CN106633217B - The preparation method of high-performance rubber - Google Patents
The preparation method of high-performance rubber Download PDFInfo
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- CN106633217B CN106633217B CN201610910331.8A CN201610910331A CN106633217B CN 106633217 B CN106633217 B CN 106633217B CN 201610910331 A CN201610910331 A CN 201610910331A CN 106633217 B CN106633217 B CN 106633217B
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- sulphur
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
- C08K3/02—Elements
- C08K3/06—Sulfur
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08L7/00—Compositions of natural rubber
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The present invention relates to materials synthesis field, a kind of claimed preparation method of high-performance rubber：Either physically or chemically by sulphur uniform deposition to the main supporting material of rubber, to form the reinforced composites of sulphur cladding；The composite material is directly added in compounding rubber link, and sulphur realizes nano-dispersion by supporting material in rubber masterbatch, effectively avoid because sulphur disperse it is uneven caused by rubber bloom and local over cure and other issues.
Description
Technical field
The present invention relates to materials synthesis field more particularly to the preparation methods of high-performance rubber product.
Background technology
Sulphur is as natural rubber and the vulcanizing agent of alkadiene synthetic rubber, but general Cosan is difficult point in sizing material
It dissipates uniform.It is to be more easy to sulphur migration occur with some reinforced fillings and used time, causes product easily occur during rubber processing
Bloom has the problems such as point (agglutinator).To solve this problem, vast related work person has done substantial amounts of effort, such as：System
Standby insoluble sulfur (reduction sulphur is dissolved in rubber masterbatch, is precipitated, agglomeration traits) prepares sulphur masterbatch (reduction sulphur
Between reunion) etc., chemical company of Japan manufactured it is a kind of be referred to as polysulfide resin-like Sulfur, prevent light vulcanizate table
There is brown sulphur spot in face, reduces product defect.But these methods are only applicable to some specific products or glue kind, no
It can thoroughly solve the problems, such as that sulphur disperses non-uniform during rubber processing.
The content of the invention
Dissolve, be precipitated in rubber masterbatch present invention aims at sulphur during solution in the prior art rubber processing,
The problem of reunion, provides the high-performance rubber that a kind of sulphur uniformly disperses in rubber masterbatch.
To solve the above problems, technical solution provided by the invention is：A kind of preparation method of high-performance rubber, including
Following steps：
1.1 prepare the reinforced composites that sulphur uniformly coats；
1.2 are added to above-mentioned composite material rubber mixing link in raw rubber；
1.3 sulfidization moldings obtain the high-performance rubber product.
An optimal technical scheme of the invention, the preparation method for the reinforced composites that step 1.1 sulphur uniformly coats
For：
2.1 are positioned over sulphur in heatable vacuum mixer；
2.2 are again positioned over reinforcing rubber material in vacuum mixer；
After 2.3 equipment vacuumize, heating unit and agitating device are opened, at the heating temperature, sulphur is by thermal evaporation, sulphur
Steam is evenly distributed on reinforcing rubber material surface, and the reinforced composites that sulphur uniformly coats are formed after cooling.
An optimal technical scheme of the invention, the heating temperature are the gasification corresponded in sulphur phasor under equilibrium vapor pressure
Temperature, such as under 0.1Pa, sulphur sublimation temperature is about 80 DEG C.
The mass ratio of an optimal technical scheme of the invention, sulphur and reinforcing rubber material is 1:1-50.It is taken out in described 2.3 true
Sky is -1Mpa~-0.1Mpa.
An optimal technical scheme of the invention, the preparation method for the reinforced composites that step 1.1 sulphur uniformly coats
For：
3.1 are uniformly mixed sulphur presoma with reinforcing rubber material；
3.2 are sent into uniformly mixed material in consersion unit, and sulphur presoma decomposites work under the conditions of certain temperature
Sulphur atom is sprinkled, the main supporting material surface of rubber is evenly distributed on, obtains sulphur uniformly rubber-coated reinforced composites.
An optimal technical scheme of the invention, the sulphur presoma are CS2、H2S, benzenethiol, thiophenol, dimethyl sulfoxide (DMSO) etc.
One or more of.
An optimal technical scheme of the invention, the certain temperature condition are 160 DEG C -500 DEG C.It is further, it is preferable to certain
Temperature conditionss are 180 DEG C -260 DEG C.
An of the invention optimal technical scheme, the reinforcing rubber material is carbon black, white carbon, carbon nanotubes, graphene, short
One or more of fiber, zinc oxide.
The one kind of the reinforcing rubber material in carbon black, white carbon, carbon nanotubes, graphene, staple fiber, zinc oxide
It is or several.
A kind of high-performance rubber preparation method technical solution provided by the invention, comprises the following steps：
(1) reinforced composites that sulphur uniformly coats are prepared：Element sulfur raw material is uniformly mixed with reinforcing rubber material, it will
Uniformly mixed material is heated, and finally obtains sulphur uniformly rubber-coated reinforced composites；
(2) reinforced composites that above-mentioned sulphur uniformly coats are added in compounding rubber link in raw rubber and be kneaded, obtained
To masterbatch；
(3) masterbatch that step (2) obtains is subjected to sulfidization molding and obtains high-performance rubber product.
The element sulfur raw material is selected from sulphur, sulphur presoma, and the sulphur presoma is CS2、H2S, benzenethiol, thiophenol, two
One or more of methyl sulfoxide etc..
When the element sulfur raw material is sulphur, in step (1), before element sulfur raw material, the stirring of reinforcing rubber material is carried out, first
It vacuumizes.For sulphur by thermal evaporation, sulphur steam is evenly distributed on reinforcing rubber material surface, obtains sulphur uniformly rubber-coated benefit
Strong composite material.
When the element sulfur raw material is sulphur presoma, sulphur is uniformly mixed with reinforcing rubber material；By what is be uniformly mixed
Material is heated, and at a certain temperature, sulphur presoma decomposites active sulphur atom, is evenly distributed on the main reinforcing material of rubber
Expect surface, obtain sulphur uniformly rubber-coated reinforced composites.
A kind of preparation method of claimed high-performance rubber.With either physically or chemically by sulphur uniform deposition
Onto the main supporting material of rubber, the reinforced composites of sulphur cladding are formed；The composite material is directly in compounding rubber link
Add in, sulphur realizes nano-dispersion by supporting material in rubber masterbatch, effectively avoid because sulphur disperse it is uneven caused by
Rubber bloom and local over cure and other issues.The present invention provides sulphur to be evenly coated at the main supporting material of rubber
The reinforced composites on surface have between part sulphur and the main supporting material of rubber with chemical key-shaped in the reinforced composites
Formula combine, can to avoid dissolved in sulphur during rubber processing in rubber masterbatch, be precipitated, reunite the problem of.Sulphur simultaneously
The main supporting material surface of rubber is coated on, increases the contact area of sulphur and rubber masterbatch, inhibits sulphur migration, reduces sulphur
Between agglomeration, it can be achieved that sulphur in rubber masterbatch uniformly disperse.
The present invention realize sulphur in rubber uniformly disperse purpose, solve due to sulphur disperse it is uneven caused by
Bloom that rubber occurs has the problems such as point.Compared with prior art, the method have the advantages that：1) present invention carries for the first time
Go out, sulphur is coated on the main supporting material surface of rubber, is then applied to rubber materials；2) product can reach sulphur in rubber
In uniformly disperse purpose.
Description of the drawings
Fig. 1 is sulphur phasor.
Fig. 2 is the TEM photos of the material prepared by embodiment 1.
Fig. 3 is the vulcanizate (A figures) of 1 gained sample preparation of embodiment with directly using the vulcanizate (B prepared by sulphur
Figure) cross-section comparison's photo.
Specific embodiment
Said program is described further below in conjunction with specific embodiment.It is to be understood that these embodiments are for illustrating
The present invention and be not limited to limit the scope of the invention.The implementation condition used in embodiment can be done according to the condition of specific producer
Further adjustment, the implementation condition being not specified is usually the condition in routine experiment.
Embodiment 1
1. m sulphur in mass ratio：M carbon nanotubes=1:2 weigh 10g sulphur and 20g carbon nanotubes；
2. sulphur and carbon nanotubes are added separately in vacuum mixer；
3. it is 0.1Pa that equipment is evacuated to pressure in equipment, will be set using the mode of heatings such as microwave, infrared, electrical heating
It is standby to be heated to 80 DEG C, while mixing plant is opened, after heating 15min, stop heating, continue stirring until material is cooled to room
Temperature obtains the reinforced composites；
It is kneaded 4. composite material rubber mixing link is added in raw rubber, obtains masterbatch；
5. obtain high-performance rubber product after masterbatch vulcanization.
Fig. 2 is the TEM photos of reinforced composites, and sulphur is evenly distributed on the surface of carbon nanotubes as seen from Figure 2.
Sulphur and the material are added separately in rubber mixing process in rubber compound by the proportioning of natural rubber basic components, vulcanized
Its section is analyzed under the microscope afterwards, as shown in Fig. 3 figures.Fig. 3 Image to left is the vulcanizate section photograph for adding sulphur
Piece, Image to right are the vulcanizate cross-section photographs for adding material of the present invention, and the two comparison is it can be found that directly use the sulphur of sulphur
Changing has a large amount of short grained sulphur aggregates in glue section, add in the vulcanizate section of material of the present invention and sulphur group do not occur
Aggressiveness illustrates that sulphur is uniformly dispersed in vulcanizate.
Embodiment 2
1. m sulphur in mass ratio：M carbon nanotubes=1:2 weigh 10g sulphur and 20g carbon nanotubes；
2. sulphur is prepared into targeting material, the laser splash area of vacuum mixer is put into；Carbon nanotubes is added to very
In empty mixer；
3. equipment is evacuated to its vacuum degree for -0.1Mpa, sulphur is gasified using laser, while opens stirring and sets
Standby, the vulcanization after gasification is adsorbed in carbon nano tube surface, stops heating, continues stirring until material is cooled to room temperature, sulphur is equal
It is even to be adsorbed in carbon nano tube surface.
It is kneaded 4. composite material rubber mixing link is added in raw rubber, obtains masterbatch；
5. obtain high-performance rubber product after masterbatch vulcanization.
Embodiment 3
1. m dimethyl sulfoxide (DMSO)s in mass ratio：M carbon nanotubes=5:4 weigh 25g dimethyl sulfoxide (DMSO)s and 20g carbon nanotubes；
2. carbon nanotubes is uniformly mixed with dimethyl sulfoxide (DMSO), carbon nanotubes/dimethyl sulfoxide (DMSO) slurry is obtained；
3. atmosphere meshbeltfurnace is warming up to 220 DEG C, carbon nanotubes/dimethyl sulfoxide (DMSO) slurry is delivered to wherein, reaction
30min obtains target product.
It is kneaded 4. composite material rubber mixing link is added in raw rubber, obtains masterbatch；
5. obtain high-performance rubber product after masterbatch vulcanization.
The foregoing examples are merely illustrative of the technical concept and features of the invention, its object is to allow the person skilled in the art to be
Present disclosure can be understood and implemented according to this, it is not intended to limit the scope of the present invention.It is all smart according to the present invention
The equivalent transformation or modification that refreshing essence is done, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of high-performance rubber, includes the following steps：
1.1 prepare the reinforced composites that sulphur uniformly coats；The preparation for the reinforced composites that step 1.1 sulphur uniformly coats
Method is：
2.1 are positioned over sulphur in heatable vacuum mixer；
2.2 are again positioned over reinforcing rubber material in vacuum mixer；
After 2.3 equipment vacuumize, heating unit and agitating device are opened, at the heating temperature, sulphur is by thermal evaporation, sulphur steam
Reinforcing rubber material surface is evenly distributed on, the reinforced composites that sulphur uniformly coats are formed after cooling；
1.2 are added to above-mentioned composite material rubber mixing link in raw rubber；
1.3 sulfidization moldings obtain the high-performance rubber product.
2. preparation method according to claim 1, which is characterized in that the heating temperature is corresponding balance in sulphur phasor
Gasification temperature under steam pressure.
3. a kind of preparation method of high-performance rubber, includes the following steps：
1.1 prepare the reinforced composites that sulphur uniformly coats；The reinforced composites that step 1.1 sulphur uniformly coats
Preparation method is：
3.1 are uniformly mixed sulphur presoma with reinforcing rubber material；
3.2 are sent into uniformly mixed material in consersion unit, and sulphur presoma decomposites active sulphur under the conditions of certain temperature
Atom is evenly distributed on the main supporting material surface of rubber, obtains sulphur uniformly rubber-coated reinforced composites；
1.2 are added to above-mentioned composite material rubber mixing link in raw rubber；
1.3 sulfidization moldings obtain the high-performance rubber product.
4. preparation method according to claim 3, which is characterized in that the sulphur presoma is CS2、H2S, benzenethiol, sulphur
One or more of phenol, dimethyl sulfoxide (DMSO).
5. preparation method according to claim 3, which is characterized in that the certain temperature condition is 160 DEG C -500 DEG C.
6. the preparation method according to claim 1 or 3, which is characterized in that the reinforcing rubber material is carbon black, hard charcoal
One or more of black, carbon nanotubes, graphene, staple fiber, zinc oxide.
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| CN201610910331.8A CN106633217B (en) | 2016-10-19 | 2016-10-19 | The preparation method of high-performance rubber |
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| CN201610910331.8A CN106633217B (en) | 2016-10-19 | 2016-10-19 | The preparation method of high-performance rubber |
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| CN107189104B (en) * | 2017-05-12 | 2019-05-17 | 北京化工大学 | A kind of preparation method being sustained sulphur |
| CN109134967A (en) * | 2018-08-15 | 2019-01-04 | 龙岩学院 | A kind of preparation method of the high antibacterial weight-reducing pull strap of high intensity |
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| JP2515976B2 (en) * | 1986-02-27 | 1996-07-10 | 日本ゼオン 株式会社 | Method for producing sulfur master batch |
| CN101698708B (en) * | 2009-10-21 | 2012-08-22 | 中国石油大学(北京) | Formula of raw materials for producing sulfur microcapsule capable of being used as rubber vulcanizing agent |
| CN102516616B (en) * | 2011-11-17 | 2014-05-21 | 特拓(青岛)轮胎技术有限公司 | Accessory ingredient pre-dispersed masterbatch used for refining sizing material and preparation method thereof |
| CN103788414B (en) * | 2013-12-23 | 2016-02-03 | 于文明 | A kind of preparation method of high-temperature stable steamed stuffed bun sulphur |
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Effective date of registration: 20181217 Address after: 221000 South Side of No.4 Road, Yangtun Town Industrial Park, Peixian County, Xuzhou City, Jiangsu Province Patentee after: Sayfo (Xuzhou) Co., nano science and technology Address before: 215123 Room 207, Building 99 Jinjihu Avenue, Suzhou Industrial Park, Jiangsu Province Patentee before: SUZHOU SAIFU DEBEI TRADE CO., LTD. |