CN112409662B - Composition for preparing rubber compound, preparation method of rubber compound and tire - Google Patents
Composition for preparing rubber compound, preparation method of rubber compound and tire Download PDFInfo
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- CN112409662B CN112409662B CN202011281740.9A CN202011281740A CN112409662B CN 112409662 B CN112409662 B CN 112409662B CN 202011281740 A CN202011281740 A CN 202011281740A CN 112409662 B CN112409662 B CN 112409662B
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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
- C08L15/00—Compositions of rubber derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0016—Compositions of the tread
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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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Abstract
The application provides a composition for preparing a rubber compound, the rubber compound, a preparation method of the rubber compound and a tire, and belongs to the technical field of rubber modification. The composition for preparing the rubber compound comprises 70-130 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber A, 5-55 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber B, 60-100 parts by weight of white carbon black, 5-15 parts by weight of carbon black, 3-7 parts by weight of vulcanization activator, 1-2 parts by weight of vulcanizing agent and 3.8-5.5 parts by weight of vulcanization accelerator. The styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20-35%, and the vinyl content is 40-60%. The modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B have higher affinity with white carbon black and can be better and fully combined, so that the rubber material prepared from the rubber compound has excellent ground grabbing performance and lower rolling resistance.
Description
Technical Field
The application relates to the technical field of rubber modification, in particular to a composition for preparing a rubber compound, the rubber compound, a preparation method of the rubber compound and a tire.
Background
With the development of semi-steel radial tires, the requirements on the tire gripping performance and the fuel performance are increasing from the safety and comfort considerations. However, improving grip performance and reducing rolling resistance are often a pair of contradictors, which tend to cancel each other out, which presents a significant challenge to existing formulation technology. The ground grabbing safety, the fuel oil economy and the environmental protection are the most important two control links of the green tire, and generally, the two large performance indexes are controlled at a higher level, so that the formulation technology needs to be changed greatly.
Disclosure of Invention
The application provides a composition for preparing a rubber compound, a preparation method thereof and a tire, which can improve the grip performance of the tire and reduce the rolling resistance at the same time.
Embodiments of the present application are implemented as follows:
in a first aspect, the present examples provide a composition for preparing a mix comprising: 70 to 130 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber A, 5 to 55 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber B, 60 to 100 weight parts of white carbon black, 5 to 15 weight parts of carbon black, 3 to 7 weight parts of vulcanization activator, 1 to 2 weight parts of vulcanizing agent and 3.8 to 5.5 weight parts of vulcanization accelerator.
Wherein, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber A is 25-40%, and the vinyl content is 25-40%.
The styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20-35%, and the vinyl content is 40-60%.
In the technical scheme, the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B have higher affinity with white carbon black and can be well and fully combined, so that the rubber material prepared from the rubber compound has excellent ground grabbing performance and lower rolling resistance.
The styrene content of the modified oil-extended solution polymerized styrene-butadiene rubber A is controlled to be 25-40%, so that the rolling resistance is not remarkably improved while the rubber material has excellent ground grabbing performance; the vinyl content is controlled to be 25-40% in order to balance better rolling resistance. The styrene content of the modified oil-extended solution polymerized styrene-butadiene rubber B is controlled to be 20-35%, and the vinyl content is controlled to be 40-60%, so that the rubber material has small hysteresis loss and low rolling resistance. The modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B have better compatibility. And the coordination of the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B can improve the conflict of the single modified oil-extended solution polymerized styrene-butadiene rubber in the directions of ground grabbing, rolling resistance and processing performance.
With reference to the first aspect, in a first possible example of the first aspect of the present application, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber a is 30 to 40%, the vinyl content is 30 to 40%, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20 to 30%, and the vinyl content is 40 to 50%.
Alternatively, the modified oil-extended solution polymerized styrene-butadiene rubber A has a weight average molecular weight M w ≥10 6 The weight average molecular weight of the modified oil-extended solution polymerized styrene-butadiene rubber B is 4 x 10 5 ～6*10 5 。
Optionally, 35 to 40phr of modified oil-extended solution polymerized styrene-butadiene rubber A and 3 to 7phr of modified oil-extended solution polymerized styrene-butadiene rubber B.
In the above examples, the high molecular weight modified oil-extended solution-polymerized styrene-butadiene rubber a can give a rubber material having better grip performance, abrasion resistance, mechanical properties, and reduced rolling resistance.
In combination with the first aspect, in a second possible example of the first aspect of the present application, the silica is precipitated hydrated silica having a BET specific surface area of 140 to 180cm 2 /g。
Optionally, the nitrogen adsorption specific surface area of the carbon black is more than or equal to 80cm 2 /g。
Alternatively, the composition used to prepare the mix includes 2 to 4 parts by weight of a white carbon dispersion agent including a mixture of zinc stearate and fatty acid esters.
Optionally, the composition used to prepare the mix comprises 6 to 15 parts by weight of a silane coupling agent.
Alternatively, the silane coupling agent comprises Si-69 solid silicon.
In the above examples, the white carbon black of the present application has a good dispersibility, and such white carbon black can be dispersed to the level of primary particles, thereby shortening the required kneading time.
The silane coupling agent can reduce the generation of ethanol, reduce the emission of VOC and improve the performance of sizing materials.
With reference to the first aspect, in a third possible example of the first aspect of the present application, the vulcanizing agent includes sulfur, and the vulcanization accelerator includes N-cyclohexyl-2-benzothiazole sulfenamide, diphenyl guanidine, and tetrabenzyl thiuram disulfide.
Optionally, the vulcanization accelerator comprises 1.5 to 2 parts by weight of N-cyclohexyl-2-benzothiazole sulfenamide, 2 to 3 parts by weight of diphenyl guanidine, and 0.3 to 0.5 part by weight of tetrabenzyl thiuram disulfide.
In a fourth possible example of the first aspect of the present application, in combination with the first aspect, the above composition for preparing a rubber compound includes 4 to 7 parts by weight of the traction resin.
Optionally, the traction resin comprises a modified alpha-methylstyrene based resin.
In the above examples, the grip resin has good compatibility with the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B, and can improve the grip performance of the rubber material prepared from the rubber compound without improving the rolling resistance.
In a fifth possible example of the first aspect of the present application, in combination with the first aspect, the composition for preparing a rubber compound includes 4 to 7 parts by weight of a biomaterial KSH-1, the biomaterial KSH-1 having a formula C 9 H 8.83 (OCH 3 ) 0.95 。
In the above examples, the biological material and the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B are matched, so that the grip performance of the rubber material prepared from the rubber compound can be improved, and the rolling resistance can be reduced.
In combination with the first aspect, in a sixth possible example of the first aspect of the present application, the composition for preparing a rubber compound described above includes 2 to 9 parts by weight of an environment-friendly aromatic oil, 4 to 7 parts by weight of an anti-aging agent, and 0.1 to 0.3 parts by weight of a scorch retarder.
In a second aspect, the present examples provide a method of preparing a masterbatch comprising sequentially performing a first-stage masterbatch mixing, a second-stage masterbatch mixing, a third-stage masterbatch mixing, and a fourth-stage masterbatch mixing.
The first master batch is prepared by mixing 70-130 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber A, 5-55 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber B, 60-100 parts by weight of white carbon black, 2-4 parts by weight of white carbon black dispersing agent, 6-15 parts by weight of silane coupling agent, 4-7 parts by weight of ground-grabbing resin, 4-7 parts by weight of biological material KSH-1, 2-4 parts by weight of vulcanization activator, 2-3 parts by weight of vulcanization accelerator, 1-3 parts by weight of age inhibitor and 2-9 parts by weight of environment-friendly aromatic oil to prepare the master batch.
The second-stage masterbatch mixing comprises the steps of mixing the prepared first masterbatch, 5-15 parts by weight of carbon black, 1-3 parts by weight of vulcanization active agent and 2-4 parts by weight of anti-aging agent to prepare a second masterbatch.
And the three-stage masterbatch mixing comprises the step of carrying out back-mixing on the prepared second masterbatch to prepare a third masterbatch.
The four-section masterbatch mixing comprises the steps of mixing the prepared third masterbatch, 1-2 parts by weight of vulcanizing agent, 1.8-2.5 parts by weight of vulcanization accelerator and 0.1-0.3 part by weight of scorch retarder for final mixing to prepare the masterbatch.
In the technical scheme, the four-section mixing process is adopted, and the four-section mixing process can ensure that the white carbon black can be fully dispersed and fully combined with the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B.
In a third aspect, the present examples provide a rubber compound prepared according to the method for preparing a rubber compound described above.
In the technical scheme, the rubber material prepared from the rubber compound has higher ground grabbing performance and lower rolling resistance.
In a fourth aspect, the present examples provide a tire made using the above-described compound.
In the technical scheme, the tire has higher ground grabbing performance and lower rolling resistance.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the synthetic reaction of the modified oil-extended solution polymerized styrene-butadiene rubber of the present application;
FIG. 2 is a schematic diagram of the combination of the modified oil-extended solution polymerized styrene-butadiene rubber and filler of the present application;
FIG. 3 is a schematic illustration of the silylation reaction of the white carbon black and rubber of the present application.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustration of the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The following is a specific description of a composition for preparing a rubber compound, a preparation method thereof and a tire according to the embodiment of the present application:
the present application provides a composition for preparing a mix comprising: 70 to 130 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber A (F-SSBR A), 5 to 55 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber B (F-SSBR B), 60 to 100 parts by weight of white carbon black, 5 to 15 parts by weight of carbon black, 3 to 7 parts by weight of vulcanization activator, 1 to 2 parts by weight of vulcanizing agent and 3.8 to 5.5 parts by weight of vulcanization accelerator.
Wherein, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber A is 25-40%, and the vinyl content is 25-40%;
the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20-35%, and the vinyl content is 40-60%.
Optionally, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber A is 30-40%, and the vinyl content is 30-40%;
the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20-30%, and the vinyl content is 40-50%.
Optionally, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber A is 32-36%, and the vinyl content is 35-40%;
the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 25-30%, and the vinyl content is 40-45%.
The modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B are both prepared by modifying the single end of 4,4 '-bis- (dialkylamino) -benzophenone, and the synthetic reaction schematic diagram of the oil-extended solution polymerized styrene-butadiene rubber with the single end modified of 4,4' -bis- (dialkylamino) -benzophenone is shown in figure 1.
The oil extension of the modified oil-extended solution polymerized styrene-butadiene rubber A is 35-40 phr, and the oil extension of the modified oil-extended solution polymerized styrene-butadiene rubber B is 3-7 phr.
Alternatively, the modified oil-extended solution polymerized styrene-butadiene rubber A has an oil extension of 37.5phr and the modified oil-extended solution polymerized styrene-butadiene rubber B has an oil extension of 5phr.
The styrene content in the present application refers to the content of the styrene structure; the vinyl content refers to the amount of vinyl bonds.
Weight average molecular weight M of modified oil-extended solution polymerized styrene-butadiene rubber A w ≥10 6 Weight average molecular weight M of modified oil-extended solution polymerized styrene-butadiene rubber B w At 4 x 10 5 ～6*10 5 Between them.
Alternatively, the modified oil-extended solution polymerized styrene-butadiene rubber A has a weight average molecular weight M w ≥1.15*10 6 Weight average molecular weight M of modified oil-extended solution polymerized styrene-butadiene rubber B w At 4.5 x 10 5 ～5.5*10 5 Between them.
The solubility parameter SP value of the modified oil-extended solution polymerized styrene-butadiene rubber A is 17.83, and the solubility parameter SP value of the modified oil-extended solution polymerized styrene-butadiene rubber A is 17.61.
The modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B have higher affinity with white carbon black, and can be better and fully combined. So that the rubber material prepared from the rubber compound has excellent ground grabbing performance and lower rolling resistance.
As shown in fig. 2, a comparison of the unmodified oil-extended solution polymerized styrene-butadiene rubber and the modified oil-extended solution polymerized styrene-butadiene rubber shows that: the functional group at the molecular chain end of the modified oil-extended solution polymerized styrene-butadiene rubber can react with the filler (silicon dioxide), so that the free chain end is reduced and better rubber-filler interaction is achieved, hysteresis loss is reduced, and better reinforcing effect is achieved. While the unmodified oil-extended solution polymerized styrene-butadiene rubber is capable of reacting with the filler in a lesser amount.
The styrene content of the modified oil-extended solution polymerized styrene-butadiene rubber A is not too high or too low, so that the rolling resistance is not remarkably improved while the rubber material has excellent ground grabbing performance; the vinyl content is controlled at a higher level in order to balance better rolling resistance properties. Meanwhile, the high molecular weight modified oil-extended solution polymerized styrene-butadiene rubber A can enable the rubber material to have better ground grabbing performance, wear resistance and mechanical performance, and reduce rolling resistance.
The styrene content of the modified oil-extended solution polymerized styrene-butadiene rubber B is controlled to be 20-35%, the vinyl content is controlled to be 40-60%, and the styrene content is 4 x 10 5 Weight average molecular weight M is less than or equal to w ≤6*10 5 The modified oil-extended solution polymerized styrene-butadiene rubber B can lead the rubber material to have small hysteresis loss and low rolling resistance.
The modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B have better compatibility. And the coordination of the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B can improve the conflict of the single modified oil-extended solution polymerized styrene-butadiene rubber in the directions of ground grabbing, rolling resistance and processing performance.
It should be noted that, in order to fully exert its effect, the dry rubber content of the modified oil-extended solution polymerized styrene-butadiene rubber B in the whole raw rubber system is not less than 20%.
The vulcanization activators include Stearic Acid (SA) and activated zinc oxide (ZnO).
Specifically, 3 to 7 parts by weight of the vulcanization activator comprises 1 to 3 parts by weight of active zinc oxide and 2 to 4 parts by weight of stearic acid.
The vulcanizing agent comprises sulfur powder.
Optionally, the composition used to prepare the mix comprises 1.2 to 1.7 parts by weight of a vulcanizing agent.
Vulcanization accelerators include N-cyclohexyl-2-benzothiazole sulfenamide (CZ), diphenyl guanidine (DPG), and tetrabenzyl thiuram disulfide (TBzTD).
Alternatively, the vulcanization accelerator is a mixture of N-cyclohexyl-2-benzothiazole sulfenamide, diphenyl guanidine, and tetrabenzylthiuram disulfide.
Specifically, 3.8 to 5.5 parts by weight of the vulcanization accelerator comprises 1.5 to 2 parts by weight of N-cyclohexyl-2-benzothiazole sulfenamide, 2 to 3 parts by weight of diphenyl guanidine and 0.3 to 0.5 part by weight of tetrabenzyl thiuram disulfide.
The present application uses moderate amounts of vulcanizing agents in combination with the vulcanization accelerators described above, and such "semi-effective vulcanization systems" are intermediate between effective vulcanization systems and conventional vulcanization systems. It can give the rubber composition good vulcanization flatness, longer scorch time, higher crosslinking density and crosslinking stability, and higher physical and mechanical properties.
The three accelerators of the present application are activated in a characteristic manner with respect to vulcanization speed and degree of crosslinking, they have a synergistic effect, which is not possible, and can ensure a suitable vulcanization speed and an extended scorch time of the rubber composition. And as a large amount of acid groups on the surface of the white carbon black can adsorb the vulcanization accelerator to delay the vulcanization speed, the inventor of the application makes long-term search on a vulcanization system, and can greatly improve the physical and mechanical properties of rubber materials and improve the durability of tires by increasing the dosage of the accelerator N-cyclohexyl-2-benzothiazole sulfenamide and the dosage of diphenyl guanidine, especially increasing the dosage of the alkaline accelerator diphenyl guanidine and reducing the dosage of sulfur powder.
The white carbon black is precipitated hydrated silicon dioxide, and the BET specific surface area is 140-180 cm 2 /g, and D50 value is 2-5 μm, and particle diameter of primary particles is 5-15 nm;
alternatively, the white carbon black is precipitated hydrated silica having a BET specific surface area of 160 to 170cm 2 /g, and D50 value is 2-3 μm, and particle diameter of primary particles is 8-10 nm;
optionally, the white carbon black is Solviwei1165MP, silicon +.>HD165MP。
The white carbon black is used for partially or completely replacing the carbon black, so that the relation between the loss factor and the temperature can be improved, the rolling resistance is greatly reduced, and the ground grabbing performance is improved.
Compared with the common white carbon black, the high-dispersion white carbon black has great difference in production process, and particularly is characterized in that the control process of the silica aggregate structure in the semi-finished product synthesis stage is more focused on the polymerization of primary silica particles and the depolymerization of secondary particles, so that a large number of small particles exist stably in uniform particle size, the interaction between the white carbon black is reduced, the formation of a network structure between the silica is reduced, and the occurrence of flocculation aggregates is reduced.
The nitrogen adsorption specific surface area of the carbon black is more than or equal to 80cm 2 /g；
Optionally, the nitrogen adsorption specific surface area of the carbon black is more than or equal to 100cm 2 /g；
Optionally, the carbon black has a nitrogen adsorption specific surface area of 132-142 cm 2 The DBP oil absorption value is 108-118 mL/100g.
Alternatively, the carbon black is CB N115.
The carbon black of the present application possesses excellent tear resistance, and can impart better durability to rubber materials.
The composition for preparing a rubber compound of the present application comprises 2 to 4 parts by weight of a white carbon black dispersant comprising a mixture of zinc stearate and fatty acid esters (RF-70).
The composition for preparing the rubber compound comprises 6-15 parts by weight of a silane coupling agent, wherein the silane coupling agent comprises Si-69 solid silicon, mono-sulfur or disulfide.
Alternatively, the silane coupling agent is Si-69 solid silicon.
The Si-69 solid silicon has relatively low price, and can control the manufacturing cost of the rubber material. If the cost of producing the rubber material is not taken into consideration, a novel silane coupling agent of mono-sulfur or disulfide may be selected.
The high-fraction white carbon black and the ethanol generated in the silanization reaction of rubber cannot be completely discharged to delay the silanization reaction, dense air holes are formed in the tread extrusion section possibly, the silane coupling agent can reduce the generation of ethanol, reduce the emission of VOC and improve the sizing material performance.
The composition for preparing the mix comprises 4 to 7 parts by weight of a grip resin comprising a modified alpha-methylstyrene based resin (CSR 6200) having a softening point of 90 to 110 ℃.
The ground-grabbing resin has good compatibility with the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B, can interact with the surface groups of the white carbon black, improves the viscoelastic performance of the rubber material, and endows the rubber material with excellent ground-grabbing performance and traction performance.
The composition for preparing the rubber compound comprises 4 to 7 weight parts of biological material KSH-1, wherein the molecular formula of the biological material KSH-1 is C 9 H 8.83 (OCH 3 ) 0.95 . The amorphous three-dimensional linear polymer material is formed by connecting phenyl propane units through ether bonds and carbon-carbon bonds, and has polar and nonpolar functional groups, and the biological material is matched with modified oil-filled solution polymerized styrene-butadiene rubber A and modified oil-filled solution polymerized styrene-butadiene rubber B, so that the ground grabbing performance of the rubber material can be improved, the rolling resistance can be reduced, and the vulcanization speed of a sizing material can be obviously reduced.
The composition for preparing the rubber compound comprises 2-9 parts by weight of environment-friendly aromatic oil, 4-7 parts by weight of anti-aging agent and 0.1-0.3 part by weight of scorch retarder.
The environment-friendly aromatic oil is used for improving the processability of the rubber material and improving the grip performance of the rubber material.
Alternatively, the environmentally friendly aromatic oil is composed of the chinese holy vivanec 500.
Alternatively, 4 to 7 parts by weight of the antioxidant includes 1 to 3 parts by weight of the Rhine Wax 111 (Wax) and 2 to 4 parts by weight of the antioxidant 6PPD (N- (1, 3-dimethylbutyl) -N' -phenyl-p-phenylenediamine).
Alternatively, the scorch retarder comprises a scorch retarder CTP (N-cyclohexylthio-phthalimide).
Optionally, the composition for preparing a rubber compound of the present application comprises: 95 to 115 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber A, 20 to 35 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber B, 65 to 85 weight parts of white carbon black, 5 to 10 weight parts of carbon black, 4 to 6 weight parts of vulcanization active agent, 1.2 to 1.7 weight parts of vulcanizing agent, 4.5 to 5.5 weight parts of vulcanization accelerator, 3 to 4 weight parts of white carbon black dispersing agent, 8 to 13 weight parts of silane coupling agent, 4 to 6 weight parts of ground-gripping resin, 4 to 6 weight parts of biological material KSH-1, 3 to 8 weight parts of environment-friendly aromatic oil, 4 to 6 weight parts of anti-aging agent and 0.1 to 0.3 weight part of scorch retarder.
The application also provides a preparation method of the rubber compound, which comprises the steps of primary master batch mixing, secondary master batch mixing, tertiary master batch mixing and quaternary master batch mixing which are sequentially carried out.
It should be noted that, although silica can react with the functional groups at the end of the molecular chain of the modified oil-extended solution polymerized styrene-butadiene rubber a and the modified oil-extended solution polymerized styrene-butadiene rubber B as the filler to realize interaction, the whole reaction process has high requirements on mixing equipment and process, and the white carbon black rubber material needs an additional mixing step to complete the reaction between the silanol of the white carbon black and the ethoxy of the coupling agent, and the reaction schematic diagram is shown in fig. 3. Typically this reaction has a minimum initiation temperature of about 130 ℃. Therefore, in actual production, the silylation reaction is usually controlled at 145-150 ℃, which is a narrower temperature reaction window, and the reaction is effective only under the higher temperature treatment effect and the longer constant temperature mixing, so that the activities of chemical adsorption, grafting and the like can occur. In addition, the surface of the rubber material is smooth, the Mooney is controlled in a proper range, and the extrusion process of the next process is satisfied, which is difficult to control for a shearing type rotor internal mixer, so that the reaction temperature and time of the high-white carbon black formula are strictly controlled, sufficient silanization reaction is ensured, a plurality of mixing stages of 150 ℃ are formed, excellent static physical properties and dynamic mechanical properties of the rubber material are ensured, and excellent conversion capability between the grip performance and rolling resistance of the rubber material and better durability are realized.
The method adopts the measures of adjusting the initial rotation speed, adjusting the number of times of lifting bolts, adjusting the rotation speed gradient, adjusting the temperature rising speed, adjusting the rotation speed during constant-temperature mixing, and basically ensuring the constant-temperature mixing time, so that the silanization reaction is sufficient.
The preparation method of the rubber compound comprises the following steps:
and (3) mixing a section of masterbatch:
the filling coefficient is 0.65-0.8. 70 to 130 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber A, 5 to 55 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber B, 60 to 100 weight parts of white carbon black, 2 to 4 weight parts of white carbon black dispersing agent, 6 to 15 weight parts of silane coupling agent, 4 to 7 weight parts of ground-grabbing resin, 4 to 7 weight parts of biological material KSH-1, 2 to 4 weight parts of stearic acid, 2 to 3 weight parts of diphenyl guanidine and 1 to 3 weight parts of Rhine wax 111 are added into a GK400 internal mixer.
The initial rotating speed adopts a higher rotating speed of 50RPM, so that the temperature rising speed in the process of breaking rubber reaches a higher level, the bolt is lifted after the temperature of the bolt is raised to 118-120 ℃ for 40-42 seconds, and the rotating speed is reduced to 45RPM; adding 9 parts by weight of environment-friendly aromatic oil, pressing the bolt for 33-35 seconds, lifting the bolt after the temperature is increased to 142-144 ℃, and reducing the rotating speed to 30RPM; pressing the bolt for 68-70 seconds, lifting the bolt after the temperature is increased to 138-140 ℃, and reducing the rotating speed to 22RPM; pressing the bolt for 48-50 seconds until the temperature is raised to 139-141 ℃, and lifting the bolt; finally, the temperature of the pressing bolt is raised to 148-150 ℃ for 33-35 seconds, the rubber is discharged, the lifting bolt opens the discharging door, and the rotating speed is restored to 40RPM. The glue discharging is controlled by time or temperature, the set glue discharging technological parameter is 260 seconds or 150 ℃, and the glue discharging is started when one set parameter is reached, so that the first master batch is prepared.
The primary master batch mixing is the most important ring in the mixing process, the silanization reaction mainly occurs in the primary master batch mixing process, the mixing temperature is controlled by forming a rotating speed decreasing gradient and lifting bolts for a plurality of times, the silanization reaction is well finished in a shearing type rotor internal mixer, the full reaction is kept in a narrower temperature window, and the mixing effect at the stage plays a role in determining the performance of the sizing material.
Mixing the two-stage masterbatch:
the filling coefficient is 0.65-0.8. The prepared first masterbatch, 5 to 15 parts by weight of carbon black, 1 to 3 parts by weight of active zinc oxide and 2 to 4 parts by weight of antioxidant 6PPD are added into a GK400 internal mixer.
The second-stage masterbatch is produced at a constant rotating speed, the rotating speed is set to 40RPM, and the bolt is lifted after the temperature of the pressing bolt is raised to 108-110 ℃ for 34-36 seconds; pressing the bolt for 20-22 seconds, lifting the bolt after the temperature is raised to 118-120 ℃; pressing the bolt for 40-45 seconds, raising the temperature to 140-145 ℃ for discharging glue, lifting the bolt and opening the discharging door. And (3) controlling the time or the temperature of the glue discharging, wherein the set glue discharging technological parameter is 130 seconds or 145 ℃, and the glue discharging is started when one set parameter is reached, so that the second master batch is prepared.
Active zinc oxide is usually added in a primary masterbatch, but in a high white carbon black formulation, the risk of scorch can be reduced by selecting a secondary production formulation.
Mixing three-section masterbatch:
the filling coefficient is 0.65-0.8. The second masterbatch was added to a GK400 internal mixer. In order to reduce the mooney of the sizing material, a recycling process is adopted in the three-stage masterbatch. Setting the initial rotating speed to 40RPM, lifting the bolt after the temperature of the pressing bolt is raised to 112-114 ℃ for 20-22 seconds, and reducing the rotating speed to 35RPM; pressing the bolt for 68-70 seconds, discharging glue after the temperature is raised to 138-140 ℃, lifting the bolt, and opening the discharging door. And (3) controlling the time or the temperature of the glue discharging, wherein the set glue discharging technological parameter is 110 seconds or 140 ℃, and when one set parameter is reached, the glue discharging is started, so that the third master batch is prepared.
Four-section masterbatch mixing:
the filling coefficient is 0.65-0.8. Adding the third masterbatch, 1-2 parts by weight of vulcanizing agent, 1.5-2 parts by weight of N-cyclohexyl-2-benzothiazole sulfenamide, 0.3-0.5 part by weight of tetrabenzyl thiuram disulfide and 0.1-0.3 part by weight of scorch retarder into a GK255 internal mixer.
Setting the initial rotating speed to be 28RPM, lifting the bolt after the temperature of the pressing bolt is increased to 90-92 ℃ for 40-42 seconds, and reducing the rotating speed to 25RPM; pressing the bolt for 32-37 seconds, then discharging glue after the temperature is raised to 100-105 ℃, lifting the bolt and opening the discharging door.
The application also provides a rubber compound, which is prepared according to the preparation method of the rubber compound.
The rubber material prepared from the rubber compound can ensure that the semi-steel radial tire meets the requirements of the hardness, the elastic modulus and other physical properties of the tread and the extrusion process, improves the dynamic rigidity retention under the change of temperature, greatly improves the ground grabbing performance of the rubber material, greatly reduces the rolling resistance and simultaneously improves the breaking strength of the rubber material.
The application also provides a tire which is prepared from the rubber compound.
The tire of the present application has higher grip performance and lower rolling resistance.
A composition for preparing a rubber compound, a rubber compound and a method for preparing the same of the present application are described in further detail below with reference to examples.
Examples 1 to 7 and comparative examples 1 to 7 each used the specific four-stage kneading process of the present application.
The formulations of examples 1 to 7 are shown in Table 1, and the formulations of comparative examples 1 to 7 are shown in Table 2.
Table 1 formulation tables of examples 1 to 7
Wherein, F-SSBR A-1 weight averageA molecular weight of 1.2 x 10 6 The styrene content is 25-40%, the vinyl content is 25-40%; F-SSBR B-1 has a weight average molecular weight of 5.2X10 5 The styrene content is 25-40%, the vinyl content is 25-40%; F-SSBR A-2 has a weight average molecular weight of 0.9X10 6 The styrene content is 25-40%, the vinyl content is 25-40%; F-SSBR B-2 has a weight average molecular weight of 3.4x10 5 The content of styrene is 20-35%, and the content of vinyl is 40-60%; F-SSBR B-3 has a weight average molecular weight of 7.5 x 10 5 The content of styrene is 20-35%, and the content of vinyl is 40-60%.
Table 2 formulas of comparative examples 1 to 7
Wherein F-SSBR A-3 has a weight average molecular weight of 5.5X10 5 The styrene content is 10-24%, the vinyl content is 41-55%; F-SSBR B-4 has a weight average molecular weight of 5.2X10 5 The styrene content is 5-19% and the vinyl content is 25-39%.
Test example 1
The compounds prepared by the formulations of examples 1 to 7 and comparative examples 1 to 3 and 6 to 7 were vulcanized at 160℃for 30min and scorched at 127℃and the Mooney viscosity characteristics at 100℃were measured, respectively, as shown in tables 3 and 4. And the physical and mechanical properties of the compounds prepared by the formulations of examples 1 to 7 and comparative examples 1 to 3 and 6 to 7 were measured after vulcanization at 160℃for 20min, as shown in tables 5 and 6.
Table 3 Mooney viscosity Properties of the compounds of examples 1 to 7 were vulcanized at 160℃for 30min and scorched at 127℃and at 100 ℃
Table 4 Cure the compounds of comparative examples 1 to 3, 6 to 7 at 160℃for 30min, scorch at 127℃and Mooney viscosity at 100 ℃
| Test item | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 6 | Comparative example 7 |
| ML | 1.49 | 2.09 | 1.48 | 1.62 | 1.72 |
| MH | 11.45 | 15.09 | 11.88 | 9.27 | 12.46 |
| TS1 | 2:33 | 0:44 | 2:59 | 2:43 | 3:20 |
| TS2 | 3:07 | 2:25 | 3:27 | 3:19 | 3:45 |
| T10 | 2:33 | 1:28 | 2:53 | 2:50 | 3:18 |
| T50 | 3:47 | 3:23 | 4:21 | 4:16 | 4:38 |
| T90 | 8:49 | 9:25 | 9:55 | 9:38 | 10:27 |
| Ts5(127℃) | 22:21 | 19:05 | 20:52 | 23:19 | 27:11 |
| ML(1+4)100℃ | 70.43 | 76.98 | 73.42 | 69.24 | 78.85 |
Table 5 physical and mechanical Properties of the compounds of examples 1 to 7 after vulcanization at 160℃for 20min
Table 6 physical and mechanical Properties of the mixes of comparative examples 1 to 3 and 6 to 7 after curing at 160℃for 20min
As is clear from tables 3 to 4, the total amounts of the two resin materials CSR6200 and KSH-1 were kept the same, the ratios were different, and the vulcanization rates were different. The greater the amount of KSH-1 used, the slower the cure rate and the corresponding longer the scorch time, the slower the cure rate of example 4 compared to examples 1-3.
As is clear from tables 5 to 6, the formulations of examples 1 to 4 are capable of better balancing the contradiction between grip performance and rolling resistance performance when using the raw rubber systems of F-SSBR A-1 and F-SSBRB-1. Example 5 the tear strength of the vulcanizate was reduced using the green combination of F-SSBR A-2 and F-SSBRB-1, and the grip and roll resistance properties of the compounds were characterized to some extent by the high and low temperature resilience in the same frame formulation, both of which were reduced to some extent. Similarly, the grip performance of examples 6 to 7 was also lowered to a certain extent. The vulcanization speed of comparative examples 4 to 5 was too slow to cure. Comparative examples 1 to 2 incorporated a raw rubber system (IR, BR) of insoluble polymerized styrene-butadiene rubber, and the grip performance and rolling resistance were remarkably lowered. The physical and mechanical properties of comparative examples 3 and 6 were significantly reduced, the grip performance of comparative example 6 was significantly reduced, and the grip performance of comparative example 7 was not well balanced.
Test example 2
The dynamic mechanical properties of the compounds prepared by the formulations of examples 1 to 7 and comparative examples 1 to 3 and 6 to 7 were measured after vulcanization at 160℃for 20min, respectively, as shown in tables 7 to 8.
Table 7 dynamic mechanical Properties of the compounds of examples 1 to 7 after vulcanization at 160℃for 20min
Wherein, DMA test condition Static 3%, dynamic 0.25X10 HzTemp@3K/MIN-40- > 120 ℃.
Table 8 dynamic mechanical Properties of the mixes of comparative examples 1 to 3, 6 to 7 after curing at 160℃for 20min
| Test item | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 6 | Comparative example 7 |
| RPA,ΔG' | 0.76 | 0.65 | 0.32 | 0.28 | 0.41 |
| tanδ(@0℃) | 0.733 | 0.535 | 1.089 | 0.612 | 0.717 |
| tanδ(@20℃) | 0.275 | 0.222 | 0.406 | 0.287 | 0.266 |
| tanδ(@60℃) | 0.115 | 0.126 | 0.087 | 0.091 | 0.120 |
| E'(Mpa)(@0℃) | 57.711 | 65.546 | 47.231 | 39.127 | 49.562 |
| E'(Mpa)(@20℃) | 16.870 | 27.823 | 9.181 | 14.635 | 12.543 |
| E'(Mpa)(@60℃) | 7.942 | 15.443 | 4.245 | 6.316 | 5.827 |
| E'(Mpa)(20-60℃) | 8.93 | 12.38 | 4.94 | 8.32 | 6.72 |
| Tg℃(@Max tanδ) | -4.6 | -8.8 | -5.5 | -6.1 | -12.3 |
Wherein, DMA test condition Static 3%, dynamic 0.25X10 HzTemp@3K/MIN-40- > 120 ℃.
As can be seen from tables 7 and 8, the RPA represents the dispersion condition of the white carbon black in the sizing material, and the smaller the value, the better the dispersion, and the mixing process adopted in the application can effectively improve the dispersibility of the sizing material, thereby improving the dynamic performance of the sizing material. tan delta (@ 20 ℃) characterizes the dry grip properties of the compounds, the higher the value, the better the grip properties; tan delta (@ 60 ℃) characterizes the rolling resistance properties of the compounds, the lower the value the better the rolling resistance properties. Examples 2 to 4 are excellent in grip performance and rolling resistance performance, and are excellent in performance. E' (20-60 ℃) represents the dynamic rigidity retention rate of the sizing material under the temperature change, the lower the value of the dynamic rigidity retention rate is used for representing the smaller the influence of the temperature change on the sizing material, the dynamic performance of all the embodiments is controlled within a lower threshold value under the influence of the temperature change, and the excellent conversion capability of the ground grabbing performance and the rolling resistance performance can be realized.
In comparative example 3, when sulfur is increased by a single variable, the dynamic performance of the rubber material is hardly affected, but the static physical properties are insufficient, and the grip performance and rolling resistance performance of comparative examples 1 to 2 and 6 to 7 are all balanced and insufficient.
The foregoing is merely a specific embodiment of the present application and is not intended to limit the present application, and various modifications and variations may be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (13)
1. A composition for preparing a rubber compound, characterized in that it comprises: 70 to 130 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber A, 5 to 55 weight parts of modified oil-filled solution polymerized styrene-butadiene rubber B, 60 to 100 weight parts of white carbon black, 5 to 15 weight parts of carbon black, 3 to 7 weight parts of vulcanization activator, 1 to 2 weight parts of vulcanizing agent and 3.8 to 5.5 weight parts of vulcanization accelerator;
wherein the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B are both modified at one end of 4,4' -bis- (dialkylamino) -benzophenone;
the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber A is 30-40%, and the vinyl content is 30-40%;
the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20-30%, and the vinyl content is 40-50%;
weight average molecular weight M of the modified oil-extended solution polymerized styrene-butadiene rubber A w ≥10 6 The weight average molecular weight of the modified oil-extended solution polymerized styrene-butadiene rubber B is 4 x 10 5 ～6*10 5 ；
The vulcanization accelerator comprises 1.5 to 2 weight parts of N-cyclohexyl-2-benzothiazole sulfenamide, 2 to 3 weight parts of diphenyl guanidine and 0.3 to 0.5 weight part of tetrabenzyl thiuram disulfide;
the composition for preparing the rubber compound comprises 4-7 parts by weight of biological material KSH-1.
2. The composition for preparing a rubber compound according to claim 1, characterized in that said modified oil-extended solution polymerized styrene-butadiene rubber a is extended with 35 to 40phr and said modified oil-extended solution polymerized styrene-butadiene rubber B is extended with 3 to 7phr.
3. The composition for preparing a rubber compound according to claim 1, wherein the silica white is precipitated hydrated silica having a BET specific surface area of 140 to 180cm 2 /g。
4. A composition for preparing a rubber compound according to claim 3, characterized in that the carbon black has a nitrogen adsorption specific surface area of 80cm or more 2 /g。
5. A composition for preparing a rubber compound according to claim 3, characterized in that it comprises 2-4 parts by weight of a white carbon dispersing agent comprising a mixture of zinc stearate and fatty acid esters.
6. A composition for preparing a rubber compound according to claim 3, characterized in that it comprises 6-15 parts by weight of silane coupling agent.
7. The composition for preparing a rubber compound according to claim 6, wherein the silane coupling agent comprises Si-69 solid silicon.
8. The composition for preparing a rubber compound according to claim 1, characterized in that it comprises 4-7 parts by weight of a traction resin.
9. The composition for preparing a rubber compound according to claim 8, characterized in that the ground-gripping resin comprises a modified alpha-methylstyrene-based resin.
10. The composition for preparing a rubber compound according to any one of claims 1 to 9, wherein the composition for preparing a rubber compound comprises 2 to 9 parts by weight of an environment-friendly aromatic oil, 4 to 7 parts by weight of an anti-aging agent and 0.1 to 0.3 part by weight of a scorch retarder.
11. The preparation method of the rubber compound is characterized by comprising the steps of sequentially carrying out primary-section masterbatch mixing, secondary-section masterbatch mixing, tertiary-section masterbatch mixing and quaternary-section masterbatch mixing;
the primary master batch mixing comprises the steps of mixing 70-130 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber A, 5-55 parts by weight of modified oil-filled solution polymerized styrene-butadiene rubber B, 60-100 parts by weight of white carbon black, 2-4 parts by weight of white carbon black dispersing agent, 6-15 parts by weight of silane coupling agent, 4-7 parts by weight of ground-grabbing resin, 4-7 parts by weight of biological material KSH-1, 2-4 parts by weight of vulcanization activator, 2-3 parts by weight of vulcanization accelerator, 1-3 parts by weight of age inhibitor and 2-9 parts by weight of environment-friendly aromatic oil to prepare a primary master batch; the modified oil-extended solution polymerized styrene-butadiene rubber A and the modified oil-extended solution polymerized styrene-butadiene rubber B are both modified at one end by 4,4' -bis- (dialkylamino) -benzophenone; the vulcanization accelerator comprises 1.5 to 2 weight parts of N-cyclohexyl-2-benzothiazole sulfenamide, 2 to 3 weight parts of diphenyl guanidine and 0.3 to 0.5 weight part of tetrabenzyl thiuram disulfide;
the two-stage masterbatch mixing comprises the steps of mixing the prepared first masterbatch, 5-15 parts by weight of carbon black, 1-3 parts by weight of vulcanization active agent and 2-4 parts by weight of anti-aging agent to prepare a second masterbatch;
the three-section masterbatch mixing comprises the step of carrying out the back mixing of the prepared second masterbatch to prepare a third masterbatch;
the four-section masterbatch mixing comprises the steps of mixing the prepared third masterbatch, 1-2 parts by weight of vulcanizing agent, 1.8-2.5 parts by weight of vulcanization accelerator and 0.1-0.3 part by weight of scorch retarder for final mixing to prepare a mixed rubber;
wherein, the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber A is 30-40%, and the vinyl content is 30-40%;
the styrene content in the modified oil-extended solution polymerized styrene-butadiene rubber B is 20-30%, and the vinyl content is 40-50%;
weight average molecular weight M of the modified oil-extended solution polymerized styrene-butadiene rubber A w ≥10 6 The weight average molecular weight of the modified oil-extended solution polymerized styrene-butadiene rubber B is 4 x 10 5 ～6*10 5 。
12. A rubber compound, characterized in that it is prepared according to the process for preparing a rubber compound according to claim 11.
13. A tyre, characterized in that its tread is obtained with the mix according to claim 12.
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