CN106608990A - Rubber composition and preparation method thereof, and vulcanized rubber - Google Patents
Rubber composition and preparation method thereof, and vulcanized rubber Download PDFInfo
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Abstract
The present invention discloses a rubber composition and a preparation method thereof, and a vulcanized rubber. The rubber composition preparation method comprises: (1) carrying out first mixing on solution polymerized styrene-butadiene rubber, white carbon black, a surface modifier and an optional cis-polybutadiene rubber to prepare white carbon black rubber master batch; (2) carrying out second mixing on the white carbon black rubber master batch, an activator, an anti-aging agent, a softening agent and an optional carbon black to prepare a second-stage rubber master batch; and (3) carrying out third mixing on the second-stage rubber master batch, an accelerator and a vulcanizing agent to obtain the final mixed rubber. According to the present invention, in the processing process, the effect of the surface modifier can be well provided, the complete interaction between the white carbon black and the polymer can be easily achieved, the strength of the vulcanized rubber prepared through the vulcanization can be improved, the heat generation of the vulcanized rubber can be reduced, and the wet skid resistance of the vulcanized rubber can be improved.
Description
Technical field
The present invention relates to rubber composition prepared by a kind of preparation method of rubber composition and the method,
With further vulcanized the vulcanite that obtains by the rubber composition.
Background technology
Impact of the dynamic lag loss performance of rubber compounding to tyre performance is particularly important, and hysteresis loss makes
Sizing material energy expenditure during dynamic deformation increases, and heat increases, flexibility decrease, and rolling resistance rises.
Heat also results in the intensity of rubber and wearability declines, and causes the Random early Detection of tire, heat can also increase
Plus the rolling resistance of tire, increase the discharge capacity of fuel consumption and carbon dioxide.
CN102382338A discloses a kind of Isoprene rubber blend, including isoprene rubber, anti-form-1,4-
Polyisoprene, reinforcer, situ-formed graft modified additive, compound rubber and the first additive.
CN103881161A discloses a kind of rubber composition containing trans-polyisoprene, and rubber is total
Measure in terms of 100 mass parts, wherein the total amount of synthesis of trans polyisoprene and synthesizing cis polyisoprene
For 5-60 mass parts, natural rubber 40-95 mass parts, white carbon 5-90 mass parts, white carbon black 5-990
Mass parts；Rubber master batch technique includes：By synthesis of trans polyisoprene or with synthesizing cis polyisoprene
Rubber composition is white carbon wood glue with white carbon, coupling agent mixing；It is with white carbon black mixing by natural rubber
Carbon black rubber master batch；Finished composition technique：By the carbon black rubber master batch, white carbon wood glue, age resistor, activating agent,
Rubber composition is made in accelerator, vulcanizing agent mixing.
CN103703072A discloses a kind of rubber composition for tire tread, its contain solution polymerized butadiene styrene rubber,
White carbon black, silicon dioxide and Polyethylene Glycol, solution polymerized butadiene styrene rubber described in the rubber constituent of 100 mass %
Content is more than 60 mass %, relative to the mass parts of the rubber constituent 100, the content of the white carbon black
Below 10 mass parts, the content of the silicon dioxide is more than 50 mass parts, the Polyethylene Glycol
Content is 0.1-3.5 mass parts.
CN103087365A discloses a kind of building rubber compound for anti-slippery wear resistance balance tire tread
Thing, the rubber composition contains diene elastomer, inorganic reinforced filling, coupling agent and plasticizer.
But the rubber that prior art is provided still can not meet the intensity of tire tread glue needs, reduce life
Heat, the requirement for improving wet and slippery performance, it is desirable to provide a kind of rubber of performance improvement.
The content of the invention
The invention aims to solve how to improve the intensity of the rubber for tire tread, reduce life
Heat, the problem for improving anti-slippery, there is provided a kind of rubber composition and preparation method thereof and vulcanite.
To achieve these goals, the present invention provides a kind of preparation method of rubber composition, the method bag
Include：(1) solution polymerized butylbenzene, white carbon, surface modifier and optional butadiene rubber are carried out into the first mixing,
Make white carbon rubber master batch；(2) by the white carbon rubber master batch, activator, age resistor, softening agent and optionally
White carbon black carry out the second mixing and make two-stage nitration rubber master batch；(3) by the two-stage nitration rubber master batch, accelerator and vulcanizing agent
Carry out the 3rd mixing and make finished composition.
Present invention also offers rubber composition prepared by a kind of method provided by the present invention.
Present invention also offers a kind of vulcanite, the vulcanite is by the rubber group that provides the present invention
Compound carries out sulfuration and is obtained, the temperature of the sulfuration is 150-170 DEG C, and the sulfuration will be
10-20MPa, the time of the sulfuration is 30-50 minutes.
The rubber composition that the present invention is provided is obtained by a kind of new compounding process, first will be molten in the method
Poly- butylbenzene, butadiene rubber, white carbon and its surface modifier are prepared by mixing into white carbon according to portfolio ratio
Rubber master batch, then again in white carbon rubber master batch according to addition white carbon black, activator, age resistor, softening agent mixing
Two-stage nitration rubber master batch is prepared, finally adds vulcanizing agent, accelerator to be prepared into according to portfolio ratio in two-stage nitration rubber master batch
Finished composition.According to each component of the composition rubber composition for so sequentially adding selection, have an advantage in that：
In the processing technique, can preferably play the effect of surface modifier, be conducive to white carbon fully with it is poly-
Compound interacts, and can preferably improve the intensity of the obtained vulcanite of further sulfuration, reduces sulfur
Change the heat of rubber, improve the anti-slippery of vulcanizate compound.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the present invention is described in detail below.It should be appreciated that this place is retouched
The specific embodiment stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The present invention provides a kind of preparation method of rubber composition, and the method includes：(1) by solution polymerized butylbenzene,
White carbon, surface modifier and optional butadiene rubber carry out the first mixing, make white carbon rubber master batch；(2)
The white carbon rubber master batch, activator, age resistor, softening agent and optional white carbon black are carried out into the second mixing system
Into two-stage nitration rubber master batch；(3) the two-stage nitration rubber master batch, accelerator and vulcanizing agent are carried out into the 3rd mixing and makes whole refining
Glue.
, according to the invention it is preferred in the case of, the inventory of each component is in the method：60-100 mass parts
Solution polymerized butylbenzene, the butadiene rubber of 0-40 mass parts, the white carbon of 50-100 mass parts, 0-20 mass parts
White carbon black, the surface modifier of 2-12 mass parts, the softening agent of 10-20 mass parts, the work of 3-8 mass parts
The age resistor of agent, the vulcanizing agent of 0.5-3 mass parts, the accelerator of 1-6 mass parts and 1-6 mass parts.
, according to the invention it is preferred in the case of, the temperature of first mixing is 120-180 DEG C, preferred institute
The temperature for stating the first mixing is 140-165 DEG C.
, according to the invention it is preferred in the case of, the time of first mixing is 2-10min, preferably described
The time of the first mixing is 5-8min.
, according to the invention it is preferred in the case of, the temperature of second mixing is 80-140 DEG C, preferably described
The temperature of the second mixing is 100-120 DEG C.
, according to the invention it is preferred in the case of, the time of second mixing is 3-10min, preferably described
The time of the second mixing is 4-6min.
, according to the invention it is preferred in the case of, the temperature of the 3rd mixing is less than 130 DEG C, preferably
110-130℃；The time of the 3rd mixing is 4-6min.
, according to the invention it is preferred in the case of, white carbon is silicon dioxide, the N2 adsorption ratio of preferred white carbon
Surface area is 10-200m2/g；The CTAB adsorption specific surface areas of white carbon black are 10-300m2/g。
Preferably, white carbon is preferably prepared by the sedimentation method.White carbon and white carbon black can pass through commercially available,
Such as white carbon is 115GR and 165GR (French Rhodia).White carbon black is N330 and N220 (east
Qi Deli Chemical Industry Science Co., Ltd of tabernaemontanus bulrush city).
, according to the invention it is preferred in the case of, the surface modifier is formula (RO)3SiCH2CH2CH2-X
The organo silane coupling agent of expression, RO is hydrolyzable groups, preferably methoxyl group, ethyoxyl or acetyl
Epoxide；X is organo-functional group, preferably amino, methacryloxy, epoxy radicals, or S
Formula Sn(CH2)3Si(OR)3The group of expression, n is the integer of 2-4；It is preferred that the organosilan is coupled
Agent is double-[γ-(triethoxysilicane) propyl group]-tetrasulfide (Si69).
, according to the invention it is preferred in the case of, the age resistor be amines antioxidants, quinoline type antioxidant,
At least one in benzimidazole age resistor and physical protection agent.Can be with commercially available, such as age resistor
4020。
, according to the invention it is preferred in the case of, the softening agent is aromatic naphtha, paraffin oil, naphthenic oil, stone
At least one in oleoresin and Polyethylene Glycol.Wherein, the weight average molecular weight of Polyethylene Glycol is in 3000-5000
In the range of so that composite has preferable processing characteristics and physical and mechanical propertiess.Can be obtained with commercially available
, such as aromatic naphtha TDAE V500, Polyethylene Glycol PEG4000.
, according to the invention it is preferred in the case of, the activator is the compositionss of metal-oxide and fatty acid,
Or fatty acid metal soap salt；The metal-oxide is Zinc Oxide and/or magnesium oxide, and the fatty acid is golden
Category soap salt is zinc stearate and/or Firebrake ZB.
, according to the invention it is preferred in the case of, the accelerator is sulfenamide type accelerators, thiazoless rush
At least one entered in agent, thuriam acceserator and guanidines.Can be with commercially available, such as
N tert butyl benzothiazole 2 sulfenamide (TBBS), diphenylguanidine (D)
, according to the invention it is preferred in the case of, the vulcanizing agent is sulfur, insoluble sulfuy, oil-filled sulfur
With at least one in sulphur-donor.Can be for example common sulfur S, oil-filled insoluble with commercially available
Sulfur IS.
Present invention also offers rubber composition prepared by a kind of method provided by the present invention.
Present invention also offers a kind of vulcanite, the vulcanite is by the rubber group that provides the present invention
Compound carries out sulfuration and is obtained, the temperature of the sulfuration is 150-170 DEG C, and the sulfuration will be
10-20MPa, the time of the sulfuration is 30-50 minutes.
Pressure used is gauge in the present invention.
Hereinafter will be described the present invention by embodiment.
The Preparation equipment of rubber composition and rubber is shown in Table 1 used in following examples and comparative example.
Table 1
| Sequence number | Device name | Model | Manufacturer |
| 1 | Banbury | 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 rubber machinery plant of Shanghai first |
The test instrunment of rubber is shown in Table 2 obtained in embodiment and comparative example, and test condition is shown in Table 3.
Table 2
Table 3
The chemical reagent that embodiment and comparative example are used is commercially available product, specific as follows：
Solution polymerized butylbenzene：2535E, Yanshan Petrochemical product (wherein, styrene-content be 23 mass %, second
Amount vinyl content is 63 mass %, is 27 mass % containing oil component；Mooney viscosity 60)；
Butadiene rubber：BR9000, Yanshan Petrochemical product (wherein, cis-content is 97.8 mass %)；
White carbon：165GR, French Rhodia, N2 adsorption specific surface area is 170m2/g；
White carbon black：N330, Dongguan City Qi Deli Chemical Industry Science Co., Ltd, CTAB adsorption specific surface areas are
75m2/g；
Surface modifier：Double-[γ-(triethoxysilicane) propyl group]-tetrasulfide (Si69), Nanjing dawn chemical industry
Company limited；
Softening agent：Environment-friendly aromatic oil TDAE V500, Xin Dayang (Ningbo) company limited；
Activator：Zinc Oxide, stearic acid, Weifang Hengfeng Chemical Co., Ltd.；
Antioxidant 4020：N- (1,3- dimethylbutyl)-N '-diphenyl-para-phenylene diamine, the holy chemistry science and technology difficult to understand in Jiangsu
Company limited；
Vulcanizing agent：Sulfur, Weifang Zhong Heng Chemical Co., Ltd.s；
Accelerator：N tert butyl benzothiazole 2 sulfenamide (TBBS), diphenylguanidine (D), Shanghai
Yong Yan Chemical Industry Science Co., Ltd；
PEG4000：Pacify petrochemical plant in Huai-Hai.
Amounts of components in following examples and comparative example is weight portion.
Embodiment 1
The present embodiment is used for the preparation of the rubber composition for illustrating present invention offer and vulcanite.
Formula (weight portion, similarly hereinafter)：Solution polymerized butylbenzene 60, butadiene rubber 40, white carbon 50, white carbon black
20th, Si69 (silane couplers) 2, TDAE (softening agent) 17, Zinc Oxide 5 (activator), Hard Fat
Sour 1 (activator), sulfur 0.5 (vulcanizing agent), TBBS (accelerator) 4, D (accelerator) 2,
4020 (age resistor) 1, PEG4000 (softening agent) 3.
Rubber composition preparation process：
White carbon rubber master batch processed：Solution polymerized butylbenzene is added in banbury, setting rotating speed is 80rpm, it is initial mixed
Refining temperature is 80 DEG C, and rubber plasticates the time for 0.5min；Butadiene rubber, white carbon and Si69 are added
The first mixing is carried out in banbury, melting temperature is 150 DEG C, and mixing time is 7min, and Linesless charcoal is obtained
Black rubber master batch；
Two-stage nitration rubber master batch processed：By white carbon black, TDAE, Zinc Oxide, stearic acid, antioxidant 4020 and PEG4000
Add in banbury, with white carbon rubber master batch the second mixing is carried out, mixing time is 6min, dump temperature
For 120 DEG C, discharge and park and make two-stage nitration rubber master batch in 4 hours；
Finished composition processed：The rotating speed for arranging banbury is 80rpm, and initial melting temperature is 40 DEG C, by two-stage nitration
Rubber master batch is plasticated after 1min, and addition vulcanizing agent, accelerator carry out the 3rd mixing, and 110 DEG C of melting temperature is mixed
The refining time is 4min, and discharging obtains finished composition, i.e., the rubber composition that the present invention is provided.
Vulcanite processed：
The rubber composition for obtaining is put in vulcanizing press and is vulcanized, curing temperature be 160 DEG C,
Sulfide stress is 15MPa, cure time is 40min, and cured rubber samples S1 is obtained.
Vulcanized rubber article S1 is carried out into performance test, 4 are the results are shown in Table.
Embodiment 2
The present embodiment is used for the preparation of the rubber composition for illustrating present invention offer and vulcanite.
Formula：Solution polymerized butylbenzene 75, butadiene rubber 25, white carbon 77, white carbon black 8, Si69 (silane idol
Connection agent) 8, TDAE (softening agent) 8, Zinc Oxide 5, stearic acid 3, sulfur 1.7 (vulcanizing agent), TBBS
(age resistor) 2, PEG4000 (softening agent) 6 of (accelerator) 1.7, D (accelerator) 1.9,4020.
Rubber composition preparation process：
White carbon rubber master batch processed：Solution polymerized butylbenzene is added in banbury, setting rotating speed is 80rpm, it is initial mixed
Refining temperature is 80 DEG C, and rubber plasticates the time for 0.5min；Butadiene rubber, white carbon and Si69 are added
The first mixing is carried out in banbury, melting temperature is 140 DEG C, and mixing time is 8min, and Linesless charcoal is obtained
Black rubber master batch；
Two-stage nitration rubber master batch processed：By white carbon black, TDAE, Zinc Oxide, stearic acid, antioxidant 4020 and PEG4000
Add in banbury, with white carbon rubber master batch the second mixing is carried out, mixing time is 4min, dump temperature
For 100 DEG C, discharge and park and make two-stage nitration rubber master batch in 4 hours；
Finished composition processed：The rotating speed for arranging banbury is 80rpm, and initial melting temperature is 40 DEG C, by two-stage nitration
Rubber master batch is plasticated after 1min, and addition vulcanizing agent, accelerator carry out the 3rd mixing, and melting temperature is 130 DEG C,
Mixing time is 6min, and discharging obtains finished composition, i.e., the rubber composition that the present invention is provided.
Vulcanite processed：
The rubber composition for obtaining is put in vulcanizing press and is vulcanized, curing temperature be 150 DEG C,
Sulfide stress is 20MPa, cure time is 50min, and cured rubber samples S2 is obtained.
Vulcanized rubber article S2 is carried out into performance test, 4 are the results are shown in Table.
Embodiment 3
The present embodiment is used for the preparation of the rubber composition for illustrating present invention offer and vulcanite.
Formula：Solution polymerized butylbenzene 100, white carbon 100, Si69 (silane coupler) 12, TDAE are (soft
Agent) 8, Zinc Oxide 2, stearic acid 1, sulfur 3 (vulcanizing agent), TBBS (accelerator) 0.5, D
(accelerator) 0.5,4020 (age resistor) 6, PEG4000 (softening agent) 2.
Rubber composition preparation process：
White carbon rubber master batch processed：Solution polymerized butylbenzene is added in banbury, setting rotating speed is 80rpm, it is initial mixed
Refining temperature is 80 DEG C, and rubber plasticates the time for 0.5min；Butadiene rubber, white carbon and Si69 are added
The first mixing is carried out in banbury, melting temperature is 165 DEG C, and mixing time is 5min, and Linesless charcoal is obtained
Black rubber master batch；
Two-stage nitration rubber master batch processed：By white carbon black, TDAE, Zinc Oxide, stearic acid, antioxidant 4020 and PEG4000
Add in banbury, with white carbon rubber master batch the second mixing is carried out, mixing time is 5min, dump temperature
For 113 DEG C, discharge and park and make two-stage nitration rubber master batch in 4 hours；
Finished composition processed：The rotating speed for arranging banbury is 80rpm, and initial melting temperature is 40 DEG C, by two-stage nitration
Rubber master batch is plasticated after 1min, and addition vulcanizing agent, accelerator carry out the 3rd mixing, and melting temperature is 120 DEG C,
Mixing time is 5min, and discharging obtains finished composition, i.e., the rubber composition that the present invention is provided.
Vulcanite processed：
The rubber composition for obtaining is put in vulcanizing press and is vulcanized, curing temperature be 170 DEG C,
Sulfide stress is 10MPa, cure time is 30min, and cured rubber samples S3 is obtained.
Vulcanized rubber article S3 is carried out into performance test, 4 are the results are shown in Table.
Embodiment 4
The present embodiment is used for the preparation of the rubber composition for illustrating present invention offer and vulcanite.
Formula：Solution polymerized butylbenzene 100, white carbon 100, Si69 (silane coupler) 12, TDAE are (soft
Agent) 15, Zinc Oxide 5, stearic acid 3, sulfur 3 (vulcanizing agent), TBBS (accelerator) 2, D
(accelerator) 2.2,4020 (age resistor) 3, PEG4000 (softening agent) 5.
Rubber composition preparation process：
White carbon rubber master batch processed：Solution polymerized butylbenzene is added in banbury, setting rotating speed is 80rpm, it is initial mixed
Refining temperature is 80 DEG C, and rubber plasticates the time for 0.5min；White carbon and Si69 are added to enter in banbury
Row first is kneaded, and melting temperature is 170 DEG C, and mixing time is 9min, and white carbon rubber master batch is obtained；
Two-stage nitration rubber master batch processed：TDAE, Zinc Oxide, stearic acid, antioxidant 4020 and PEG4000 are added
Enter in banbury, with white carbon rubber master batch the second mixing is carried out, mixing time is 3min, and dump temperature is
130 DEG C, discharge and park and make two-stage nitration rubber master batch in 4 hours；
Finished composition processed：The rotating speed for arranging banbury is 80rpm, and initial melting temperature is 40 DEG C, by two-stage nitration
Rubber master batch is plasticated after 1min, and addition vulcanizing agent, accelerator carry out the 3rd mixing, and melting temperature is 116 DEG C,
Mixing time is 4min, and discharging obtains finished composition, i.e., the rubber composition that the present invention is provided.
Vulcanite processed：
The rubber composition for obtaining is put in vulcanizing press and is vulcanized, curing temperature be 160 DEG C,
Sulfide stress is 15MPa, cure time is 40min, and cured rubber samples S4 is obtained.
Vulcanized rubber article S4 is carried out into performance test, 4 are the results are shown in Table.
Comparative example 1
Formula：Solution polymerized butylbenzene 30, butadiene rubber 70, white carbon 40, white carbon black 35, Si69 (silane idol
Connection agent) 1, TDAE (softening agent) 4, Zinc Oxide 1.5, stearic acid 1, sulfur 1.5 (vulcanizing agent),
TBBS (accelerator) 3, D (accelerator) 4,4020 (age resistor) 0.5, PEG4000 (softens
Agent) 4.
According to the rubber composition processed of embodiment 1 and the method for vulcanite, vulcanized rubber article D1 is obtained.
Vulcanized rubber article D1 is carried out into performance test, 4 are the results are shown in Table.
Comparative example 2
Formula：Solution polymerized butylbenzene 75, butadiene rubber 25, white carbon 77, white carbon black 8, Si69 (silane idol
Connection agent) 8, TDAE (softening agent) 8, Zinc Oxide 5, stearic acid 3, sulfur 1.7 (vulcanizing agent), TBBS
(age resistor) 2, PEG4000 (softening agent) 6 of (accelerator) 1.7, D (accelerator) 1.9,4020.
Rubber composition preparation process：
Solution polymerized butylbenzene is added in banbury, setting rotating speed is 80rpm, initial melting temperature is 80 DEG C,
Rubber plasticates the time for 0.5min；By butadiene rubber, white carbon, Si69, white carbon black, TDAE, oxidation
Zinc, stearic acid, antioxidant 4020 and PEG4000 are added and kneaded in banbury, and mixing time is
10min, dump temperature is 175 DEG C, discharges and parks and makes rubber master batch in 4 hours；
The rotating speed for arranging banbury is 80rpm, and initial melting temperature is 40 DEG C, and rubber master batch is plasticated 1min
Afterwards, add vulcanizing agent, accelerator to be kneaded, melting temperature is 115 DEG C, and mixing time is 4min,
Discharging obtains finished composition, i.e., the rubber composition that the present invention is provided.
Vulcanite processed：
The rubber composition for obtaining is put in vulcanizing press and is vulcanized, curing temperature be 160 DEG C,
Sulfide stress is 15MPa, cure time is 40min, and cured rubber samples D2 is obtained.
Vulcanized rubber article D2 is carried out into performance test, 4 are the results are shown in Table.
Comparative example 3
Formula：Solution polymerized butylbenzene 75, butadiene rubber 25, white carbon 77, white carbon black 8, Si69 (silane idol
Connection agent) 8, TDAE (softening agent) 8, Zinc Oxide 5, stearic acid 3, sulfur 1.7 (vulcanizing agent), TBBS
(age resistor) 2, PEG4000 (softening agent) 6 of (accelerator) 1.7, D (accelerator) 1.9,4020.
Calendering process according to the embodiment 1 of CN103881161A prepares rubber composition and sulfuration rubber
Glue：
One section of mixing adhesive process：
Carbon black rubber master batch technique：After adding solution polymerized butylbenzene to plasticate 60 seconds in rotating speed is for the banbury of 45rpm
Floating weight is carried, white carbon black is added, mixing proposes floating weight cleaning after 60 seconds, then kneads 60 seconds dumpings；Pressurization
Mixing time is 180 seconds, and dump temperature is 165 DEG C；
White carbon rubber master batch technique：Carry after the solution polymerized butylbenzene mixing second is added in rotating speed is for the banbury of 45rpm
Floating weight, adds butadiene rubber, white carbon, Si69, mixing that floating weight is carried after 60 seconds, kneads 30 seconds
Floating weight is carried, then kneads 60 seconds dumpings；Pressurization mixing time is 210 seconds, and dump temperature is 160 DEG C；
Two-stage mixing process：
Carbon black rubber master batch and white carbon rubber master batch, mixing is added to carry for 80 seconds in rotating speed is for the banbury of 40rpm
Floating weight, adds Zinc Oxide, stearic acid, antioxidant 4020, TDAE and PEG4000, mixing 70
Second cleans, then kneads 30 seconds dumpings, and pressurization mixing time is 180 seconds, and dump temperature is 155 DEG C, is obtained
To two-stage mixing rubber master batch.
Finished composition calendering process：
Two-stage mixing rubber master batch, mixing is added to carry floating weight within 30 seconds and add in rotating speed is for the banbury of 20rpm
Accelerator, vulcanizing agent, knead 60 seconds and clean, then knead 30 seconds dumpings, and pressurization mixing time is 120
Second, dump temperature is 105 DEG C.Obtain finished composition, i.e. rubber composition.
Vulcanite processed：
The rubber composition for obtaining is put in vulcanizing press and is vulcanized, curing temperature be 160 DEG C,
Sulfide stress is 15MPa, cure time is 40min, and cured rubber samples D3 is obtained.
Vulcanized rubber article D3 is carried out into performance test, 4 are the results are shown in Table.
Table 4
As can be seen from the above results, the rubber composition preparation method for being provided using the present invention, can make
Prepare each component of rubber has more preferable dispersibility in rubber composition, so that sulfur made by further
Changing rubber can have raising intensity, reduce heat, improve the excellent combination properties such as anti-slippery.Phase
Than under, using building rubber compound composition formula similarly to Example 2 but using different rubber compositions
During preparation method (comparative example 2 and 3), the vulcanite D2 and D3 for further preparing in performance not
As vulcanite S2, such as breaking strength will be less than S2, it is higher than S2 that compression heats up, and resilience is less than S2,
DIN abrasion are higher than S2；The dynamic mechanical of embodiment S2 shows less rolling resistance, preferably
Anti-slippery, pendant Buddhist nun effect data also illustrate the carbon black dispersion of embodiment S2 be better than comparative example D2,
D3。
In addition, Rubber compositions same as Example 1 used in comparative example 1, but each component
In the composition of the rubber composition that the dosage for using no longer application claims are limited, the same sulfuration rubber for obtaining
The performance of glue D1 is not so good as S1.
Because the preparation method that the present invention is provided can make the vulcanite of acquisition have better performance, should
In for automobile tire tyre surface, the durability of tire can be improved, improve the fuel economy of automobile, be improved
The safety of automobile.
Claims (13)
1. a kind of preparation method of rubber composition, the method includes：
(1) solution polymerized butylbenzene, white carbon, surface modifier and optional butadiene rubber are carried out into first to mix
Refining, makes white carbon rubber master batch；
(2) the white carbon rubber master batch, activator, age resistor, softening agent and optional white carbon black are carried out
Two-stage nitration rubber master batch is made in second mixing；
(3) the two-stage nitration rubber master batch, accelerator and vulcanizing agent are carried out into the 3rd mixing and makes finished composition.
2. preparation method according to claim 1, wherein, the inventory of each component in the method
For：The solution polymerized butylbenzene of 60-100 mass parts, the butadiene rubber of 0-40 mass parts, 50-100 mass parts it is white
White carbon black, the white carbon black of 0-20 mass parts, the surface modifier of 2-12 mass parts, the softening of 10-20 mass parts
Agent, the activator of 3-8 mass parts, the vulcanizing agent of 0.5-3 mass parts, the accelerator of 1-6 mass parts and 1-6
The age resistor of mass parts.
3. preparation method according to claim 1 and 2, wherein, the temperature of first mixing
For 120-180 DEG C, the temperature of preferably described first mixing is 140-165 DEG C；The time of first mixing
For 2-10min, the time of preferably described first mixing is 5-8min.
4. preparation method according to claim 1 and 2, wherein, the temperature of second mixing
For 80-140 DEG C, the temperature of preferably described second mixing is 100-120 DEG C；The time of second mixing
For 3-10min, the time of preferably described second mixing is 4-6min.
5. preparation method according to claim 1 and 2, wherein, the temperature of the 3rd mixing
Less than 130 DEG C, preferably 110-130 DEG C；The time of the 3rd mixing is 4-6min.
6. preparation method according to claim 1 and 2, wherein, white carbon is silicon dioxide,
It is preferred that the N2 adsorption specific surface area of white carbon is 10-200m2/g；The CTAB adsorption specific surface areas of white carbon black are
10-300m2/g。
7. preparation method according to claim 1 and 2, wherein, the surface modifier is logical
Formula (RO)3SiCH2CH2CH2The organo silane coupling agent that-X is represented, RO is hydrolyzable groups, preferably
Methoxyl group, ethyoxyl or acetoxyl group；X is organo-functional group, preferably amino, methacryl
Epoxide, epoxy radicals, or formula Sn(CH2)3Si(OR)3The group of expression, n is the integer of 2-4；It is excellent
The organo silane coupling agent is selected for double-[γ-(triethoxysilicane) propyl group]-tetrasulfide.
8. preparation method according to claim 1 and 2, wherein, the age resistor is anti-for amine
At least one in old agent, quinoline type antioxidant, benzimidazole age resistor and physical protection agent.
9. preparation method according to claim 1 and 2, wherein, the softening agent be aromatic naphtha,
At least one in paraffin oil, naphthenic oil, Petropols and Polyethylene Glycol.
10. preparation method according to claim 1 and 2, wherein, the activator is metal oxygen
The compositionss of compound and fatty acid, or fatty acid metal soap salt；The metal-oxide be Zinc Oxide and
/ or magnesium oxide, the fatty acid metal soap salt is zinc stearate and/or Firebrake ZB.
11. preparation methoies according to claim 1 and 2, wherein, the accelerator is time sulphonyl
At least one in amine type accelerator, thiazole accelerator, thuriam acceserator and guanidines,
The vulcanizing agent is at least one in sulfur, insoluble sulfuy, oil-filled sulfur and sulphur-donor.
Rubber composition prepared by a kind of 12. methods by described in any one in claim 1-11.
A kind of 13. vulcanites, the vulcanite is by by the rubber composition described in claim 12
Carry out sulfuration to be obtained, the temperature of the sulfuration is 150-170 DEG C, the sulfuration will be 10-20MPa,
The time of the sulfuration is 30-50 minutes.
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