CN117866301B - Shoulder pad rubber material for all-steel radial tire and preparation method thereof - Google Patents
Shoulder pad rubber material for all-steel radial tire and preparation method thereof Download PDFInfo
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 150
- 239000005060 rubber Substances 0.000 title claims abstract description 150
- 239000000463 material Substances 0.000 title claims abstract description 28
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 22
- 239000010959 steel Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000945 filler Substances 0.000 claims abstract description 83
- 238000002156 mixing Methods 0.000 claims abstract description 52
- 239000002131 composite material Substances 0.000 claims abstract description 49
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052582 BN Inorganic materials 0.000 claims abstract description 22
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 22
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 13
- -1 modifying Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 74
- 238000003756 stirring Methods 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 21
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 238000009210 therapy by ultrasound Methods 0.000 claims description 16
- 230000004048 modification Effects 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 14
- 239000006229 carbon black Substances 0.000 claims description 14
- 244000043261 Hevea brasiliensis Species 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- HDMXIELEUKTYFR-UHFFFAOYSA-N bis(2-ethylhexyl) butanedioate;sodium Chemical compound [Na].CCCCC(CC)COC(=O)CCC(=O)OCC(CC)CCCC HDMXIELEUKTYFR-UHFFFAOYSA-N 0.000 claims description 12
- 229920003052 natural elastomer Polymers 0.000 claims description 12
- 229920001194 natural rubber Polymers 0.000 claims description 12
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000021355 Stearic acid Nutrition 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 230000008878 coupling Effects 0.000 claims description 10
- 238000010168 coupling process Methods 0.000 claims description 10
- 238000005859 coupling reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 10
- 229940075507 glyceryl monostearate Drugs 0.000 claims description 10
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 10
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 10
- 239000012188 paraffin wax Substances 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 239000005011 phenolic resin Substances 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 239000008117 stearic acid Substances 0.000 claims description 10
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 239000011593 sulfur Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000004939 coking Methods 0.000 claims 1
- 230000020169 heat generation Effects 0.000 abstract description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 5
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000011231 conductive filler Substances 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011246 composite particle Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000003068 static effect Effects 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
-
- 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
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- 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)
Abstract
The invention provides a shoulder pad rubber material for an all-steel radial tire and a preparation method thereof, belonging to the technical field of shoulder pad rubber materials; the preparation method comprises the steps of preparing the heat conducting filler, preparing the composite filler, modifying, rubber pretreatment and mixing; adding polyvinyl alcohol and cetyltrimethylammonium bromide into nano alumina for ball milling treatment, controlling the ball milling rotation speed to be 306-320rpm, the ball material ratio to be 12-16:1, and the ball milling time to be 30-35min, then adding hexagonal boron nitride, reducing the rotation speed to be 250-262rpm, continuing ball milling for 15-20min, and obtaining the heat conducting filler after the ball milling treatment is finished; the shoulder pad rubber material prepared by the invention has good heat conducting property, low heat generation and good and stable mechanical property.
Description
Technical Field
The invention belongs to the technical field of shoulder pad rubber materials, and particularly relates to a shoulder pad rubber material for an all-steel radial tire and a preparation method thereof.
Background
With the improvement of the living standard of people, automobiles are becoming more and more popular and faster, an all-steel radial tire generates great heat under periodic load due to the viscoelastic property of rubber, the heat conduction property of the rubber is poor, the heat generation is difficult to discharge in time, a tire shoulder is the joint part of a tread and a tire body material and is the thickest part in the whole tire, and in the running process of the tire, the strain frequency of the tire shoulder part is high, the heat generation is high, the heat dissipation is difficult, the shoulder empty phenomenon of the tire shoulder part is caused, and the service performance of the tire is influenced;
Therefore, in order to solve the shoulder hole problem and improve the endurance performance of the tire, it is necessary to reduce the heat generating property of the shoulder pad and improve the heat conducting property.
In the prior art, the filler with heat-conducting property such as alumina is generally added, and only a larger amount of the filler such as alumina can exert better heat-conducting property, so that the heat-conducting property is improved to a certain extent, the temperature rise in the rubber material is reduced, the dynamic fatigue life of the cushion rubber is prolonged, but the dispersion property of the inorganic filler in the rubber matrix is poor due to the influence of factors such as particle size, interface and the like, so that the static mechanical property of the cushion rubber is obviously reduced;
in the prior art, the silane coupling agent is used for carrying out organic treatment on the white carbon black, and then the white carbon black after the organic treatment is filled into a rubber system, so that the dispersion performance of the white carbon black in the rubber system is good, a certain mechanical property can be improved, but the dynamic heat generation is large, and the white carbon black is not beneficial to use in dynamic occasions;
In addition, the applicant also finds that the shoulder pad rubber material for the all-steel radial tire prepared by the prior art is hardened in the northern cold environment, and the mechanical property of the pad rubber is seriously affected;
Therefore, the shoulder pad rubber material for the all-steel radial tire and the preparation method thereof are provided, the heat conducting performance is improved, the mechanical performance is still at a higher level, the heat generation is low, and the mechanical performance is stable, so that the technical problem to be solved in the prior art is urgent.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the shoulder pad rubber material for the all-steel radial tire and the preparation method thereof, which ensure higher mechanical property, low heat generation and stable mechanical property while improving the heat conducting property.
Aiming at the technical problems, the invention adopts the following technical scheme:
on one hand, the preparation method of the shoulder pad rubber material for the all-steel radial tire comprises the steps of preparing a heat conducting filler, preparing a composite filler, modifying, rubber pretreatment and mixing, and specifically comprises the following steps:
1. Preparation of thermally conductive filler
Adding polyvinyl alcohol and hexadecyl trimethyl ammonium bromide into nano alumina for ball milling treatment, controlling the ball milling rotation speed to be 306-320rpm, the ball material ratio to be 12-16:1, the ball milling time to be 30-35min, then adding hexagonal boron nitride, reducing the rotation speed to be 250-262rpm, continuing ball milling for 15-20min, and obtaining the heat conducting filler after the ball milling treatment is finished;
the particle size of the nano alumina is 154-165nm;
the particle size of the hexagonal boron nitride is 100-120nm;
The mass ratio of the nano aluminum oxide to the polyvinyl alcohol to the hexadecyl trimethyl ammonium bromide to the hexagonal boron nitride is 30-35:1.4-1.6:0.8-1.2:8-10.
2. Preparation of composite filler
Mixing a heat conducting filler with absolute ethyl alcohol, adding sodium bis (2-ethylhexyl) succinate sulfonate for ultrasonic treatment for 10-15min, wherein the ultrasonic frequency is 25-29kHz, the ultrasonic power is 284-295W, preparing heat conducting slurry after the ultrasonic treatment is finished, adding ammonia water and deionized water into the heat conducting slurry, heating to 40-44 ℃, uniformly stirring, slowly dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 0.08-0.12ml/min, stirring while dropwise adding until the reaction is completed, and centrifuging, washing and drying after the reaction is completed to prepare the composite filler;
The mass volume ratio of the heat conducting filler, the absolute ethyl alcohol and the sodium bis (2-ethylhexyl) succinate sulfonate is 0.8-1.2g:92-106ml:0.10-0.13g;
The volume ratio of the heat conduction slurry to the ammonia water to the deionized water to the tetraethoxysilane is 94-105:3.7-3.9:4.4-4.8:12.0-12.5;
3. Modification
Mixing a silane coupling agent kH550 and an ethanol solution, and then adding sodium lignin sulfonate to prepare a coupling solution; spraying the coupling liquid to the composite filler, after the spraying is finished, raising the temperature to 72-76 ℃, continuously stirring for 1.0-1.4h at the stirring speed of 118-132rpm, and drying after the stirring is finished to obtain the modified composite filler;
The mass concentration of the ethanol solution is 40-44%;
The mass ratio of the silane coupling agent kH550 to the ethanol solution to the sodium lignin sulfonate to the composite filler is 0.8-1.2:122-128:1.0-1.3:13-16.
4. Rubber pretreatment
Mixing natural rubber and styrene-butadiene rubber, heating to 56-59 ℃, adding absolute ethyl alcohol, polyvinylpyrrolidone and glyceryl monostearate, stirring for 13-18min at 178-188rpm, and drying after stirring to obtain pretreated rubber;
the mass ratio of the natural rubber to the styrene-butadiene rubber to the absolute ethyl alcohol to the polyvinylpyrrolidone to the glyceryl monostearate is 18-22:2.9-3.3:65-70:0.8-1.2:1.7-2.0.
5. Mixing
Adding the pretreated rubber into an internal mixer for banburying for 24-26s, wherein the rotating speed of the internal mixer is 50-54rpm, adding white carbon black, modified composite filler, zinc oxide, stearic acid, an antioxidant MB, phenolic resin and paraffin for mixing, wherein the mixing time is 21-25s, the temperature of the rubber reaches 125-127 ℃, lifting weight is 6-8s, the mixing of the rubber by a pressure weight is 42-44s, the temperature of the rubber is 145-150 ℃, the rubber is completely mixed, naturally cooling to room temperature, mixing in the internal mixer again, the rotating speed of the rotor is 48-52rpm, the pressure of the rubber is 0.64-0.68MPa, the mixing of the rubber by a pressure weight is 34-38s, the temperature of the rubber reaches 125-129 ℃, the lifting weight is 7-9s, the mixing of the rubber is continued for 30-35s, the temperature of the rubber reaches 148-152 ℃, after the mixing is completed, the rubber is naturally cooled to the room temperature, the sulfur, the accelerator NS and the antioxidant CTP are added, the rubber is placed in a mixing chamber of the internal mixer again, the rotating speed of the rotor is 25-27rpm, the pressure of the rubber is 0.52-0.55MPa, the pressure of the rubber is 0.64-0.68MPa, the pressure of the rubber is 20-9 s, the temperature of the rubber is continuously mixed for 20-102 s, and the rubber is continuously mixed after the rolling is completed;
The mass ratio of the pretreated rubber to the white carbon black to the modified composite filler to the zinc oxide to the stearic acid to the antioxidant MB to the phenolic resin to the paraffin to the sulfur to the accelerator NS to the scorch retarder CTP is 108-113:5.0-5.4:15.2-15.5:3.0-3.2:1.0-1.4:1.8-2.2:1.5-1.9:1.1-1.4:1.5-1.7:1.1-1.3:0.2-0.4.
On the other hand, the shoulder pad rubber material for the all-steel radial tire is prepared by adopting the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1. According to the invention, a specific method is adopted to prepare the heat-conducting filler, wherein polyvinyl alcohol and cetyl trimethyl ammonium bromide are compounded, and the heat-conducting filler is subjected to cooperative ball milling treatment, so that agglomeration of nano aluminum oxide and hexagonal boron nitride is avoided, and the heat-conducting filler has good dispersion performance and good lubricating performance; in the step of preparing the modified composite filler, under the synergistic effect of sodium bis (2-ethylhexyl) succinate sulfonate and ultrasonic treatment, the tetraethoxysilane is hydrolyzed to generate silicon dioxide, which is uniformly dispersed on the surface of the heat conducting filler, and the modified composite filler prepared by the further silane modification step has the advantages of enhancing the heat conducting property of the composite filler, reducing the friction among particles, reducing the heat generating property, uniformly dispersing in a rubber system, ensuring the particle integrity of the modified composite filler, enhancing the mechanical property and ensuring the stability of the mechanical property;
The rubber is pretreated by adopting a specific method, aggregation among rubber particles is weakened, compatibility with modified composite particles is enhanced, and further, uniform dispersibility of the cushion rubber sizing material is improved, and the heat conducting property is improved, meanwhile, higher mechanical property is ensured, heat generation is low, and mechanical property is stable;
2. the tensile strength of the shoulder pad rubber material for the all-steel radial tire is 33.4-34.7MPa, the elongation at break is 607-612%, and the 300% elongation is 17.6-18.3MPa (GB/T528);
The tearing strength of the shoulder pad rubber material for the all-steel radial tire is 143.7-146.2KN/m (GB/T529);
The tire shoulder pad rubber material for the all-steel radial tire prepared by the invention has the compression fatigue temperature rise of 6.7-7.0 ℃ and the compression permanent deformation of 2.5-2.8% under the conditions of the experimental temperature of 55 ℃, the load of 1.5MPa and the compression frequency of 30Hz (GB/T1687-1993);
the heat conductivity coefficient of the shoulder pad rubber material for the all-steel radial tire is 0.392-0.397W/mK (GB/T11205-2009);
3. The shoulder pad rubber material for the all-steel radial tire is frozen at the temperature of minus 40 ℃ for 10 days, the tensile strength is 32.8-34.3MPa, the elongation at break is 588-597%, the 300% elongation is 17.2-18.0MPa, and the tearing strength is 139.4-142.4KN/m.
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, specific embodiments of the present invention will be described.
Example 1 preparation method of shoulder pad rubber for all-Steel radial tire
1. Preparation of thermally conductive filler
Adding polyvinyl alcohol and hexadecyl trimethyl ammonium bromide into nano alumina for ball milling treatment, controlling the ball milling rotation speed to be 314rpm, the ball-material ratio to be 14:1, the ball milling time to be 32min, then adding hexagonal boron nitride, reducing the rotation speed to 256rpm, continuing ball milling for 17min, and obtaining the heat conducting filler after the ball milling treatment is finished;
the particle size of the nano alumina is 160nm;
the particle size of the hexagonal boron nitride is 110nm;
the mass ratio of the nano aluminum oxide to the polyvinyl alcohol to the hexadecyl trimethyl ammonium bromide to the hexagonal boron nitride is 32:1.5:1.0:9.
2. Preparation of composite filler
Mixing a heat conducting filler with absolute ethyl alcohol, adding sodium bis (2-ethylhexyl) succinate sulfonate for ultrasonic treatment, wherein the ultrasonic treatment time is 12min, the ultrasonic frequency is 27kHz, the ultrasonic power is 290W, preparing heat conducting slurry after ultrasonic treatment is finished, adding ammonia water and deionized water into the heat conducting slurry, heating to 42 ℃, uniformly stirring, slowly dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 0.1ml/min, stirring while dropwise adding until the reaction is finished, and centrifuging, washing and drying after the reaction is finished to prepare a composite filler;
The mass volume ratio of the heat conducting filler, the absolute ethyl alcohol and the sodium bis (2-ethylhexyl) succinate sulfonate is 1g to 100ml to 0.12g;
the volume ratio of the heat conduction slurry to the ammonia water to the deionized water to the tetraethoxysilane is 100:3.8:4.6:12.3;
3. Modification
Mixing a silane coupling agent kH550 and an ethanol solution, and then adding sodium lignin sulfonate to prepare a coupling solution; spraying the coupling liquid to the composite filler, after the spraying is finished, raising the temperature to 74 ℃, continuously stirring for 1.2 hours, wherein the stirring speed is 125rpm, and drying after the stirring is finished to obtain the modified composite filler;
The mass concentration of the ethanol solution is 42%;
the mass ratio of the silane coupling agent kH550 to the ethanol solution to the sodium lignin sulfonate to the composite filler is 1.0:125:1.2:14.
4. Rubber pretreatment
Mixing natural rubber and styrene-butadiene rubber, heating to 57 ℃, adding absolute ethyl alcohol polyvinylpyrrolidone and glyceryl monostearate, stirring for 15min at 184rpm, and drying after stirring to obtain pretreated rubber;
The mass ratio of the natural rubber to the styrene-butadiene rubber to the absolute ethyl alcohol to the polyvinylpyrrolidone to the glyceryl monostearate is 20:3.1:68:1.0:1.8.
5. Mixing
Adding the pretreated rubber into an internal mixer for banburying for 25 seconds, wherein the rotating speed of the internal mixer is 52rpm, adding white carbon black, modified composite filler, zinc oxide, stearic acid, an anti-aging agent MB, phenolic resin and paraffin for mixing, wherein the mixing time is 23 seconds, the temperature of the rubber reaches 126 ℃, the pressure of the rubber is raised for 7 seconds, the pressure of the rubber is raised for 43 seconds, the temperature of the rubber is 148 seconds, the rubber is discharged after mixing, naturally cooling to room temperature, placing the rubber into the internal mixer again for mixing, the rotating speed of the rotor is 50rpm, the pressure of the rubber is 0.66MPa, the temperature of the rubber is raised for 36 seconds, the temperature of the rubber reaches 127 ℃, the pressure of the rubber is raised for 8 seconds, the pressure of the rubber is continued for 32 seconds, the temperature of the rubber reaches 150 ℃, after mixing is completed, adding sulfur, an accelerator NS and an anti-scorching agent CTP into the internal mixer for mixing, the rotor is rotated for 26rpm, the pressure of the rubber is 0.54MPa, the pressure of the rubber is raised for 25 seconds, the rubber is continued to be pressed for 22 seconds, the temperature of the rubber is 103 ℃, and the rubber is discharged after the rubber is mixed into a tire shoulder to obtain a rubber pad;
The mass ratio of the pretreated rubber to the white carbon black to the modified composite filler to the zinc oxide to the stearic acid to the antioxidant MB to the phenolic resin to the paraffin to the sulfur to the accelerator NS to the scorch retarder CTP is 110:5.2:15.3:3.1:1.2:2.0:1.8:1.3:1.6:1.2:0.3.
Example 2 preparation method of shoulder pad rubber for all-Steel radial tire
1. Preparation of thermally conductive filler
Adding polyvinyl alcohol and hexadecyl trimethyl ammonium bromide into nano alumina for ball milling treatment, controlling the ball milling rotation speed to be 306rpm, the ball-material ratio to be 12:1, the ball milling time to be 30min, then adding hexagonal boron nitride, reducing the rotation speed to 250rpm, continuing ball milling for 15min, and obtaining the heat conducting filler after the ball milling treatment is finished;
the particle size of the nano aluminum oxide is 154nm;
The particle size of the hexagonal boron nitride is 100nm;
The mass ratio of the nano aluminum oxide to the polyvinyl alcohol to the hexadecyl trimethyl ammonium bromide to the hexagonal boron nitride is 30:1.4:0.8:8.
2. Preparation of composite filler
Mixing a heat conducting filler with absolute ethyl alcohol, adding sodium bis (2-ethylhexyl) succinate sulfonate for ultrasonic treatment, wherein the ultrasonic treatment time is 10min, the ultrasonic frequency is 25kHz, the ultrasonic power is 284W, preparing heat conducting slurry after the ultrasonic treatment is finished, adding ammonia water and deionized water into the heat conducting slurry, heating to 40 ℃, uniformly stirring, slowly dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 0.08ml/min, stirring while dropwise adding until the reaction is finished, and centrifuging, washing and drying after the reaction is finished to prepare a composite filler;
the mass volume ratio of the heat conducting filler, the absolute ethyl alcohol and the sodium bis (2-ethylhexyl) succinate sulfonate is 0.8g:92ml:0.10g;
the volume ratio of the heat conduction slurry to the ammonia water to the deionized water to the tetraethoxysilane is 94:3.7:4.4:12.0;
3. Modification
Mixing a silane coupling agent kH550 and an ethanol solution, and then adding sodium lignin sulfonate to prepare a coupling solution; spraying the coupling liquid on the composite filler, after the spraying is finished, raising the temperature to 72 ℃, continuously stirring for 1.0h, wherein the stirring speed is 118rpm, and drying after the stirring is finished to obtain the modified composite filler;
the mass concentration of the ethanol solution is 40%;
the mass ratio of the silane coupling agent kH550 to the ethanol solution to the sodium lignin sulfonate to the composite filler is 0.8:122:1.0:13.
4. Rubber pretreatment
Mixing natural rubber and styrene-butadiene rubber, heating to 56 ℃, adding absolute ethyl alcohol, polyvinylpyrrolidone and glyceryl monostearate, stirring for 13min at 178rpm, and drying after stirring to obtain pretreated rubber;
The mass ratio of the natural rubber to the styrene-butadiene rubber to the absolute ethyl alcohol to the polyvinylpyrrolidone to the glyceryl monostearate is 18:2.9:65:0.8:1.7.
5. Mixing
Adding the pretreated rubber into an internal mixer for banburying for 24 seconds, wherein the rotating speed of the internal mixer is 50rpm, adding white carbon black, modified composite filler, zinc oxide, stearic acid, an anti-aging agent MB, phenolic resin and paraffin for mixing, wherein the mixing time is 21 seconds, the temperature of the rubber reaches 125 ℃, the pressure of the rubber is raised for 42 seconds, the temperature of the rubber is 145 ℃, the rubber is discharged after mixing, the rubber is naturally cooled to room temperature, the rubber is placed in the internal mixer again for mixing, the rotating speed of the rotor is 48rpm, the pressure of the rubber is 0.64MPa, the temperature of the rubber reaches 125 ℃, the pressure of the rubber is raised for 7 seconds, the pressure of the rubber is continued to be mixed for 30 seconds, the temperature of the rubber reaches 148 ℃, after the mixing is completed, the rubber is naturally cooled to room temperature, sulfur, an accelerator NS and an anti-scorching agent CTP are added, the rubber is placed in a mixing chamber again, the rotating speed of the rotor is 25rpm, the pressure of the rubber is 0.52MPa, the pressure of the rubber is raised for 24 seconds, the rubber is continued to be pressed for 20 seconds, the temperature of the rubber is 102 ℃, and the rubber is discharged after the rubber is mixed at the temperature of the tire shoulder, and the rubber is discharged;
The mass ratio of the pretreated rubber to the white carbon black to the modified composite filler to the zinc oxide to the stearic acid to the antioxidant MB to the phenolic resin to the paraffin to the sulfur to the accelerator NS to the scorch retarder CTP is 108:5.0:15.2:3.0:1.0:1.8:1.5:1.1:1.5:1.1:0.2.
Example 3 preparation method of shoulder pad rubber for all-Steel radial tire
1. Preparation of thermally conductive filler
Adding polyvinyl alcohol and hexadecyl trimethyl ammonium bromide into nano alumina for ball milling treatment, controlling the ball milling rotation speed to be 320rpm, the ball-material ratio to be 16:1, the ball milling time to be 35min, then adding hexagonal boron nitride, reducing the rotation speed to 262rpm, continuing ball milling for 20min, and obtaining the heat conducting filler after the ball milling treatment is finished;
the particle size of the nano alumina is 165nm;
the particle size of the hexagonal boron nitride is 120nm;
The mass ratio of the nano aluminum oxide to the polyvinyl alcohol to the hexadecyl trimethyl ammonium bromide to the hexagonal boron nitride is 35:1.6:1.2:10.
2. Preparation of composite filler
Mixing a heat conducting filler with absolute ethyl alcohol, adding sodium bis (2-ethylhexyl) succinate sulfonate for ultrasonic treatment, wherein the ultrasonic treatment time is 15min, the ultrasonic frequency is 29kHz, the ultrasonic power is 295W, a heat conducting slurry is prepared after the ultrasonic treatment is finished, ammonia water and deionized water are added into the heat conducting slurry, the temperature is raised to 44 ℃, after uniform stirring, ethyl orthosilicate is slowly added dropwise, the dropwise acceleration is controlled to be 0.12ml/min, stirring is carried out while dropwise adding until the reaction is completed, and after the reaction is completed, the composite filler is prepared by centrifugation, washing and drying;
the mass volume ratio of the heat conducting filler, the absolute ethyl alcohol and the sodium bis (2-ethylhexyl) succinate sulfonate is 1.2g:106ml:0.13g;
the volume ratio of the heat conduction slurry to the ammonia water to the deionized water to the tetraethoxysilane is 105:3.9:4.8:12.5;
3. Modification
Mixing a silane coupling agent kH550 and an ethanol solution, and then adding sodium lignin sulfonate to prepare a coupling solution; spraying the coupling liquid to the composite filler, after the spraying is finished, raising the temperature to 76 ℃, continuously stirring for 1.4 hours, wherein the stirring speed is 132rpm, and drying after the stirring is finished to obtain the modified composite filler;
the mass concentration of the ethanol solution is 44%;
The mass ratio of the silane coupling agent kH550 to the ethanol solution to the sodium lignin sulfonate to the composite filler is 1.2:128:1.3:16.
4. Rubber pretreatment
Mixing natural rubber and styrene-butadiene rubber, heating to 59 ℃, adding absolute ethyl alcohol, polyvinylpyrrolidone and glyceryl monostearate, stirring for 18min at 188rpm, and drying after stirring to obtain pretreated rubber;
The mass ratio of the natural rubber to the styrene-butadiene rubber to the absolute ethyl alcohol to the polyvinylpyrrolidone to the glyceryl monostearate is 22:3.3:70:1.2:2.0.
5. Mixing
Adding the pretreated rubber into an internal mixer for banburying for 26s, wherein the rotating speed of the internal mixer is 54rpm, adding white carbon black, modified composite filler, zinc oxide, stearic acid, an anti-aging agent MB, phenolic resin and paraffin for mixing, wherein the mixing time is 25s, the temperature of the rubber reaches 127 ℃, the pressure of the rubber is 8s, the pressure of the rubber is 44s, the temperature of the rubber is 150 ℃, the rubber is discharged after mixing, the rubber is naturally cooled to room temperature, the rubber is placed in the internal mixer again for mixing, the rotating speed of the rotor is 52rpm, the pressure of the rubber is 0.68MPa, the temperature of the rubber reaches 129 ℃, the pressure of the rubber is 9s, the pressure of the rubber is continuously mixed for 35s, the temperature of the rubber reaches 152 ℃, after mixing is completed, the rubber is naturally cooled to room temperature, sulfur, an accelerator NS and an anti-scorching agent CTP are added, the rubber is placed in a mixing room of the internal mixer again, the rotating speed of the rotor is 27rpm, the pressure of the rubber is 0.55MPa, the pressure of the rubber is 26s, the rubber is continuously pressed for mixing for 24s, the rubber is 104 ℃, and the rubber is discharged after the rubber is mixed at the temperature of the tire shoulder;
The mass ratio of the pretreated rubber to the white carbon black to the modified composite filler to the zinc oxide to the stearic acid to the antioxidant MB to the phenolic resin to the paraffin to the sulfur to the accelerator NS to the scorch retarder CTP is 113:5.4:15.5:3.2:1.4:2.2:1.9:1.4:1.7:1.3:0.4.
Comparative example 1
Based on example 1, the modification was that,
① In the step of preparing the heat conducting filler, only nano alumina and hexagonal boron nitride are uniformly mixed to prepare the heat conducting filler; the particle size of the nano alumina is 160nm; the particle size of the hexagonal boron nitride is 110nm; the mass ratio of the nano aluminum oxide to the hexagonal boron nitride is 32:9;
② The modification step comprises the steps of mixing a silane coupling agent kH550 and an ethanol solution, then adding a composite filler, raising the temperature to 74 ℃, continuously stirring for 1.2 hours, wherein the stirring speed is 125rpm, and drying to obtain a modified composite filler;
The mass concentration of the ethanol solution is 42%;
the mass ratio of the silane coupling agent kH550 to the ethanol solution to the composite filler is 1.0:125:14;
The rest of the operations are the same.
Comparative example 2
On the basis of the embodiment 1, the modification is that the rubber pretreatment step is omitted, natural rubber and styrene-butadiene rubber which are not subjected to any treatment are directly adopted, the mass ratio of the natural rubber to the styrene-butadiene rubber is 20:3.1, and the rest operations are the same.
Test examples
The products obtained in examples 1-3 and comparative examples 1-2 were placed on a press vulcanizer and vulcanized for 30min at 151℃to obtain test specimens, and the performance test was conducted as follows:
mechanical property detection
Tensile properties were measured according to GB/T528; tear properties were measured according to GB/T529;
Heat buildup test
Compression heat generation is detected according to GB/T1687-1993, the experimental temperature is 55 ℃, the load is 1.5MPa, and the compression frequency is 30Hz;
thermal conductivity testing
The heat conductivity was measured according to GB/T11205-2009.
(1) Basic Properties
(2) Low temperature resistance
The test specimens were frozen at-40℃for 10d and again subjected to performance testing, with the following test results:
according to the invention, a specific method is adopted to prepare the heat-conducting filler, wherein polyvinyl alcohol and cetyl trimethyl ammonium bromide are compounded, and the heat-conducting filler is subjected to cooperative ball milling treatment, so that agglomeration of nano aluminum oxide and hexagonal boron nitride is avoided, and the heat-conducting filler has good dispersion performance and good lubricating performance; in the step of preparing the modified composite filler, under the synergistic effect of sodium bis (2-ethylhexyl) succinate sulfonate and ultrasonic treatment, the tetraethoxysilane is hydrolyzed to generate silicon dioxide, which is uniformly dispersed on the surface of the heat conducting filler, and the modified composite filler prepared by the further silane modification step has the advantages of enhancing the heat conducting property of the composite filler, reducing the friction among particles, reducing the heat generating property, uniformly dispersing in a rubber system, ensuring the particle integrity of the modified composite filler, enhancing the mechanical property and ensuring the stability of the mechanical property;
The invention adopts a specific method to pretreat the rubber, weakens aggregation among rubber particles, enhances compatibility with modified composite particles, further improves uniform dispersibility of the cushion rubber sizing material, further realizes that the heat conducting property is improved, and simultaneously ensures higher mechanical property, low heat generation and stable mechanical property.
According to the experiment of comparative example 1, in comparative example 1, nano aluminum oxide and hexagonal boron nitride are uniformly mixed to prepare a heat-conducting filler, then only a silane coupling agent is added in a modification step, and drying is carried out, wherein the product prepared in comparative example 1 has poor mechanical properties, poor heat conductivity and high heat generation; the heat-conducting filler prepared in comparative example 1 has poor dispersion performance, agglomeration phenomenon among particles is shown, coupling effect is influenced in the modification process, the integrity of the particles cannot be ensured, so that the compatibility with a rubber system is poor, on one hand, the mechanical property and the mechanical stability are influenced, and on the other hand, the heat generation is high and the heat conduction effect is poor.
According to the experiment of comparative example 2, the pretreatment step of rubber is omitted, so that the modified composite filler cannot be uniformly dispersed in a rubber system, and further the mechanical property and mechanical stability are reduced, and the heat generation is high and the heat conduction effect is poor.
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. 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 (4)
1. The preparation method of the shoulder wedge rubber material for the all-steel radial tire is characterized by comprising the steps of preparing a heat conducting filler, preparing a composite filler, modifying, rubber pretreatment and mixing;
Adding polyvinyl alcohol and cetyltrimethylammonium bromide into nano alumina for ball milling treatment, controlling the ball milling rotation speed to be 306-320rpm, the ball material ratio to be 12-16:1, and the ball milling time to be 30-35min, then adding hexagonal boron nitride, reducing the rotation speed to be 250-262rpm, continuing ball milling for 15-20min, and obtaining the heat conducting filler after the ball milling treatment is finished;
The mass ratio of the nano aluminum oxide to the polyvinyl alcohol to the hexadecyl trimethyl ammonium bromide to the hexagonal boron nitride is 30-35:1.4-1.6:0.8-1.2:8-10;
Mixing a heat conducting filler with absolute ethyl alcohol, adding sodium bis (2-ethylhexyl) succinate sulfonate for ultrasonic treatment, wherein the ultrasonic treatment time is 10-15min, the ultrasonic frequency is 25-29kHz, the ultrasonic power is 284-295W, preparing a heat conducting slurry after the ultrasonic treatment is finished, adding ammonia water and deionized water into the heat conducting slurry, heating to 40-44 ℃, uniformly stirring, slowly dropwise adding tetraethoxysilane, controlling the dropwise adding speed to be 0.08-0.12ml/min, stirring until the reaction is completed, and centrifuging, washing and drying to prepare the composite filler after the reaction is completed;
The mass volume ratio of the heat conducting filler, the absolute ethyl alcohol and the sodium bis (2-ethylhexyl) succinate sulfonate is 0.8-1.2g:92-106ml:0.10-0.13g;
The volume ratio of the heat conduction slurry to the ammonia water to the deionized water to the tetraethoxysilane is 94-105:3.7-3.9:4.4-4.8:12.0-12.5;
The modification step is that a silane coupling agent kH550 and an ethanol solution are mixed, and then sodium lignin sulfonate is added to prepare a coupling solution; spraying the coupling liquid to the composite filler, after the spraying is finished, raising the temperature to 72-76 ℃, continuously stirring for 1.0-1.4h at the stirring speed of 118-132rpm, and drying after the stirring is finished to obtain the modified composite filler;
The mass ratio of the silane coupling agent kH550 to the ethanol solution to the sodium lignin sulfonate to the composite filler is 0.8-1.2:122-128:1.0-1.3:13-16;
Mixing natural rubber and styrene-butadiene rubber, raising the temperature to 56-59 ℃, adding absolute ethyl alcohol, polyvinylpyrrolidone and glyceryl monostearate, stirring for 13-18min at 178-188rpm, and drying after stirring to obtain pretreated rubber;
The mass ratio of the natural rubber to the styrene-butadiene rubber to the absolute ethyl alcohol to the polyvinylpyrrolidone to the glyceryl monostearate is 18-22:2.9-3.3:65-70:0.8-1.2:1.7-2.0;
The method comprises the steps of adding pretreated rubber into an internal mixer for banburying for 24-26s, wherein the rotating speed of the internal mixer is 50-54rpm, adding white carbon black, modified composite filler, zinc oxide, stearic acid, an antioxidant MB, phenolic resin and paraffin for mixing for 21-25s, carrying out rubber lifting for 6-8s at the temperature of 125-127 ℃, carrying out rubber lifting for 42-44s at the temperature of 145-150 ℃, naturally cooling to room temperature, carrying out mixing in the internal mixer again at the rotating speed of 48-52rpm, the pressure of 0.64-0.68MPa, the pressure of 34-38s at the temperature of 125-129 ℃, carrying out rubber lifting for 7-9s, continuing to carry out rubber lifting for 30-35s at the temperature of 148-152 ℃, carrying out rubber lifting after the temperature of the rubber lifting, adding sulfur, an accelerator NS and an anti-coking agent CTP again into a mixing chamber of the internal mixer, carrying out rubber lifting for 24-9 s at the rotating speed of 25-27rpm, carrying out rubber lifting for 0.64-0.68MPa, carrying out rubber lifting for 24-104 s at the temperature of the rubber lifting for 20-104 s, and carrying out rubber lifting for 2-104 s;
The mass ratio of the pretreated rubber to the white carbon black to the modified composite filler to the zinc oxide to the stearic acid to the antioxidant MB to the phenolic resin to the paraffin to the sulfur to the accelerator NS to the scorch retarder CTP is 108-113:5.0-5.4:15.2-15.5:3.0-3.2:1.0-1.4:1.8-2.2:1.5-1.9:1.1-1.4:1.5-1.7:1.1-1.3:0.2-0.4.
2. The method for producing a shoulder wedge compound for all-steel radial tires according to claim 1, characterized in that,
In the step of preparing the heat conducting filler, the particle size of the nano aluminum oxide is 154-165nm;
the particle size of the hexagonal boron nitride is 100-120nm.
3. The method for producing a shoulder wedge compound for all-steel radial tires according to claim 1, characterized in that,
In the modification step, the mass concentration of the ethanol solution is 40-44%.
4. A shoulder wedge compound for all-steel radial tires produced by the production method according to any one of claims 1 to 3.
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