirement, and in one embodiment of the present invention, the amino-terminated polyurethane is prepared according to the preparation method of amino-terminated linear polyurethane in example 1 of chinese patent CN 106750144B.
Preferably, the high boiling point solvent is any one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone; the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the preparation method of the copolymer resin comprises the following steps: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 3-5 hours at 50-65 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the copolymer resin.
Preferably, the mass ratio of the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, the 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, the styrene, the acrylonitrile, the vinyl trimethoxy silane, the azobisisobutyronitrile and the dimethyl sulfoxide is (3-5):1 (1-2): 0.8-1.2):1 (0.06-0.1): 20-30.
Preferably, the polyamide thermoplastic elastomer is polyether block amide Pebax 4033 SA 01.
Preferably, the butadiene rubber is raw butadiene rubber BR9000 with the number average molecular weight of 71000.
Preferably, the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
Another object of the present invention is to provide a method for preparing the high tear, cut and flex resistant tire tread material, which comprises the following steps: the components are mixed in sequence according to the parts by weight, mixed evenly on an open mill, and then vulcanized to prepare the high-tearing-property cutting-resistant flexing-resistant tire tread material.
Preferably, the vulcanization processing is two-stage vulcanization, the one-stage vulcanization temperature is 180-190 ℃, and the vulcanization time is 6-10 minutes; the secondary vulcanization temperature is 150-160 ℃, and the vulcanization time is 2-4 hours.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) The high-tearing-resistance cutting-resistance flexing-resistance tire tread material disclosed by the invention is prepared by sequentially carrying out mixing and vulcanization processing, does not need special equipment and a complex process, is simple in preparation method, convenient to operate and control, low in energy consumption, high in preparation efficiency, suitable for continuous large-scale production, and has a high popularization and application value.
(2) The high-tearing-resistance cutting-resistance flexing-resistance tire tread material disclosed by the invention takes the blending of hydrogenated nitrile rubber, butadiene rubber and a polyamide thermoplastic elastomer as a base material of the tread material, combines the excellent performances of the materials, so that the prepared material has good mechanical property and good wear resistance, and can be matched with other components to act together, so that the tread material can be endowed with excellent tear resistance, cutting-resistance flexing resistance, gripping performance and aging resistance, and the service life of the tire tread material is long.
(3) The invention discloses a high-tearing cutting-resistant flexing-resistant tire tread material, wherein the copolymer resin is prepared by the free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane; a fluorine-containing phenyl structure is introduced, so that the aging resistance, wear resistance, tear resistance, cutting resistance and flexibility resistance can be improved; the acrylonitrile structural unit and the hydrogenated nitrile rubber have similar nitrile group structures, and the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide and the polyamide thermoplastic elastomer contain similar amide group structures, so that the compatibility between the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide and the polyamide thermoplastic elastomer is good, the molecular structure of the material is more compact, and the service life is longer. The quinoline, amide and polyurethane structures are introduced into the molecular structure of the quinolyl polyurethane based polyamide polycondensate, and the quinolyl polyurethane based polyamide polycondensate can further improve the wear resistance, tear resistance, flex resistance and cutting resistance under the combined action with other structures, so that the service life is further prolonged.
(4) According to the high-tearing-property cutting-resistant and flexing-resistant tire tread material disclosed by the invention, the addition of sulfonated poly (aryl ether ketone-benzimidazole) can play a role in enhancing and improving the tearing-resistant, flexing-resistant and cutting-resistant properties, and a sulfonic group on the sulfonated poly (aryl ether ketone-benzimidazole) is subjected to a chemical reaction with benzene rings on copolymer resin and quinolyl polyurethane based polyamide polycondensate under the catalytic action of phosphorus pentoxide and polyphosphoric acid and is matched with a vulcanization system to form a multiple interpenetrating network structure in a molecular structure, so that the physical property and the performance stability are effectively improved, and the service life is prolonged; the prepared tire tread material has good tear resistance, cutting resistance and flexing resistance, excellent ground gripping performance, aging resistance and wear resistance and long service life.
(5) The invention discloses a high-tearing-resistance cutting-resistance flexing-resistance tire tread material, wherein a filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to a mass ratio of 1 (1-3) to (3-5) to (4-6); the components have a better reinforcing effect under the coordination effect, and the fillers have good compatibility with the base material; the fly ash belongs to resource recycling, so that waste is changed into valuable, and the ecological value is high.
Detailed Description
The following description is provided to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments described below are by way of example only, and other obvious variations will occur to those skilled in the art.
The sulfonated poly (aryl ether ketone-benzimidazole) in each embodiment of the invention is prepared by the preparation method of the five-polymer 5-1 in the embodiment of the Chinese patent CN 101230137B; the amino-terminated polyurethane is prepared according to a preparation method of linear polyurethane taking amino as a terminal group in embodiment 1 of Chinese patent CN 106750144B.
Example 1
A high-tearing-property cutting-resistant flexing-resistant tire tread material comprises the following components in parts by weight: 35 parts of hydrogenated nitrile rubber, 50 parts of butadiene rubber, 8 parts of polyamide thermoplastic elastomer, 5 parts of copolymer resin, 3 parts of quinolyl polyurethane based polyamide polycondensate, 1 part of sulfonated poly (aryl ether ketone-benzimidazole), 1 part of Luck H-518 tear resistant auxiliary agent, 1 part of anti-aging agent, 1 part of stearic acid, 30 parts of filler, 1 part of coupling agent, 2 parts of vulcanizing agent, 1 part of accelerator, 1 part of phosphorus pentoxide and 0.8 part of polyphosphoric acid; the copolymer resin is prepared by free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane.
The accelerator is accelerator NS; the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to the mass ratio of 3: 1; the coupling agent is a silane coupling agent KH 550.
The filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to a mass ratio of 1:1:3: 4; the granularity of the filler is 800 meshes; the average diameter of the nano boron fiber is 300nm, and the length-diameter ratio is 15: 1; the anti-aging agent is a mixture formed by mixing an anti-aging agent RD and an anti-aging agent 4020 in a mass ratio of 1: 1.
The preparation method of the quinolyl polyurethane based polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting at 130 ℃ under normal pressure for 3 hours, heating to 230 ℃, carrying out polycondensation reaction at 350Pa for 10 hours, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3 times, and drying in a vacuum drying oven at 85 ℃ to constant weight to obtain the quinolyl polyurethane based polyamide polycondensate; the molar ratio of the 2, 3-quinolinedicarboxylic acid to the amino-terminated polyurethane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling-point solvent is 1:1:0.8:0.6: 15; the high boiling point solvent is dimethyl sulfoxide; the inert gas is nitrogen.
The preparation method of the copolymer resin comprises the following steps: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 3 hours at 50 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying oven at 85 ℃ to constant weight to obtain copolymer resin; the mass ratio of the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, the 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, the styrene, the acrylonitrile, the vinyl trimethoxy silane, the azobisisobutyronitrile and the dimethyl sulfoxide is 3:1:1:0.8:1:0.06: 20.
The polyamide thermoplastic elastomer is polyether block amide Pebax 4033 SA 01; the butadiene rubber is raw butadiene rubber BR9000 with the number average molecular weight of 71000; the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
A preparation method of the high-tearing-property cutting-resistance flexing-resistance tire tread material comprises the following steps: sequentially mixing the components in parts by weight, uniformly mixing on an open mill, and then carrying out vulcanization processing to prepare the high-tearing-property cutting-resistant flexing-resistant tire tread material; the vulcanization processing is two-stage vulcanization, wherein the first-stage vulcanization temperature is 180 ℃, and the vulcanization time is 6 minutes; the secondary vulcanization temperature is 150 ℃, and the vulcanization time is 2 hours.
Example 2
A high-tearing-resistance cutting-resistance flexing-resistance tire tread material comprises the following components in parts by weight: 37 parts of hydrogenated nitrile rubber, 53 parts of butadiene rubber, 9 parts of polyamide thermoplastic elastomer, 7 parts of copolymer resin, 3.5 parts of quinolyl polyurethane based polyamide polycondensate, 1.5 parts of sulfonated poly (aryl ether ketone-benzimidazole), 1.5 parts of Luck H-518 tear resistant auxiliary agent, 1.5 parts of anti-aging agent, 1.5 parts of stearic acid, 33 parts of filler, 1.2 parts of coupling agent, 2.5 parts of vulcanizing agent, 1.2 parts of accelerator, 1.3 parts of phosphorus pentoxide and 0.9 part of polyphosphoric acid; the copolymer resin is prepared by free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane.
The accelerator is accelerator NS; the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to a mass ratio of 3.5: 1; the coupling agent is a silane coupling agent KH 560; the filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to the mass ratio of 1:1.5:3.5: 4.5; the granularity of the filler is 900 meshes; the average diameter of the nano boron fiber is 350nm, and the length-diameter ratio is 17: 1; the anti-aging agent is a mixture formed by mixing an anti-aging agent RD and an anti-aging agent 4020 in a mass ratio of 1: 1.3.
The preparation method of the quinolyl polyurethane based polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 3.5 hours at the normal pressure and the temperature of 135 ℃, heating to 233 ℃, carrying out polycondensation reaction for 12 hours at the pressure of 400Pa, cooling to the room temperature, adjusting to the normal pressure, precipitating in water, washing the precipitated polymer for 4 times with ethanol, and drying in a vacuum drying oven at the temperature of 87 ℃ to constant weight to obtain the quinolinyl polyurethane based polyamide polycondensate; the molar ratio of the 2, 3-quinolinedicarboxylic acid to the amino-terminated polyurethane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling-point solvent is 1:1:0.9:0.65: 17; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The preparation method of the copolymer resin comprises the following steps: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 3.5 hours at 55 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 4 times, and finally drying in a vacuum drying oven at 87 ℃ to constant weight to obtain copolymer resin; the mass ratio of the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, the 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, the styrene, the acrylonitrile, the vinyl trimethoxy silane, the azobisisobutyronitrile and the dimethyl sulfoxide is 3.5:1:1.3:0.9:1:0.07: 23.
The polyamide thermoplastic elastomer is polyether block amide Pebax 4033 SA 01; the butadiene rubber is raw butadiene rubber BR9000 with the number average molecular weight of 71000; the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
A preparation method of the high-tearing-property cutting-resistance flexing-resistance tire tread material comprises the following steps: sequentially mixing the components in parts by weight, uniformly mixing on an open mill, and then carrying out vulcanization processing to prepare the high-tearing-property cutting-resistant flexing-resistant tire tread material; the vulcanization processing is two-stage vulcanization, the first-stage vulcanization temperature is 183 ℃, and the vulcanization time is 7 minutes; the secondary vulcanization temperature was 153 ℃ and the vulcanization time was 2.5 hours.
Example 3
A high-tearing-property cutting-resistant flexing-resistant tire tread material comprises the following components in parts by weight: 40 parts of hydrogenated nitrile rubber, 55 parts of butadiene rubber, 10 parts of polyamide thermoplastic elastomer, 9 parts of copolymer resin, 4 parts of quinolyl polyurethane-based polyamide polycondensate, 2 parts of sulfonated poly (aryl ether ketone-benzimidazole), 2 parts of Luck H-518 tear-resistant assistant, 2 parts of anti-aging agent, 2 parts of stearic acid, 35 parts of filler, 1.5 parts of coupling agent, 3 parts of vulcanizing agent, 1.5 parts of accelerator, 1.5 parts of phosphorus pentoxide and 1 part of polyphosphoric acid; the copolymer resin is prepared by free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane.
The accelerator is accelerator NS; the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to a mass ratio of 4: 1; the coupling agent is a silane coupling agent KH 570; the filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to a mass ratio of 1:2:4: 5; the granularity of the filler is 1000 meshes; the average diameter of the nano boron fiber is 400nm, and the length-diameter ratio is 18: 1; the anti-aging agent is a mixture formed by mixing an anti-aging agent RD and an anti-aging agent 4020 in a mass ratio of 1: 1.5.
The preparation method of the quinolyl polyurethane based polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 4 hours at 138 ℃ under normal pressure, heating to 235 ℃, carrying out polycondensation reaction for 13 hours under 450Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer for 5 times with ethanol, and drying in a vacuum drying oven at 90 ℃ to constant weight to obtain the quinolyl polyurethane based polyamide polycondensate; the molar ratio of the 2, 3-quinolinedicarboxylic acid to the amino-terminated polyurethane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling-point solvent is 1:1:1:0.7: 18; the high boiling point solvent is N-methyl pyrrolidone; the inert gas is neon.
The preparation method of the copolymer resin comprises the following steps: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 4 hours at 59 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 5 times, and finally drying in a vacuum drying oven at 90 ℃ to constant weight to obtain copolymer resin; the mass ratio of the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, the 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, the styrene, the acrylonitrile, the vinyl trimethoxy silane, the azobisisobutyronitrile and the dimethyl sulfoxide is 4:1:1.5:1:1:0.08: 25.
The polyamide thermoplastic elastomer is polyether block amide Pebax 4033 SA 01; the butadiene rubber is raw butadiene rubber BR9000 with the number average molecular weight of 71000; the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
A preparation method of the high-tearing-property cutting-resistance flexing-resistance tire tread material comprises the following steps: sequentially mixing the components in parts by weight, uniformly mixing on an open mill, and then carrying out vulcanization processing to prepare the high-tearing-property cutting-resistant flexing-resistant tire tread material; the vulcanization processing is two-stage vulcanization, wherein the first-stage vulcanization temperature is 185 ℃, and the vulcanization time is 8 minutes; the secondary vulcanization temperature is 155 ℃, and the vulcanization time is 3 hours.
Example 4
A high-tearing-property cutting-resistant flexing-resistant tire tread material comprises the following components in parts by weight: 43 parts of hydrogenated nitrile rubber, 58 parts of butadiene rubber, 11 parts of polyamide thermoplastic elastomer, 11 parts of copolymer resin, 4.5 parts of quinolyl polyurethane based polyamide polycondensate, 2.5 parts of sulfonated poly (aryl ether ketone-benzimidazole), 2.5 parts of Luck H-518 tear resistant auxiliary agent, 2.5 parts of anti-aging agent, 3 parts of stearic acid, 38 parts of filler, 1.8 parts of coupling agent, 3.5 parts of vulcanizing agent, 1.8 parts of accelerator, 1.8 parts of phosphorus pentoxide and 1.1 parts of polyphosphoric acid; the copolymer resin is prepared by free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane.
The accelerant is accelerant NS; the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to the mass ratio of 4.5: 1; the coupling agent is a mixture formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:3: 2; the filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to the mass ratio of 1:2.5:4.5: 5.5; the granularity of the filler is 1100 meshes; the average diameter of the nano boron fiber is 450nm, and the length-diameter ratio is 19: 1; the anti-aging agent is a mixture formed by mixing an anti-aging agent RD and an anti-aging agent 4020 in a mass ratio of 1: 1.9.
The preparation method of the quinolyl polyurethane based polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 4.5 hours at the temperature of 143 ℃ under normal pressure, heating to 238 ℃, carrying out polycondensation reaction for 15 hours under 530Pa, cooling to room temperature, adjusting to the normal pressure, precipitating in water, washing the precipitated polymer for 6 times with ethanol, and drying in a vacuum drying oven at the temperature of 93 ℃ to constant weight to obtain the quinolinyl polyurethane based polyamide polycondensate; the molar ratio of the 2, 3-quinolinedicarboxylic acid to the amino-terminated polyurethane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling-point solvent is 1:1:1.1:0.75: 19; the high boiling point solvent is dimethyl sulfoxide; the inert gas is argon.
The preparation method of the copolymer resin comprises the following steps: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 4.5 hours at 63 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 6 times, and finally drying in a vacuum drying oven at 93 ℃ to constant weight to obtain copolymer resin; the mass ratio of the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, the 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, the styrene, the acrylonitrile, the vinyl trimethoxy silane, the azobisisobutyronitrile and the dimethyl sulfoxide is 4.5:1:1.8:1.1:1:0.09: 28.
The polyamide thermoplastic elastomer is polyether block amide Pebax 4033 SA 01; the butadiene rubber is butadiene rubber BR9000 crude rubber, and the number average molecular weight is 71000; the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
A preparation method of the high-tearing-property cutting-resistance flexing-resistance tire tread material comprises the following steps: sequentially mixing the components in parts by weight, uniformly mixing on an open mill, and then carrying out vulcanization processing to prepare the high-tearing-property cutting-resistant flexing-resistant tire tread material; the vulcanization processing is two-stage vulcanization, the first-stage vulcanization temperature is 188 ℃, and the vulcanization time is 9.5 minutes; the secondary vulcanization temperature was 158 ℃ and the vulcanization time was 3.5 hours.
Example 5
A high-tearing-property cutting-resistant flexing-resistant tire tread material comprises the following components in parts by weight: 45 parts of hydrogenated nitrile rubber, 60 parts of butadiene rubber, 12 parts of polyamide thermoplastic elastomer, 12 parts of copolymer resin, 5 parts of quinolyl polyurethane based polyamide polycondensate, 3 parts of sulfonated poly (aryl ether ketone-benzimidazole), 3 parts of Luck H-518 tear resistant auxiliary agent, 3 parts of anti-aging agent, 3 parts of stearic acid, 40 parts of filler, 2 parts of coupling agent, 4 parts of vulcanizing agent, 2 parts of accelerator, 2 parts of phosphorus pentoxide and 1.2 parts of polyphosphoric acid; the copolymer resin is prepared by free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane.
The accelerator is accelerator NS; the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to a mass ratio of 5: 1; the coupling agent is a silane coupling agent KH 550; the filler is a mixture formed by mixing lignin, nano boron fiber, fly ash and white carbon black according to a mass ratio of 1:3:5: 6; the particle size of the filler is 1200 meshes; the average diameter of the nano boron fiber is 500nm, and the length-diameter ratio is 20: 1; the anti-aging agent is a mixture formed by mixing an anti-aging agent RD and an anti-aging agent 4020 in a mass ratio of 1: 2.
The preparation method of the quinolyl polyurethane based polyamide polycondensate comprises the following steps: uniformly mixing 2, 3-quinolinedicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the reaction kettle with inert gas, reacting for 5 hours at 145 ℃ under normal pressure, heating to 240 ℃, carrying out polycondensation reaction for 16 hours under 550Pa, cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the precipitated polymer for 6 times with ethanol, and drying in a vacuum drying oven at 95 ℃ to constant weight to obtain the quinolyl polyurethane based polyamide polycondensate; the molar ratio of the 2, 3-quinolinedicarboxylic acid to the amino-terminated polyurethane to the N, N-diisopropylethylamine to the 4-dimethylaminopyridine to the high-boiling-point solvent is 1:1:1.2:0.8: 20; the high boiling point solvent is N, N-dimethylformamide; the inert gas is argon.
The preparation method of the copolymer resin comprises the following steps: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 5 hours at 65 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 6 times, and finally drying in a vacuum drying oven at 95 ℃ to constant weight to obtain copolymer resin; the mass ratio of the N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, the 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, the styrene, the acrylonitrile, the vinyl trimethoxy silane, the azobisisobutyronitrile and the dimethyl sulfoxide is 5:1:2:1.2:1:0.1: 30.
The polyamide thermoplastic elastomer is polyether block amide Pebax 4033 SA 01; the butadiene rubber is butadiene rubber BR9000 crude rubber, and the number average molecular weight is 71000; the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
A preparation method of the high-tearing-resistance cutting-resistance flexing-resistance tire tread material comprises the following steps: sequentially mixing the components in parts by weight, uniformly mixing on an open mill, and then carrying out vulcanization processing to prepare the high-tearing-resistance cutting-resistance flexing-resistance tire tread material; the vulcanization processing is two-stage vulcanization, the first-stage vulcanization temperature is 190 ℃, and the vulcanization time is 10 minutes; the secondary vulcanization temperature is 160 ℃, and the vulcanization time is 4 hours.
Comparative example 1
The invention provides a high tear, cut and flex resistant tire tread material having a formulation and method of manufacture similar to example 1, except without the addition of a polyamide-based thermoplastic elastomer and N- (4-cyano-3-trifluoromethylphenyl) methacrylamide.
Comparative example 2
The present invention provides a high tear, cut and flex resistant tire tread material having a formulation and method of manufacture similar to example 1, except that no quinolinyl polyurethane based polyamide condensation polymer and no sulfonated poly (aryl ether ketone-benzimidazole) are added.
In order to further illustrate the beneficial technical effects of the high tearing cutting resistant and flexing resistant tire tread material prepared by each embodiment of the invention, the high tearing cutting resistant and flexing resistant tire tread material prepared by each embodiment is subjected to physical property tests comprising mechanical property, cutting resistant and flexing resistant property according to the current national standard or conventional method in China; wherein, the cutting resistance is tested by a dynamic cutting resistance instrument by continuously cutting for 20 minutes at the frequency of 120 times/minute, and the smaller the cutting weight loss rate is, the better the cutting resistance is; the smaller the 10 ten thousand flex crack rating, the better the flex resistance. The aging resistance is obtained by placing each product in hot air at 100 ℃ for 100 hours, and testing and calculating the retention rate of tensile strength, wherein the larger the value, the better the heat aging resistance.
TABLE 1
| Item | Tensile strength | Thermal aging resistance | Tear strength | Cutting weight loss ratio of 20 minutes | 10 million flex crack rating |
| Unit of | MPa | % | KN·m-1 | % | Stage |
| Example 1 | 28.2 | 98.8 | 96.9 | 6.2 | 2 |
| Example 2 | 28.9 | 99.3 | 97.3 | 5.9 | 2 |
| Example 3 | 29.4 | 99.6 | 98.0 | 5.3 | 1 |
| Example 4 | 30.2 | 99.7 | 98.8 | 4.9 | 1 |
| Example 5 | 30.6 | 99.9 | 99.3 | 4.1 | 1 |
| Comparative example 1 | 25.3 | 95.3 | 88.5 | 9.8 | 3 |
| Comparative example 2 | 24.7 | 93.8 | 86.6 | 10.6 | 5 |
As can be seen from Table 1, the high-tear, cut-resistant and flex-resistant tire tread material disclosed in the examples of the present invention has more excellent mechanical properties, tear resistance, thermal aging resistance, cut resistance and flex resistance than the comparative product, which is the result of the synergistic effect of the components. The addition of a polyamide-based thermoplastic elastomer, N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, a quinolylpolyurethane-based polyamide polycondensate and a sulfonated poly (aryletherketone-benzimidazole) are all beneficial for improving the above properties.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The high-tearing-resistance cutting-resistance flexing-resistance tire tread material is characterized by comprising the following components in parts by weight: 35-45 parts of hydrogenated nitrile rubber, 50-60 parts of butadiene rubber, 8-12 parts of polyamide thermoplastic elastomer, 5-12 parts of copolymer resin, 3-5 parts of quinolyl polyurethane based polyamide polycondensate, 1-3 parts of sulfonated poly (aryl ether ketone-benzimidazole), 1-3 parts of Luck H-518 tear-resistant auxiliary agent, 1-3 parts of anti-aging agent, 1-3 parts of stearic acid, 30-40 parts of filler, 1-2 parts of coupling agent, 2-4 parts of vulcanizing agent, 1-2 parts of accelerator, 1-2 parts of phosphorus pentoxide and 0.8-1.2 parts of polyphosphoric acid; the copolymer resin is prepared by free radical polymerization of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile and vinyl trimethoxy silane.
2. The high tear, cut and flex resistant tire tread material of claim 1, wherein the accelerator is accelerator NS; the vulcanizing agent is a mixture formed by mixing sulfur and dicumyl peroxide according to a mass ratio of (3-5) to 1; the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
3. The high-tear, cutting-resistant and flexing-resistant tire tread material as claimed in claim 1, wherein the filler is a mixture of lignin, nano boron fiber, fly ash and white carbon black in a mass ratio of 1 (1-3) to (3-5) to (4-6); the granularity of the filler is 800-1200 meshes; the average diameter of the nano boron fiber is 300-500nm, and the length-diameter ratio is (15-20): 1.
4. The high tear, cut and flex resistant tire tread material according to claim 1, wherein the antioxidant is a mixture of antioxidant RD and antioxidant 4020 mixed in a mass ratio of 1 (1-2).
5. The high tear, cut and flex resistant tire tread material of claim 1 wherein said quinolinyl polyurethane based polyamide condensation polymer is prepared by a process comprising the steps of: uniformly mixing 2, 3-quinoline dicarboxylic acid, amino-terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine and a high-boiling-point solvent to form a solution, adding the solution into a reaction kettle, replacing air in the kettle with inert gas, reacting at the temperature of 130 ℃ and 145 ℃ for 3-5 hours under normal pressure, heating to the temperature of 230 ℃ and 240 ℃, carrying out polycondensation reaction at the pressure of 350 ℃ and 550Pa for 10-16 hours, cooling to room temperature, adjusting to the normal pressure, precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and drying in a vacuum drying oven at the temperature of 85-95 ℃ to constant weight to obtain the quinolyl polyurethane based polyamide polycondensate.
6. The high tear, cut resistant and flex resistant tire tread material of claim 5 wherein the molar ratio of 2, 3-quinolinedicarboxylic acid, amino terminated polyurethane, N-diisopropylethylamine, 4-dimethylaminopyridine, high boiling point solvent is 1:1 (0.8-1.2) to (0.6-0.8) to (15-20); the high boiling point solvent is any one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone; the inert gas is any one of nitrogen, helium, neon and argon.
7. The high tear, cut and flex resistant tire tread material of claim 1, wherein the method of making the copolymer resin comprises the steps of: adding N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyl trimethoxy silane and azobisisobutyronitrile into dimethyl sulfoxide, stirring and reacting for 3-5 hours at 50-65 ℃ in a nitrogen atmosphere, then precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the copolymer resin.
8. The high tear, cut and flex resistant tire tread material of claim 7 wherein the mass ratio of N- (4-cyano-3-trifluoromethylphenyl) methacrylamide, 2-acrylic acid-hexahydro-4, 7-methylene-1H-indenyl ester, styrene, acrylonitrile, vinyltrimethoxysilane, azobisisobutyronitrile, dimethyl sulfoxide is (3-5):1 (1-2): 0.8-1.2):1 (0.06-0.1): 20-30.
9. The high tear cut resistant flex tire tread material of claim 1, wherein the polyamide based thermoplastic elastomer is polyether block amide Pebax ® 4033 SA 01; the butadiene rubber is butadiene rubber BR9000 crude rubber, and the number average molecular weight is 71000; the hydrogenated nitrile rubber is hydrogenated nitrile rubber HNBR 2157 crude rubber.
10. A method of making a high tear, cut and flex resistant tire tread material as in any one of claims 1-9, comprising the steps of: sequentially mixing the components in parts by weight, uniformly mixing on an open mill, and then carrying out vulcanization processing to prepare the high-tearing-property cutting-resistant flexing-resistant tire tread material; the vulcanization processing is two-stage vulcanization, the first-stage vulcanization temperature is 180-190 ℃, and the vulcanization time is 6-10 minutes; the secondary vulcanization temperature is 150-160 ℃, and the vulcanization time is 2-4 hours.
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| CN115181345A (en) * | 2022-08-05 | 2022-10-14 | 扬州东星橡胶股份有限公司 | Flame-retardant antistatic rubber material for conveyor belt covering layer and preparation method thereof |
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