CN104497035A - Production method for enhancing yield of octamethylcyclotetrasiloxane - Google Patents
Production method for enhancing yield of octamethylcyclotetrasiloxane Download PDFInfo
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Abstract
The invention relates to the technical field of chemical industry, particularly a production method for enhancing yield of octamethylcyclotetrasiloxane. The method comprises the following steps: after dimethyl hydrolyzate is subjected to cracking rearrangement and ring rectification, the separated D3, D5, D6, light component and high-boiling-point component can be returned to a rearrangement kettle to perform rearrangement, thereby obtaining the cracking substance mainly composed of D4; and carrying out the repeated process of cracking, rectification, cracking, rectification and the like, thereby enhancing the yield of the D4 to 95% above.
Description
Technical field
The present invention relates to a kind of production method improving octamethylcyclotetrasiloxane yield, belong to chemical technology field.
Background technology
Based on the polysiloxane of dimethyl silicone oil, dimethyl silicone rubber owing to having the performance of many excellences, as high temperature resistant, low temperature resistant, insulation, hydrophobic, weather-resistant and physiological inertia etc., be widely used in aerospace, aviation, electrically, the every field such as electronics, light industry, machinery, chemical industry, medical science, and be deep into the industry-by-industry of people's life, becoming the outstanding person of new chemical materials, is type material important in national economy.Polysiloxane is mainly hydrolyzed the hydrolyzate that obtains and hydrolyzate cracking with dimethyldichlorosilane(DMCS) and resets the mixed methylcyclosiloxane that obtains for raw material and obtain.Along with the development of national economy and the raising of specification of quality, composition in diformazan hydrolyzate and mixed methylcyclosiloxane is more, be unfavorable for obtaining stay-in-grade polysiloxane, it is single that octamethylcyclotetrasiloxane (D4) has composition, be easy to the characteristic of ring-opening polymerization, become the main raw material of production high-quality, high request polysiloxane.
In current octamethylcyclotetrasiloxane production method be, hydrolyzate is obtained after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate is reset through cracking and is obtained lysate, the quality group of lysate becomes hexamethyl cyclotrisiloxane (D3) 10-15%, octamethylcyclotetrasiloxane (D4) 45-60%, decamethylcyclopentaandoxane (D5) 20-25%, ten diformazan basic ring six siloxanes (D6) 5% and small part Light ends and high boiling point component, lysate isolates D4 through ring body rectifying tower, the D3 separated, D5, D6, part D4 and Light ends, high boiling point component mixing composition mixed methylcyclosiloxane, because D4 consists of 45-60%, D4 yield is less than 50%.
Summary of the invention
The object of this invention is to provide a kind of production method improving octamethylcyclotetrasiloxane yield.Principle of the present invention be D3, D5, D6 and Light ends, high boiling point component under the effect of potassium hydroxide catalyst, cracking can reset and obtain D4; According to this principle, cracking can be turned back to through ring body rectifying separation D3, D5, D6 out and Light ends, high boiling point component to reset still and carry out cracking rearrangement, obtain the lysate that D4 content is 45-60% further, simultaneously in cracking rearrangement process, other impurity can react with potassium hydroxide and remove.Through repetitive processes such as cracking-rectifying-cracking-rectifying, the yield of D4 is improved, and can reach more than 95%.
A kind of production method improving octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.08-0.098Mpa and 130-180 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls as 130-150 DEG C, de-low tower top temperature control is made as 80-100 DEG C, vacuum tightness is 0.05-0.09Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, bottom temperature controls as 140-160 DEG C, and top temperature control is made as 100-130 DEG C, vacuum tightness 0.05-0.098Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
Advantage of the present invention is: in the process of producing octamethylcyclotetrasiloxane, and hydrolyzate is through repetitive processes such as cracking-rectifying-cracking-rectifying, and not only technique is simple, and the yield of D4 is improved, and can reach more than 95%.
Specific embodiment
Embodiment 1:
A kind of production method improving octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.08-0.09Mpa and 130-150 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls to be 130 DEG C, de-low tower top temperature control is made as 80 DEG C, vacuum tightness is 0.05Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, it is 140 DEG C that bottom temperature controls, and top temperature control is made as 100 DEG C, vacuum tightness 0.05Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
Embodiment 2:
A kind of production method improving octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.095-0.098Mpa and 130-180 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls to be 140 DEG C, de-low tower top temperature control is made as 90 DEG C, vacuum tightness is 0.095Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, it is 150 DEG C that bottom temperature controls, and top temperature control is made as 120 DEG C, vacuum tightness 0.098Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
Embodiment 3:
A kind of production method improving octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.09-0.095Mpa and 150-180 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls to be 150 DEG C, de-low tower top temperature control is made as 100 DEG C, vacuum tightness is 0.09Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, it is 160 DEG C that bottom temperature controls, and top temperature control is made as 130 DEG C, vacuum tightness 0.098Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
Embodiment 4:
A kind of production method improving octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.08Mpa and 120 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls to be 120 DEG C, de-low tower top temperature control is made as 70 DEG C, vacuum tightness is 0.04Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, it is 130 DEG C that bottom temperature controls, and top temperature control is made as 90 DEG C, vacuum tightness 0.04Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
Embodiment 5:
A kind of production method improving octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.1Mpa and 190 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls to be 160 DEG C, de-low tower top temperature control is made as 110 DEG C, vacuum tightness is 0.1Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, it is 170 DEG C that bottom temperature controls, and top temperature control is made as 140 DEG C, vacuum tightness 0.1Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
The octamethylcyclotetrasiloxane yield that each embodiment obtains is as shown in the table
As can be seen from upper table result, the yield of the embodiment 1-3 in present invention process parameter is apparently higher than the enforcement 4,5 outside processing range and the yield not adopting the inventive method, wherein the highest with the yield of embodiment 2, the specific technique of visible employing the present invention and parameter, can obtain the octamethylcyclotetrasiloxane that yield is higher.
Claims (3)
1. improve a production method for octamethylcyclotetrasiloxane yield, it is characterized in that it carries out in the steps below:
Cracking can be turned back to reset still through ring body rectifying separation D3, D5, D6 out and Light ends, high boiling point component, cracking rearrangement is carried out together with hydrolyzate, obtain the lysate that D4 content is 45-60% further, lysate carries out ring body rectifying separation again and obtains target product D4, with D3, D5, D6 and the byproduct such as Light ends, high boiling point component, the latter returns again cracking and resets still cracking rearrangement, and through repetitive processes such as cracking-rectifying-cracking-rectifying, the yield of D4 is improved.
2. one kind is improved the production method of octamethylcyclotetrasiloxane yield, concrete steps are: obtain hydrolyzate after dimethyldichlorosilane(DMCS) hydrolysis, it is characterized in that: hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.08-0.098Mpa and 130-180 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls as 130-150 DEG C, de-low tower top temperature control is made as 80-100 DEG C, vacuum tightness is 0.05-0.09Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, bottom temperature controls as 140-160 DEG C, and top temperature control is made as 100-130 DEG C, vacuum tightness 0.05-0.098Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
3. a kind of production method improving octamethylcyclotetrasiloxane yield as claimed in claim 2, it is characterized in that: hydrolyzate and potassium hydroxide add in the rearrangement still of band stirring, at vacuum tightness 0.095-0.098Mpa and 130-180 DEG C, cracking is reset, generate quality composition hexamethyl cyclotrisiloxane 10-15%, octamethylcyclotetrasiloxane 45-60%, decamethylcyclopentaandoxane 20-25%, the lysate of ten diformazan basic ring six siloxanes 5% and small part Light ends and high boiling point component, lysate first isolates hexamethyl cyclotrisiloxane and Light ends through de-low tower from tower top, the control condition of de-low tower is that bottom temperature controls to be 140 DEG C, de-low tower top temperature control is made as 90 DEG C, vacuum tightness is 0.098Mpa, de-low tower tower bottoms isolates octamethylcyclotetrasiloxane and the high boiling material containing decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component through octamethylcyclotetrasiloxane tower again, and octamethylcyclotetrasiloxane is from tower top discharging, it is 150 DEG C that bottom temperature controls, and top temperature control is made as 120 DEG C, vacuum tightness 0.098Mpa, the high boiling material of hexamethyl cyclotrisiloxane and Light ends and decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes, high boiling point component turns back to cracking by pipeline and resets still, carry out cracking rearrangement together with hydrolyzate, obtaining containing octamethylcyclotetrasiloxane is main lysate.
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Cited By (8)
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| CN108164556A (en) * | 2018-01-05 | 2018-06-15 | 王谌树 | A kind of organosilicon hydrolyzation oil continuous cracking technique |
| CN108675309A (en) * | 2018-05-15 | 2018-10-19 | 湖北兴瑞硅材料有限公司 | A kind of method of gas-phase silica raw materials for production supply |
| CN108929343A (en) * | 2018-06-27 | 2018-12-04 | 合盛硅业（泸州）有限公司 | A method of purification octamethylcy-clotetrasiloxane |
| CN109096322A (en) * | 2018-07-19 | 2018-12-28 | 芜湖维软新材料有限公司 | The preparation method of octamethylcy-clotetrasiloxane is produced using liquid methane |
| CN109096323A (en) * | 2018-10-18 | 2018-12-28 | 江西星火狮达科技有限公司 | Utilize the preparation method of organosilicon cracking dregs of fat production organosilicon hybrid ring body |
| CN110591097A (en) * | 2019-09-30 | 2019-12-20 | 唐山三友硅业有限责任公司 | Cation catalytic ring-opening process of hexamethylcyclotrisiloxane |
| CN113769820A (en) * | 2021-08-26 | 2021-12-10 | 上海精日新材料科技有限公司 | Environment-friendly organosilicon production line |
| WO2022213890A1 (en) | 2021-04-09 | 2022-10-13 | 江西蓝星星火有机硅有限公司 | Process for producing organosilicon linear body |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108164556A (en) * | 2018-01-05 | 2018-06-15 | 王谌树 | A kind of organosilicon hydrolyzation oil continuous cracking technique |
| CN108164556B (en) * | 2018-01-05 | 2020-12-08 | 王谌树 | Continuous cracking process for organic silicon hydrolyzed oil |
| CN108675309A (en) * | 2018-05-15 | 2018-10-19 | 湖北兴瑞硅材料有限公司 | A kind of method of gas-phase silica raw materials for production supply |
| CN108675309B (en) * | 2018-05-15 | 2020-02-14 | 湖北兴瑞硅材料有限公司 | Method for supplying raw materials for producing fumed silica |
| CN108929343A (en) * | 2018-06-27 | 2018-12-04 | 合盛硅业（泸州）有限公司 | A method of purification octamethylcy-clotetrasiloxane |
| CN109096322A (en) * | 2018-07-19 | 2018-12-28 | 芜湖维软新材料有限公司 | The preparation method of octamethylcy-clotetrasiloxane is produced using liquid methane |
| CN109096323A (en) * | 2018-10-18 | 2018-12-28 | 江西星火狮达科技有限公司 | Utilize the preparation method of organosilicon cracking dregs of fat production organosilicon hybrid ring body |
| CN109096323B (en) * | 2018-10-18 | 2020-07-17 | 江西星火狮达科技有限公司 | Preparation method for producing organic silicon mixed ring body by using organic silicon cracking oil residue |
| CN110591097A (en) * | 2019-09-30 | 2019-12-20 | 唐山三友硅业有限责任公司 | Cation catalytic ring-opening process of hexamethylcyclotrisiloxane |
| WO2022213890A1 (en) | 2021-04-09 | 2022-10-13 | 江西蓝星星火有机硅有限公司 | Process for producing organosilicon linear body |
| CN113769820A (en) * | 2021-08-26 | 2021-12-10 | 上海精日新材料科技有限公司 | Environment-friendly organosilicon production line |
| CN113769820B (en) * | 2021-08-26 | 2023-02-28 | 上海精日新材料科技有限公司 | Environment-friendly organosilicon production line |
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Effective date of registration: 20161215 Address after: 330319 Jiangxi province Jiujiang Yongxiu County Yangjialing Applicant after: JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE CO., LTD. Address before: Xinghuo Industrial Park in Jiangxi province Jiujiang Yongxiu County 330319 Applicant before: Jiangxi Xinghuo Organo-Silicon Plant, Lanxing Chemical New Material Co., Ltd. |
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