CN105254658A - Preparation method for methyl trialkoxy silane - Google Patents
Preparation method for methyl trialkoxy silane Download PDFInfo
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- CN105254658A CN105254658A CN201510585300.5A CN201510585300A CN105254658A CN 105254658 A CN105254658 A CN 105254658A CN 201510585300 A CN201510585300 A CN 201510585300A CN 105254658 A CN105254658 A CN 105254658A
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- trichloro silane
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Abstract
The invention provides a preparation method for methyl trialkoxy silane. The preparation method comprises the following four procedures: an alcoholysis reaction between methyl trichlorosilane and absolute alcohol; neutralization; filtering; and distillation. The alcoholysis reaction comprises the following concrete steps: introducing drying neutral gas-loaded methyl trichlorosilane steam into absolute alcohol and carrying out a continuous stirring reaction for 1 to 4 h at a normal pressure and a temperature of 30 to 80 DEG C so as to obtain methyl trialkoxy silane. According to the invention, hydrogen chloride gas produced in the process is expelled by using heating reflux and drying neutral gas, which facilitates implementation of the main reaction, reduces by-products and improves yield and quality of methyl trialkoxy silane.
Description
Technical field
The present invention relates to the preparation method of organoalkoxysilane, particularly relate to a kind of preparation method improving methyl trialkoxysilane productive rate.
Technical background
Methyl trialkoxysilane prepares the important intermediate of polysiloxane, is mainly used in silicone rubber crosslinking agent, modified synthetic resin, fireproofing agent, the base paint of plastics hard coat, hydrophober, has very large using value and wide market.The preparation method of present methyl trialkoxysilane carries out esterification by METHYL TRICHLORO SILANE and absolute alcohol, through neutralization, obtains after filtration, distillation.Domestic also have corresponding report, and as Li Wen first in 2000, Ji Chengjie, waited in people CN1320600A and report, under laboratory adopts sherwood oil to exist, carries out two-way dropping obtain vinyltrimethoxy silane by vinyl trichloro silane and methyl alcohol; What army in 2003, Liu Yunmei adopts sherwood oil to prepare Trimethoxy silane etc. as solvent in laboratory, their reactive mode is mostly that the mode dripped is reacted, its raw materials used cost or processing unit require high, product cost is caused to remain high, urgent need finds a kind of raw materials cost low, and technique is simple, improves the method for productive rate.
Summary of the invention
The object of the invention is at ambient pressure, temperature is under 30 ~ 80 DEG C of comparatively gentle reaction conditionss, provides that a kind of high-level efficiency, high yield, high quality, technique are simple, the preparation method of the methyl trialkoxysilane of low cost.
Technical scheme of the present invention: methyl trialkoxysilane carries out esterification by METHYL TRICHLORO SILANE and absolute alcohol, is prepared from totally through neutralizing, filtering, distill four operations.Improvements are that described reaction is different from traditional dropping mode, but by the neutral gas of drying, METHYL TRICHLORO SILANE steam is loaded in absolute alcohol, dry neutral gas flow rate control is at 0.05L ~ 0.15L/min, react under normal pressure 30 ~ 80 DEG C of conditions, namely the way of contact of reactant is gas-liquid contact type reaction, different from the liquid drop add mode of routine, and pass into dry neutral gas in reaction process always, can be very fast reaction in HCl discharge system outside, advantageously in the carrying out of forward reaction, reduce by product, improve productive rate; Also add the condensation effect of condensing works simultaneously, reduce METHYL TRICHLORO SILANE and overflow reaction system with carrier gas and affect productive rate.Reaction equation:
CH
3SiCl
3(g)+3ROH→CH
3Si(RO)
3+3HCl。
Above-mentioned reaction, all adds completely in METHYL TRICHLORO SILANE, and continue to pass into dry neutral gas, constant temperature 1 ~ 4 hour, drives the hydrogen chloride gas produced in reaction, impels reaction to carry out to positive dirction, then carries out being neutralized to pH=8 ~ 9 with ammonia.
Described METHYL TRICHLORO SILANE and absolute alcohol 1:2.9 ~ 3.2 in molar ratio.Described absolute alcohol is C1-C5 alcohol.
More preferably described absolute alcohol is methyl alcohol, ethanol, propyl alcohol or Virahol.
In reaction process of the present invention, the neutral gas of drying is loaded into METHYL TRICHLORO SILANE in absolute alcohol, after obtaining methyl trialkoxysilane generation to reaction system, when system is constant without content of Cl element, stop logical dry neutral gas, now, passing into pH in ammonia to system is 8-9, and after filtration, at 141-143 DEG C, air distillation can obtain methyl trialkoxysilane.
Described condensation adopts condensation reflux unit to carry out, and condensation reflux unit 2-3 root passes into the prolong of chilled brine, and its temperature controls at 0 ~ 5 DEG C.
In the present invention, under atmospheric low-temperature condition, pass into dry neutral gas and adopt ammonia to be neutralizing agent, processing unit is simple, and easy to operate, cheap, productive rate is high, and the ammonium chloride produced after neutralization may be used for fertilizer, is conducive to green production.
The present invention is further illustrated by following instance.
Embodiment
Embodiment 1
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 1000ml four-hole boiling flask A in add 200.1g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:2.9, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 250ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 91.76%.
Embodiment 2
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 1000ml four-hole boiling flask A in add 205.3g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 500ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 97.83%.
Embodiment 3
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 1000ml four-hole boiling flask A in add 203.5g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.1, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 500ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 94.31%.
Embodiment 4
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 1000ml four-hole boiling flask A in add 199.7g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.2, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 500ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 degree Celsius simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 94.35%.
Embodiment 5
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 1000ml four-hole boiling flask A in add 403.7g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 500ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 degree Celsius simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 98.87%.
Embodiment 6
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 1000ml four-hole boiling flask A in add 430g monomethyl trichlorosilane, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 500ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 80 DEG C simultaneously, when dehydrated alcohol seethes with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 96.18%.
Embodiment 7
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 2000ml four-hole boiling flask A in add 600.5g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 1000ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 98.96%.
Embodiment 8
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 2000ml four-hole boiling flask A in add 800.0g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 1000ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 99.1%.
Embodiment 9
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 2000ml four-hole boiling flask A in add 900.3g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 1000ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 98.96%.
Embodiment 10
Thermometer is had equipment one, mechanical stirrer, (serpentine condenser passing into icy salt solution is equipped with in its upper end for airway and spherical condenser, surge flask and HCl absorption unit) 2000ml four-hole boiling flask A in add 1000.1g dehydrated alcohol, according to mol ratio METHYL TRICHLORO SILANE: dehydrated alcohol=1:3.0, in addition with two airways, namely one end airway to be passed in A below reaction solution liquid level, METHYL TRICHLORO SILANE is added in 1000ml there-necked flask B in the nitrogen that the access of another airway is dry, heat A to 60 DEG C, open icy salt solution water coolant, heat B to 65 DEG C simultaneously, when METHYL TRICHLORO SILANE is seethed with excitement, dry nitrogen is passed in B, feed in raw material, A is warming up to 80 DEG C, backflow 3 as a child stopped heating, after being cooled to normal temperature, pass into ammonia and be neutralized to pH=8 ~ 9, filter, distillation, collect the cut of 143 DEG C, the productive rate obtained is 99.05%.
Claims (6)
1. the preparation method of a methyl trialkoxysilane, alcoholysis reaction is carried out by METHYL TRICHLORO SILANE and absolute alcohol, through neutralization, filtration, distillation, condensation totally four operations complete, and it is characterized in that, concrete alcoholysis reaction is in absolute alcohol, pass into the METHYL TRICHLORO SILANE steam be loaded into by the neutral gas of drying, at normal pressure and 30-80 DEG C, continuously stirring reaction 1-4 hour, obtain methyl trialkoxysilane, its reaction equation is:
CH
3SiCl
3(g)+3ROH→CH
3Si(RO)
3+3HCl。
2. the preparation method of methyl trialkoxysilane according to claim 1, is characterized in that, METHYL TRICHLORO SILANE and absolute alcohol 1:2.9 ~ 3.2 in molar ratio.
3. the preparation method of methyl trialkoxysilane according to claim 1, is characterized in that, described absolute alcohol is C1-C5 alcohol.
4. the preparation method of methyl trialkoxysilane according to claim 3, is characterized in that, described absolute alcohol is methyl alcohol, ethanol, propyl alcohol or Virahol.
5. the preparation method of methyl trialkoxysilane according to claim 1, it is characterized in that, in reaction process, the neutral gas of drying is loaded in absolute alcohol METHYL TRICHLORO SILANE, after obtaining methyl trialkoxysilane generation to reaction system, when system is constant without content of Cl element, stop logical dry neutral gas, now, passing into pH in ammonia to system is 8-9, and after filtration, at 141-143 DEG C, air distillation can obtain methyl trialkoxysilane.
6. the preparation method of methyl trialkoxysilane according to claim 1, is characterized in that, condensation adopts condensation reflux unit to carry out, and condensation reflux unit 2-3 root passes into the prolong of chilled brine, and its temperature controls at 0 ~ 5 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083912A (en) * | 2016-06-17 | 2016-11-09 | 吉林化工学院 | The novel synthesizing progress method of one of methyl ethoxy dichlorosilane |
| CN114805427A (en) * | 2022-04-06 | 2022-07-29 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of vinyl trimethoxy silane |
| CN115677752A (en) * | 2022-07-11 | 2023-02-03 | 杭州师范大学 | Safe and efficient ethylene silicon synthesis method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262380A (en) * | 2014-08-21 | 2015-01-07 | 湖北兴发化工集团股份有限公司 | Preparation method of methyltrialkoxysilane |
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- 2015-09-15 CN CN201510585300.5A patent/CN105254658A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262380A (en) * | 2014-08-21 | 2015-01-07 | 湖北兴发化工集团股份有限公司 | Preparation method of methyltrialkoxysilane |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083912A (en) * | 2016-06-17 | 2016-11-09 | 吉林化工学院 | The novel synthesizing progress method of one of methyl ethoxy dichlorosilane |
| CN114805427A (en) * | 2022-04-06 | 2022-07-29 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of vinyl trimethoxy silane |
| CN114805427B (en) * | 2022-04-06 | 2024-05-14 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of vinyl trimethoxy silane |
| CN115677752A (en) * | 2022-07-11 | 2023-02-03 | 杭州师范大学 | Safe and efficient ethylene silicon synthesis method |
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Application publication date: 20160120 |
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