CN102127228B - Production process for synthesizing methyl vinyl silicone rubber - Google Patents
Production process for synthesizing methyl vinyl silicone rubber Download PDFInfo
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- CN102127228B CN102127228B CN 201110021460 CN201110021460A CN102127228B CN 102127228 B CN102127228 B CN 102127228B CN 201110021460 CN201110021460 CN 201110021460 CN 201110021460 A CN201110021460 A CN 201110021460A CN 102127228 B CN102127228 B CN 102127228B
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- polymerizer
- time
- low molecule
- raw material
- tubular type
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 7
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 title abstract description 8
- 229920002379 silicone rubber Polymers 0.000 title abstract description 8
- 239000004945 silicone rubber Substances 0.000 title abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- -1 dimethyl cyclic siloxane Chemical class 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 238000007701 flash-distillation Methods 0.000 claims description 12
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 229920001971 elastomer Polymers 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 125000003368 amide group Chemical group 0.000 claims description 2
- 235000021050 feed intake Nutrition 0.000 claims description 2
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- 238000005987 sulfurization reaction Methods 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000007799 cork Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention relates to a production process for synthesizing methyl vinyl silicone rubber, characterized by adopting a tubular polymerizer and a two-flash technology, using dimethyl cyclic siloxane or octamethylcy-clotetrasiloxane as a raw material, and comprising the concrete steps of: measuring, dehydrating, adding auxiliaries, polymerizing, cracking a catalyst, flashing for the first time and flashing for the second time. The production process provided by the invention has high operating flexibility and strong process controllability, and has a good mass transfer device and a sufficientheat exchange area, thus improving the molecular weight distribution; the flow direction of material can be easily changed by communicating pipelines at the inlet/outlet of the tubular polymerizer, thus removing and cleaning the tubular polymerizer in time; the reaction condition in the tubular polymerizer can be analyzed on line at any time, thus facilitating intermediate control and adjustment of the process formula and processing conditions in time; and an additional flash device is arranged, thus being conductive to the reduction of burden of a vacuum system and stabilization of the product quality.
Description
Technical field
The present invention relates to rubber production, particularly a kind of production technique of synthesizing methyl vinylsiloxane rubber.
Background technology
The historical evolution of high temperature vulcanized methyl vinyl silicone rubber synthesis technique is very long.Be combined to from initial intermittence, develop into, stir the application of polymerization and high temperature high vacuum flash evaporation technology, thereby completed the operation of serialization.Be subject at that time the limitation of whole mechanical process capacity, and can't have made the device extension of single cover, therefore also just be confined to the ability of pilot scale.So also just development, changed the main body of static mixer as polyreaction into.But, from having moved the situation of several years, the throughput of unit, demand that still far away can't satisfying the market.And after operation for many years, also found this streamline, also exist limitation itself that can't go beyond.In order to improve matter exchange and heat exchange, improve the efficient of polyreaction for this reason.Be also methyl ethylene high temperature to be vulcanized the demand of the multiple trade mark in order to adapt to market, and on stand-alone device, switching that can be convenient has developed again the stirring reaction operational path with helical-ribbon type.
Above-mentioned production technique is each has something to recommend him, cuts both ways.
Summary of the invention
In order further to improve the unit production capacity, more effectively improve matter exchange and heat exchange in polyreaction, make the molecular weight distribution of product more reasonable, improve processing characteristics and the quality of product, the invention provides a kind of production technique of synthesizing methyl vinylsiloxane rubber.
The production technique of synthesizing methyl vinylsiloxane rubber of the present invention has adopted the tubular type polymerizer, and has configured flash evaporation technology twice;
Its concrete steps are as follows:
1) the dimethyl cyclosiloxane raw material in feed sump uses vacuum to be pumped into the raw material scale tank, carries out accurate-metering;
2) by the design according to formula of the low molecule that produces in the dimethyl cyclosiloxane raw material after accurate measurement and reaction process, enter in vacuum dewatering plant, the Trace water that removes in material divides;
3) material after dewatering process is completed and catalyzer, molecular weight regulator and other auxiliary agent enter batching kettle, stir;
4) use rare gas element that material is pressed in the tubular type polymerizer, through different tube diameters scientific combination, pass through the tubular type continuous break-in of polymerizer internal part and backflow, make material carry out sufficient heat exchange and matter exchange, the pressure that gives by rare gas element guarantees the enough polymerization time of material in polymerizer;
5) material flows into for the first time in flash distillation plant, top at the first flasher makes the catalyst decomposes inoperative novel compound of this product in pairs through high temperature, then under the promotion of rare gas element, the bottom of the first flasher is again high vacuum, shifts out the low molecule of unreacted;
6) material flows into second stage flash distillation plant, more further removes low molecule, to ensure the quality of products fully;
7) the low molecule that produces in vacuum dewatering plant, tubular type polymerizer, first step flash distillation plant and second stage flash distillation plant, turn back in low molecule storage tank, incorporate dimethyl cyclosiloxane raw material into and jointly enter into vacuum dewatering plant participation reaction after low molecule scale tank metering.
Described catalyzer adopts: with the organic hydroxide of amido; Organic hydroxide with the phosphorus base; Or alkali-metal oxyhydroxide, its add-on is 5/100000ths to 2/10000ths of the total amount that feeds intake.
Described molecular weight regulator adopts: R
1[(CH
3)
2SiO]
nR
2, R wherein
1And R
2Can be identical, also can be different.R
1And R
2Alkyl or be alkylene, n is the positive integer of 1-20, its add-on is to feed intake one of the percentage of total amount to ten Percent.
Described auxiliary agent adopts: [R
3R
1SiO]
M, R
2Alkyl, R
1Be alkylene, m is the positive integer of 1-8; Can be also that its molecule signal formula is: (CH with the polymkeric substance of the linearity of the Si oxide of polyenoid alkyl
3)
3[R
5R
6SiO]
a(CH
3)
3, R wherein
5Alkyl, R
6It is alkylene.Its add-on is the 0-5% of total amount of feeding intake.
Described dimethyl cyclosiloxane and octamethylcyclotetrasiloxane all can use.
The production technique of the synthetic sulfuration of the present invention methyl vinyl silicone rubber has following superiority:
1) turndown ratio is large, and process controllability is strong;
2) device of good matter exchange and the area of heat exchange are fully arranged, improved molecular weight distribution, be conducive to next step the processing characteristics of this product;
3) occur to flow when smooth when material, perhaps when just driving, UNICOM's pipeline of import and export that can be by the tubular type polymerizer changes the flow direction of material like a cork, in time gets rid of and clears up the tubular type polymerizer;
4) response situation of on-line analysis at any time in the tubular type polymerizer, be convenient to intermediate controlled, in time adjusting process composition and engineering condition;
5) increased by a cover flash distillation plant, be conducive to alleviate the burden of vacuum system, more be beneficial to the stable of quality product;
Description of drawings
Fig. 1 is the schema of the production technique of the synthetic sulfuration of the present invention methyl vinyl silicone rubber.
Embodiment
Below in conjunction with embodiment, the production technique of the synthetic sulfuration of the present invention methyl vinyl silicone rubber is done detailed explanation.
Fig. 1 is the schema of the production technique of the synthetic sulfuration of the present invention methyl vinyl silicone rubber.
The production technique of the synthetic sulfuration of the present invention methyl vinyl silicone rubber has adopted the tubular type polymerizer, and has configured flash evaporation technology twice; Can use dimethyl cyclosiloxane (DMC) to make raw material, also can use octamethylcyclotetrasiloxane (D4) to make raw material;
Its concrete steps are as follows:
1) the dimethyl cyclosiloxane in feed sump or octamethylcyclotetrasiloxane raw material use vacuum to be pumped into the raw material scale tank, carry out accurate-metering;
2) by the design according to formula of the low molecule that produces in the dimethyl cyclosiloxane after accurate measurement or octamethylcyclotetrasiloxane raw material and reaction process, enter in vacuum dewatering plant, the Trace water that removes in material divides; The condition of vacuum hydro-extraction is that interior temperature control is at 35-75 ℃; Vacuum degree control is at-750mmHg--650mm Hg; Dewatering time is 1-4 hour; The amount of blasting of rare gas element must be that material stirs uniformly, constantly updates liquid level, and the vacuum tightness of dehydration is kept in the scope of technique license.
3) material after dewatering process is completed and catalyzer (), molecular weight regulator () and other auxiliary agent () enter batching kettle, stir;
4) use rare gas element that material is pressed in the tubular type polymerizer, through different tube diameters scientific combination, pass through the tubular type continuous break-in of polymerizer internal part and backflow, make material carry out sufficient heat exchange and matter exchange, the pressure that gives by rare gas element guarantees the enough polymerization time of material in polymerizer; The processing condition of polyreaction are that the temperature of charge of controlling in the pipeline polymerizer is between 95 ℃-115 ℃, and interior temperature cannot be over 115 ℃; Keep the residence time of material in the tubular type polymerizer to be not less than 3 hours, whole polymerization is to carry out under the protection of rare gas element.
5) material flows into for the first time in flash distillation plant, top at the first flasher makes the catalyst decomposes inoperative novel compound of this product in pairs through high temperature, require the temperature of catalyst breakage to be strict controlled in 145 ℃-160 ℃, make material in the residence time 〉=0.5, top of flasher hour.Applying 0-1.0Pa. above flasher by rare gas element then under the promotion at rare gas element, the bottom of the first flasher is again high vacuum, its vacuum tightness requires at-750mm Hg--720mm Hg, the chuck of flasher below is by the continuous heating cycle of thermal barrier, require the temperature of thermal barrier to be controlled between 175 ℃-190 ℃, under the severe condition of high vacuum and high temperature, shift out unreacted low molecule and be decomposed into polymkeric substance is not had effective novel compound.
6) material flows into second stage flash distillation plant, more further removes low molecule, to ensure the quality of products fully; The same with in the first flasher of concrete processing requirement.
7) the low molecule that produces in vacuum dewatering plant, tubular type polymerizer, first step flash distillation plant and second stage flash distillation plant, turn back in low molecule storage tank, incorporate dimethyl cyclosiloxane raw material into and jointly enter into vacuum dewatering plant participation reaction after low molecule scale tank metering.
Claims (1)
1. the production technique of a synthesizing methyl vinylsiloxane rubber, adopted the tubular type polymerizer, and configured flash evaporation technology twice, it is characterized in that: described production technique concrete steps are as follows:
1) the dimethyl cyclosiloxane raw material in feed sump uses vacuum to be pumped into the raw material scale tank, carries out accurate-metering;
2) by the design according to formula of the low molecule that produces in the dimethyl cyclosiloxane raw material after accurate measurement and reaction process, enter in vacuum dewatering plant, the Trace water that removes in material divides;
3) material after dewatering process is completed and catalyzer, molecular weight regulator and other auxiliary agent enter batching kettle, stir;
Described catalyzer adopts: with organic hydroxide or the alkali-metal oxyhydroxide of amido; Its add-on is 5/100000ths to 2/10000ths of the total amount that feeds intake;
Described molecular weight regulator adopts: R
1[(CH
3)
2SiO]
nR
2, R wherein
1And R
2Identical, or different, R
1And R
2For alkyl or be alkylene, n is the positive integer of 1-20, and its add-on is to feed intake one of the percentage of total amount to ten Percent;
Described auxiliary agent adopts: [R
3R
4SiO]
M, R
3Alkyl, R
4Be alkylene, m is the positive integer of 3-10; Or with the polymkeric substance of the linearity of the Si oxide of polyenoid alkyl, its molecule signal formula is: (CH
3)
3[R
5R
6SiO]
a(CH
3)
3, R wherein
5Alkyl, R
6Be alkylene, its add-on is the 0-5% of total amount of feeding intake;
4) use rare gas element that material is pressed in the tubular type polymerizer, through different tube diameters scientific combination, pass through the tubular type continuous break-in of polymerizer internal part and backflow, make material carry out sufficient heat exchange and matter exchange, the pressure that gives by rare gas element guarantees the enough polymerization time of material in polymerizer;
5) material flows into the first flasher, and broken matchmaker is on the top of flasher, and at high temperature catalyst decomposes is reacted inoperative novel compound in pairs;
6) material after broken matchmaker the upper pressure bottom that rare gas element arranged with the first flasher of high vacuum in device, shift out the low molecule of unreacted;
7) material flows into second stage flash distillation plant, more further removes low molecule, to ensure the quality of products fully;
8) the low molecule that produces in vacuum dewatering plant, tubular type polymerizer, first step flash distillation plant, second stage flash distillation plant, turn back in low molecule storage tank, incorporate dimethyl cyclosiloxane raw material into and jointly enter into vacuum dewatering plant participation reaction after low molecule scale tank metering.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110021460 CN102127228B (en) | 2011-01-19 | 2011-01-19 | Production process for synthesizing methyl vinyl silicone rubber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110021460 CN102127228B (en) | 2011-01-19 | 2011-01-19 | Production process for synthesizing methyl vinyl silicone rubber |
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|---|---|
| CN102127228A CN102127228A (en) | 2011-07-20 |
| CN102127228B true CN102127228B (en) | 2013-06-19 |
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044684A (en) * | 2011-10-17 | 2013-04-17 | 颜建平 | 35000-ton-scale intermittent kettle type methyl vinyl silicone rubber production process |
| CN104592517A (en) * | 2014-12-23 | 2015-05-06 | 安徽助成信息科技有限公司 | Synthesis method of methyl vinyl silicone raw rubber |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787876A (en) * | 2003-06-04 | 2006-06-14 | 埃克森美孚化学专利公司 | Tubular polymerization reactors and polymerization process using same |
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|---|---|---|---|---|
| US20040109853A1 (en) * | 2002-09-09 | 2004-06-10 | Reactive Surfaces, Ltd. | Biological active coating components, coatings, and coated surfaces |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1787876A (en) * | 2003-06-04 | 2006-06-14 | 埃克森美孚化学专利公司 | Tubular polymerization reactors and polymerization process using same |
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