CN106279244A - A kind of methoxytrimethylsilane alcoholysis process - Google Patents
A kind of methoxytrimethylsilane alcoholysis process Download PDFInfo
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- CN106279244A CN106279244A CN201610655816.7A CN201610655816A CN106279244A CN 106279244 A CN106279244 A CN 106279244A CN 201610655816 A CN201610655816 A CN 201610655816A CN 106279244 A CN106279244 A CN 106279244A
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- reaction tower
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
Abstract
The present invention relates to chemical field, especially a kind of methoxytrimethylsilane alcoholysis process.The present invention is that by the top of reaction tower, trim,ethylchlorosilane is entered reactor, and methanol enters reactor from the bottom of reaction tower, and methyl trichlorosilane, when solvent is at reactor, is simultaneously introduced ferric chloride and makees catalyst, and reaction temperature is at 50 ~ 80 DEG C.Present invention process is stable, it is easy to operation, and by-product can continue reaction with methanol, can separate as solvent, product and by-product, and utilization rate is higher, and up to 90%, product content is more than 96%, and total chlorine is at below 50ppm.
Description
Technical field
The present invention relates to chemical field, especially a kind of methoxytrimethylsilane alcoholysis process.
Background technology
Methoxytrimethylsilane is as a kind of organosilicon cross-linking agent, coupling agent, generally as the primary raw material of silicones
With the major auxiliary burden of room temperature vulcanized silicone rubber, also apply relatively wide in other field of chemical industry, to improve the mechanical strength of goods, resistance to
Hot property, humidity resistance.Methoxytrimethylsilane is to be reacted by trim,ethylchlorosilane and Methanolysis to obtain, its primary response
For (CH3) 3SiCl+CH3OH(CH3) 3SiOCH3+HCl.Chlorosilane alcoholysis production process is one-pot operation at present, chlorine
Silane and alcohols 1:1 in molar ratio instill mixing reactor and carry out alcoholysis reaction；Also have and use continuity method operation, methanol warp
Vaporizing and enter reaction tower by stripper, chlorosilane enters from reaction tower top, and the two is alcoholysis reaction in reaction tower, and reaction is produced
Raw substantial amounts of HCl gas, this large amount of solvents of needs and at a fairly low condensation temperature, the requirement to condensing unit is higher, produces into
This and energy consumption are bigger；Generally reaction temperature is 70 ~ 104 DEG C, and at such a temperature, hydrogen chloride and methanol can produce side reaction, HCl
+ CH3OH CH3Cl+H2O, produces chloromethanes and water, and water produces hydrolysis with main material trim,ethylchlorosilane again,
Methoxyl group trimethylsilane yield is declined, only about 90%, and the hydrolysate of trim,ethylchlorosilane can cause reaction
Device, the blocking of tower, affect the normal production of MTMS.
Summary of the invention
It is an object of the invention to: provide a kind of generation reducing side reaction and by-product, it is to avoid by-product is to reaction
Device, the blocking of tower, it is ensured that the normal production of trimethylmethoxysilane, reduce the use of solvent simultaneously, and can improve trimethyl
The utilization rate of chlorosilane and the methoxytrimethylsilane alcoholysis process of methoxytrimethylsilane yield.
The technical scheme is that
A kind of oxygen methyltrimethylsilane alcoholysis process, it is characterised in that it comprises the following steps:
1), incomplete alcoholysis reaction:
Use dosing pump respectively trim,ethylchlorosilane and methanol to be at the uniform velocity added dropwise to alcoholysis reaction tower and carry out alcoholysis reaction, trimethyl
Chlorosilane drips from the bottom of reaction tower, and methanol drips from the upper end of reaction tower；Methyl trimethoxy epoxide silicon is added in reactor
Alkane, is simultaneously introduced ferric chloride and makees catalyst, and the temperature of reactor controls at 50 80 DEG C, and by-product HCl is from alcoholysis reaction tower
Top is overflowed, and the incomplete alcoholysate that reaction generates flows in reactor；
2), complete alcoholysis reaction:
By the still temperature rise of reactor to 60 105 DEG C, make the vaporization backflow of incomplete alcoholysate, methanol is vaporized through methyl alcohol vaporizing device
After from reaction tower bottom enter reaction tower, with in reaction tower backflow incomplete alcoholysate continue alcoholysis, methyl alcohol vaporizing device oil
Bath temperature controls at 90 120 DEG C；The HCl produced in alcoholysis reaction tower overflows from alcoholysis reaction tower top, thick finished product methoxy
Base trimethyl silane is back to reactor, the methoxytrimethylsilane crude yield obtained be more than 75%, content 96 97%,
Acid content is less than 150ppm, creates good condition for the neutralization of lower step, rectification.
The principle of the present invention is traditional methoxytrimethylsilane one-pot or continuous print one step alcoholysis reaction to be optimized for
The tower reaction of continuous print two step, first allows methyl trichlorosilane and methanol at room temperature carry out incomplete alcoholysis reaction, cannot generate completely
Full alcoholysate, it is to avoid the generation of side reaction, reduces the by-product impact on producing；Incomplete alcoholysate is allowed to carry out with methanol again
Complete alcoholysis is reacted；Second step raises temperature of reaction kettle, promotes the vaporization of incomplete alcoholysate to go successively to alcoholysis in reaction tower, keeps away
Exempt from alcoholysis reaction incomplete.
It is an advantage of the current invention that:
The present invention carries out alcoholysis reaction at low temperatures, and product purity is improved；Side reaction is avoided to occur, catalyst ferric chloride
Addition avoid the blocking that reactor, tower cause by the hydrolysate of trim,ethylchlorosilane, reduce the use of solvent, side reaction simultaneously
The by-product produced can flow directly into reactor and works as solvent, can carry high product yield, it is ensured that MTMS normal
Produce；Process stabilizing, it is easy to operation, uses manpower and material resources sparingly.
Detailed description of the invention
Embodiment 1:
Dosing pump is used respectively the trim,ethylchlorosilane of 543g and the methanol of 128g at the uniform velocity to be dripped entrance alcoholysis reaction, trimethyl
Chlorosilane drips from the bottom of reaction tower, and methanol drips from the upper end of reaction tower, adds 100g methyl trimethoxy epoxide in reactor
Silane, the ferric chloride being simultaneously introduced 2g makees catalyst, and the temperature of reactor controls at 60 DEG C, and by-product HCl is from alcoholysis reaction
Tower top overflows, and the incomplete alcoholysate that reaction generates flows in reactor；
By the still temperature rise of reactor to 75 DEG C, make the vaporization backflow of incomplete alcoholysate, the methanol of 32g is vaporized through methyl alcohol vaporizing device
After from reaction tower bottom enter reaction tower, with in reaction tower backflow incomplete alcoholysate continue alcoholysis, methyl alcohol vaporizing device oil
It is 110 DEG C that bath temperature controls；The HCl produced in alcoholysis reaction tower overflows from alcoholysis reaction tower top, thick finished product methoxyl group front three
Base silane is back to reactor.By in thick product zinc powder and after, rectification, collect column temperature at the product of about 78 DEG C, produced
The yield of product is 71%, content 96.6%, total chlorine 37ppm.
Embodiment 2:
Dosing pump is used respectively the trim,ethylchlorosilane of 543g and the methanol of 120g at the uniform velocity to be dripped entrance alcoholysis reaction, trimethyl
Chlorosilane drips from the bottom of reaction tower, and methanol drips from the upper end of reaction tower, adds 100g methyl trimethoxy epoxide in reactor
Silane, the ferric chloride being simultaneously introduced 2g makees catalyst, and the temperature of reactor controls at 60 DEG C, and by-product HCl is from alcoholysis reaction
Tower top overflows, and the incomplete alcoholysate that reaction generates flows in reactor；
By the still temperature rise of reactor to 70 DEG C, make the vaporization backflow of incomplete alcoholysate, the methanol of 30g is vaporized through methyl alcohol vaporizing device
After from reaction tower bottom enter reaction tower, with in reaction tower backflow incomplete alcoholysate continue alcoholysis, methyl alcohol vaporizing device oil
It is 110 DEG C that bath temperature controls；The HCl produced in alcoholysis reaction tower overflows from alcoholysis reaction tower top, thick finished product methoxyl group three
Methyl-monosilane is back to reactor.By in thick product zinc powder and after, rectification, collect column temperature at the product of about 78 DEG C, obtain
The yield of product is 65%, content 95.5%, total chlorine 76ppm.
Embodiment 3
Dosing pump is used respectively the trim,ethylchlorosilane of 543g and the methanol of 128g at the uniform velocity to be dripped entrance alcoholysis reaction, trimethyl
Chlorosilane drips from the bottom of reaction tower, and methanol drips from the upper end of reaction tower, adds 100g methyl trimethoxy epoxide in reactor
Silane, the ferric chloride being simultaneously introduced 2g makees catalyst, and the temperature of reactor controls at 60 DEG C, and by-product HCl is from alcoholysis reaction
Tower top overflows, and the incomplete alcoholysate that reaction generates flows in reactor；
By the still temperature rise of reactor to 75 DEG C, make the vaporization backflow of incomplete alcoholysate, by the methanol of 42g through methyl alcohol vaporizing device vapour
Enter reaction tower after change from reaction tower bottom, continue alcoholysis, methyl alcohol vaporizing device with the incomplete alcoholysate of backflow in reaction tower
It is 110 DEG C that oil bath temperature controls；The HCl produced in alcoholysis reaction tower overflows from alcoholysis reaction tower top, thick finished product methoxyl group
Trimethyl silane is back to reactor.By in thick product zinc powder and after, rectification, collect column temperature at the product of about 78 DEG C,
Yield to product is 69%, content 96.8%, total chlorine 31ppm.
Claims (1)
1. an oxygen methyltrimethylsilane alcoholysis process, it is characterised in that it comprises the following steps:
1), incomplete alcoholysis reaction:
Use dosing pump respectively trim,ethylchlorosilane and methanol to be at the uniform velocity added dropwise to alcoholysis reaction tower and carry out alcoholysis reaction, trimethyl
Chlorosilane drips from the bottom of reaction tower, and methanol drips from the upper end of reaction tower；Methyl trimethoxy epoxide silicon is added in reactor
Alkane, is simultaneously introduced ferric chloride and makees catalyst, and the temperature of reactor controls at 50 80 DEG C, and by-product HCl is from alcoholysis reaction tower
Top is overflowed, and the incomplete alcoholysate that reaction generates flows in reactor；
2), complete alcoholysis reaction:
By the still temperature rise of reactor to 60 105 DEG C, make the vaporization backflow of incomplete alcoholysate, methanol is vaporized through methyl alcohol vaporizing device
After from reaction tower bottom enter reaction tower, with in reaction tower backflow incomplete alcoholysate continue alcoholysis, methyl alcohol vaporizing device oil
Bath temperature controls at 90 120 DEG C；The HCl produced in alcoholysis reaction tower overflows from alcoholysis reaction tower top, thick finished product methoxy
Base trimethyl silane is back to reactor, the methoxytrimethylsilane crude yield obtained be more than 75%, content 96 97%,
Acid content is less than 150ppm, creates good condition for the neutralization of lower step, rectification.
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| CN201610655816.7A CN106279244B (en) | 2016-08-12 | 2016-08-12 | A kind of methoxytrimethylsilane alcoholysis process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232633A (en) * | 2018-11-16 | 2019-01-18 | 江西晨光新材料股份有限公司 | A kind of one methoxy silane of trimethyl-hexamethyldisilazane combined preparation process |
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| US2695307A (en) * | 1947-09-20 | 1954-11-23 | Union Chimique Belge Sa | Process of manufacturing polymerized organic silicon compounds |
| JPH09157277A (en) * | 1995-12-06 | 1997-06-17 | Shin Etsu Chem Co Ltd | Production of alkoxysilane |
| CN101613367A (en) * | 2009-07-22 | 2009-12-30 | 吉林新亚强生物化工有限公司 | The preparation method of trimethylethoxysilane |
| CN102887916A (en) * | 2012-09-29 | 2013-01-23 | 中昊晨光化工研究院有限公司 | Alkoxy silicon resin intermediate and preparation method thereof |
| CN103012460A (en) * | 2012-12-25 | 2013-04-03 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Alcoholysis process for methyltrimethoxysilane |
-
2016
- 2016-08-12 CN CN201610655816.7A patent/CN106279244B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2695307A (en) * | 1947-09-20 | 1954-11-23 | Union Chimique Belge Sa | Process of manufacturing polymerized organic silicon compounds |
| JPH09157277A (en) * | 1995-12-06 | 1997-06-17 | Shin Etsu Chem Co Ltd | Production of alkoxysilane |
| CN101613367A (en) * | 2009-07-22 | 2009-12-30 | 吉林新亚强生物化工有限公司 | The preparation method of trimethylethoxysilane |
| CN102887916A (en) * | 2012-09-29 | 2013-01-23 | 中昊晨光化工研究院有限公司 | Alkoxy silicon resin intermediate and preparation method thereof |
| CN103012460A (en) * | 2012-12-25 | 2013-04-03 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Alcoholysis process for methyltrimethoxysilane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232633A (en) * | 2018-11-16 | 2019-01-18 | 江西晨光新材料股份有限公司 | A kind of one methoxy silane of trimethyl-hexamethyldisilazane combined preparation process |
| CN109232633B (en) * | 2018-11-16 | 2020-12-25 | 江西晨光新材料股份有限公司 | Combined preparation method of trimethyl monomethoxysilane-hexamethyldisilazane |
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Address after: Luochang Town, Shashi District, Jingzhou City, Hubei Province Patentee after: Hubei Jianghan New Material Co.,Ltd. Address before: 434000 No.2 Road, Shashi District Economic and Technological Development Zone, Jingzhou City, Hubei Province Patentee before: JINGZHOU JIANGHAN FINE CHEMICAL Co.,Ltd. |
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