CN104672583B - A kind of preparation method of rubber modifier - Google Patents
A kind of preparation method of rubber modifier Download PDFInfo
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- CN104672583B CN104672583B CN201510060241.XA CN201510060241A CN104672583B CN 104672583 B CN104672583 B CN 104672583B CN 201510060241 A CN201510060241 A CN 201510060241A CN 104672583 B CN104672583 B CN 104672583B
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- white carbon
- aminodiphenylamine
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Abstract
The present invention relates to the preparation method of a kind of rubber modifier, its technical scheme is: 4-aminodiphenylamine and white carbon mass ratio are 9:1 4:1；The preparation of rubber antioxidant comprises the following steps that: first puts in reactor by block 4-aminodiphenylamine, guarantees that the temperature of reactor is more than 80 DEG C simultaneously；Keeping the reaction temperature in reactor to control in 80 150 degree Celsius range, the stir speed (S.S.) of reactor can be 0 to 50 revs/min；Become liquid after 4-aminodiphenylamine melts completely, white carbon is slowly added into and is stirred continuously；Pulverulent mixture is cooled down, then sieves, grind, pack.The invention has the beneficial effects as follows: the serviceability of rubber can be substantially improved, after interpolation, make rubber have more preferable crosslinked action.
Description
Technical field
The present invention relates to a kind of chemical manufacturing process, particularly to the preparation method of a kind of rubber modifier.
Background technology
ADPA-S is to be mixed by adsorption reaction according to a certain percentage by 4-aminodiphenylamine and white carbon.4-aminodiphenylamine has another name called 4-
Aminodiphenylamine, English name is 4-Amino diphenylamine, No. CAS be 101-54-2 molecular formula be C12H12N2, molecule
Amount is 184.2371, is mainly used as the intermediate of dyestuff and auxiliary agent.White carbon be white powder X-ray amorphous silicic acid and
The general name of silicate product, is primarily referred to as precipitated silica, aerosil, superfine silicon dioxide gel and aeroge,
Also powder synthetic aluminium silicate and calcium silicates etc. are included.White carbon is porous material, and the available SiO2 nH2O of its composition represents,
Wherein nH2O is presented in surface hydroxyl.Can be dissolved in caustic alkali and Fluohydric acid., (fluoric acid removes for water insoluble, solvent and acid
Outward).High temperature resistant, do not fire, tasteless, odorless, there is good electrical insulating property.No. CAS is 10279-57-9, and molecular formula is H2O·
xO2Si.White carbon industry in developed country's startings such as America and Europes relatively early, starts to realize industry metaplasia during World War II
Produce.Since 20th century middle nineteen seventies, along with white carbon research is deepened continuously by western countries, it produces and application
Aspect has obtained developing on a large scale very much.To 2006, the production capacity of whole world white carbon about 1,300,000 tons (without China), it was Sino-German
The production capacity of state's Degussa, France Luo Na and the big multinational corporations of U.S. PPG tri-exceedes the half of world's total capacity.China's Linesless charcoal
Black-labour industry is started in 1958, originally slower development, and within 1984, output of white carbon black is 2,600 tons, and nineteen ninety output of white carbon black carries
High to 20,000 tons.Recently as the development of rubber industry, yield rapidly increases, and within 2008, Chinese output of white carbon black reaches
71.2 ten thousand tons, yield ranks first in the world, and has become the net exporter of white carbon.At present, Chinese white white carbon black industry defines
Foreign capitals (joint) company and domestic corporation the market competition structure deposited, the market competition is abundant.
The problem that presently, there are: the use value of white carbon and 4-aminodiphenylamine is low, currently used rubber modifier affects rubber
The serviceability of glue goods, the rubber impact of performance is poor, and after rubber modifier interpolation, the crosslinked action of rubber is poor.
Summary of the invention
The purpose of the present invention is aiming at the drawbacks described above that prior art exists, it is provided that the preparation side of a kind of rubber modifier
Method, is substantially improved the serviceability of rubber, makes rubber have more preferable crosslinked action after interpolation.
The preparation method of the rubber modifier that the present invention mentions, its technical scheme is: include 4-aminodiphenylamine and white carbon, and RT trains
Department and white carbon mass ratio are 9:1 4:1；
Its preparation method comprises the following steps that:
A, first block 4-aminodiphenylamine is put in reactor, guarantee that the temperature of reactor, more than 80 DEG C, makes training department simultaneously
Slowly can melt completely；
Reaction temperature in B, holding reactor controls in 80-150 degree Celsius range, and the stir speed (S.S.) of reactor can be
0 to 50 revs/min；
C, after 4-aminodiphenylamine melts completely, become liquid, white carbon is slowly added into and is stirred continuously, along with white carbon
It is continuously added solution and is gradually become pureed by liquid, after all being added by white carbon, become uniform powder, color under light
For darkviolet；
D, by pulverulent mixture cool down, then sieve, grind, pack, the screen cloth of employing is 80 eye mesh screens, pulverulent mixture
The percent of pass of middle particle diameter 1-0.1 accounts for 98%.
The above-mentioned reaction temperature in reactor is 125-135 degree Celsius.
The stir speed (S.S.) of above-mentioned reactor is 11-20 rev/min.
The invention has the beneficial effects as follows: the modified rubber agent composition that 4-aminodiphenylamine is made new advances by reaction preparation with white carbon
After, the serviceability of rubber can be substantially improved as new rubber modifier, after interpolation, make rubber have more preferably crosslinking
Effect, thus it is greatly improved the use value of white carbon and 4-aminodiphenylamine, it is applied to the interpolation of rubber chemicals, promotes market simultaneously
Competitiveness.
Detailed description of the invention
Embodiment 1: the preparation method of the rubber modifier that the present invention mentions is as follows:
Raw material includes that 4-aminodiphenylamine and white carbon, 4-aminodiphenylamine and white carbon mass ratio are 9:1, wherein 4-aminodiphenylamine, has another name called 4-ammonia
Base diphenylamines；The preparation of rubber modifier comprises the following steps that:
First block 4-aminodiphenylamine is put in reactor, guarantee that the temperature of reactor, at 80-150 DEG C, makes training department slow simultaneously
Slowly can melt completely, keep the temperature in reactor in certain temperature range, then control certain stir speed (S.S.), preferably
Speed control be 11-20 rev/min, white carbon is slowly added in liquid and constantly stir after 4-aminodiphenylamine melts completely
Mix, along with the solution that is continuously added of white carbon is gradually become pureed by liquid, after all being added by white carbon, become uniform powder
End, under light, color is darkviolet, is cooled down by pulverulent mixture, then sieves, grinds, and the size controlling after grinding is necessarily
Scope, screen cloth is 80 eye mesh screens, and in pulverulent mixture, the percent of pass of particle diameter 1-0.1 accounts for 98%, uses sealed barrier package,
This product can be substantially improved the serviceability of rubber, makes rubber have more preferable crosslinked action after interpolation.
Following table is that embodiment 1 does sample result, and effect is preferable
| Sequence number | Project | Measurement result | Remarks |
| 1 | Heating loss | 0.37% | |
| 2 | Ash | 25.35% | |
| 3 | Particle diameter | 13.33% | 80 mesh net percent of pass, 1-0.1 accounts for 98% |
| 4 | Fusing point | Existence conditions does not measures |
Embodiment 2: the preparation method of the rubber modifier that the present invention mentions is as follows:
Raw material includes that 4-aminodiphenylamine and white carbon, 4-aminodiphenylamine and white carbon mass ratio are 4:1, wherein 4-aminodiphenylamine, has another name called 4-ammonia
Base diphenylamines；The preparation of rubber modifier comprises the following steps that:
First block 4-aminodiphenylamine is put in reactor, guarantee that the temperature of reactor, at 80-150 DEG C, makes training department slow simultaneously
Slowly can melt completely, keep the temperature in reactor in certain temperature range, then control certain stir speed (S.S.), preferably
Speed control be 11-20 rev/min, white carbon is slowly added in liquid and constantly stir after 4-aminodiphenylamine melts completely
Mix, along with the solution that is continuously added of white carbon is gradually become pureed by liquid, after all being added by white carbon, become uniform powder
End, under light, color is darkviolet, is cooled down by pulverulent mixture, then sieves, grinds, and the size controlling after grinding is necessarily
Scope, screen cloth is 80 eye mesh screens, and in pulverulent mixture, the percent of pass of particle diameter 1-0.1 accounts for 98%, uses sealed barrier package,
This product can be substantially improved the serviceability of rubber, makes rubber have more preferable crosslinked action after interpolation.
Following table is that embodiment 1 does sample result, and effect is preferable
| Sequence number | Project | Measurement result | Remarks |
| 1 | Heating loss | 0.36% | |
| 2 | Ash | 23.35% | |
| 3 | Particle diameter | 14.33% | 80 mesh net percent of pass, 1-0.1 accounts for 98% |
| 4 | Fusing point | Existence conditions does not measures |
Embodiment 3: the preparation method of the rubber modifier that the present invention mentions is as follows:
Raw material includes that 4-aminodiphenylamine and white carbon, 4-aminodiphenylamine and white carbon mass ratio are 6:1, wherein 4-aminodiphenylamine, has another name called 4-ammonia
Base diphenylamines；The preparation of rubber modifier comprises the following steps that:
First block 4-aminodiphenylamine is put in reactor, guarantee that the temperature of reactor, at 125-135 DEG C, makes training department slow simultaneously
Slowly can melt completely, keep the temperature in reactor in certain temperature range, then control certain stir speed (S.S.), preferably
Speed control be 11-20 rev/min, white carbon is slowly added in liquid and constantly stir after 4-aminodiphenylamine melts completely
Mix, along with the solution that is continuously added of white carbon is gradually become pureed by liquid, after all being added by white carbon, become uniform powder
End, under light, color is darkviolet, is cooled down by pulverulent mixture, then sieves, grinds, and the size controlling after grinding is necessarily
Scope, screen cloth is 80 eye mesh screens, and in pulverulent mixture, the percent of pass of particle diameter 1-0.1 accounts for 98%, uses sealed barrier package,
This product can be substantially improved the serviceability of rubber, makes rubber have more preferable crosslinked action after interpolation.
Following table is that embodiment 3 does sample result, and effect is preferable
| Sequence number | Project | Measurement result | Remarks |
| 1 | Heating loss | 0.34% | |
| 2 | Ash | 25.65% | |
| 3 | Particle diameter | 13.23% | 80 mesh net percent of pass, 1-0.1 accounts for 98% |
| 4 | Fusing point | Existence conditions does not measures |
Above-mentioned 3 embodiments can be substantially improved the serviceability of rubber as new rubber modifier, after interpolation
Making rubber have more preferable crosslinked action, thus be greatly improved the use value of white carbon and 4-aminodiphenylamine, it is applied to rubber chemicals
Interpolation, promote the competitiveness in market simultaneously.
Claims (1)
1. a preparation method for rubber modifier, is characterized in that: include 4-aminodiphenylamine and white carbon, 4-aminodiphenylamine and white carbon quality
Ratio is 6:1；Its preparation method comprises the following steps that:
A, first block 4-aminodiphenylamine is put in reactor, guarantee that the temperature of reactor, more than 80 DEG C, makes training department slowly simultaneously
Can melt completely；
Reaction temperature in B, holding reactor controls in 125-135 degree Celsius range, and the stir speed (S.S.) of reactor can be 11-
20 revs/min；
C, after 4-aminodiphenylamine melts completely, become liquid, white carbon is slowly added into and is stirred continuously, continuous along with white carbon
Adding solution and gradually become pureed by liquid, become uniform powder after all being added by white carbon, under light, color is deep
Purple；
D, by pulverulent mixture cool down, then sieve, grind, pack, the screen cloth of employing is 80 eye mesh screens, grain in pulverulent mixture
The percent of pass in footpath 1-0.1 accounts for 98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510060241.XA CN104672583B (en) | 2015-02-05 | 2015-02-05 | A kind of preparation method of rubber modifier |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510060241.XA CN104672583B (en) | 2015-02-05 | 2015-02-05 | A kind of preparation method of rubber modifier |
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|---|---|
| CN104672583A CN104672583A (en) | 2015-06-03 |
| CN104672583B true CN104672583B (en) | 2017-01-04 |
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| US9284443B2 (en) * | 2011-06-21 | 2016-03-15 | E. I. Du Pont De Nemours And Company | Heat-stabilized acrylate elastomer composition and process for its production |
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Effective date of registration: 20170601 Address after: 257000 Dongying Port Economic Development Zone, Shandong Port Road, north of Hong Kong, west of Port Road, west of the road three Patentee after: Shandong EKESEN Chemical Co., Ltd. Address before: 257000 Dongying Port Economic Development Zone, Shandong Port Road, north of Hong Kong, west of Port Road, west of the road three Patentee before: Shandong Ai Kesen novel material company limited |
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