CN108084504A - A kind of method for synthesizing ageing-resistant natural rubber - Google Patents
A kind of method for synthesizing ageing-resistant natural rubber Download PDFInfo
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- CN108084504A CN108084504A CN201611023348.8A CN201611023348A CN108084504A CN 108084504 A CN108084504 A CN 108084504A CN 201611023348 A CN201611023348 A CN 201611023348A CN 108084504 A CN108084504 A CN 108084504A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/04—Carbon
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
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Abstract
The invention belongs to technical field of rubber material, are related to a kind of method for synthesizing ageing-resistant natural rubber.A kind of method for synthesizing ageing-resistant natural rubber, including（1）Old silane coupling agent is prevented in synthesis：γ glycidyl ether oxygen propyl trimethoxy silicanes and mutual-amido two polyaniline are added in reaction kettle, are passed through 0.2 0.6MPa of nitrogen, 120 150 DEG C of heating temperature, anti-old silane coupling agent is made in 100 120r/min of speed of agitator, 1 1.5h of mixing time；（2）In-situ modified filler：It weighs carbon black, white carbon and prevents that old silane coupling agent is put into reaction kettle, lead to N20.1 0.2 MPa of gas is heated to 50 60 DEG C, and in-situ modified filler is made in 100 120r/min of speed of agitator, 1 1.5h of mixing time.Preparation method of the present invention improves the ageing-resistant physical property of rubber using the anti-old coupling agent modified filler preparation anti-aging natural rubber of addition, and easy to operate, and ageing-resistant rubber prepared by the present invention has many advantages, such as that intensity is high and ageing-resistant performance is strong.
Description
Technical field
The invention belongs to technical field of rubber material, are related to a kind of method for synthesizing ageing-resistant natural rubber.
Background technology
Natural rubber (NR) is most widely used general purpose rubber, but double bond excessive in its molecular structure causes to make
Product are easy to aging.The application of anti-aging agent substantially prolongs the service life of rubber, but general anti-aging agent is readily volatilized and migrates,
This not only causes product properties to be deteriorated, while also pollutes environment, endangers human health.And it is used in rubber industry silane coupled
Agent is almost silane coupler containing sulfur entirely, particularly multi-sulfur silane coupling agent.Traditional coupling agent Si69 needs mixed in use
It is high to refine temperature, easily causes sizing material incipient scorch, and there are the sizing material porosity it is higher the drawbacks of.
With the structure of silane coupling agent to improve rubber/filler interaction as simple purpose, if it can be in coupling agent
One end other functional groups of grafting, can just be assigned while white carbon reinforcing property is improved its corresponding function can be on
The report of this respect work is seldom, and therefore, developing a kind of ageing-resistant rubber of new anti-old coupling agent filling is very important.
The content of the invention
In view of the problems of the existing technology, it is an object of the invention to provide a kind of sides for synthesizing ageing-resistant natural rubber
Method.Preparation method of the present invention prepares anti-aging natural rubber using the anti-old coupling agent modified filler of addition and improves the resistance to old of rubber
Change physical property, and it is easy to operate.Ageing-resistant rubber prepared by the present invention has many advantages, such as that intensity is high and ageing-resistant performance is strong.
In order to solve the above technical problems, the technical solution adopted by the present invention is.
A kind of method for synthesizing ageing-resistant natural rubber, step are as follows：
（1）Old silane coupling agent is prevented in synthesis
γ-glycidyl ether oxygen propyl trimethoxy silicane and mutual-amido two polyaniline are added in reaction kettle, are passed through nitrogen 0.2-
0.6MPa, 120-150 DEG C of heating temperature, speed of agitator 100-120r/min, mixing time 1-1.5h are made anti-old silane coupled
Agent；
（2）In-situ modified filler
It weighs carbon black, white carbon and prevents that old silane coupling agent is put into reaction kettle, lead to N2Gas 0.1-0.2 MPa, heat temperature raising
To 50-60 DEG C, in-situ modified filler is made in speed of agitator 100-120r/min, mixing time 1-1.5h；
（3）It plasticates
It weighs natural rubber to be put into open mill, thin 8-10 times logical, adjustment roll spacing is 0.3-0.8mm, makes sizing material bag roller；
（4）It is kneaded
By step（3）Sizing material put into kneading machine, add in in-situ modified filler, then sequentially add zinc oxide, stearic acid, anti-
Old agent, accelerating agent and vulcanizing agent are kneaded, rotor speed 80-100r/min, time 10-35min, then are put into out
Mixed packing clot is carried out in mill, it is thin 5-8 times logical, roll spacing is 1-1.5mm slices；
（5）Vulcanization
By step（4）Product be placed on vulcanizing press and vulcanize, curing temperature is 170-190 DEG C, vulcanization time 10-
15min is to get finished product.
The step（1）In the γ-glycidyl ether oxygen propyl trimethoxy silicane and the mutual-amido two polyaniline
Molar ratio be 1:1-2.
The step（2）In by ratio of weight and the number of copies be carbon black：White carbon：Prevent old silane coupling agent=1:1.5-2:0.2-
0.5。
The step（4）In packing number for 3-5 time, clot number is 2-6 times.
Beneficial effects of the present invention：The present invention reduces the viscosity of rubber material using the addition for preventing old coupling agent, sulfuric
Change time shortening, the dispersiveness of modified white carbon is improved significantly with preferable thermal stability, preferable aging
Energy.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply for the feature and advantage that further illustrate the present invention rather than to the claims in the present invention
Limitation.
Embodiment 1
A kind of ageing-resistant native rubber composite material, is prepared by the raw material of following parts by weight：It is 135 parts of natural rubber, white
45 parts of carbon black VN3,35 parts of carbon black N330,6 parts of zinc oxide, 4 parts of stearic acid, anti-old 3 parts of coupling agent, 8 parts of captax and sulphur
3 parts of agent sulphur.
Preparation method, step are as follows：
（1）Old silane coupling agent is prevented in synthesis
γ-glycidyl ether oxygen propyl trimethoxy silicane and mutual-amido two polyaniline are added in reaction kettle, the γ-shrink is sweet
The molar ratio of oily ether oxygen propyl trimethoxy silicane and the mutual-amido two polyaniline is 1:1-2 is passed through nitrogen 0.2-0.6MPa, adds
Anti- old silane coupling agent is made in hot 120-150 DEG C of temperature, speed of agitator 100-120r/min, mixing time 1-1.5h；
（2）In-situ modified filler
It weighs carbon black, white carbon and prevents that old silane coupling agent is put into reaction kettle, lead to N2Gas 0.1-0.2 MPa, heat temperature raising
To 50-60 DEG C, in-situ modified filler is made in speed of agitator 100-120r/min, mixing time 1-1.5h；
（3）It plasticates
It weighs natural rubber to be put into open mill, thin 8-10 times logical, adjustment roll spacing is 0.3-0.8mm, makes sizing material bag roller；
（4）It is kneaded
By step（3）Sizing material put into kneading machine, add in in-situ modified filler, then sequentially add zinc oxide, stearic acid, anti-
Old agent, accelerating agent and vulcanizing agent are kneaded, rotor speed 80-100r/min, time 10-35min, then are put into out
Carried out in mill it is mixed be packaged clot, it is 3-5 time to be packaged number, and clot number is 2-6 times, thin 5-8 times logical, roll spacing is 1-
1.5mm slice；
（5）Vulcanization
By step（4）Product be placed on vulcanizing press and vulcanize, curing temperature is 170-190 DEG C, vulcanization time 10-
15min is to get finished product.
Embodiment 2
A kind of ageing-resistant native rubber composite material, is prepared by the raw material of following parts by weight：It is 130 parts of natural rubber, white
44 parts of carbon black VN3,38 parts of carbon black N330,7 parts of zinc oxide, 4 parts of stearic acid, anti-old 3 parts of coupling agent, 7 parts of diphenylguanidine and sulphur
3 parts of agent sulphur.
Preparation method, step are as follows：
（1）Old silane coupling agent is prevented in synthesis
γ-glycidyl ether oxygen propyl trimethoxy silicane and mutual-amido two polyaniline are added in reaction kettle, the γ-shrink is sweet
The molar ratio of oily ether oxygen propyl trimethoxy silicane and the mutual-amido two polyaniline is 1:1-2 is passed through nitrogen 0.2-0.6MPa, adds
Anti- old silane coupling agent is made in hot 120-150 DEG C of temperature, speed of agitator 100-120r/min, mixing time 1-1.5h；
（2）In-situ modified filler
It weighs carbon black, white carbon and prevents that old silane coupling agent is put into reaction kettle, lead to N2Gas 0.1-0.2 MPa, heat temperature raising
To 50-60 DEG C, in-situ modified filler is made in speed of agitator 100-120r/min, mixing time 1-1.5h；
（3）It plasticates
It weighs natural rubber to be put into open mill, thin 8-10 times logical, adjustment roll spacing is 0.3-0.8mm, makes sizing material bag roller；
（4）It is kneaded
By step（3）Sizing material put into kneading machine, add in in-situ modified filler, then sequentially add zinc oxide, stearic acid, anti-
Old agent, accelerating agent and vulcanizing agent are kneaded, rotor speed 80-100r/min, time 10-35min, then are put into out
Carried out in mill it is mixed be packaged clot, it is 3-5 time to be packaged number, and clot number is 2-6 times, thin 5-8 times logical, roll spacing is 1-
1.5mm slice；
（5）Vulcanization
By step（4）Product be placed on vulcanizing press and vulcanize, curing temperature is 170-190 DEG C, vulcanization time 10-
15min is to get finished product.
Embodiment 3
A kind of ageing-resistant native rubber composite material, is prepared by the raw material of following parts by weight：It is 140 parts of natural rubber, white
48 parts of carbon black VN3,39 parts of carbon black N330,8 parts of zinc oxide, 4 parts of stearic acid, anti-old 3 parts of coupling agent, 8 parts of captax and sulphur
4 parts of agent sulphur.
Preparation method, step are as follows：
（1）Old silane coupling agent is prevented in synthesis
γ-glycidyl ether oxygen propyl trimethoxy silicane and mutual-amido two polyaniline are added in reaction kettle, the γ-shrink is sweet
The molar ratio of oily ether oxygen propyl trimethoxy silicane and the mutual-amido two polyaniline is 1:1-2 is passed through nitrogen 0.2-0.6MPa, adds
Anti- old silane coupling agent is made in hot 120-150 DEG C of temperature, speed of agitator 100-120r/min, mixing time 1-1.5h；
（2）In-situ modified filler
It weighs carbon black, white carbon and prevents that old silane coupling agent is put into reaction kettle, lead to N2Gas 0.1-0.2 MPa, heat temperature raising
To 50-60 DEG C, in-situ modified filler is made in speed of agitator 100-120r/min, mixing time 1-1.5h；
（3）It plasticates
It weighs natural rubber to be put into open mill, thin 8-10 times logical, adjustment roll spacing is 0.3-0.8mm, makes sizing material bag roller；
（4）It is kneaded
By step（3）Sizing material put into kneading machine, add in in-situ modified filler, then sequentially add zinc oxide, stearic acid, anti-
Old agent, accelerating agent and vulcanizing agent are kneaded, rotor speed 80-100r/min, time 10-35min, then are put into out
Carried out in mill it is mixed be packaged clot, it is 3-5 time to be packaged number, and clot number is 2-6 times, thin 5-8 times logical, roll spacing is 1-
1.5mm slice；
（5）Vulcanization
By step（4）Product be placed on vulcanizing press and vulcanize, curing temperature is 170-190 DEG C, vulcanization time 10-
15min is to get finished product.
First, performance detection
Hardness（Shao Er A）It is tested according to GB/T 531-1999；Tensile strength and elongation rate of tensile failure are according to GB/T 528-
1998 are tested；Thermogravimetic analysis (TGA) is tested according to ISO11358-1997.
1st, performance detection, comparison knot are carried out to embodiment 1-3 and the comparative example 1 ageing-resistant native rubber composite material prepared
Fruit such as table 1.
Ageing-resistant native rubber composite material rationality index contrast table prepared by 1 embodiment 1-3 of table and comparative example 1.
| Project/number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Tensile strength/MPa | 28 | 29 | 30 | 20 |
| Elongation rate of tensile failure/% | 798 | 826 | 815 | 736 |
| Hardness（Shao Er A） | 67 | 65 | 64 | 56 |
| Elongation rate of tensile failure variation/%（300 DEG C × 48h agings） | -28 | -26 | -28 | -32 |
| Firmness change rate, % | -4.56 | -3.78 | -3.79 | -10.66 |
| Tensile strength change rate, % | -13.7 | -13.8 | -12.5 | -23.56 |
As shown in Table 1, it is of the invention in tensile strength, elongation rate of tensile failure, hardness（Shao Er A）, elongation rate of tensile failure variation/%
（300 DEG C × 48h agings）, firmness change rate and tensile strength change rate etc. better than comparative example 1, illustrate that the present invention has
Good ageing-resistant performance.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
The described technical solution of inventive embodiments, it will be understood by those of ordinary skill in the art that, still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect；As long as meeting using needs, all protection scope of the present invention it
It is interior.
Claims (4)
- A kind of 1. method for synthesizing ageing-resistant natural rubber, which is characterized in that step is as follows：（1）Old silane coupling agent is prevented in synthesisγ-glycidyl ether oxygen propyl trimethoxy silicane and mutual-amido two polyaniline are added in reaction kettle, are passed through nitrogen 0.2- 0.6MPa, 120-150 DEG C of heating temperature, speed of agitator 100-120r/min, mixing time 1-1.5h are made anti-old silane coupled Agent；（2）In-situ modified fillerIt weighs carbon black, white carbon and prevents that old silane coupling agent is put into reaction kettle, lead to N2Gas 0.1-0.2 MPa, are heated to 50-60 DEG C, in-situ modified filler is made in speed of agitator 100-120r/min, mixing time 1-1.5h；（3）It plasticatesIt weighs natural rubber to be put into open mill, thin 8-10 times logical, adjustment roll spacing is 0.3-0.8mm, makes sizing material bag roller；（4）It is kneadedBy step（3）Sizing material put into kneading machine, add in in-situ modified filler, then sequentially add zinc oxide, stearic acid, anti- Old agent, accelerating agent and vulcanizing agent are kneaded, rotor speed 80-100r/min, time 10-35min, then are put into out Mixed packing clot is carried out in mill, it is thin 5-8 times logical, roll spacing is 1-1.5mm slices；（5）VulcanizationBy step（4）Product be placed on vulcanizing press and vulcanize, curing temperature is 170-190 DEG C, vulcanization time 10- 15min is to get finished product.
- 2. the method for the ageing-resistant natural rubber of synthesis according to claim 1, which is characterized in that the step（1）In The molar ratio of the γ-glycidyl ether oxygen propyl trimethoxy silicane and the mutual-amido two polyaniline is 1:1-2.
- 3. the method for the ageing-resistant natural rubber of synthesis according to claim 1, it is characterised in that：The step（2）In It is carbon black by ratio of weight and the number of copies：White carbon：Prevent old silane coupling agent=1:1.5-2:0.2-0.5.
- 4. the method for the ageing-resistant natural rubber of synthesis according to claim 1, it is characterised in that：The step（4）In It is 3-5 times to be packaged number, and clot number is 2-6 times.
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| CN201611023348.8A CN108084504A (en) | 2016-11-21 | 2016-11-21 | A kind of method for synthesizing ageing-resistant natural rubber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864690A (en) * | 2018-06-13 | 2018-11-23 | 无锡市华美电缆有限公司 | A kind of fatigue proof composite cable material of flexibility and preparation method thereof |
| CN109135345A (en) * | 2018-08-01 | 2019-01-04 | 安徽锦华氧化锌有限公司 | A kind of method of the rubber product anti-old coupling agent modified Nano carbon white of ionic liquid- |
| CN109879903A (en) * | 2019-01-09 | 2019-06-14 | 青岛科技大学 | One kind is novel to prevent old silane coupling agent and preparation method thereof |
| CN112521609A (en) * | 2020-12-31 | 2021-03-19 | 常州市五洲化工有限公司 | Preparation method of oil-resistant sealing modified anti-aging agent |
| CN114685903A (en) * | 2022-05-07 | 2022-07-01 | 安徽潜隆机电科技有限公司 | Rubber for gas mask cover |
| CN114957812A (en) * | 2022-06-08 | 2022-08-30 | 江苏麒祥高新材料有限公司 | Rubber composition, preparation method thereof and rubber product |
| CN116063759A (en) * | 2023-03-06 | 2023-05-05 | 三门县质量技术服务中心(三门县产品质量检验所、三门县计量检定测试所) | Method for preparing rubber composition and rubber obtained by same |
| CN117511006A (en) * | 2023-07-31 | 2024-02-06 | 云南国为机械科技有限公司 | Rubber shock pad and preparation process thereof |
-
2016
- 2016-11-21 CN CN201611023348.8A patent/CN108084504A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864690A (en) * | 2018-06-13 | 2018-11-23 | 无锡市华美电缆有限公司 | A kind of fatigue proof composite cable material of flexibility and preparation method thereof |
| CN109135345A (en) * | 2018-08-01 | 2019-01-04 | 安徽锦华氧化锌有限公司 | A kind of method of the rubber product anti-old coupling agent modified Nano carbon white of ionic liquid- |
| CN109879903A (en) * | 2019-01-09 | 2019-06-14 | 青岛科技大学 | One kind is novel to prevent old silane coupling agent and preparation method thereof |
| CN112521609A (en) * | 2020-12-31 | 2021-03-19 | 常州市五洲化工有限公司 | Preparation method of oil-resistant sealing modified anti-aging agent |
| CN114685903A (en) * | 2022-05-07 | 2022-07-01 | 安徽潜隆机电科技有限公司 | Rubber for gas mask cover |
| CN114957812A (en) * | 2022-06-08 | 2022-08-30 | 江苏麒祥高新材料有限公司 | Rubber composition, preparation method thereof and rubber product |
| CN116063759A (en) * | 2023-03-06 | 2023-05-05 | 三门县质量技术服务中心(三门县产品质量检验所、三门县计量检定测试所) | Method for preparing rubber composition and rubber obtained by same |
| CN117511006A (en) * | 2023-07-31 | 2024-02-06 | 云南国为机械科技有限公司 | Rubber shock pad and preparation process thereof |
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