CN114874518A - Tire tread rubber composition containing pretreated white carbon black, preparation method and application thereof, and tire - Google Patents
Tire tread rubber composition containing pretreated white carbon black, preparation method and application thereof, and tire Download PDFInfo
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- CN114874518A CN114874518A CN202210561741.1A CN202210561741A CN114874518A CN 114874518 A CN114874518 A CN 114874518A CN 202210561741 A CN202210561741 A CN 202210561741A CN 114874518 A CN114874518 A CN 114874518A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0016—Compositions of the tread
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- 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
Abstract
The invention belongs to the field of rubber tire manufacturing, and particularly relates to a tread rubber composition containing pretreated white carbon black, a preparation method and application thereof, and a tire. The rubber composition comprises the following raw materials in parts by weight based on 100 parts of the sum of rubber materials: 20-40 parts of butadiene rubber and 60-80 parts of solution polymerized styrene butadiene rubber; 80-95 parts of pretreated white carbon black and 10-78 parts of silane coupling agent C2; the pretreated white carbon black is silane coupling agent A modified precipitated white carbon black; the silane coupling agent A and C are selected from one of Si69, Si75, OTES and Si 363; the mixing method of the rubber composition comprises a first-stage mixing stage, a second-stage mixing stage and a final mixing stage; wherein, when the mixing temperature of the first-stage mixing reaches 110-130 ℃, the silane coupling agent component C is added. The tread rubber provided by the invention has the advantages that the hysteresis loss, the wet-grip resistance, the tensile strength, the elongation at break and the like are obviously improved.
Description
Technical Field
The invention belongs to the field of rubber tire manufacturing, and particularly relates to a tread rubber composition containing pretreated white carbon black, a preparation method and application thereof, and a tire.
Background
The labeling method for tires sets forth requirements for wet grip and rolling resistance of the tire. The white carbon black is used in the tire tread of the tire and has the effects of reducing rolling resistance and improving wet grip. However, the hydrophilic white carbon black has a large amount of silicon hydroxyl groups on the surface, and has poor compatibility with lipophilic rubber. Therefore, during the mixing process of the white carbon black and the rubber, a silane coupling agent is often added to improve the lipophilicity of the white carbon black. Generally, silane coupling agents contain ethoxy groups, and the silane coupling agents and white carbon black can generate a silanization reaction to generate ethanol in a mixing process; on the other hand, the reaction efficiency is not high, and the silane coupling agent does not modify the surface of the white carbon black completely.
In order to solve the problem of ethanol release in the reaction process and improve the reaction efficiency, lipophilic groups are introduced on the surface of the white carbon black in the manufacturing process of the white carbon black, namely, the silanization reaction is carried out in the manufacturing process of the white carbon black in advance, so that an effective solution to the above problem is provided. As IN the U.S. Momentive patent IN201821015006A, NXT silane pre-treated white carbon black and the use of this white carbon black IN all natural rubber treads significantly reduced the hysteresis loss of the compound at 60 ℃.
As also disclosed in U.S. patent EP2722361B to Goodyear corporation, a silane pretreated white carbon black having the trade name Agilon400 was used as a surface material in a tread composition for a tire, and 2phr (calculated as 100phr of the rubber in the formulation) of solid Si69 and solid Si75 (50% of carbon black in solid silane) was additionally added during mixing, resulting in a tread rubber with lower hysteresis loss and better abrasion resistance.
In the prior art, after the surface of the white carbon black is pretreated by using a silane coupling agent, the surface of the white carbon black is subjected to oleophylic modification, and the white carbon black can be well dispersed into oleophylic rubber. Therefore, the silane coupling agent does not need to be added again during the kneading process. However, the inventors found that although the surface of the pretreated white carbon has been coated with the silane coupling agent, the agglomerate of the white carbon is opened by the large shearing force of the rotor of the internal mixer, and the inside of the white carbon particle is exposed. The exposed part of the white carbon black is still very hydrophilic without silane pretreatment, so that the reaggregation among particles is caused to deteriorate the dispersibility of the white carbon black, and the rolling resistance and the wet-grip resistance of the tread rubber are finally influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a rubber composition containing pretreated white carbon black and a preparation method thereof. According to the invention, different silane coupling agents are selected to pretreat the white carbon black, and then the silane coupling agents are added again after a certain mixing temperature is reached during a first mixing period, so that the rubber composition is prepared by the method. The rubber composition has remarkably improved hysteresis loss, wet grip resistance, tensile strength and elongation at break.
In order to achieve the above object, the present invention adopts the following technical solutions:
the tread rubber composition containing the pretreated white carbon black comprises the following components in parts by weight based on 100 parts of the sum of rubber materials:
the pretreated white carbon black is silane coupling agent A modified precipitated white carbon black;
the silane coupling agent A and C are selected from one of Si69, Si75, OTES and Si 363;
the mixing method of the rubber composition comprises a first-stage mixing stage, a second-stage mixing stage and a final mixing stage; wherein, when the mixing temperature of the first-stage mixing reaches 110-130 ℃, the silane coupling agent component C is added.
Preferably, the raw material formula of the rubber composition comprises the following components in parts by weight based on 100 parts by weight of the sum of the rubber compounds:
preferably, the raw material formula of the rubber composition further comprises the following components: 1.5-3.5 parts of zinc oxide, 1-3 parts of stearic acid, 1-3 parts of microcrystalline wax, 1-3 parts of antioxidant 4020, 0.5-2.5 parts of antioxidant RD, 1-3 parts of sulfur and 0.5-2.5 parts of promoter CZ.
Preferably, the raw material formula of the rubber composition further comprises the following components: 2.5 parts of zinc oxide, 2 parts of stearic acid, 2 parts of microcrystalline wax, 2 parts of an anti-aging agent 4020, 1.5 parts of an anti-aging agent RD, 2 parts of sulfur and 1.8 parts of a promoter CZ.
Preferably, the specific surface area BET of the precipitated silica is 100-200m 2 /g。
Preferably, the silanization modification rate of the pretreated white carbon black is 5-10%.
Preferably, the preparation method of the pretreated white carbon black comprises the following steps:
1) adding a large amount of ethanol and a small amount of water into a specific container, adjusting the pH to 3.5-5.0 by using acetic acid, adding a silane coupling agent A (8-16% of the weight ratio of precipitated silica) and performing hydrolysis ionization reaction for 10-20 hours;
2) adding precipitated white carbon black, and stirring at 40-100 ℃ for 48 hours to complete the pretreatment reaction;
3) and finally, drying the slurry to obtain the white carbon black pretreatment powder.
Further, the present application provides a method for preparing the rubber composition, which comprises the following steps:
1) all rubber, pretreated white carbon black, zinc oxide, stearic acid, microcrystalline wax, an anti-aging agent 4020 and an anti-aging agent RD are added together at the initial stage of mixing; adding the silane coupling agent C when the first-stage mixing temperature reaches 110 ℃, and discharging rubber after the mixing temperature reaches 170 ℃;
2) mixing in the second stage, wherein no material is added into the master batch, and discharging rubber after the mixing temperature reaches 170 ℃;
3) and (3) final refining, namely adding the second-stage masterbatch, sulfur, the accelerator CZ and the accelerator DPG together in the initial stage, and discharging the rubber when the temperature of the rubber reaches 110 ℃.
Further, the application provides the application of the rubber composition in the preparation and production of tires.
Further, the present application provides a tire having a tread compound vulcanized using the rubber composition.
According to the invention, due to the adoption of the technical scheme, the inventors use OTES, or Si69, or Si75 to implement pre-modification in the white carbon black manufacturing process; meanwhile, during the mixing process, part of silane, or OTES, or Si69, or Si75, or NXT is continuously added, and the process optimization in the in-situ reaction is carried out, so that the tread composition of the ideal tread is finally obtained. The pretreatment of white carbon black by using Si75 or Si69 is not related to patent EP2722361B, and meanwhile, the pretreatment of white carbon black by using a plurality of silanes in the series, the supplement of silane in the mixing process, the control of the in-situ reaction temperature of various silanes and the regulation and control of other materials in the tread composition are not related to patent EP 2722361B. On the other hand, compared with the commercially available pretreated silane Agilon400, the tensile strength and the elongation at break of the tread composition designed by the invention are also greatly improved.
Drawings
FIG. 1: hydrolysis ionization reaction of Si69 under specific conditions.
Detailed Description
The technical solutions in the embodiments of the present invention will be examined and completely described below with reference to the embodiments of the present invention, so as to further explain the invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. Given the embodiments of the present invention, all other embodiments that can be obtained by a person of ordinary skill in the art without any inventive step are within the scope of the present invention.
Pretreatment of white carbon black surface
A comparative surface area of 165m 2 The precipitated silica (trade name 1165MP, product of Sorburv, Qingdao) is subjected to surface pretreatment and modification.
The method specifically comprises the following steps:
1) 1000L of ethanol and 30L of water were charged into a specified vessel, pH was adjusted to 4.5 using acetic acid, and a silane coupling agent A10kg was added to conduct hydrolysis for 10 hours, resulting in conversion of ethoxy group to hydroxyl group.
2) Adding 100kg of precipitated white carbon black, stirring for 48 hours at 70 ℃ to complete the pretreatment reaction, and drying to obtain powder. And cleaning the powder by using acetone, removing unreacted silane coupling agent on the surface of the white carbon black, and drying to obtain the final pretreated white carbon black.
Tread composition containing pretreated white carbon black and preparation process thereof
The tread formula is as follows: 30phr of butadiene rubber, 70phr of solution polymerized styrene-butadiene rubber, 88phr of pretreated white carbon black, 2phr of silane coupling agent C, 2.5phr of zinc oxide, 2phr of stearic acid, 2phr of microcrystalline wax, 2phr of anti-aging agent 4020, 1.5phr of anti-aging agent RD, 2phr of sulfur, 1.8phr of accelerator CZ and 1.0phr of accelerator DPG.
The preparation process of the tread composition comprises the following steps:
1) all rubber, pretreated white carbon black, zinc oxide, stearic acid, microcrystalline wax, an anti-aging agent 4020 and an anti-aging agent RD are put into the mixer at the initial stage of mixing.
2) And adding the silane coupling agent C when the first-stage mixing temperature reaches 110 ℃, and discharging rubber after the mixing temperature reaches 170 ℃.
3) And (3) two-stage mixing, wherein no material is added into the master batch, and rubber is discharged after the mixing temperature reaches 170 ℃.
4) And (3) final refining, namely adding the second-stage masterbatch, sulfur, the accelerator CZ and the accelerator DPG together in the initial stage, and discharging the rubber when the temperature of the rubber reaches 110 ℃.
Characterization of the Properties of pretreated white carbon and Tread rubber
The surface of the silica after silane pretreatment was analyzed using a thermogravimetric analyzer (TGA). The principle is as follows: after the unreacted silane coupling agent on the surface of the white carbon black treated by the silane coupling agent is cleaned by acetone, the white carbon black is heated by TGA. The percentage of weight reduction at high temperature in the heating process of TGA is used to determine the amount of silane reacted to the surface of the white carbon black, i.e. the modification rate of silane to white carbon black. The test method comprises the following steps: heating up to 600 ℃ from room temperature of 20 ℃ under the protection of nitrogen at a heating rate of 10 ℃/min. In the data processing, the weight reduction rate of 150-600 ℃ is used as the modification rate of the silane to the white carbon black.
The tan delta value at 60 ℃ was used as an indication of the rolling resistance of the tread rubber. A dynamic thermal mechanical analyzer model VR-7120 (DMA, manufactured by Shanghai, Japan) was used. The test conditions were: a stretching mode; frequency, 12 Hz; static strain is 7%, and dynamic strain is 0.25%; temperature rise rate, 2 ℃/min. The tan delta value at 60 ℃ was used to characterize the rolling resistance of the vulcanizate. Calculated on the tan delta value of comparative example 1 at 60 ℃ as 100, the higher the value, the lower the rolling resistance.
The tan delta value of 0 ℃ was used as an indication of the wet grip resistance of the tread rubber. A dynamic thermal mechanical analyzer model VR-7120 (DMA, manufactured by Shanghai, Japan) was used. The test conditions were: a stretching mode; frequency, 12 Hz; static strain is 7%, and dynamic strain is 0.25%; temperature rise rate, 2 ℃/min. The tan delta value at 0 ℃ was used to characterize the wet grip resistance of the vulcanizate. Calculated as tan δ value at 0 ℃ of comparative example 1 being 100, the higher the value, the higher the wet grip resistance.
Strain scanning at 80 ℃ using a Rubber Processing Analyzer (RPA) was used as a characterization of the degree of filler dispersion in the tread rubber (Payne effect refers to the difference in elastic modulus G' at large magnitude strain). And (3) testing conditions are as follows: at 80 deg.C, the strain sweep ranges from 0.28-100%, and the frequency is 20 Hz. Calculated on the value of G' 0.28-42% of comparative example 1 as 100, the larger the value, the larger the Payne effect, and the worse the dispersion of the filler in the tread rubber.
Steps of particular embodiments
Commercial pretreated white carbon black Aglion400 used in comparative examples 1 and 2, pretreated silane used on the surface and the kind thereof were not known.
Comparative example 1 used a non-silane treated white carbon black, model 1165MP, product of solvay corporation.
Comparative example 2 compares the temperature difference of the silane coupling agent C input.
Comparative example 3 no silane coupling agent C was added during the kneading, and the Payne effect, tan δ at 60 ℃, etc. were less effective.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention, including any reference to the above-mentioned embodiments. Various modifications to these embodiments will be readily apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The tread rubber composition containing the pretreated white carbon black is characterized in that the raw material formula of the rubber composition comprises the following components in parts by weight based on 100 parts by weight of the sum of rubber materials:
20-40 parts of butadiene rubber
60-80 parts of solution polymerized styrene-butadiene rubber
70-95 parts of pretreated white carbon black
2-10 parts of a silane coupling agent C;
the pretreated white carbon black is silane coupling agent A modified precipitated white carbon black;
the silane coupling agent A and C are selected from one of Si69, Si75, OTES and Si 363;
the mixing method of the rubber composition comprises a first-stage mixing stage, a second-stage mixing stage and a final mixing stage; wherein, when the mixing temperature of the first-stage mixing reaches 110-130 ℃, the silane coupling agent component C is added.
2. The rubber composition according to claim 1, wherein the raw material formulation of the rubber composition comprises the following components in parts by weight based on 100 parts by weight of the sum of the rubber compounds:
25-35 parts of butadiene rubber
65-75 parts of solution polymerized styrene-butadiene rubber
85-90 parts of pretreated white carbon black
And 2-5 parts of a silane coupling agent C.
3. The rubber composition of claim 1, wherein the rubber composition further comprises the following components: 1.5-3.5 parts of zinc oxide, 1-3 parts of stearic acid, 1-3 parts of microcrystalline wax, 1-3 parts of antioxidant 4020, 0.5-2.5 parts of antioxidant RD, 1-3 parts of sulfur and 0.5-2.5 parts of promoter CZ.
4. The rubber composition according to claim 3, wherein the raw material formulation of the rubber composition further comprises the following components: 2.5 parts of zinc oxide, 2 parts of stearic acid, 2 parts of microcrystalline wax, 2 parts of an anti-aging agent 4020, 1.5 parts of an anti-aging agent RD, 2 parts of sulfur and 1.8 parts of a promoter CZ.
5. The rubber composition of claim 1, wherein the precipitation whitening is performedThe specific surface area BET of the carbon black is 100-200m 2 /g。
6. The rubber composition of claim 1, wherein the silanization modification rate of the pretreated white carbon black is 5% -10%.
7. The rubber composition according to claim 1, wherein the preparation method of the pretreated white carbon black comprises the following steps:
1) adding a large amount of ethanol and a small amount of water into a specific container, adjusting the pH to 3.5-5.0 by using acetic acid, adding a silane coupling agent A (8-16 percent of the weight proportion of precipitated white carbon black), and performing hydrolysis ionization reaction for 10-20 hours;
2) adding precipitated white carbon black, and stirring at 40-100 ℃ for 48 hours to complete the pretreatment reaction;
3) and finally, drying the slurry to obtain the white carbon black pretreatment powder.
8. A process for preparing a rubber composition according to any one of claims 1 to 7, characterized in that it comprises the steps of:
all rubber, pretreated white carbon black, zinc oxide, stearic acid, microcrystalline wax, an anti-aging agent 4020 and an anti-aging agent RD are put into the mixer at the initial stage of mixing; adding the silane coupling agent C when the first-stage mixing temperature reaches 110 ℃, and discharging rubber after the mixing temperature reaches 170 ℃;
mixing in the second stage, wherein no material is added into the master batch, and discharging rubber after the mixing temperature reaches 170 ℃;
and (3) final refining, namely adding the second-stage masterbatch, sulfur, the accelerator CZ and the accelerator DPG together in the initial stage, and discharging the rubber when the temperature of the rubber reaches 110 ℃.
9. Use of a rubber composition according to any one of claims 1 to 7 in the manufacture of a tire.
10. A tire, characterized in that the tread compound of said tire is obtained by vulcanizing the rubber composition according to any one of claims 1 to 7.
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| CN202210561741.1A CN114874518B (en) | 2022-05-23 | 2022-05-23 | Tread rubber composition containing pretreated white carbon black, preparation method and application thereof, and tire |
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| CN202210561741.1A CN114874518B (en) | 2022-05-23 | 2022-05-23 | Tread rubber composition containing pretreated white carbon black, preparation method and application thereof, and tire |
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| CN110869433A (en) * | 2017-07-19 | 2020-03-06 | 住友橡胶工业株式会社 | Rubber composition for tread and pneumatic tire |
| CN111491998A (en) * | 2017-12-05 | 2020-08-04 | 大陆轮胎德国有限公司 | Sulfur-crosslinkable rubber mixture, vulcanized rubber of rubber mixture and vehicle tire |
| CN113861533A (en) * | 2021-09-29 | 2021-12-31 | 中策橡胶集团有限公司 | White carbon black filled tire tread rubber composition, mixing method and tire |
| CN113896965A (en) * | 2021-10-11 | 2022-01-07 | 中策橡胶集团有限公司 | White carbon black filled tread rubber composition, mixing method and wear-resistant tire |
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2022
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| EP0638610A1 (en) * | 1993-08-09 | 1995-02-15 | The Goodyear Tire & Rubber Company | Tire with silica reinforced tread |
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