CN117887152A - Tire belt rubber composition and preparation method thereof - Google Patents
Tire belt rubber composition and preparation method thereof Download PDFInfo
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- CN117887152A CN117887152A CN202410288920.1A CN202410288920A CN117887152A CN 117887152 A CN117887152 A CN 117887152A CN 202410288920 A CN202410288920 A CN 202410288920A CN 117887152 A CN117887152 A CN 117887152A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 102
- 239000000203 mixture Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 109
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000006229 carbon black Substances 0.000 claims abstract description 62
- 238000002156 mixing Methods 0.000 claims abstract description 58
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims description 25
- 239000011268 mixed slurry Substances 0.000 claims description 25
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 239000000853 adhesive Substances 0.000 claims description 18
- 230000001070 adhesive effect Effects 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 13
- 239000010456 wollastonite Substances 0.000 claims description 13
- 229910052882 wollastonite Inorganic materials 0.000 claims description 13
- 235000021355 Stearic acid Nutrition 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 12
- 239000008117 stearic acid Substances 0.000 claims description 12
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 claims description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 claims description 11
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 11
- RZRNAYUHWVFMIP-HXUWFJFHSA-N glycerol monolinoleate Natural products CCCCCCCCC=CCCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-HXUWFJFHSA-N 0.000 claims description 11
- CMAUJSNXENPPOF-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)-n-cyclohexylcyclohexanamine Chemical compound C1CCCCC1N(C1CCCCC1)SC1=NC2=CC=CC=C2S1 CMAUJSNXENPPOF-UHFFFAOYSA-N 0.000 claims description 11
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 11
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 11
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 11
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 11
- 239000011593 sulfur Substances 0.000 claims description 11
- 229910052717 sulfur Inorganic materials 0.000 claims description 11
- 239000011787 zinc oxide Substances 0.000 claims description 11
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 10
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 10
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 10
- 239000000701 coagulant Substances 0.000 claims description 10
- 229940073507 cocamidopropyl betaine Drugs 0.000 claims description 10
- 239000002480 mineral oil Substances 0.000 claims description 10
- 235000010446 mineral oil Nutrition 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinyl group Chemical group C1(O)=CC(O)=CC=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 8
- 239000010433 feldspar Substances 0.000 claims description 8
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 230000001965 increasing effect Effects 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000003712 anti-aging effect Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 230000020169 heat generation Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 9
- 230000002776 aggregation Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000015271 coagulation Effects 0.000 description 4
- 238000005345 coagulation Methods 0.000 description 4
- 244000043261 Hevea brasiliensis Species 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920003052 natural elastomer Polymers 0.000 description 3
- 229920001194 natural rubber Polymers 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- -1 thiocarboxylic acid ester Chemical class 0.000 description 1
- 239000003190 viscoelastic substance Substances 0.000 description 1
Classifications
-
- 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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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a tire belt rubber composition and a preparation method thereof, belonging to the technical field of rubber compositions; the preparation method comprises the steps of preparing dispersible white carbon black, preparing powder rubber mixture and mixing; the preparation of the dispersible white carbon black comprises the steps of placing the white carbon black into impregnating solution, stirring uniformly, carrying out primary standing for 6-10min under the pressure of 2.0-2.2MPa, carrying out secondary standing after the primary standing is finished for 5-7min under the pressure of 2.6-2.8MPa, and drying after the standing is finished to obtain the dispersible white carbon black; the rubber composition prepared by the invention has low heat generation, strong and stable mechanical property and excellent heat conduction property.
Description
Technical Field
The invention belongs to the technical field of rubber compositions, and particularly relates to a tire belt rubber composition and a preparation method thereof.
Background
The belt layer is also called a supporting layer, a hard buffer layer and a stabilizing layer, and is a material layer which is used for hooping the carcass in the circumferential direction of the central line of the tread under the tread base parts of the radial tire and the belt bias tire; the belt ply mainly plays a role in hooping the tire body and also plays a role in buffering and impacting; it is also the main stress part for radial tyre, so it should use high strength, high modulus and small angle arranged cord as its reinforcing material, and at the same time it is covered with high stretching, high hardness glue.
The rubber is a viscoelastic material, hysteresis loss is generated in the rubber material, mechanical energy in the tire deformation process is converted into heat energy, more heat is generated at the belt layer part, and the long-term service performance of the rubber material is further affected;
on the one hand, the kind of carbon black may be changed to lower the heat buildup, but it has a problem of poor mechanical properties;
on the other hand, the patent with application number 2008100027653 discloses a belt steel cord adhesive, and specifically discloses that thiocarboxylic acid ester silane coupling agent and white carbon black are added in the formula, so that the dispersity of the white carbon black can be improved, and the hysteresis loss of the adhesive can be reduced; but still suffer from poor mechanical properties;
in addition, the mechanical properties of the conventional belt rubber composition are greatly reduced after long-time ultraviolet irradiation, the service performance is seriously influenced, and the service life is further shortened.
Therefore, the tire belt rubber composition and the preparation method thereof are provided, the hysteresis loss of rubber materials is reduced, the mechanical properties are improved, and the ultraviolet irradiation resistance is enhanced, 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 a tire belt rubber composition and a preparation method thereof, which can reduce hysteresis loss of rubber materials, improve mechanical properties and enhance ultraviolet irradiation resistance.
Aiming at the technical problems, the invention adopts the following technical scheme:
the preparation method of the tire belt rubber composition comprises the steps of preparing dispersible white carbon black, preparing powder rubber mixture and mixing, and specifically comprises the following steps:
1. preparation of dispersible white carbon black
Placing the white carbon black into the impregnating solution, stirring uniformly, carrying out primary standing for 6-10min under the pressure of 2.0-2.2MPa, carrying out secondary standing after the primary standing is finished, carrying out standing for 5-7min under the pressure of 2.6-2.8MPa, and drying after the standing is finished to obtain the dispersible white carbon black;
the particle size of the white carbon black is 130-150nm;
the mass ratio of the white carbon black to the impregnating solution is 1:3.5-3.9;
the impregnating solution consists of deionized water, fatty alcohol-polyoxyethylene ether and sodium dodecyl benzene sulfonate, wherein the mass ratio of the deionized water to the fatty alcohol-polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 76-80:2.3-2.5:2.8-3.2.
2. Preparation of powder rubber mixtures
(1) Preparation of functional powder
Calcining aluminum nitride powder at 246-254 ℃ for 1.0-1.4h, calcining wollastonite powder at 315-325 ℃ for 0.8-1.2h, cooling to room temperature respectively after calcining, and mixing to obtain a primary mixed material; adding polyethylene glycol 400 into the primary mixed material, performing ball milling treatment for 42-48min at a ball milling rotating speed of 204-213rpm, and obtaining functional powder after ball milling;
the grain diameter of the aluminum nitride powder is 95-105nm;
the particle size of the calcium feldspar powder is 115-140nm, and the mass content of the silicon dioxide is 65.4-66.0%;
the mass ratio of the aluminum nitride powder to the wollastonite powder is 1.4-1.6:1.1-1.3;
the mass ratio of the primary mixed material to the polyethylene glycol 400 is 93-97:1.7-1.9;
(2) Preparation of Mixed slurry
Mixing functional powder with deionized water, stirring uniformly, adding KH570 and cocamidopropyl betaine, stirring at 74-80deg.C for 2.2-2.4 hr, and cooling to room temperature to obtain suspension; adding natural latex with 25% of solid content and glycerol monooleate into the suspension, homogenizing under 6.0-6.4MPa for 4-6min to obtain mixed slurry;
the mass ratio of the functional powder to the deionized water to the KH570 to the cocamidopropyl betaine is 12-14:122-128:1.0-1.2:0.44-0.50;
the mass ratio of the natural latex to the glycerol monooleate to the suspension is 258-262:2.1-2.3:320-325;
(3) Coagulation
Adding CaCl with mass concentration of 2% into the mixed slurry 2 Solidifying the coagulant, and then washing and drying to obtain a powder rubber mixture;
the mass ratio of the mixed slurry to the coagulant is 100:0.21-0.25.
3. Mixing
Adding the powder rubber mixture, zinc oxide, an auxiliary agent and an anti-aging agent RD into an internal mixer for mixing, controlling the temperature to be 79-81 ℃, the pressure to be 13-15MPa, the rotor rotating speed to be 52-56rpm, and the mixing time to be 29-31s, so as to prepare a section of mixed rubber; adding the first-stage mixed rubber, the dispersible white carbon black, the carbon black and the adhesive into an internal mixer for mixing, controlling the temperature to be 158-162 ℃, the pressure to be 12-14MPa, the rotating speed of a rotor to be 48-52rpm, and the mixing time to be 44-46s to prepare a second-stage mixed rubber; adding the second-stage mixed rubber, sulfur and accelerator DZ into an internal mixer, mixing for 91-93s at the rotor rotating speed of 22-24rpm, and discharging rubber to prepare a tire belt rubber composition;
the mass ratio of the powder rubber mixture to the zinc oxide to the auxiliary agent to the antioxidant RD to the dispersible white carbon black to the adhesive to the sulfur to the accelerator DZ is 156-160:2.4-2.6:1.4-1.6:2.8-3.2:7.1-7.7:12-14:2.8-3.0:1.8-2.2:2.1-2.5;
the adhesive is resorcinol;
the preparation method of the auxiliary agent comprises the steps of mixing stearic acid and carboxymethyl cellulose, increasing the temperature to 40-44 ℃, stirring for 12-14min at 130-134rpm, then adding mineral oil, and continuously stirring for 6-8min to obtain the auxiliary agent;
the mass ratio of the stearic acid to the carboxymethyl cellulose to the mineral oil is 3.6-3.8:1.8-2.2:1.0-1.2.
A tire belt rubber composition is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of the tire belt rubber composition has the advantages that the dispersible white carbon black prepared by adopting a specific method has good dispersibility and high surface activity; the functional powder is prepared by adopting a specific method, so that the agglomeration phenomenon is avoided, the functional powder is treated by a silane coupling agent and then is mixed with rubber by a wet method, the compatibility and the dispersibility of the functional powder in the rubber are improved, the damage to rubber molecules is avoided, the functional powder is combined with specific auxiliary agents and other technical means, the mixing uniformity of other components is improved, the structural stability of the inside of the rubber composition is enhanced, and the purposes of improving the heat conductivity, reducing hysteresis loss, reducing heat generation, and enhancing the mechanical property and mechanical stability are realized;
2. the tire belt rubber composition prepared by the invention adopts dynamic mechanical analysis to test a sample, wherein the test mode is a stretching mode, the dynamic strain is 0.25%, the static strain is 1%, and the test tan delta is 0.035-0.038 at 60 ℃;
the heat conductivity coefficient is 0.391-0.395W/mK according to GB/T11205-2009;
tested according to GB/T528-2009, the tensile strength is 32.9-33.8MPa, the elongation at break is 538-547%, the 100% elongation is 8.5-8.9MPa, and the 300% elongation is 20.7-21.6%;
the tearing strength is 133.6-135.7kN/m according to GB/T529-2008;
3. the tire belt rubber composition prepared by the invention is irradiated for 192 hours by a 1600W high-pressure mercury lamp, the ultraviolet wavelength is 390nm, the tensile strength is 31.7-32.9MPa, the elongation at break is 513-527%, the 100% elongation is 8.2-8.7MPa, the 300% elongation is 20.0-21.2%, and the tearing strength is 130.5-133.8kN/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 tire Belt rubber composition
1. Preparation of dispersible white carbon black
Placing the white carbon black into the impregnating solution, stirring uniformly, carrying out primary standing for 8min under the pressure of 2.1MPa, carrying out secondary standing after the primary standing is completed, carrying out standing for 6min under the pressure of 2.7MPa, and drying after the standing is completed to obtain the dispersible white carbon black;
the particle size of the white carbon black is 140nm;
the mass ratio of the white carbon black to the impregnating solution is 1:3.7;
the impregnating solution consists of deionized water, fatty alcohol-polyoxyethylene ether and sodium dodecyl benzene sulfonate, wherein the mass ratio of the deionized water to the fatty alcohol-polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 78:2.4:3.0.
2. Preparation of powder rubber mixtures
(1) Preparation of functional powder
Calcining aluminum nitride powder at 250 ℃ for 1.2 hours, calcining wollastonite powder at 320 ℃ for 1.0 hour, cooling to room temperature respectively after the calcining is finished, and mixing to obtain a primary mixed material; adding polyethylene glycol 400 into the primary mixed material, performing ball milling treatment for 45min at the ball milling rotating speed of 210rpm, and obtaining functional powder after ball milling;
the grain diameter of the aluminum nitride powder is 100nm;
the particle size of the calcium feldspar powder is 125nm, and the mass content of the silicon dioxide is 65.8%;
the mass ratio of the aluminum nitride powder to the wollastonite powder is 1.5:1.2;
the mass ratio of the primary mixed material to the polyethylene glycol 400 is 95:1.8;
(2) Preparation of Mixed slurry
Mixing functional powder with deionized water, stirring uniformly, adding KH570 and cocamidopropyl betaine, stirring at 76 ℃ for 2.3h, and cooling to room temperature after stirring to obtain suspension; adding natural latex with 25% of solid content and glycerol monooleate into the suspension, homogenizing under 6.2MPa for 5min to obtain mixed slurry;
the mass ratio of the functional powder to the deionized water to the KH570 to the cocamidopropyl betaine is 13:125:1.1:0.47;
the mass ratio of the natural latex to the glycerol monooleate to the suspension is 260:2.2:323;
(3) Coagulation
Adding CaCl with mass concentration of 2% into the mixed slurry 2 Solidifying the coagulant, and then washing and drying to obtain a powder rubber mixture;
the mass ratio of the mixed slurry to the coagulant is 100:0.23.
3. Mixing
Adding the powder rubber mixture, zinc oxide, an auxiliary agent and an anti-aging agent RD into an internal mixer for mixing, controlling the temperature to be 80 ℃, the pressure to be 14MPa, the rotating speed of a rotor to be 54rpm, and the mixing time to be 30s to prepare a section of mixed rubber; adding the first-stage mixed rubber, the dispersible white carbon black, the carbon black and the adhesive into an internal mixer for mixing, controlling the temperature to 160 ℃, the pressure to 13MPa, the rotor rotating speed to 50rpm and the mixing time to 45s, and preparing a second-stage mixed rubber; adding the second-stage mixed rubber, sulfur and accelerator DZ into an internal mixer, mixing for 92 seconds at the rotor rotating speed of 23rpm, and discharging rubber to prepare a tire belt rubber composition;
the mass ratio of the powder rubber mixture to the zinc oxide to the auxiliary agent to the antioxidant RD to the dispersible white carbon black to the adhesive to the sulfur to the accelerator DZ is 158:2.5:1.5:3.0:7.4:13:2.9:2.0:2.3;
the adhesive is resorcinol;
the preparation method of the auxiliary agent comprises the steps of mixing stearic acid and carboxymethyl cellulose, increasing the temperature to 42 ℃, stirring for 13min at 132rpm, then adding mineral oil, and continuing stirring for 7min to obtain the auxiliary agent;
the mass ratio of the stearic acid to the carboxymethyl cellulose to the mineral oil is 3.7:2.0:1.1.
Example 2 preparation method of tire Belt rubber composition
1. Preparation of dispersible white carbon black
Placing the white carbon black into the impregnating solution, stirring uniformly, carrying out primary standing for 6min under the pressure of 2.0MPa, carrying out secondary standing after the primary standing is completed, carrying out standing for 5min under the pressure of 2.6MPa, and drying after the standing is completed to obtain the dispersible white carbon black;
the particle size of the white carbon black is 130nm;
the mass ratio of the white carbon black to the impregnating solution is 1:3.5;
the impregnating solution consists of deionized water, fatty alcohol-polyoxyethylene ether and sodium dodecyl benzene sulfonate, wherein the mass ratio of the deionized water to the fatty alcohol-polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 76:2.3:2.8.
2. Preparation of powder rubber mixtures
(1) Preparation of functional powder
Calcining aluminum nitride powder at 246 ℃ for 1.0h, calcining wollastonite powder at 315 ℃ for 1.2h, cooling to room temperature respectively after calcining, and mixing to obtain a primary mixed material; adding polyethylene glycol 400 into the primary mixed material, performing ball milling treatment for 42min at a ball milling rotating speed of 204rpm, and obtaining functional powder after ball milling;
the grain diameter of the aluminum nitride powder is 95nm;
the particle size of the calcium feldspar powder is 115nm, and the mass content of the silicon dioxide is 65.4%;
the mass ratio of the aluminum nitride powder to the wollastonite powder is 1.6:1.3;
the mass ratio of the primary mixed material to the polyethylene glycol 400 is 93:1.7;
(2) Preparation of Mixed slurry
Mixing functional powder with deionized water, stirring uniformly, adding KH570 and cocamidopropyl betaine, stirring at 74 ℃ for 2.2h, and cooling to room temperature after stirring to obtain suspension; adding natural latex with 25% of solid content and glycerol monooleate into the suspension, homogenizing under 6.0MPa for 6min to obtain mixed slurry;
the mass ratio of the functional powder to the deionized water to the KH570 to the cocamidopropyl betaine is 12:122:1.0:0.44;
the mass ratio of the natural latex to the glycerol monooleate to the suspension is 258:2.1:320;
(3) Coagulation
Adding CaCl with mass concentration of 2% into the mixed slurry 2 Solidifying the coagulant, and then washing and drying to obtain a powder rubber mixture;
the mass ratio of the mixed slurry to the coagulant is 100:0.21.
3. Mixing
Adding the powder rubber mixture, zinc oxide, an auxiliary agent and an anti-aging agent RD into an internal mixer for mixing, controlling the temperature to be 79 ℃, the pressure to be 13MPa, the rotating speed of a rotor to be 52rpm, and the mixing time to be 29s to prepare a section of mixed rubber; adding the first-stage mixed rubber, the dispersible white carbon black, the carbon black and the adhesive into an internal mixer for mixing, controlling the temperature to 158 ℃, the pressure to 12MPa, the rotor rotating speed to 48rpm and the mixing time to 44s, and preparing a second-stage mixed rubber; adding the second-stage mixed rubber, sulfur and accelerator DZ into an internal mixer, mixing for 91s at the rotor rotating speed of 22rpm, and discharging rubber to prepare a tire belt rubber composition;
the mass ratio of the powder rubber mixture to the zinc oxide to the auxiliary agent to the antioxidant RD to the dispersible white carbon black to the adhesive to the sulfur to the accelerator DZ is 156:2.4:1.4:2.8:7.1:12:2.8:1.8:2.1;
the adhesive is resorcinol;
the preparation method of the auxiliary agent comprises the steps of mixing stearic acid and carboxymethyl cellulose, increasing the temperature to 40 ℃, stirring for 12min at 130rpm, then adding mineral oil, and continuing stirring for 6min to obtain the auxiliary agent;
the mass ratio of the stearic acid to the carboxymethyl cellulose to the mineral oil is 3.6:1.8:1.0.
Example 3 preparation method of tire Belt rubber composition
1. Preparation of dispersible white carbon black
Placing the white carbon black into the impregnating solution, stirring uniformly, carrying out primary standing for 10min under the pressure of 2.2MPa, carrying out secondary standing after the primary standing is completed, carrying out standing for 7min under the pressure of 2.8MPa, and drying after the standing is completed to obtain the dispersible white carbon black;
the particle size of the white carbon black is 150nm;
the mass ratio of the white carbon black to the impregnating solution is 1:3.9;
the impregnating solution consists of deionized water, fatty alcohol-polyoxyethylene ether and sodium dodecyl benzene sulfonate, wherein the mass ratio of the deionized water to the fatty alcohol-polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 80:2.5:3.2.
2. Preparation of powder rubber mixtures
(1) Preparation of functional powder
Calcining aluminum nitride powder at 254 ℃ for 1.4 hours, calcining wollastonite powder at 325 ℃ for 0.8 hours, cooling to room temperature respectively after the calcining is finished, and mixing to obtain a primary mixed material; adding polyethylene glycol 400 into the primary mixed material, performing ball milling treatment for 48min at a ball milling rotating speed of 213rpm, and obtaining functional powder after ball milling;
the grain diameter of the aluminum nitride powder is 105nm;
the particle size of the calcium feldspar powder is 140nm, and the mass content of the silicon dioxide is 66.0%;
the mass ratio of the aluminum nitride powder to the wollastonite powder is 1.4:1.1;
the mass ratio of the primary mixed material to the polyethylene glycol 400 is 97:1.9;
(2) Preparation of Mixed slurry
Mixing functional powder with deionized water, stirring uniformly, adding KH570 and cocamidopropyl betaine, stirring at 80deg.C for 2.4 hr, and cooling to room temperature to obtain suspension; adding natural latex with 25% of solid content and glycerol monooleate into the suspension, homogenizing under 6.4MPa for 4min to obtain mixed slurry;
the mass ratio of the functional powder to the deionized water to the KH570 to the cocamidopropyl betaine is 14:128:1.2:0.50;
the mass ratio of the natural latex to the glycerol monooleate to the suspension is 262:2.3:325;
(3) Coagulation
Adding CaCl with mass concentration of 2% into the mixed slurry 2 Solidifying the coagulant, and then washing and drying to obtain a powder rubber mixture;
the mass ratio of the mixed slurry to the coagulant is 100:0.25.
3. Mixing
Adding the powder rubber mixture, zinc oxide, an auxiliary agent and an anti-aging agent RD into an internal mixer for mixing, controlling the temperature to be 81 ℃, the pressure to be 15MPa, the rotating speed of a rotor to be 56rpm, and the mixing time to be 31s to prepare a section of mixed rubber; adding the first-stage mixed rubber, the dispersible white carbon black, the carbon black and the adhesive into an internal mixer for mixing, controlling the temperature to 162 ℃, the pressure to 14MPa, the rotor rotating speed to 52rpm and the mixing time to 46s, and preparing a second-stage mixed rubber; adding the second-stage mixed rubber, sulfur and accelerator DZ into an internal mixer, mixing for 93s at the rotor rotating speed of 24rpm, and discharging rubber to prepare a tire belt rubber composition;
the mass ratio of the powder rubber mixture to the zinc oxide to the auxiliary agent to the antioxidant RD to the dispersible white carbon black to the adhesive to the sulfur to the accelerator DZ is 160:2.6:1.6:3.2:7.7:14:3.0:2.2:2.5;
the adhesive is resorcinol;
the preparation method of the auxiliary agent comprises the steps of mixing stearic acid and carboxymethyl cellulose, increasing the temperature to 44 ℃, stirring for 14min at 134rpm, then adding mineral oil, and continuing stirring for 8min to obtain the auxiliary agent;
the mass ratio of the stearic acid to the carboxymethyl cellulose to the mineral oil is 3.8:2.2:1.2.
Comparative example 1
On the basis of the embodiment 1, the preparation of the powder rubber mixture is omitted, the powder rubber mixture is replaced by a mixture of aluminum nitride powder and calcium feldspar powder and natural rubber in the mixing process, the mass ratio of the natural rubber to the aluminum nitride powder to the calcium feldspar powder is 65:16.7:13.3, and the rest operations are the same.
Comparative example 2
Based on example 1, the modification was that,
(1) omitting the step of preparing the dispersible white carbon black, and directly adopting white carbon black which is not subjected to any treatment, wherein the particle size of the white carbon black is 140nm;
(2) in the mixing step, the auxiliary agent is replaced by stearic acid; the mass ratio of the powder rubber mixture to the zinc oxide to the stearic acid to the antioxidant RD to the dispersible white carbon black to the adhesive to the sulfur to the accelerator DZ is 158:2.5:1.5:3.0:7.4:13:2.9:2.0:2.3;
the rest of the operations are the same.
Comparative example 3
Based on example 1, the specific method for preparing the powder rubber mixture is,
(1) preparation of functional powder
Calcining aluminum nitride powder at 250 ℃ for 1.2 hours, calcining wollastonite powder at 320 ℃ for 1.0 hour, cooling to room temperature respectively after the calcining is finished, and mixing to obtain functional powder;
the grain diameter of the aluminum nitride powder is 100nm;
the particle size of the calcium feldspar powder is 125nm, and the mass content of the silicon dioxide is 65.8%;
the mass ratio of the aluminum nitride powder to the wollastonite powder is 1.5:1.2;
(2) preparation of Mixed slurry
Mixing the functional powder with deionized water, stirring uniformly, adding KH570, stirring at 76 ℃ for 2.3h, and cooling to room temperature after stirring to obtain suspension; adding natural latex with 25% of solid content into the suspension, and uniformly stirring to obtain mixed slurry;
the mass ratio of the functional powder to the deionized water to the KH570 is 13:125:1.1;
the mass ratio of the natural latex to the suspension is 260:323;
the rest of the operations are the same.
Test examples
The rubber compositions prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance tests according to the following criteria:
mechanical properties were tested according to GB/T528-2009; tear properties were tested according to GB/T529-2008; the heat conduction performance is tested according to GB/T11205-2009; the DMA test is to test a sample by dynamic mechanical analysis, wherein the test mode is a stretching mode, the dynamic strain is 0.25%, the static strain is 1%, and the tan delta is tested at 60 ℃;
the vulcanizing conditions are 160 ℃ for 20min, and the performance test results are as follows:
the dispersible white carbon black prepared by the invention, sodium dodecyl benzene sulfonate and fatty alcohol polyoxyethylene ether are used as the surfactant, the pressure is increased in order to thoroughly impregnate the white carbon black in the standing process, and the combination of the surfactant avoids the agglomeration of the white carbon black, and improves the dispersibility of the white carbon black in a rubber system;
according to the invention, the functional powder is prepared by adopting a specific method, the heat conduction performance can be improved, the strength performance is enhanced, polyethylene glycol 400 in the preparation process is used as a surfactant, the surface of the functional powder is dispersed by combining ball milling treatment, the functional powder is treated by a silane coupling agent, and then the functional powder is mixed with rubber by combining homogenization treatment and a wet method, so that the compatibility and the dispersibility of the functional powder in the rubber are improved, and the rubber molecules are prevented from being damaged; the auxiliary agent prepared by the invention mainly has the functions of dispersion lubrication and stabilization; in the mixing process, the specific powder rubber mixture is combined with specific auxiliary agents, dispersible white carbon black and other technical means, so that the mixing uniformity of other components is improved, the structural stability of the inside of the rubber composition is enhanced, and the purposes of improving the heat conductivity, reducing hysteresis loss, reducing heat generation and enhancing the mechanical property and mechanical stability are achieved.
According to the experiment of the comparative example 1, the inorganic filler and the natural rubber are subjected to simple dry mixing, agglomeration easily occurs in the mixing process, the dispersion performance is poor, the internal dispersion of the rubber composition is uneven, the phenomenon of particle aggregation occurs, rubber molecules are easily damaged by thermal oxidation and the like, the mechanical property and the heat conducting property are further influenced, the heat generation is high, and the strength loss after ultraviolet irradiation is more;
according to comparative example 2, the white carbon black is not treated in comparative example 2, the white carbon black particles are in an aggregation state, and the auxiliary agent is omitted in the mixing step, so that the components cannot be uniformly dispersed, the heat conductivity and the reinforcing property cannot be fully exerted, the heat generation is high, the comprehensive performance of the rubber composition is further influenced, and the service life is shortened;
according to the experiment of comparative example 3, the simple mixing of the wollastonite powder and the aluminum nitride powder in comparative example 3 cannot eliminate the agglomeration phenomenon among particles, in the step of preparing the mixed slurry, the cocoamidopropyl betaine component, the glycerol monooleate component and the homogenizing treatment step are omitted, the functional powder still presents an aggregation state, the aggregated functional powder can cause the silane coupling agent to not sufficiently react with the functional powder, the mixing uniformity performance is poor when the functional powder is mixed with the natural latex, and the comprehensive application of the rubber composition is finally affected.
The proportions described in the invention are mass proportions, and the percentages are mass percentages unless otherwise specified.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. 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 (7)
1. The preparation method of the tire belt rubber composition is characterized by comprising the steps of preparing dispersible white carbon black, preparing powder rubber mixture and mixing;
the preparation method of the dispersible white carbon black comprises the steps of placing the white carbon black into impregnating solution, stirring uniformly, carrying out primary standing for 6-10min under the pressure of 2.0-2.2MPa, carrying out secondary standing for 5-7min under the pressure of 2.6-2.8MPa, and drying after standing to obtain the dispersible white carbon black;
the impregnating solution consists of deionized water, fatty alcohol-polyoxyethylene ether and sodium dodecyl benzene sulfonate, wherein the mass ratio of the deionized water to the fatty alcohol-polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 76-80:2.3-2.5:2.8-3.2;
the preparation of the powder rubber mixture comprises the steps of preparing functional powder, preparing mixed slurry and solidifying;
the preparation method of the functional powder comprises the steps of placing aluminum nitride powder at 246-254 ℃ for calcination for 1.0-1.4h, placing wollastonite powder at 315-325 ℃ for calcination for 0.8-1.2h, cooling to room temperature after the calcination, and mixing to obtain a primary mixed material; adding polyethylene glycol 400 into the primary mixed material, performing ball milling treatment for 42-48min at a ball milling rotating speed of 204-213rpm, and obtaining functional powder after ball milling;
the preparation method of the mixed slurry comprises the steps of mixing functional powder with deionized water, stirring uniformly, adding KH570 and cocamidopropyl betaine, stirring at 74-80 ℃ for 2.2-2.4h, and cooling to room temperature after stirring to obtain suspension; adding natural latex with 25% of solid content and glycerol monooleate into the suspension, homogenizing under 6.0-6.4MPa for 4-6min to obtain mixed slurry;
the mixing step is that the powder rubber mixture, zinc oxide, auxiliary agent and anti-aging agent RD are added into an internal mixer to be mixed, the temperature is controlled to be 79-81 ℃, the pressure is controlled to be 13-15MPa, the rotating speed of a rotor is 52-56rpm, and the mixing time is 29-31s, so that a section of mixed rubber is prepared; adding the first-stage mixed rubber, the dispersible white carbon black, the carbon black and the adhesive into an internal mixer for mixing, controlling the temperature to be 158-162 ℃, the pressure to be 12-14MPa, the rotating speed of a rotor to be 48-52rpm, and the mixing time to be 44-46s to prepare a second-stage mixed rubber; adding the second-stage mixed rubber, sulfur and accelerator DZ into an internal mixer, mixing for 91-93s at the rotor rotating speed of 22-24rpm, and discharging rubber to prepare a tire belt rubber composition;
the preparation method of the auxiliary agent comprises the steps of mixing stearic acid and carboxymethyl cellulose, increasing the temperature to 40-44 ℃, stirring for 12-14min at 130-134rpm, then adding mineral oil, and continuously stirring for 6-8min to obtain the auxiliary agent.
2. A process for producing a tire belt rubber composition as claimed in claim 1, wherein,
in the step of preparing the dispersible white carbon black, the particle size of the white carbon black is 130-150nm;
the mass ratio of the white carbon black to the impregnating solution is 1:3.5-3.9.
3. A process for producing a tire belt rubber composition as claimed in claim 1, wherein,
in the step of preparing the functional powder, the grain diameter of the aluminum nitride powder is 95-105nm;
the particle size of the calcium feldspar powder is 115-140nm, and the mass content of the silicon dioxide is 65.4-66.0%;
the mass ratio of the aluminum nitride powder to the wollastonite powder is 1.4-1.6:1.1-1.3;
the mass ratio of the primary mixed material to the polyethylene glycol 400 is 93-97:1.7-1.9.
4. A process for producing a tire belt rubber composition as claimed in claim 1, wherein,
in the step of preparing the mixed slurry, the mass ratio of the functional powder to the deionized water to the KH570 to the cocamidopropyl betaine is 12-14:122-128:1.0-1.2:0.44-0.50;
the mass ratio of the natural latex to the glycerol monooleate to the suspension is 258-262:2.1-2.3:320-325.
5. A process for producing a tire belt rubber composition as claimed in claim 1, wherein,
the solidification step is to add CaCl with mass concentration of 2% into the mixed slurry 2 Solidifying the coagulant, and then washing and drying to obtain a powder rubber mixture;
the mass ratio of the mixed slurry to the coagulant is 100:0.21-0.25.
6. A process for producing a tire belt rubber composition as claimed in claim 1, wherein,
the mass ratio of the powder rubber mixture to the zinc oxide to the auxiliary agent to the antioxidant RD to the dispersible white carbon black to the adhesive to the sulfur to the accelerator DZ is 156-160:2.4-2.6:1.4-1.6:2.8-3.2:7.1-7.7:12-14:2.8-3.0:1.8-2.2:2.1-2.5;
the adhesive is resorcinol;
the mass ratio of the stearic acid to the carboxymethyl cellulose to the mineral oil is 3.6-3.8:1.8-2.2:1.0-1.2.
7. A tire belt rubber composition produced by the production method according to any one of claims 1 to 6.
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