CN102516283A - Method for producing DMC material by silicone low-ring opening process - Google Patents
Method for producing DMC material by silicone low-ring opening process Download PDFInfo
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- CN102516283A CN102516283A CN2011104022010A CN201110402201A CN102516283A CN 102516283 A CN102516283 A CN 102516283A CN 2011104022010 A CN2011104022010 A CN 2011104022010A CN 201110402201 A CN201110402201 A CN 201110402201A CN 102516283 A CN102516283 A CN 102516283A
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- dmc
- low
- open loop
- ring
- producing
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 238000007142 ring opening reaction Methods 0.000 title abstract 5
- 229920001296 polysiloxane Polymers 0.000 title abstract 3
- 238000005336 cracking Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005070 sampling Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- -1 temperature control Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Silicon Polymers (AREA)
Abstract
The present invention relates to a method for producing a DMC material, and especially relates to the method for producing the DMC material by silicone low-ring opening process through using a silicone low-ring opening technology. The method comprises the following steps delivering the low-ring material from a low ring tank to a reactor; heating the material to 65 DEG C, standing for a period to stratify and drain the lower acidic water; adding a KOH catalyst and keeping the temperature at 65-100 DEG C for carrying out D3 ring opening; sampling and observing the state of the open-loop material, adding water when the requirement is satisfied; conversing the material from the reactor to the tank, waiting for cracking, distilling to produce the DMC. The invention adopts the KOH catalyst, temperature control, water addition and other means to make D3 in low ring react ring opening as far as possible to obtain the material with a small amount of D3 and low viscosity which can be used for cracking and distilling to produce the DMC. This invention possesses high operationality, thereby production cost of DMC can be reduced, and the production capacity of DMC can be increased.
Description
Technical field:
The present invention relates to the working method of DMC raw material, particularly a kind of method of utilizing the low ring of organosilicon open loop technique to produce the DMC raw material by the low ring of organosilicon open loop operation.
Background technology:
Known organosilicon DMC production process is: an organosilane monomer dimethyldichlorosilane(DMCS) (abbreviation diformazan) is hydrolyzed dechlorination; Obtain the hydrolyzate of diformazan; This hydrolyzate is through vacuum cracking rearrangement, rectifying, and obtaining a kind of is master's organosilicon major product DMC with D4, D5.
The low ring of known organosilicon production process is down: hydrolyzate is reset through vacuum cracking, obtains lysate siloxanes mixed methylcyclosiloxane (mainly being grouped into by one-tenth such as D3, D4, D5, D6, D7, D8, D9).In the process of this mixed methylcyclosiloxane component before distillation system is removed D3 and D3, having formed a kind of is main with D3, contains the low ring of material-----organosilicon material of a small amount of D4.
DMC and organosilicon are low to encircle material ratio, and the DMC quality is high, and purposes is wide, and price is high.As the low ring of organosilicon material is sold with by product, obviously be uneconomic.And utilize the low ring of organosilicon material to produce DMC again, it is low because of boiling point to need to solve low ring, in returning the high-temperature vacuum cracking still, can't carry out the problem that (mainly being that this material boiling point is low, too short in the high-temperature vacuum cracking still residence time) reset in cracking.Otherwise can cause a large amount of D3 cracking not reset formation D4, D5, cause the DMC per pass conversion too low, cost is higher.As will hang down earlier be used further to cracking after the D3 open loop in the ring, DMC is produced in rectifying, must guarantee open loop material viscosity low (molecular chain length is shorter), is convenient to pipe-line transportation and cracking, and this material D3 is residual will lack.At present, the method for utilizing the low ring of organosilicon open loop technique to produce the DMC raw material does not both at home and abroad still have bibliographical information.
Summary of the invention:
The present invention aims to provide a kind of method of producing the DMC raw material by the low ring of organosilicon open loop operation, makes the low ring of organosilicon obtain a kind of low cost, LV, material that D3 content is low again through open loop technique, is used for cracking, DMC is produced in rectifying.
The technical scheme that the present invention adopts is:
A kind of method of producing the DMC raw material by the low ring of organosilicon open loop operation, carry out as follows:
A, will hang down the ring material and be transported to reaction kettle by low ring basin;
B, material is warming up to 65 ℃, leaving standstill for some time carries out layering, drains lower floor's sour water;
C, adding KOH catalyzer, controlled temperature carries out the D3 open loop at 65 ℃-100 ℃;
Open loop material state is observed in d, sampling, reaches requirement and adds water afterwards;
E, with the mass transport in the reaction kettle to basin, wait for that cracking, rectifying produces DMC.
The unusual effect of technical scheme of the present invention is:
1. technology is simple, and is easy to operate.
2. the most of D3 in the low ring material handles through open loop, and D3 is residual to tail off, and forms a kind of material that is similar to hydrolyzate.It is more that this open loop material is reset the D4, the D5 that are formed with usefulness through cracking, and the DMC per pass conversion increases.
3. through the KOH catalyzer, temperature control adds means such as water, makes the very low of low ring open loop material viscosity change, is convenient to pipe-line transportation.
4. it is low because of viscosity lowly to encircle the open loop material, is convenient to cracking, saves the cracking time.
5. floor space is little, and primary device only needs a reaction kettle, and operator are few.
6. required other material mainly is made up of the KOH of water and minute quantity, and is cheap, and production cost is extremely low.
7. every still is operated weak point consuming time, and productive rate is high.
8. the low ring of rectifying (by product) is turned waste into wealth, obtain great economic benefit.
9. production process does not have waste water, exhaust gas emission, and environment protecting is good.
As a kind of preferred version of the present invention, the open loop temperature among the step C is 75 or 76 or 77 ℃ or 78 ℃.
As a kind of preferred version of the present invention, the amount that adds KOH among the said step B is 10ppm.
As a kind of preferred version of the present invention, add water 500L among the said step D.
Concrete embodiment:
Below in conjunction with embodiment the present invention is detailed.
Following table has provided 8 embodiment relevant art parameter values.
| ? | The weight of the low ring of organosilicon | The content (%) of D3 in the low ring | The open loop temperature (℃) | The amount that adds KOH | Material viscosity after the open loop | The content of D3 in the material after the open loop |
| 1 | 1400 | 53.67 | 75 | 10ppm | 97mpa.s | 3.91% |
| 2 | 1500 | 53.67 | 78 | 10ppm | 85mpa.s | 3.72% |
| 3 | 1600 | 66.71 | 76 | 10ppm | 110 mpa.s | 2.95% |
| 4 | 1700 | 66.71 | 76 | 10ppm | 97mpa.s | 3.71% |
| 5 | 1800 | 75.72 | 77 | 10ppm | 102 mpa.s | 3.52% |
| 6 | 1900 | 75.72 | 78 | 10ppm | 87 mpa.s | 3.05% |
| 7 | 2000 | 61.53 | 78 | 10ppm | 89 mpa.s | 3.71% |
| 8 | 1700 | 61.53 | 75 | 10ppm | 80mpa.s | 3.23% |
The weight part proportioning of said embodiment (1,2,3,4,5,6,7,8) raw material is: the low ring of organosilicon 1400L to 2000L does not wait, and Pottasium Hydroxide is respectively 10ppm; The water yield of adding is respectively 500L after the open loop.
The working method of embodiment 1 is following:
1) the low ring of 1400L organosilicon material is transported in the reaction kettle by low ring basin.
2) the low ring of machine silicon material is warming up to 65 ℃, leaving standstill for some time carries out layering, drains lower floor's sour water.
3) the KOH solution of adding 10ppm, 75 ℃ of control D3 open loop temperature.
4) open loop material state is observed in sampling, reaches the water that 500L is added in requirement afterwards.
5) sampling analysis material viscosity, D3 residual quantity 3.91%.
6) material pipe is transported to the hydrolyzate basin, waits for cracking, rectifying production DMC.
The parameters of other embodiment 2 to embodiment 8 is referring to expressed numerical value in the table; Its concrete working method is with embodiment 1 described each step; It is concrete parameter value difference.
More than its kinetic viscosity of open loop material of obtaining of each indivedual embodiment all less than below 110 mpa.s, be convenient to carry and cracking, and D3 remains in about 3.8%, highly beneficial to producing DMC.
Claims (4)
1. method of producing the DMC raw material by the low ring of organosilicon open loop operation, carry out as follows:
A, will hang down the ring material and be transported to reaction kettle by low ring basin;
B, material is warming up to 65 ℃, leaving standstill for some time carries out layering, drains lower floor's sour water;
C, adding KOH catalyzer, controlled temperature carries out the D3 open loop at 65 ℃～100 ℃;
Open loop material state is observed in d, sampling, reaches requirement and adds water afterwards;
E, with the mass transport in the reaction kettle to basin, wait for that cracking, rectifying produces DMC.
2. method of producing the DMC raw material by the low ring of organosilicon open loop operation according to claim 1, it is characterized in that: the open loop temperature among the step C is 75 or 76 or 77 ℃ or 78 ℃.
3. method of producing the DMC raw material by the low ring of organosilicon open loop operation according to claim 1, it is characterized in that: the amount that adds KOH among the said step B is 10ppm.
4. method of producing the DMC raw material by the low ring of organosilicon open loop operation according to claim 1 is characterized in that: add water 500L among the said step D.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110402201.0A CN102516283B (en) | 2011-12-07 | 2011-12-07 | The method of DMC raw material is produced by the low ring operated open-loop of organosilicon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110402201.0A CN102516283B (en) | 2011-12-07 | 2011-12-07 | The method of DMC raw material is produced by the low ring operated open-loop of organosilicon |
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| CN102516283A true CN102516283A (en) | 2012-06-27 |
| CN102516283B CN102516283B (en) | 2015-08-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151348A (en) * | 2014-07-21 | 2014-11-19 | 鲁西化工集团股份有限公司硅化工分公司 | Recovery process for by-products produced by cracking of organosilicone monomers |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837262A (en) * | 2006-04-24 | 2006-09-27 | 广州吉必时科技实业有限公司 | Process for synthesis of polysiloxane |
| CN101148455A (en) * | 2006-09-21 | 2008-03-26 | 蓝星化工新材料股份有限公司 | Continuous cracking method for dimethyl polysiloxane with end sealed by hydroxyl group and rectifying method for the same to preparing cyclosiloxane |
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2011
- 2011-12-07 CN CN201110402201.0A patent/CN102516283B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837262A (en) * | 2006-04-24 | 2006-09-27 | 广州吉必时科技实业有限公司 | Process for synthesis of polysiloxane |
| CN101148455A (en) * | 2006-09-21 | 2008-03-26 | 蓝星化工新材料股份有限公司 | Continuous cracking method for dimethyl polysiloxane with end sealed by hydroxyl group and rectifying method for the same to preparing cyclosiloxane |
Non-Patent Citations (2)
| Title |
|---|
| 幸松民等,: "《有机硅合成工艺及产品应用》", 30 September 2000, 化学工业出版社 * |
| 陈献新等,: "聚硅氧烷的研究进展", 《绝缘材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151348A (en) * | 2014-07-21 | 2014-11-19 | 鲁西化工集团股份有限公司硅化工分公司 | Recovery process for by-products produced by cracking of organosilicone monomers |
| CN104151348B (en) * | 2014-07-21 | 2016-06-08 | 鲁西化工集团股份有限公司硅化工分公司 | A kind of organosilane monomer cracking byproduct recovery process |
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| CN102516283B (en) | 2015-08-19 |
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Address after: 063305 Nanpu Development Zone, Hebei, Tangshan City Patentee after: Tangshan Sanyou Silicon Industry Co.,Ltd. Address before: 063305 Nanpu Development Zone, Hebei, Tangshan City Patentee before: SANYOU SILICON INDUSTRY Co.,Ltd. |
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