CN106608990B - A kind of rubber composition and preparation method thereof and vulcanized rubber - Google Patents

A kind of rubber composition and preparation method thereof and vulcanized rubber Download PDF

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CN106608990B
CN106608990B CN201510691474.XA CN201510691474A CN106608990B CN 106608990 B CN106608990 B CN 106608990B CN 201510691474 A CN201510691474 A CN 201510691474A CN 106608990 B CN106608990 B CN 106608990B
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rubber
preparation
carbon black
kneaded
agent
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CN106608990A (en
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王丽丽
解希铭
王丽静
李静
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Abstract

The invention discloses a kind of rubber composition and preparation method thereof and vulcanized rubbers.The preparation method of the rubber composition includes: that solution polymerized butylbenzene, white carbon black, surface modifier and optional butadiene rubber progress first are kneaded by (1), and white carbon black rubber master batch is made;(2) the white carbon black rubber master batch, activator, anti-aging agent, softening agent and optional carbon black are subjected to the second mixing and two sections of rubber master batch is made;(3) two sections of rubber master batch, promotor and vulcanizing agent are subjected to third mixing and finished composition is made.In the processing technology, the effect in surface modifier can be preferably played, is conducive to white carbon black and sufficiently vulcanizes the intensity of vulcanized rubber obtained with interpolymer interaction, raising, reduce the heat of vulcanized rubber, improve the anti-slippery of vulcanized rubber.

Description

A kind of rubber composition and preparation method thereof and vulcanized rubber
Technical field
The present invention relates to rubber compositions prepared by a kind of preparation method of rubber composition and this method, and by the rubber The vulcanized rubber that glue composition further vulcanizes.
Background technique
Influence of the dynamic lag loss performance of rubber compounding to tyre performance is particularly important, and hysteresis loss makes sizing material dynamic Energy consumption increases in state deformation process, and heat increases, flexibility decrease, and rolling resistance rises.Heat also results in the strong of rubber Degree and wearability decline, cause the Random early Detection of tire, and heat also will increase the rolling resistance of tire, increase fuel consumption and two The discharge amount of carbonoxide.
CN102382338A discloses a kind of Isoprene rubber blend, including isoprene rubber, anti-form-1, the poly- isoamyl two of 4- Alkene, reinforcing filler, situ-formed graft modified additive, compound rubber and the first additive.
CN103881161A discloses a kind of rubber composition containing trans-polyisoprene, and rubber total amount is with 100 matter Part meter is measured, wherein the total amount of synthesis of trans polyisoprene and synthesizing cis polyisoprene is 5-60 mass parts, natural rubber 40-95 mass parts, white carbon black 5-90 mass parts, carbon black 5-990 mass parts;Rubber master batch technique includes: by the poly- isoamyl two of synthesis of trans Alkene is kneaded with synthesizing cis polyisoprene rubber composition and white carbon black, coupling agent as white carbon black wood glue;By natural rubber It is carbon black rubber master batch that glue and carbon black, which are kneaded,;Finished composition technique: by the carbon black rubber master batch, white carbon black wood glue, anti-aging agent, activating agent, rush Rubber composition is made into agent, vulcanizing agent mixing.
CN103703072A discloses a kind of rubber composition for tire tread, contains solution polymerized butadiene styrene rubber, carbon black, titanium dioxide Silicon and polyethylene glycol, the content of solution polymerized butadiene styrene rubber described in the rubber constituent of 100 mass % are 60 mass % or more, relative to 100 mass parts of rubber constituent, below the mass for 10, the content of the silica is 50 mass to the content of the carbon black Part or more, the content of the polyethylene glycol is 0.1-3.5 mass parts.
CN103087365A discloses a kind of rubber composition for anti-slippery wear resistance balance tire tread, the rubber group It closes object and contains diene elastomer, inorganic reinforced filling, coupling agent and plasticizer.
But the rubber that prior art provides still is not able to satisfy the intensity of tire tread glue needs, reduces heat, improves A kind of requirement of wet and slippery performance, it is desirable to provide rubber of performance improvement.
Summary of the invention
The purpose of the present invention is to solve how to improve the intensity of the rubber for tire tread, reduce heat, raising The problem of anti-slippery, provides a kind of rubber composition and preparation method thereof and vulcanized rubber.
To achieve the goals above, the present invention provides a kind of preparation method of rubber composition, this method comprises: (1) will Solution polymerized butylbenzene, white carbon black, surface modifier and optional butadiene rubber carry out first and are kneaded, and white carbon black rubber master batch is made;(2) by institute White carbon black rubber master batch, activator, anti-aging agent, softening agent and optional carbon black progress second is stated to be kneaded and two sections of rubber master batch are made;(3) by institute It states two sections of rubber master batch, promotor and vulcanizing agent progress third mixing and finished composition is made.
The present invention also provides a kind of rubber compositions of method preparation provided by the present invention.
The present invention also provides a kind of vulcanized rubber, the vulcanized rubber is by carrying out rubber composition provided by the invention Vulcanization is made, and the temperature of the vulcanization is 150-170 DEG C, and the vulcanization will be 10-20MPa, and the time of the vulcanization is 30- 50 minutes.
Rubber composition provided by the invention is obtained by a kind of new mixing method, in this method first by solution polymerized butylbenzene, Butadiene rubber, white carbon black and its surface modifier are prepared by mixing into white carbon black rubber master batch according to portfolio ratio, then again in white carbon black In rubber master batch according to carbon black is added, activator, anti-aging agent, softening agent are mixed with two sections of rubber master batch, finally in two sections of rubber master batch according to Vulcanizing agent is added in portfolio ratio, promotor is prepared into finished composition.According to the composition rubber composition for so sequentially adding selection Each component, the advantage is that: can preferably play the effect of surface modifier in the processing technology, be conducive to white carbon black Sufficiently and interpolymer interaction, the intensity for further vulcanizing vulcanized rubber obtained can be preferably improved, vulcanization rubber is reduced The heat of glue improves the anti-slippery of vulcanizate compound.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of preparation method of rubber composition, this method comprises: (1) is by solution polymerized butylbenzene, white carbon black, table Face modifying agent and optional butadiene rubber carry out first and are kneaded, and white carbon black rubber master batch is made;(2) by the white carbon black rubber master batch, activation Agent, anti-aging agent, softening agent and optional carbon black carry out the second mixing and two sections of rubber master batch are made;(3) by two sections of rubber master batch, promotors Third mixing is carried out with vulcanizing agent, and finished composition is made.
In the case of, according to the invention it is preferred to, the inventory of each component in this method are as follows: 60-100 mass parts contain intermingle with fourth Benzene, the butadiene rubber of 0-40 mass parts, the white carbon black of 50-100 mass parts, the carbon black of 0-20 mass parts, 2-12 mass parts table Face modifying agent, the softening agent of 10-20 mass parts, the activator of 3-8 mass parts, the vulcanizing agent of 0.5-3 mass parts, 1-6 mass parts Promotor and 1-6 mass parts anti-aging agent.
In the case of, according to the invention it is preferred to, the described first temperature being kneaded is 120-180 DEG C, and preferably described first is kneaded Temperature be 140-165 DEG C.
In the case of, according to the invention it is preferred to, the described first time being kneaded was 2-10min, preferably described first mixing Time is 5-8min.
In the case of, according to the invention it is preferred to, the described second temperature being kneaded is 80-140 DEG C, preferably described second mixing Temperature is 100-120 DEG C.
In the case of, according to the invention it is preferred to, the described second time being kneaded was 3-10min, preferably described second mixing Time is 4-6min.
In the case of, according to the invention it is preferred to, the temperature that the third is kneaded is no more than 130 DEG C, preferably 110-130 DEG C; The time that the third is kneaded is 4-6min.
In the case of, according to the invention it is preferred to, white carbon black is silica, and the N2 adsorption specific surface area of preferably white carbon black is 10-200m2/g;The CTAB adsorption specific surface area of carbon black is 10-300m2/g。
Preferably, white carbon black is preferably prepared by the precipitation method.White carbon black and carbon black can be commercially available, such as hard charcoal Black is 115GR and 165GR (French Rhodia).Carbon black is N330 and N220 (the limited public affairs of Dongguan City Qi Deli chemical science and technology Department).
In the case of, according to the invention it is preferred to, the surface modifier is general formula (RO)3SiCH2CH2CH2- X indicates organic Silane coupling agent, RO are hydrolyzable groups, preferably methoxyl group, ethyoxyl or acetoxyl group;X is organo-functional group, preferably For amino, methacryloxy, epoxy group or S general formula Sn(CH2)3Si(OR)3The group of expression, n are the integer of 2-4; It is preferred that the organo silane coupling agent is double-[γ-(triethoxysilicane) propyl]-tetrasulfide (Si69).
In the case of, according to the invention it is preferred to, the anti-aging agent is amines antioxidants, quinoline type antioxidant, benzimidazole At least one of anti-aging agent and physical protection agent.Can be commercially available, such as antioxidant 4020.
In the case of, according to the invention it is preferred to, the softening agent is aromatic naphtha, paraffin oil, naphthenic oil, Petropols and poly- second At least one of glycol.Wherein, the weight average molecular weight of polyethylene glycol is within the scope of 3000-5000, so that composite material has Preferable processing performance and physical mechanical property.Can be commercially available, such as aromatic naphtha TDAE V500, polyethylene glycol PEG4000。
In the case of, according to the invention it is preferred to, the activator is the composition of metal oxide and fatty acid, or fat Sour metallic soap salt;The metal oxide be zinc oxide and/or magnesia, the fatty acid metal soap salt be zinc stearate and/ Or zinc borate.
In the case of, according to the invention it is preferred to, the promotor is sulfenamide type accelerators, thiazole accelerator, Qiu Lan At least one of nurse class promotor and guanidines.Can be commercially available, such as N- tert-butyl -2-[4-morpholinodithio time sulphonyl Amine (TBBS), diphenylguanidine (D)
In the case of, according to the invention it is preferred to, the vulcanizing agent is that sulphur, insoluble sulfuy, oil-filled Sulfur and Sulfur are given At least one of body.Can be commercially available, such as common sulphur S, oil-filled insoluble sulfur IS.
The present invention also provides a kind of rubber compositions of method preparation provided by the present invention.
The present invention also provides a kind of vulcanized rubber, the vulcanized rubber is by carrying out rubber composition provided by the invention Vulcanization is made, and the temperature of the vulcanization is 150-170 DEG C, and the vulcanization will be 10-20MPa, and the time of the vulcanization is 30- 50 minutes.
Pressure used is gauge in the present invention.
The present invention will be described in detail by way of examples below.
1 is shown in Table using the Preparation equipment of rubber composition and rubber in following embodiment and comparative example.
Table 1
Serial number Device name Model Manufacturer
1 Mixer BR1600 Farrel Corp. (US) 25 Main Street, Ansonia, CT 06401, U.S.A. of the U.S.
2 Vulcanizing press XLB-D400*400*2 The first rubber machinery plant of Shanghai
The test equipment of rubber made from embodiment and comparative example is shown in Table 2, and test condition is shown in Table 3.
Table 2
Table 3
The chemical reagent that embodiment and comparative example uses is commercially available product, specific as follows:
Solution polymerized butylbenzene: 2535E, (wherein, styrene-content is 23 mass %, contents of ethylene 63 to Yanshan Petrochemical product Quality % is 27 mass % containing oil component;Mooney viscosity 60);
Butadiene rubber: BR9000, Yanshan Petrochemical product (wherein, cis-content is 97.8 mass %);
White carbon black: 165GR, French Rhodia, N2 adsorption specific surface area are 170m2/g;
Carbon black: N330, Dongguan City Qi Deli Chemical Industry Science Co., Ltd, CTAB adsorption specific surface area are 75m2/g;
Surface modifier: double-[γ-(triethoxysilicane) propyl]-tetrasulfide (Si69), the limited public affairs of Nanjing dawn chemical industry Department;
Softening agent: environment-friendly aromatic oil TDAE V500, Xin Dayang (Ningbo) Co., Ltd;
Activator: zinc oxide, stearic acid, Weifang Hengfeng Chemical Co., Ltd.;
Antioxidant 4020: N- (1,3- dimethylbutyl)-N '-diphenyl-para-phenylene diamine, the limited public affairs of the holy chemistry science and technology difficult to understand in Jiangsu Department;
Vulcanizing agent: sulphur, Weifang Zhong Heng Chemical Co., Ltd.;
Promotor: N tert butyl benzothiazole 2 sulfenamide (TBBS), diphenylguanidine (D), chemical science and technology is ground in Shanghai forever to be had Limit company;
PEG4000: pacify petrochemical plant in Huai-Hai.
Amounts of components in following embodiment and comparative example is parts by weight.
Embodiment 1
The present embodiment is used to illustrate the preparation and vulcanized rubber of rubber composition provided by the invention.
Be formulated (parts by weight, similarly hereinafter): solution polymerized butylbenzene 60, butadiene rubber 40, white carbon black 50, carbon black 20, Si69 are (silane coupled Agent) 2, TDAE (softening agent) 17, zinc oxide 5 (activator), stearic acid 1 (activator), sulphur 0.5 (vulcanizing agent), TBBS (promotion Agent) 4,2,4020 (anti-aging agent) 1 of D (promotor), PEG4000 (softening agent) 3.
Rubber composition preparation process:
White carbon black rubber master batch processed: solution polymerized butylbenzene is added in mixer, and setting revolving speed is 80rpm, and initial melting temperature is 80 DEG C, raw rubber plasticates the time as 0.5min;Butadiene rubber, white carbon black and Si69 are added in mixer and carry out the first mixing, is kneaded Temperature is 150 DEG C, mixing time 7min, and white carbon black rubber master batch is made;
It makes two sections of rubber master batch: carbon black, TDAE, zinc oxide, stearic acid, antioxidant 4020 and PEG4000 is added in mixer, It carries out second with white carbon black rubber master batch to be kneaded, mixing time 6min, dump temperature is 120 DEG C, and discharging and parking 4 hours is made two Section rubber master batch;
Finished composition processed: the revolving speed that mixer is arranged is 80rpm, and initial melting temperature is 40 DEG C, and two sections of rubber master batch are plasticated After 1min, addition vulcanizing agent, promotor carry out third mixing, and 110 DEG C of melting temperature, mixing time 4min, discharging obtains end Refining glue, i.e., rubber composition provided by the invention.
Vulcanized rubber processed:
Obtained rubber composition is put into vulcanizing press and is vulcanized, curing temperature is 160 DEG C, sulfide stress is Cured rubber samples S1 is made in 15MPa, vulcanization time 40min.
Vulcanized rubber article S1 is tested for the property, the results are shown in Table 4.
Embodiment 2
The present embodiment is used to illustrate the preparation and vulcanized rubber of rubber composition provided by the invention.
Formula: solution polymerized butylbenzene 75, butadiene rubber 25, white carbon black 77, carbon black 8, Si69 (silane coupling agent) 8, TDAE (softening Agent) 8, zinc oxide 5, stearic acid 3, sulphur 1.7 (vulcanizing agent), TBBS (promotor) 1.7, D (promotor) 1.9,4020 it is (anti-old Agent) 2, PEG4000 (softening agent) 6.
Rubber composition preparation process:
White carbon black rubber master batch processed: solution polymerized butylbenzene is added in mixer, and setting revolving speed is 80rpm, and initial melting temperature is 80 DEG C, raw rubber plasticates the time as 0.5min;Butadiene rubber, white carbon black and Si69 are added in mixer and carry out the first mixing, is kneaded Temperature is 140 DEG C, mixing time 8min, and white carbon black rubber master batch is made;
It makes two sections of rubber master batch: carbon black, TDAE, zinc oxide, stearic acid, antioxidant 4020 and PEG4000 is added in mixer, It carries out second with white carbon black rubber master batch to be kneaded, mixing time 4min, dump temperature is 100 DEG C, and discharging and parking 4 hours is made two Section rubber master batch;
Finished composition processed: the revolving speed that mixer is arranged is 80rpm, and initial melting temperature is 40 DEG C, and two sections of rubber master batch are plasticated After 1min, addition vulcanizing agent, promotor carry out third mixing, and melting temperature is 130 DEG C, and mixing time 6min, discharging obtains Finished composition, i.e., rubber composition provided by the invention.
Vulcanized rubber processed:
Obtained rubber composition is put into vulcanizing press and is vulcanized, curing temperature is 150 DEG C, sulfide stress is Cured rubber samples S2 is made in 20MPa, vulcanization time 50min.
Vulcanized rubber article S2 is tested for the property, the results are shown in Table 4.
Embodiment 3
The present embodiment is used to illustrate the preparation and vulcanized rubber of rubber composition provided by the invention.
Formula: solution polymerized butylbenzene 100, white carbon black 100, Si69 (silane coupling agent) 12, TDAE (softening agent) 8, zinc oxide 2, Stearic acid 1, sulphur 3 (vulcanizing agent), TBBS (promotor) 0.5,0.5,4020 (anti-aging agent) 6 of D (promotor), PEG4000 (softening Agent) 2.
Rubber composition preparation process:
White carbon black rubber master batch processed: solution polymerized butylbenzene is added in mixer, and setting revolving speed is 80rpm, and initial melting temperature is 80 DEG C, raw rubber plasticates the time as 0.5min;Butadiene rubber, white carbon black and Si69 are added in mixer and carry out the first mixing, is kneaded Temperature is 165 DEG C, mixing time 5min, and white carbon black rubber master batch is made;
It makes two sections of rubber master batch: carbon black, TDAE, zinc oxide, stearic acid, antioxidant 4020 and PEG4000 is added in mixer, It carries out second with white carbon black rubber master batch to be kneaded, mixing time 5min, dump temperature is 113 DEG C, and discharging and parking 4 hours is made two Section rubber master batch;
Finished composition processed: the revolving speed that mixer is arranged is 80rpm, and initial melting temperature is 40 DEG C, and two sections of rubber master batch are plasticated After 1min, addition vulcanizing agent, promotor carry out third mixing, and melting temperature is 120 DEG C, and mixing time 5min, discharging obtains Finished composition, i.e., rubber composition provided by the invention.
Vulcanized rubber processed:
Obtained rubber composition is put into vulcanizing press and is vulcanized, curing temperature is 170 DEG C, sulfide stress is Cured rubber samples S3 is made in 10MPa, vulcanization time 30min.
Vulcanized rubber article S3 is tested for the property, the results are shown in Table 4.
Embodiment 4
The present embodiment is used to illustrate the preparation and vulcanized rubber of rubber composition provided by the invention.
Formula: solution polymerized butylbenzene 100, white carbon black 100, Si69 (silane coupling agent) 12, TDAE (softening agent) 15, zinc oxide 5, Stearic acid 3, sulphur 3 (vulcanizing agent), TBBS (promotor) 2,2.2,4020 (anti-aging agent) 3 of D (promotor), PEG4000 (softening Agent) 5.
Rubber composition preparation process:
White carbon black rubber master batch processed: solution polymerized butylbenzene is added in mixer, and setting revolving speed is 80rpm, and initial melting temperature is 80 DEG C, raw rubber plasticates the time as 0.5min;White carbon black and Si69 are added in mixer and carry out the first mixing, melting temperature 170 DEG C, white carbon black rubber master batch is made in mixing time 9min;
It makes two sections of rubber master batch: TDAE, zinc oxide, stearic acid, antioxidant 4020 and PEG4000 is added in mixer, and it is white Carbon black rubber master batch carries out second and is kneaded, and mixing time 3min, dump temperature is 130 DEG C, and discharging and parking is made two sections of mothers for 4 hours Glue;
Finished composition processed: the revolving speed that mixer is arranged is 80rpm, and initial melting temperature is 40 DEG C, and two sections of rubber master batch are plasticated After 1min, addition vulcanizing agent, promotor carry out third mixing, and melting temperature is 116 DEG C, and mixing time 4min, discharging obtains Finished composition, i.e., rubber composition provided by the invention.
Vulcanized rubber processed:
Obtained rubber composition is put into vulcanizing press and is vulcanized, curing temperature is 160 DEG C, sulfide stress is Cured rubber samples S4 is made in 15MPa, vulcanization time 40min.
Vulcanized rubber article S4 is tested for the property, the results are shown in Table 4.
Comparative example 1
Formula: solution polymerized butylbenzene 30, butadiene rubber 70, white carbon black 40, carbon black 35, Si69 (silane coupling agent) 1, TDAE are (soft Agent) 4, zinc oxide 1.5, stearic acid 1, sulphur 1.5 (vulcanizing agent), TBBS (promotor) 3, D (promotor) 4,4020 it is (anti-old Agent) 0.5, PEG4000 (softening agent) 4.
According to the method for 1 rubber composition processed and vulcanized rubber of embodiment, vulcanized rubber article D1 is made.
Vulcanized rubber article D1 is tested for the property, the results are shown in Table 4.
Comparative example 2
Formula: solution polymerized butylbenzene 75, butadiene rubber 25, white carbon black 77, carbon black 8, Si69 (silane coupling agent) 8, TDAE (softening Agent) 8, zinc oxide 5, stearic acid 3, sulphur 1.7 (vulcanizing agent), TBBS (promotor) 1.7, D (promotor) 1.9,4020 it is (anti-old Agent) 2, PEG4000 (softening agent) 6.
Rubber composition preparation process:
Solution polymerized butylbenzene is added in mixer, setting revolving speed is 80rpm, and initial melting temperature is 80 DEG C, when raw rubber is plasticated Between be 0.5min;By butadiene rubber, white carbon black, Si69, carbon black, TDAE, zinc oxide, stearic acid, antioxidant 4020 and PEG4000 It is added in mixer and is kneaded, mixing time 10min, dump temperature is 175 DEG C, and discharging and parking 4 hours is made rubber master batch;
The revolving speed that mixer is arranged is 80rpm, and initial melting temperature is 40 DEG C, and rubber master batch is plasticated after 1min, addition vulcanization Agent, promotor are kneaded, and melting temperature is 115 DEG C, mixing time 4min, and discharging obtains finished composition, i.e., the present invention provides Rubber composition.
Vulcanized rubber processed:
Obtained rubber composition is put into vulcanizing press and is vulcanized, curing temperature is 160 DEG C, sulfide stress is Cured rubber samples D2 is made in 15MPa, vulcanization time 40min.
Vulcanized rubber article D2 is tested for the property, the results are shown in Table 4.
Comparative example 3
Formula: solution polymerized butylbenzene 75, butadiene rubber 25, white carbon black 77, carbon black 8, Si69 (silane coupling agent) 8, TDAE (softening Agent) 8, zinc oxide 5, stearic acid 3, sulphur 1.7 (vulcanizing agent), TBBS (promotor) 1.7, D (promotor) 1.9,4020 it is (anti-old Agent) 2, PEG4000 (softening agent) 6.
Rubber composition and vulcanized rubber are prepared according to the calendering process of the embodiment 1 of CN103881161A:
One section of mixing adhesive process:
Carbon black rubber master batch technique: it is added after solution polymerized butylbenzene is plasticated 60 seconds in the mixer that revolving speed is 45rpm and mentions floating weight, added Enter carbon black, floating weight cleaning is proposed after being kneaded 60 seconds, then be kneaded 60 seconds dumpings;The mixing time that pressurizes is 180 seconds, and dump temperature is 165℃;
White carbon black rubber master batch technique: it is added after solution polymerized butylbenzene is kneaded the second in the mixer that revolving speed is 45rpm and mentions floating weight, added Enter butadiene rubber, white carbon black, Si69, floating weight is mentioned after being kneaded 60 seconds, is kneaded 30 seconds and mentions floating weight, then be kneaded 60 seconds dumpings;Add Pressing mixing time is 210 seconds, and dump temperature is 160 DEG C;
Two-stage mixing process:
Carbon black rubber master batch and white carbon black rubber master batch are added in the mixer that revolving speed is 40rpm, is kneaded 80 seconds and mentions floating weight, is added Zinc oxide, stearic acid, antioxidant 4020, TDAE and PEG4000 are kneaded 70 seconds and clean, then be kneaded 30 seconds dumpings, when pressurization is kneaded Between be 180 seconds, dump temperature be 155 DEG C, obtain two-stage mixing rubber master batch.
Finished composition calendering process:
Two-stage mixing rubber master batch is added in the mixer that revolving speed is 20rpm, mixing mentions floating weight for 30 seconds and adds promotor, vulcanization Agent is kneaded 60 seconds and cleans, then is kneaded 30 seconds dumpings, and pressurization mixing time is 120 seconds, and dump temperature is 105 DEG C.Obtain whole refining Glue, i.e. rubber composition.
Vulcanized rubber processed:
Obtained rubber composition is put into vulcanizing press and is vulcanized, curing temperature is 160 DEG C, sulfide stress is Cured rubber samples D3 is made in 15MPa, vulcanization time 40min.
Vulcanized rubber article D3 is tested for the property, the results are shown in Table 4.
Table 4
As can be seen from the above results, using rubber composition preparation method provided by the invention, can make to prepare rubber Each component have better dispersibility in rubber composition, thus make further made of vulcanized rubber to can have raising strong Degree reduces heat, improves the excellent comprehensive performances such as anti-slippery.In contrast, using rubber group similarly to Example 2 Close composition formula but when using different rubber composition preparation methods (comparative example 2 and 3), the vulcanized rubber D2 further prepared and D3 is not so good as vulcanized rubber S2 in performance, and if breaking strength will be lower than S2, compression heating is higher than S2, and resilience is lower than S2, DIN mill Consumption is higher than S2;The dynamic mechanical of embodiment S2 shows lesser rolling resistance, preferable anti-slippery, pendant Buddhist nun's effect number It is better than comparative example D2, D3 according to the carbon black dispersion for also illustrating embodiment S2.
In addition, Rubber compositions same as Example 1 are used in comparative example 1, but the dosage that each component uses No longer the present invention claims in the composition of the rubber composition of restriction, the performance of the vulcanized rubber D1 equally obtained is not so good as S1.
Since preparation method provided by the invention can make the vulcanized rubber obtained have better performance, it is applied to automobile In tire tread, the durability of tire can be improved, improve the fuel economy of automobile, improve the safety of automobile.

Claims (19)

1. a kind of preparation method of rubber composition, this method comprises:
(1) solution polymerized butylbenzene, white carbon black, surface modifier and optional butadiene rubber are carried out first to be kneaded, white carbon black mother is made Glue;
(2) the white carbon black rubber master batch, activator, anti-aging agent, softening agent and optional carbon black are subjected to the second mixing and are made two sections Rubber master batch;
(3) two sections of rubber master batch, promotor and vulcanizing agent are subjected to third mixing and finished composition is made.
2. preparation method according to claim 1, wherein the inventory of each component in this method are as follows: 60-100 mass parts Solution polymerized butylbenzene, the butadiene rubber of 0-40 mass parts, the white carbon black of 50-100 mass parts, the carbon black of 0-20 mass parts, 2-12 matter Measure the surface modifier of part, the softening agent of 10-20 mass parts, the activator of 3-8 mass parts, 0.5-3 mass parts vulcanizing agent, 1- The promotor of 6 mass parts and the anti-aging agent of 1-6 mass parts.
3. preparation method according to claim 1 or 2, wherein the described first temperature being kneaded is 120-180 DEG C;It is described First time being kneaded was 2-10min.
4. preparation method according to claim 3, wherein the described first temperature being kneaded is 140-165 DEG C;Described first The time of mixing is 5-8min.
5. preparation method according to claim 1 or 2, wherein the described second temperature being kneaded is 80-140 DEG C;Described Two times being kneaded were 3-10min.
6. preparation method according to claim 5, wherein the described second temperature being kneaded is 100-120 DEG C;Described second The time of mixing is 4-6min.
7. preparation method according to claim 1 or 2, wherein the temperature that the third is kneaded is no more than 130 DEG C;It is described The time that third is kneaded is 4-6min.
8. preparation method according to claim 7, wherein the temperature that the third is kneaded is 110-130 DEG C.
9. preparation method according to claim 1 or 2, wherein white carbon black is silica;Table is compared in the CTAB absorption of carbon black Area is 10-300m2/g。
10. preparation method according to claim 9, wherein the N2 adsorption specific surface area of white carbon black is 10-200m2/g。
11. preparation method according to claim 1 or 2, wherein the surface modifier is general formula (RO)3SiCH2CH2CH2The organo silane coupling agent that-X is indicated, RO is hydrolyzable groups;X is organo-functional group.
12. preparation method according to claim 11, wherein RO is methoxyl group, ethyoxyl or acetoxyl group;X be amino, Methacryloxy, epoxy group or general formula Sn(CH2)3Si(OR)3The group of expression, n are the integer of 2-4.
13. preparation method according to claim 12, wherein the organo silane coupling agent is double-[γ-(triethoxy Silicon) propyl]-tetrasulfide.
14. preparation method according to claim 1 or 2, wherein the anti-aging agent is amines antioxidants, quinolines are anti-old At least one of agent, benzimidazole anti-aging agent and physical protection agent.
15. preparation method according to claim 1 or 2, wherein the softening agent be aromatic naphtha, paraffin oil, naphthenic oil, At least one of Petropols and polyethylene glycol.
16. preparation method according to claim 1 or 2, wherein the activator is the group of metal oxide and fatty acid Close object or fatty acid metal soap salt;The metal oxide is zinc oxide and/or magnesia, the fatty acid metal soap salt For zinc stearate and/or zinc borate.
17. preparation method according to claim 1 or 2, wherein the promotor is sulfenamide type accelerators, thiazole At least one of class promotor, thuriam acceserator and guanidines, the vulcanizing agent be Sulfur, insoluble sulfuy, At least one of oil-filled Sulfur and sulphur-donor.
18. a kind of rubber composition of the preparation of the method as described in any one of claim 1-17.
19. a kind of vulcanized rubber, which is made by the way that rubber composition described in claim 18 is carried out vulcanization, institute The temperature for stating vulcanization is 150-170 DEG C, and the pressure of the vulcanization is 10-20MPa, and the time of the vulcanization is 30-50 minutes.
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