CN108178853A - Modified host rubber and preparation method thereof and rubber composition and vulcanization rubber and its preparation method and application - Google Patents
Modified host rubber and preparation method thereof and rubber composition and vulcanization rubber and its preparation method and application Download PDFInfo
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- CN108178853A CN108178853A CN201611122718.3A CN201611122718A CN108178853A CN 108178853 A CN108178853 A CN 108178853A CN 201611122718 A CN201611122718 A CN 201611122718A CN 108178853 A CN108178853 A CN 108178853A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0016—Compositions of the tread
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/548—Silicon-containing compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/06—Copolymers with styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
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Abstract
The present invention relates to rubber materials, disclose a kind of modified host rubber and preparation method thereof and rubber composition and vulcanization rubber and its preparation method and application.The method for preparing modified host rubber includes：Main rubber is kneaded in advance with silane coupling agent or with silane coupling agent and reinforcing agent, the temperature of the pre- mixing is 130 200 DEG C, and the time being kneaded in advance is 1 20min.There is higher-strength, higher abrasion resistance, while there is relatively low rolling resistance and high wet-sliding resistant performance by the vulcanization rubber that the modified host rubber is prepared, and the vulcanization rubber can be used in preparing green tire tread rubber.
Description
Technical field
The present invention relates to rubber materials, and in particular, to a kind of modified host rubber, a kind of modified host rubber for preparing
Method and the modified host rubber being prepared by this method, a kind of vulcanization rubber, a kind of prepare sulphur at a kind of rubber composition
Change the method for rubber and by the vulcanization rubber that this method is prepared and application of the vulcanization rubber as tire tread material.
Background technology
With popularizing for automobile, the dosage of oil and the discharge capacity of carbon dioxide are higher and higher, and consequently lead to stone
The in short supply and global climate of oily resource warms.Therefore, the auto industry revolution of a reduction oil consumption has directly caused automobile system
Make requirement of the quotient to reduction tire drag.
In the resistance that automobile is hindered to advance, rolling resistance accounts for 18-30%, and rolling resistance energy consumption accounts for about fuel consumption
14.4%, it means that rolling resistance reduces by 30%, then can fuel-economizing 4.5-6%.While rolling resistance is reduced, tire should also
Could meet the needs of commercial Application with preferable wet-sliding resistant performance.
Under normal conditions, the fissipation factor that anti-slippery and rolling resistance can respectively by vulcanization rubber in 0 DEG C and 60 DEG C
Tan δ values characterize.Tan δ values at 0 DEG C are bigger, and anti-slippery is better；Tan δ values at 60 DEG C are smaller, and rolling resistance is lower.
Sizing material is made to obtain good comprehensive performance, tan δ values when should increase 0 DEG C as possible, and tan δ values when reducing 60 DEG C as possible.
CN101962423A passes through the conjugated-diolefin/uni-vinyl-arene copolymer rubber to being prepared by polymerisation in solution
Glue carry out the study found that using asymmetrical ether and anion surfactant compounding structure regulation system, can prepare and provide
There are relatively low polystyrene micro-blocks content, the high wet-sliding resistant of medium vinyl content and the terpolymer rubber of low-rolling-resistance.
Tan δ values during 0 DEG C of the terpolymer are 0.25-0.96, and tan δ values at 60 DEG C are less than 0.12.CN101319064A passes through
Silane coupling agent sealing end is added in solution polymerized butadiene styrene rubber polymerization latter stage, solution polymerized butadiene styrene rubber glue of the end with siloxane group is made
Liquid is sufficiently stirred after adding in white carbon black powder in glue, and molecular end and the secured key of filler are obtained after co-agglomeration, heat treatment
The composite material connect.The nanocomposite has excellent filler-rubber interactions and interface cohesion, shows high moisture-resistant
Slip, low-rolling-resistance and excellent composition machine performance.The rubber composition that CN101113217A is provided is included not less than 10 weight
Part have not less than 22nm average grain diameters silica and not less than 5 parts by weight have be less than 22nm be averaged primary grain
The silica of diameter, two of which silica total amount are 15-150 parts by weight.The tread-rubber composite material obtained can be with
The wet-sliding resistant performance, wear hardness and manipulation stability of tire are effectively improved, while reduces the rolling resistance of tire.
Methods of the CN103159998A by adding nanometer silicon carbide powder, can reduce the rolling resistance of tire, while not influence
The wear-resisting property of tyre surface, especially by the wet-sliding resistant performance that nm-class silicon carbide material is used to substantially increase tire.At present, generation
Some major companies also gradually release that rolling resistance is relatively low, the preferable rubber tyre of wet-sliding resistant performance, and titled with " green is taken turns in boundary
The good name of tire ".
However, the filling system of " green tire " is based on white carbon, since white carbon has higher polarity, it is difficult to
It is uniformly dispersed in rubber matrix, the quality of the dispersing uniformity of white carbon directly affects the dynamic property of product, intensity, wearability
Performance.Therefore, it can be obtained with higher-strength, higher abrasion resistance, while had relatively low with providing one kind by studying
The rubber composition of the vulcanization rubber of rolling resistance and high wet-sliding resistant performance has great importance.
Invention content
It is a kind of with higher-strength, higher abrasion resistance the purpose of the present invention is obtaining, while there is relatively low rolling resistance
With the vulcanization rubber that can be used in preparing green tire tread rubber of high wet-sliding resistant performance.
The present inventor has found after research, using pre- mixing technology, before main rubber mixing, certain
Under the conditions of temperature and time, silane coupling agent is keyed in a manner of chemical bond on the rubber molecular chain of main rubber, is increased
The polarity of main rubber, can be promoted white carbon or and dispersing uniformity of other additives in main rubber, obtain
The vulcanization rubber of excellent combination property, so as to complete the present invention.
To achieve these goals, in a first aspect, the present invention provides a kind of method for preparing modified host rubber, this method
Including：Main rubber is kneaded in advance with silane coupling agent or with silane coupling agent and reinforcing agent, the temperature of the pre- mixing
It is 130-200 DEG C to spend, and the time being kneaded in advance is 1-20min.
Second aspect, the present invention provide a kind of modified host rubber being prepared by preceding method.
The third aspect, the present invention provide a kind of with connatural modified main with modified host rubber phase described in second aspect
Body rubber.
Fourth aspect, the present invention provide a kind of rubber composition, in the composition containing modified host rubber, vulcanizing agent,
Vulcanization accelerator, activator, anti-aging agent, carbon black, white carbon and dispersant and optionally contain softening agent, the modified host
Rubber is the modified host rubber described in second aspect of the present invention and/or the third aspect.
5th aspect, the present invention provide a kind of method for preparing vulcanization rubber, and this method includes：By fourth aspect present invention
Each component in the rubber composition other than vulcanizing agent and vulcanization accelerator carries out first and is kneaded, and obtains the first mixing
Glue；Then it adds in vulcanizing agent and vulcanization accelerator carries out second and is kneaded, obtain the second rubber compound；Then to second rubber compound
Vulcanized.
6th aspect, the present invention provide a kind of method for preparing vulcanization rubber, and this method includes：
(1) modified host rubber is prepared using the method described in first aspect present invention；
(2) the modified host rubber and activator, anti-aging agent, carbon black, white carbon and dispersant obtained step (1) is optional
Ground and softening agent carry out first and are kneaded, and obtain the first rubber compound；
(3) first rubber compound and vulcanizing agent and vulcanization accelerator are carried out second to be kneaded, obtains the second rubber compound；
(4) second rubber compound is vulcanized.
7th aspect, the present invention provide a kind of method as described in fifth aspect present invention and/or the 6th aspect and are prepared into
The vulcanization rubber arrived.
Eighth aspect, present invention offer one kind has and the 7th aspect vulcanization connatural vulcanization rubber of rubber phase.
9th aspect, the present invention provide application of the aforementioned vulcanization rubber as tire tread material.
It is provided by the invention vulcanization rubber have higher-strength, higher abrasion resistance, at the same have relatively low rolling resistance and
High wet-sliding resistant performance, and vulcanization rubber provided by the invention can be used in preparing green tire tread rubber.
The preparation of the present invention vulcanizes the simple for process of rubber, that is, the present invention can be prepared under simple process conditions
The vulcanization rubber with excellent combination property is obtained, which is highly suitable for preparing the tread rubber for green tire.
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 is 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 endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood to comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It between the endpoint value of a range and individual point value and can be individually combined with each other between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
First aspect, the present invention provides a kind of method for preparing modified host rubber, this method includes：By main rubber
It is kneaded in advance with silane coupling agent or with silane coupling agent and reinforcing agent, the temperature of the pre- mixing is 130-200 DEG C, in advance
The time of mixing is 1-20min.
It was found by the inventors of the present invention that by main rubber and silane coupling agent or and reinforcing agent within specified temperatures
Modified host rubber can be obtained by being kneaded the specific time in advance, have higher using the vulcanization rubber that the modified host rubber is formed
Intensity, higher wearability, while there is lower rolling resistance and higher wet-sliding resistant performance.The present inventor is also
It was found that particularly, when the temperature of the pre- mixing is 140-170 DEG C, and the time being kneaded in advance is 1.5-5min, the modification of acquisition
Main rubber enables to the comprehensive performance of vulcanization rubber being thus prepared more excellent.
Preferably, relative to the main rubber of 100 parts by weight, the dosage of the silane coupling agent is 3.5-6 parts by weight, institute
The dosage for stating reinforcing agent is 0-20 parts by weight；It is highly preferred that relative to the main rubber of 100 parts by weight, the silane coupling agent
Dosage for 4.2-5.5 parts by weight, the dosage of the reinforcing agent is 0-10 parts by weight.
It was found by the inventors of the present invention that when the main rubber relative to 100 parts by weight, the dosage of the silane coupling agent is
4.2-5.5 parts by weight when the dosage of the reinforcing agent is 0-10 parts by weight, coordinate aforementioned specific pre- mixing temperature and time,
Enable to the comprehensive performance of vulcanization rubber that thus obtained modified host rubber is prepared more excellent.
Preferably, the main rubber is solution polymerized butadiene styrene rubber and/or emulsion polymerized styrene butadiene rubber.
Preferably, the styrol structural unit content in the solution polymerized butadiene styrene rubber is 15-35 weight %；Contents of ethylene
For 40-80 weight %；Mooney viscosity is 55-67；Oil-filled number is 0-45phr.When the oil-filled number of the solution polymerized butadiene styrene rubber
When being 0, the solution polymerized butadiene styrene rubber is non-oil-filled solution polymerized butadiene styrene rubber.
Preferably, it is 100-200m that the reinforcing agent, which is specific surface area,2One kind in the white carbon of/g or at least two
Mixture.
It is particularly preferred that it is 165-185m that the reinforcing agent, which is specific surface area,2One kind in the white carbon of/g or at least
Two kinds of mixture.It was found by the inventors of the present invention that it is 165-185m when reinforcing agent is specific surface area2One in the white carbon of/g
When kind or at least two mixture, coordinate aforementioned specific pre- mixing temperature and time, enable to thus obtained change
Property main rubber be prepared vulcanization rubber comprehensive performance it is more excellent.
Preferably, the silane coupling agent is the silane coupling agent containing alkoxy and containing sulphur atom or amino；More
Preferably, the silane coupling agent is Si69 (double-[γ-(triethoxysilicane) propyl]-tetrasulfide), KH550 (γ-ammonia third
At least one of ethyl triethoxy silicane alkane) and Si75 (double-[γ-(triethoxysilicane) propyl]-disulphide).
Second aspect, the present invention provides a kind of modified host rubber being prepared by preceding method.
In the second aspect of the present invention, the method that the modified host rubber provided is provided by the first aspect of the present invention
It is prepared.
The third aspect, the present invention provides one kind to have and the connatural modification of modified host rubber phase described in second aspect
Main rubber.
In the third aspect of the present invention, have and modified host rubber phase is connatural described in second aspect changes to preparing
Property main rubber method there is no particular limitation, also, the third aspect of the present invention it is claimed be with the present invention the
Modified host rubber described in two aspects has the modified host rubber of same nature.
Fourth aspect, the present invention provides a kind of rubber composition, contain modified host rubber, vulcanization in the composition
Agent, vulcanization accelerator, activator, anti-aging agent, carbon black, white carbon and dispersant and optionally contain softening agent, the modification
Main rubber is the modified host rubber described in second aspect of the present invention and/or the third aspect.
In the fourth aspect, involved modified host rubber is aforementioned second aspect of the invention and the third
Modified host rubber described in aspect, in order to avoid repeating, details are not described herein by the present invention.
Described " and optionally containing softening agent " refers to, can contain softening agent in the rubber composition of the invention
Softening agent can not also be contained.Those skilled in the art can add in or be added without according to actual needs the softening agent.
In the fourth aspect of the present invention, the type of the white carbon can be mended with the conduct in first aspect present invention
The type of the white carbon of strong agent is identical or different.Contain modified host in rubber composition described in the fourth aspect of the present invention
Rubber and white carbon, and contain reinforcing agent in modified host rubber, which is white carbon in the preferred case.Change when described
Property main rubber by be used as the white carbon of reinforcing agent carried out together with silane coupling agent and main rubber premix refining be prepared
When, represent that the present invention has white carbon addition in the mixing process of pre- mixing process and rubber composition, that is, white carbon point
Two steps are added in the system for preparing vulcanization rubber.
Preferably, relative to the main rubber of 100 parts by weight, the content of the vulcanizing agent is 0.5-4 parts by weight, the sulphur
The content for changing accelerating agent is 1-8 parts by weight, and the content of the activator is 2-8 parts by weight, and the content of the anti-aging agent is 1-8 weights
Part is measured, the content of the carbon black is 1-20 parts by weight, and the content of the white carbon is 50-75 parts by weight, and the dispersant contains
It measures as 1-6 parts by weight, the content of the softening agent is 0-50 parts by weight；It is highly preferred that the main body rubber relative to 100 parts by weight
Glue, the content of the vulcanizing agent is 1-2 parts by weight, and the content of the vulcanization accelerator is 2-5 parts by weight, and the activator contains
It measures as 3-5 parts by weight, the content of the anti-aging agent is 3-5 parts by weight, and the content of the carbon black is 3-12 parts by weight, the hard charcoal
Black content is 55-65 parts by weight, and the content of the dispersant is 2-4 parts by weight, and the content of the softening agent is 0-30 weight
Part.Particularly, the parts by weight of white carbon involved in the part are only the parts by weight of the white carbon in rubber composition, without
The white carbon as reinforcing agent that may be used including modified host rubber in order to obtain.
Particularly, it is unless otherwise indicated, described " relative to the main body of 100 parts by weight in the rubber composition of the present invention
Do not include the weight of filling oil that may contain in main rubber in rubber ", if that is, containing filling in the main rubber
Oil, then " relative to the main rubber of 100 parts by weight " in 100 parts by weight in be eliminate filling oil part weight.And
And the type of the filling oil of the present invention can be identical with the type of softening agent.
Preferably, the vulcanizing agent is sulphur, two thio morpholines and four vulcanize at least one of two morpholines.It is more excellent
Selection of land, the vulcanizing agent are sulphur.The sulphur for example can be common sulphur, insoluble sulfur IS60-10 and pre-dispersed sulphur
At least one of sulphur S-80.
Preferably, the vulcanization accelerator is sulfenamide vulcanization accelerator and/or guanidine vulcanization accelerator.More preferably
Ground, the vulcanization accelerator for diphenylguanidine (diphenylguanidine), N- tertiary butyls -2-[4-morpholinodithio base sulfenamide (accelerator TBBS),
2,2'- dibenzothiazyl disulfides (altax), N- tertiary butyls-bis- (2-[4-morpholinodithio) sulfenamide (accelerator TBSI)
At least one of with N- cyclohexyl-bis- (2-mercaptobenzothiazoles) sulfenamide (accelerant CZ).
Preferably, the activator is selected from least one of zinc oxide, magnesia and stearic acid.It is it is highly preferred that described
Activator is zinc oxide and stearic acid.
Preferably, the anti-aging agent is selected from least one of amines antioxidants, quinoline type antioxidant and microwax；It is described
Amines antioxidants can be N- isopropyls-N '-diphenyl-para-phenylene diamine (antioxidant 4010NA), N- (1,3- dimethylbutyls)-N '-
In diphenyl-para-phenylene diamine (antioxidant 4020) and N, N '-bis- (1,4- dimethyl amyl groups) p-phenylenediamine (anti-aging agent 77PD) at least
It is a kind of.And the quinoline type antioxidant can be 2,2,4- trimethyl -1,2- dihyaroquinolines condensates (anti-aging agent RD) and/
Or 6- ethyoxyl -2,2,4- trimethyl -1,2- dihyaroquinolines (antioxidant A W).
According to a kind of preferred embodiment, the anti-aging agent is for microwax and selected from amines antioxidants and quinolines
The mixture of at least one of anti-aging agent substance.
Preferably, the fusing point of the microwax is 60-95 DEG C, molecular weight 580-700.Particularly, the microwax master
It will be by C20-60Cycloalkane and it is a small amount of just, isoparaffin composition.
Preferably, the dispersant is the polyethylene glycol that molecular weight is 1000-10000.
Preferably, the softening agent is aromatic naphtha and/or naphthenic oil；For example, the softening agent can be TDAE (through processing
Aromatic naphtha (Treated Distillate Aromatic Extract)), RAE (raffinate oil (Residual by residual aromatics
At least one of Aromatic Extract)) and NAP (naphthenic oil (Napthtenics)).The rubber composition pair of the present invention
There is no particular limitation for the property of the aromatic naphtha and the naphthenic oil, can be the various virtues of ordinary meaning in the art
Hydrocarbon ils and the naphthenic oil.
Preferably, the carbon black is 8# reference blacks and/or carbon black N330.
5th aspect, the present invention provides a kind of method for preparing vulcanization rubber, this method includes：By present invention four directions
Each component in rubber composition described in face other than vulcanizing agent and vulcanization accelerator carries out first and is kneaded, and it is mixed to obtain first
Refining glue；Then it adds in vulcanizing agent and vulcanization accelerator carries out second and is kneaded, obtain the second rubber compound；Then it is kneaded to described second
Glue is vulcanized.
It is provided by the invention prepare vulcanization rubber method in, it is described first be kneaded and described second be kneaded method and
Condition can be the conventional selection of this field.Usually, the mixing can carry out in open mill or mixer, and the
Mixing sequence in one mixing process between each substance can be carried out at the same time, can also carry out step by step, and preferably substep carries out.
A kind of specific embodiment according to the present invention, it is described prepare vulcanization rubber method can as follows into
Row：In mixer, add in the component other than vulcanizing agent and vulcanization accelerator in aforementioned rubber composition of the present invention into
Row first is kneaded；Then on a mill by three times, obtaining the first rubber compound；By first rubber compound in kneading machine and
Vulcanizing agent and vulcanization accelerator thin logical bottom sheet on a mill, obtain the second rubber compound, by the second rubber compound after vulcanization
To vulcanization rubber.
Preferably, the condition of the vulcanization includes the temperature of vulcanization for 140-160 DEG C, and the pressure of vulcanization is 5-15MPa, sulphur
The time of change is 10-50 minutes.
6th aspect, the present invention provides a kind of method for preparing vulcanization rubber, this method includes：
(1) modified host rubber is prepared using the method described in first aspect present invention；
(2) the modified host rubber and activator, anti-aging agent, carbon black, white carbon and dispersant obtained step (1) is optional
Ground and softening agent carry out first and are kneaded, and obtain the first rubber compound；
(3) first rubber compound and vulcanizing agent and vulcanization accelerator are carried out second to be kneaded, obtains the second rubber compound；
(4) second rubber compound is vulcanized.
A kind of preferred embodiment according to the present invention, the method for preparing vulcanization rubber can be according to as follows
Mode carries out：
(1) in mixer, main rubber is premixed with silane coupling agent or with silane coupling agent and reinforcing agent
Refining, the temperature of the pre- mixing is 130-200 DEG C, and the time being kneaded in advance is 1-20min, obtains modified host rubber；
(2) in mixer, by the modified host rubber and activator or with activator and at least part white carbon
It is kneaded；
(3) anti-aging agent, carbon black and dispersant are added in optionally and softening agent and remainder white carbon, treats sizing material temperature
Mixing 5-7min unloads sizing material at such a temperature after reaching 150-160 DEG C；
(4) by sizing material on the open mill that roll spacing is 3-7mm, roller temperature is 50 ± 5 DEG C by least three times, by the mixed of acquisition
Material glue parks 3-5h；
(5) batch mixing glue and the vulcanizing agent and vulcanization accelerator obtained step (4) is kneaded at 40 ± 5 DEG C of initial temperature,
When sizing material temperature reaches 100-120 DEG C, sizing material is unloaded during mixing 2-4min at such a temperature；
(6) by step (5) obtain sizing material on the open mill that roll spacing is 0.4-0.6mm, roller temperature is 50 ± 5 DEG C by extremely
It is few primary, roll spacing is then adjusted to 2-4mm, then by least twice；The rubber compound of acquisition is parked into 18-30h；
(7) sizing material that step (6) obtains under 140-160 DEG C, 5-15Mpa pressure is vulcanized 10-50 minutes, is vulcanized
Rubber.
Preferably, the white carbon added in step (2) accounts for the 50-100 weights of the white carbon weight as rubber composition
Measure %.
7th aspect, the present invention provides a kind of methods as described in fifth aspect present invention or the 6th aspect to be prepared
Vulcanization rubber.
Vulcanization rubber described in seventh aspect present invention is prepared by using the method described in the 5th aspect or the 6th aspect
It obtains.
Eighth aspect, the present invention provides one kind to have and the 7th aspect vulcanization connatural vulcanization rubber of rubber phase
Glue.
The vulcanization rubber of eighth aspect present invention offer has the property same with the 7th aspect vulcanization rubber phase, and simultaneously
The method described in the 6th aspect or the 7th aspect using the present invention is not limited to be prepared.That is, the of the present invention
Vulcanize rubber as all vulcanization rubber with the property same with the 7th aspect vulcanization rubber phase in eight aspects, and to it
There is no particular limitation for preparation method.
9th aspect, the present invention provides application of the aforementioned vulcanization rubber as tire tread material.
It can be used using the vulcanization rubber system of the present invention for the technique of tire tread material for routine in the art
Various techniques, the present invention specific technique for applying is not particularly limited.
The present invention will be described in detail by way of examples below.
Disclosure used below is as follows：
Non- oil-filled solution polymerized butadiene styrene rubber (SSBR2506) is the commodity purchased from sinopec Yanshan Petrochemical company, wherein, benzene second
The content of alkene structural unit is 26 weight %, and contents of ethylene is 56 weight %, and Mooney viscosity 65, oil-filled number is 0phr.
Oil-filled solution polymerized butadiene styrene rubber (SSBR2636) combinated styrene content content is 25 weight %, and contents of ethylene is 63 weights
%, Mooney viscosity 62 are measured, oil-filled number is 37.5phr.
White carbon is is respectively 165GR (specific surface area 165m purchased from Rhodia (Qingdao) Co., Ltd trade mark2/ g) and
175GR (specific surface area 185m2/ g) commodity.
The commodity that it is IRB8# purchased from ConUS carbon black company manufactures' trade mark that 8# reference blacks (carbon black), which are,.
TDAE (softening agent) is the commodity for moistening limited rubber company purchased from Qingzhou City Ostwald-Folin.
Si69, Si75 (silane coupling agent) are the commodity purchased from Shanghai Rui Shi Chemical Industry Science Co., Ltd.
Zinc oxide and stearic acid (activator) are the commodity purchased from Sinopharm Chemical Reagent Co., Ltd..
Antioxidant 4010 (anti-aging agent) is the commodity purchased from Gaoyi County profit and Chemical Co., Ltd..
Diphenylguanidine (vulcanization accelerator) is the commodity purchased from Shijiazhuang City first rays of the morning sun Chemical Co., Ltd..
Accelerator TBBS (vulcanization accelerator) is the commodity purchased from Guangdong Du Ba new materials Science and Technology Ltd..
Sulphur (vulcanizing agent) is the commodity purchased from Sinopharm Chemical Reagent Co., Ltd..
The commodity that it is W-445 purchased from the Tianjin Heng Shengxin sources International Trading Company Ltd trade mark that microwax, which is, carbon atom number
For 20-50.
PEG4000 (dispersant) is commodity purchased from Nanjing Run Bang Chemical Co., Ltd.s, molecular weight 4000.
Mixer is Shanghai Kechuang rubber and plastics machine equipment Co., Ltd XSM-1/10-120 types, and mold cavity volume 1L is heated
System is electrical heating, has refrigerating function.
Vulcanizing press is produced for industrial (Anhui) Co., Ltd of huge rock oil pressure, model P-50-PCD-3L.
The total amount of rubber composition involved in following embodiment is identical, is 1200g.
Embodiment 1：Prepare vulcanization rubber S1
(1) in mixer, under 80rpm rotating speeds, main rubber is mixed with silane coupling agent at a temperature of 160 DEG C
3min；
(2) start mixer cooling system, the temperature of charge in mixer is dropped to 80 DEG C；Obtain modified host rubber；
(3) in mixer, under 80rpm rotating speeds, add in account for white carbon total weight 3/4 white carbon and whole
Activator is kneaded 2.5min；
(4) anti-aging agent, carbon black, remainder white carbon and dispersant and softening agent are added in, treats that sizing material temperature reaches 150
Sizing material is unloaded after being kneaded 6min at such a temperature after DEG C；
(5) by sizing material on the open mill that roll spacing is 5mm, roller temperature is 50 ± 5 DEG C by the way that three times, the batch mixing glue of acquisition is stopped
Put 4h；
(6) the batch mixing glue and vulcanizing agent and vulcanization accelerator obtained step (5) is under 40rpm rotating speeds, initial temperature 40
It is kneaded at ± 5 DEG C, when sizing material temperature reaches 100 DEG C, sizing material is unloaded when being kneaded 4min at such a temperature；
(7) by step (6) obtain sizing material on the open mill that roll spacing is 0.5mm, roller temperature is 50 ± 5 DEG C by primary,
Then roll spacing is adjusted to 3mm, then by twice；The rubber compound of acquisition is parked for 24 hours；
(8) sizing material that step (6) obtains under 160 DEG C, 15Mpa pressure is vulcanized 35 minutes, obtains vulcanization rubber S1.
In substance classes during the pre- mixing for preparing modified host rubber and mixing process in the present embodiment
The type and dosage of each component in rubber composition are listed in Table 1 below.
Embodiment 2：Prepare vulcanization rubber S2
(1) in mixer, under 80rpm rotating speeds, main rubber is mixed with silane coupling agent at a temperature of 170 DEG C
2min；
(2) start mixer cooling system, the temperature of charge in mixer is dropped to 80 DEG C；Obtain modified host rubber；
(3) in mixer, under 80rpm rotating speeds, 80% white carbon and whole for accounting for white carbon total weight are added in
Activator be kneaded 2.5min；
(4) anti-aging agent, carbon black, remainder white carbon and dispersant are added in, in the temperature after sizing material temperature reaches 150 DEG C
Sizing material is unloaded after the lower mixing 6min of degree；
(5) by sizing material on the open mill that roll spacing is 5mm, roller temperature is 50 ± 5 DEG C by the way that three times, the batch mixing glue of acquisition is stopped
Put 4h；
(6) the batch mixing glue and vulcanizing agent and vulcanization accelerator obtained step (5) is under 40rpm rotating speeds, initial temperature 40
It is kneaded at ± 5 DEG C, when sizing material temperature reaches 100 DEG C, sizing material is unloaded when being kneaded 4min at such a temperature；
(7) by step (6) obtain sizing material on the open mill that roll spacing is 0.5mm, roller temperature is 50 ± 5 DEG C by primary,
Then roll spacing is adjusted to 3mm, then by twice；The rubber compound of acquisition is parked for 24 hours；
(8) sizing material that step (6) obtains under 155 DEG C, 10Mpa pressure is vulcanized 40 minutes, obtains vulcanization rubber S2.
In substance classes during the pre- mixing for preparing modified host rubber and mixing process in the present embodiment
The type and dosage of each component in rubber composition are listed in Table 1 below.
Embodiment 3：Prepare vulcanization rubber S3
(1) in mixer, under 80rpm rotating speeds, by main rubber and silane coupling agent and the pre- white carbon that is kneaded 150
4.5min is mixed at a temperature of DEG C；
(2) start mixer cooling system, the temperature of charge in mixer is dropped to 80 DEG C；Obtain modified host rubber；
(3) it in mixer, under 80rpm rotating speeds, adds in and accounts for total component as in rubber composition (including pre-
90% white carbon of the white carbon total weight dosage in mixing, similarly hereinafter) and the activator of whole are kneaded 2.5min；
(4) anti-aging agent, carbon black, remainder white carbon and dispersant and softening agent are added in, treats that sizing material temperature reaches 150
Sizing material is unloaded after being kneaded 6min at such a temperature after DEG C；
(5) by sizing material on the open mill that roll spacing is 5mm, roller temperature is 50 ± 5 DEG C by the way that three times, the batch mixing glue of acquisition is stopped
Put 4h；
(6) the batch mixing glue and vulcanizing agent and vulcanization accelerator obtained step (5) is under 40rpm rotating speeds, initial temperature 40
It is kneaded at ± 5 DEG C, when sizing material temperature reaches 100 DEG C, sizing material is unloaded when being kneaded 4min at such a temperature；
(7) by step (6) obtain sizing material on the open mill that roll spacing is 0.5mm, roller temperature is 50 ± 5 DEG C by primary,
Then roll spacing is adjusted to 3mm, then by twice；The rubber compound of acquisition is parked for 24 hours；
(8) sizing material that step (6) obtains under 150 DEG C, 8Mpa pressure is vulcanized 50 minutes, obtains vulcanization rubber S3.
In substance classes during the pre- mixing for preparing modified host rubber and mixing process in the present embodiment
The type and dosage of each component in rubber composition are listed in Table 1 below.
Embodiment 4：Prepare vulcanization rubber S4
The present embodiment prepares vulcanization rubber using method similar to Example 1, the difference is that the system in the present embodiment
The pre- mixing step of standby modified host rubber is different, and specifically, step (1) is：
In mixer, under 80rpm rotating speeds, main rubber is mixed into 3min with silane coupling agent at a temperature of 180 DEG C.
Remaining is in the same manner as in Example 1, obtains vulcanization rubber S4.
Embodiment 5：Prepare vulcanization rubber S5
The present embodiment prepares vulcanization rubber using method similar to Example 1, the difference is that the system in the present embodiment
The pre- mixing step of standby modified host rubber is different, and specifically, step (1) is：
In mixer, under 80rpm rotating speeds, main rubber is mixed into 3min with silane coupling agent at a temperature of 130 DEG C.
Remaining is in the same manner as in Example 1, obtains vulcanization rubber S5.
Embodiment 6：Prepare vulcanization rubber S6
The present embodiment prepares vulcanization rubber using method similar to Example 2, the difference is that the system in the present embodiment
The pre- mixing step of standby modified host rubber is different, and specifically, step (1) is：
In mixer, under 80rpm rotating speeds, main rubber is mixed with silane coupling agent at a temperature of 170 DEG C
10min。
Remaining is in the same manner as in Example 2, obtains vulcanization rubber S6.
Embodiment 7：Prepare vulcanization rubber S7
The present embodiment prepares vulcanization rubber using method similar to Example 2, the difference is that the system in the present embodiment
The pre- mixing step of standby modified host rubber is different, and specifically, step (1) is：
In mixer, under 80rpm rotating speeds, main rubber is mixed into 1min with silane coupling agent at a temperature of 170 DEG C.
Remaining is in the same manner as in Example 2, obtains vulcanization rubber S7.
Embodiment 8：Prepare vulcanization rubber S8
This comparative example is carried out using method similar to Example 3, the difference is that the preparation in this comparative example is modified master
The dosage of the silane coupling agent used in body rubber is different from embodiment 3, specifically, in the present embodiment, relative to 100 weight
The main rubber of part, the dosage of the silane coupling agent is 6 parts by weight.That is, the type of the silane coupling agent in the present embodiment
It is in the same manner as in Example 3, the difference is that the dosage of silane coupling agent.
Remaining is in the same manner as in Example 3, obtains vulcanization rubber S8.
Comparative example 1：Prepare vulcanization rubber DS1
This comparative example is carried out using method similar to Example 1, the difference is that the main rubber in this comparative example is not
It is directly kneaded by pre- mixing process, specifically：
(1) in mixer, under 80rpm rotating speeds, at 80 DEG C, 3/4 white carbon for accounting for white carbon total weight is added in
And whole activator, whole main rubbers and silane coupling agents is kneaded 2.5min；
(2) anti-aging agent, carbon black, remainder white carbon and dispersant are added in, in the temperature after sizing material temperature reaches 150 DEG C
Sizing material is unloaded after the lower mixing 6min of degree；
(3) by sizing material on the open mill that roll spacing is 5mm, roller temperature is 50 ± 5 DEG C by the way that three times, the batch mixing glue of acquisition is stopped
Put 4h；
(4) the batch mixing glue and vulcanizing agent and vulcanization accelerator obtained step (3) is under 40rpm rotating speeds, initial temperature 40
It is kneaded at ± 5 DEG C, when sizing material temperature reaches 100 DEG C, sizing material is unloaded when being kneaded 4min at such a temperature；
(5) by step (4) obtain sizing material on the open mill that roll spacing is 0.5mm, roller temperature is 50 ± 5 DEG C by primary,
Then roll spacing is adjusted to 3mm, then by twice；The rubber compound of acquisition is parked for 24 hours；
(6) sizing material that step (5) obtains under 160 DEG C, 15Mpa pressure is vulcanized 35 minutes, obtains vulcanization rubber DS1.
The total dosage and type of each substance involved in this comparative example are in the same manner as in Example 1.
Comparative example 2：Prepare vulcanization rubber DS2
This comparative example is carried out using method similar to Example 2, the difference is that the preparation in this comparative example is modified master
The pre- mixing step of body rubber is different, and specifically, step (1) is：
In mixer, under 80rpm rotating speeds, main rubber is mixed into 2min with silane coupling agent at a temperature of 120 DEG C.
Remaining is in the same manner as in Example 2, obtains vulcanization rubber DS2.
Comparative example 3：Prepare vulcanization rubber DS3
This comparative example is carried out using method similar to Example 3, the difference is that the preparation in this comparative example is modified master
The pre- mixing step of body rubber is different, and specifically, step (1) is：
In mixer, under 80rpm rotating speeds, by main rubber and silane coupling agent and white carbon at a temperature of 220 DEG C
Mix 2min.
Remaining is in the same manner as in Example 3, obtains vulcanization rubber DS3.
Table 1
| S1 | S2 | S3 | |
| SSBR2506 | 100 | -- | 100 |
| SSBR2636 | -- | 137.5 | -- |
| Si69 | 4.8 | -- | 5.2 |
| Si75 | -- | 4.5 | -- |
| TDAE | 15 | -- | 25 |
| It is pre- to be kneaded white carbon 165GR (reinforcing agent) | -- | -- | 3 |
| White carbon 165GR during mixing | 60 | -- | 62 |
| White carbon 175GR during mixing | -- | 55 | -- |
| 8# reference blacks | 10 | 12 | 5 |
| Zinc oxide | 3.0 | 2.0 | 1.5 |
| Stearic acid | 2.0 | 2.0 | 1.5 |
| Antioxidant 4010 | 3.0 | 3.5 | 3.0 |
| Microwax | 1.5 | 1.5 | 2.0 |
| PEG4000 | 3.0 | 3.0 | 2.0 |
| Sulphur | 1.5 | 1.2 | 1.8 |
| Accelerator TBBS | 1.5 | 1.2 | 1.8 |
| Diphenylguanidine | 1.5 | 1.8 | 1.5 |
Test case：The performance of vulcanization rubber that testing example and comparative example are prepared as follows
Mooney viscosity：According to GB/T 1232.1-2000 standard testings.It is preheated 1 minute at 100 ± 0.5 DEG C, tests 4 points
Clock.
Tensile property is tested：According to national standard《GB/T 1040-92 plastic tensile method for testing performances》In method test,
The AG-20KNG of puller system model Shimadzu Corporation production；Rate of extension is 500mm/min, and test temperature is 23 DEG C.Sample
Live part length is 25mm, width 6mm.For every group of sample, 10 parallel laboratory tests are carried out, results are averaged.Gained
The results are shown in Table 2.(" tensile strength/MPa ", " 100% stretches/MPa surely ", " 300% stretches/MPa surely ", " elongation in table 2
Rate/% " and " tearing strength/(kN/m) " data).
Dynamic mechanical：Temperature scanning is on German GABO companies EPLEXOR-500N dynamic thermomechanical analysis apparatus to sample
The viscoelastic behavior of product is tested.Sample length is 35mm, width 8mm, thickness 1.0mm.Test is surveyed using stretch mode
Try frequency be 11Hz, temperature range be -80~80 DEG C, heating rate be 3 DEG C/min, static strain 1%, dynamic strain
0.25%.Acquired results are as shown in table 2 (" tan δ (0 DEG C) ", " tan δ (60 DEG C) " and " Tg/ DEG C " data in table 2).
DIN is worn away：According to national standard《(rotating roller cartridge type is worn away the measure of GB/T 9867-2008 vulcanization rubber wear-resisting performances
Machine method)》Regulation, using the phase of the test of DIN abrasion instruments (GT-7012-D, Taiwan high ferro instrument detection Co., Ltd) vulcanization rubber
To volume worn amount.
Table 2
It can be seen from the results above that using main rubber and silane coupling agent or main rubber and silane coupling agent and
The modified host rubber that the method that white carbon is kneaded in advance obtains significantly improves the vulcanization rubber of acquisition when preparing and vulcanizing rubber
The tensile strength of glue, tearing strength, elongation at break, wearability and dynamic property also promote a level.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail, within the scope of the technical concept of the present invention, a variety of simple variants can be carried out to technical scheme of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (14)
1. a kind of method for preparing modified host rubber, this method include：By main rubber and silane coupling agent or and silane
Coupling agent and reinforcing agent are kneaded in advance, and the temperature of the pre- mixing is 130-200 DEG C, and the time being kneaded in advance is 1-20min.
2. according to the method described in claim 1, wherein, the temperature of the pre- mixing is 140-170 DEG C, and the time being kneaded in advance is
1.5-5min。
3. method according to claim 1 or 2, wherein, it is described silane coupled relative to the main rubber of 100 parts by weight
The dosage of agent is 3.5-6 parts by weight, and the dosage of the reinforcing agent is 0-20 parts by weight；Preferably,
Relative to the main rubber of 100 parts by weight, the dosage of the silane coupling agent is 4.2-5.5 parts by weight, the reinforcing agent
Dosage be 0-10 parts by weight.
4. according to the method described in any one in claim 1-3, wherein, the main rubber for solution polymerized butadiene styrene rubber and/
Or emulsion polymerized styrene butadiene rubber；Preferably,
Styrol structural unit content in the solution polymerized butadiene styrene rubber is 15-35 weight %；Contents of ethylene is 40-80 weights
Measure %；Mooney viscosity is 55-67；Oil-filled number is 0-45phr.
5. according to the method described in any one in claim 1-5, wherein, the reinforcing agent is that specific surface area is 100-
200m2A kind of in the white carbon of/g or at least two mixture；Preferably,
The reinforcing agent is that specific surface area is 165-185m2A kind of in the white carbon of/g or at least two mixture；It is preferred that
Ground,
The silane coupling agent is the silane coupling agent containing alkoxy and containing sulphur atom or amino, and preferably described silane is even
Join agent for double-[γ-(triethoxysilicane) propyl]-tetrasulfide, gamma-aminopropyl-triethoxy-silane and double-[γ-(three ethoxies
At least one of base silicon) propyl]-disulphide.
6. the modified host rubber or claim 1-5 that be prepared as the method described in any one in claim 1-5
Modified host rubber described in middle any one.
7. a kind of rubber composition, modified host rubber, vulcanizing agent, vulcanization accelerator, activator, anti-old is contained in the composition
Agent, carbon black, white carbon and dispersant and optionally contain softening agent, which is characterized in that the modified host rubber is right
It is required that the modified host rubber described in 6.
8. rubber composition according to claim 7, wherein, relative to the main rubber of 100 parts by weight, the vulcanizing agent
Content for 0.5-4 parts by weight, the content of the vulcanization accelerator is 1-8 parts by weight, and the content of the activator is 2-8 weight
Part, the content of the anti-aging agent is 1-8 parts by weight, and the content of the carbon black is 1-20 parts by weight, and the white carbon is 50-75 weights
Part is measured, the content of the dispersant is 1-6 parts by weight, and the content of the softening agent is 0-50 parts by weight；Preferably,
Relative to the main rubber of 100 parts by weight, the content of the vulcanizing agent is 1-2 parts by weight, and the vulcanization accelerator contains
It measures as 2-5 parts by weight, the content of the activator is 3-5 parts by weight, and the content of the anti-aging agent is 3-5 parts by weight, the charcoal
Black content is 3-12 parts by weight, and the white carbon is 55-65 parts by weight, and the content of the dispersant is 2-4 parts by weight, described
The content of softening agent is 0-30 parts by weight.
9. rubber composition according to claim 7 or 8, wherein, the vulcanizing agent is sulphur, two thio morpholines and four
Vulcanize at least one of two morpholines；
The vulcanization accelerator is sulfenamide vulcanization accelerator and/or guanidine vulcanization accelerator；
The activator is selected from least one of zinc oxide, magnesia and stearic acid；
The anti-aging agent is selected from least one of amines antioxidants, quinoline type antioxidant and microwax；
The dispersant is the polyethylene glycol that molecular weight is 1000-10000；
The softening agent is aromatic naphtha and/or naphthenic oil；Preferably,
The fusing point of the microwax is 60-95 DEG C, molecular weight 580-700；Preferably,
The carbon black is 8# reference blacks and/or carbon black N330.
10. a kind of method for preparing vulcanization rubber, this method include：By the rubber group described in any one in claim 7-9
It closes each component in object other than vulcanizing agent and vulcanization accelerator and carries out the first mixing, obtain the first rubber compound；Then it adds in
Vulcanizing agent and vulcanization accelerator carry out second and are kneaded, and obtain the second rubber compound；Then second rubber compound is vulcanized.
11. according to the method described in claim 10, wherein, the temperature that the condition of the vulcanization includes vulcanization is 140-160 DEG C,
The pressure of vulcanization is 5-15MPa, and the time of vulcanization is 10-50 minutes.
12. a kind of method for preparing vulcanization rubber, this method include：
(1) modified host rubber is prepared using the method described in any one in claim 1-5；
(2) the modified host rubber for obtaining step (1) and activator, anti-aging agent, carbon black, white carbon and dispersant optionally with
And softening agent carries out first and is kneaded, and obtains the first rubber compound；
(3) first rubber compound and vulcanizing agent and vulcanization accelerator are carried out second to be kneaded, obtains the second rubber compound；
(4) second rubber compound is vulcanized.
13. in the vulcanization rubber or claim 11-13 that be prepared as the method described in any one in claim 10-12
Vulcanization rubber described in any one.
14. application of the vulcanization rubber as tire tread material described in claim 13.
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| CN109824952A (en) * | 2018-09-11 | 2019-05-31 | 万力轮胎股份有限公司 | A kind of tire in-situ modified rubber composition and tire and preparation method thereof |
| CN115850826A (en) * | 2021-09-23 | 2023-03-28 | 中国石油化工股份有限公司 | Rubber auxiliary agent, rubber composition, vulcanized rubber, and preparation method and application thereof |
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