CN106699800A - Preparation method of methyl trialkoxysilane - Google Patents
Preparation method of methyl trialkoxysilane Download PDFInfo
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- CN106699800A CN106699800A CN201510789380.6A CN201510789380A CN106699800A CN 106699800 A CN106699800 A CN 106699800A CN 201510789380 A CN201510789380 A CN 201510789380A CN 106699800 A CN106699800 A CN 106699800A
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Abstract
The invention provides a preparation method of methyl trialkoxysilane. The preparation method comprises following steps: an absolute alcohol compound is delivered into a reaction container A, one end of a gas-guide tube is inserted into the liquid in the reaction container A, and the other end of the gas-guide tube is connected with a container B, wherein methyl trichlorosilane is delivered into the container B; the absolute alcohol compound in the reaction container A is heated to 55 to 63 DEG C, methyl trichlorosilane in the container B is heated to 62 to 68 DEG C, N2 is introduced into the container B, an obtained mixed solution in the reaction container A is heated to 75 to 88 DEG C, refluxing and thermal insulation reaction is carried out for 1 to 4h, and then heating is stopped so as to obtain a product; ammonia gas is added so as to adjust pH value to 8 to 9 via neutralization and obtain methyl trialkoxysilane. According to the preparation method, dried neutral gas is added, and ammonia gas is taken as a neutralizer; technology equipment is simple; operation is convenient; cost is low; yield is high; ammonium chloride obtained via neutralization can be used for producing fertilizer; and the preparation method is beneficial for green production.
Description
Technical field
The present invention relates to the preparation method of alkoxy silane, more particularly to a kind of raising methyl trialkoxysilane yield
Preparation method.
Background technology
Methyl trialkoxysilane is the important intermediate for preparing polysiloxanes, is mainly used in silicone rubber crosslinking agent, is modified and closes
Resin, fireproof agent, the primer of plastics hard conating, hydrophober, with very big application value and wide market.
The preparation method of present methyl trialkoxysilane is to carry out esterification by methyl trichlorosilane and absolute alcohol, neutralized,
Obtained after filtering, distillation.Also there are a corresponding report, such as Li Wen first in 2000 in the country, Ji Chengjie, et al. CN 1320600A
Middle report, in the presence of laboratory uses petroleum ether, carries out two-way dropwise addition and ethene is obtained by vinyl trichlorosilane and methyl alcohol
Base trimethoxy silane；What army in 2003, Liu Yunmei prepares trimethoxy silane using petroleum ether in laboratory as solvent
Etc., their reactive mode is mostly that the mode being added dropwise is reacted, and its raw materials used cost or process equipment requirement are high,
Product cost is caused to remain high, it is low that urgent need finds a kind of cost of material, process is simple, the method for improving yield.
The content of the invention
The purpose of the present invention is that at ambient pressure, temperature is under 55~88 DEG C of comparatively gentle reaction conditions, there is provided a kind of efficient
Rate, high yield, high-quality, process is simple, the preparation method of the methyl trialkoxysilane of low cost.
Technical scheme：A kind of preparation method of methyl trialkoxysilane, comprises the following steps：
1. toward equipped with thermometer, mechanical agitator, wireway and condenser reaction vessel A in add absolute alcohol, air guide
One end of pipe is passed through to reaction vessel liquid level, and the other end of wireway accesses the container B equipped with methyl trichlorosilane
In；
2. the absolute alcohol in heating response container A is to 55-63 DEG C, and turn on agitator is stirred, and opens condenser, and heating is held
Methyl trichlorosilane in device B when methyl trichlorosilane seethes with excitement, to N2 is passed through in container B, is passed through to 62-68 DEG C
The flow of nitrogen is 0.05L~0.15L/min, and N2 is N2 of the moisture less than 5%, treats the methyl trichlorine silicon in container B
Alkane is added completely into reaction vessel A, continues to be passed through N2 toward container B, by the mixed solution liter in reaction vessel A
Temperature flows back and insulation reaction 1-4h to 75-88 DEG C；
3. stop heating after backflow and insulation reaction 1-4h, obtain product, product is naturally cooled into normal temperature, be passed through ammonia
PH is neutralized to for 8-9, filtering, distillation, the cut liquid for reclaiming 140-143 DEG C obtain methyl trialkoxysilane；
Specifically reaction equation is：
CH3SiCl3(g)+3ROH→CH3Si(RO)3+3HCl。
R is：Methyl, ethyl, propyl group, butyl, isopropyl.
Described methyl trichlorosilane is 1 with the mol ratio of absolute alcohol：2.5-4.0.
The way of contact of reactant is gas liquid reaction in course of reaction of the invention, different from conventional liquid drop add mode,
And dry neutral gas is passed through in course of reaction always, can be quickly the HCl gas discharge systems in reaction outside,
Advantageously in the carrying out of forward reaction, then carried out being neutralized to pH=8~9 with ammonia, reduce accessory substance, improve yield.
In the present invention, under the conditions of atmospheric low-temperature, it is nertralizer to be passed through dry neutral gas and use ammonia, and technique sets
Standby simple, easy to operate, cheap, yield is high, and the ammonium chloride produced after neutralization can be used for fertilizer, be conducive to green
Color is produced.
Specific embodiment
The present invention is further illustrated by following instance.
Embodiment 1
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 1000ml four-hole boiling flasks A in add 200.1g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% absolute ethyl alcohol=1:2.9, one end of wireway is passed into A
Below reaction solution liquid level, methyl three is added in the 250ml there-necked flasks B in the other end dry nitrogen of access of wireway
Chlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 DEG C of heating, when methyl trichlorosilane boiling
When rising, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating, cold
But to after normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the yield for obtaining is collected in distillation
It is 91.76%.
Embodiment 2
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 1000ml four-hole boiling flasks A in add 205.3g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% absolute ethyl alcohol=1:3.0, one end of wireway is passed into A
Below reaction solution liquid level, methyl three is added in the 500ml there-necked flasks B in the other end dry nitrogen of access of wireway
Chlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 DEG C of heating, when methyl trichlorosilane boiling
When rising, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating, cold
But to after normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the yield for obtaining is collected in distillation
It is 97.83%.
Embodiment 3
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 1000ml four-hole boiling flasks A in add 203.5g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% absolute methanol=1:3.1, one end of wireway is passed into A
Below reaction solution liquid level, methyl three is added in the 500ml there-necked flasks B in the other end dry nitrogen of access of wireway
Chlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 DEG C of heating, when methyl trichlorosilane boiling
When rising, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating, cold
But to after normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the yield for obtaining is collected in distillation
It is 94.31%.
Embodiment 4
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 1000ml four-hole boiling flasks A in add 199.7g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% anhydrous propyl alcohol=1:3.2, one end of wireway is passed into
In A below reaction solution liquid level, first is added in the 500ml there-necked flasks B in the other end dry nitrogen of access of wireway
Base trichlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 degrees Celsius of heating, when methyl three
When chlorosilane seethes with excitement, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stopped
Heating, after being cooled to normal temperature, is passed through ammonia and is neutralized to pH=8~9, filters, and 143 DEG C of cut is collected in distillation, is obtained
The yield for arriving is 94.35%.
Embodiment 5
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 1000ml four-hole boiling flasks A in add 403.7g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% anhydrous isopropyl alcohol=1:3.0, one end of wireway is passed through
To in A below reaction solution liquid level, added in the 500ml there-necked flasks B in the other end dry nitrogen of access of wireway
Methyl trichlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 degrees Celsius of heating, works as methyl
When trichlorosilane seethes with excitement, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stopped
Only heat, after being cooled to normal temperature, be passed through ammonia and be neutralized to pH=8~9, filter, 143 DEG C of cut is collected in distillation,
The yield for obtaining is 98.87%.
Embodiment 6
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 1000ml four-hole boiling flasks A in add 430g monomethyl trichlorines
Silane, according to mol ratio methyl trichlorosilane：Mass fraction is 99.5% anhydrous butanol=1:3.0, one end of wireway is passed through
To in A below reaction solution liquid level, added in the 500ml there-necked flasks B in the other end dry nitrogen of access of wireway
Methyl trichlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 80 DEG C of heating, works as absolute ethyl alcohol
During boiling, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating,
After being cooled to normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the product for obtaining is collected in distillation
Rate is 96.18%.
Embodiment 7
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 2000ml four-hole boiling flasks A in add 600.5g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% absolute ethyl alcohol=1:3.0, one end of wireway is passed into A
Below reaction solution liquid level, methyl three is added in the 1000ml there-necked flasks B in the other end dry nitrogen of access of wireway
Chlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 DEG C of heating, when methyl trichlorosilane boiling
When rising, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating, cold
But to after normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the yield for obtaining is collected in distillation
It is 98.96%.
Embodiment 8
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 2000ml four-hole boiling flasks A in add 800.0g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% absolute ethyl alcohol=1:3.0, one end of wireway is passed into
In A below reaction solution liquid level, first is added in the 1000ml there-necked flasks B in the other end dry nitrogen of access of wireway
Base trichlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 DEG C of heating, when methyl trichlorine silicon
When alkane seethes with excitement, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating,
After being cooled to normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the product for obtaining is collected in distillation
Rate is 99.1%.
Embodiment 9
(its upper end is equipped with being passed through brine ice to have thermometer, mechanical agitator, wireway and ball condenser in equipment one
Serpentine condenser, surge flask and HCl absorption plants) 2000ml four-hole boiling flasks A in add 900.3g absolute ethyl alcohols,
According to mol ratio methyl trichlorosilane：Mass fraction is 99.5% absolute methanol=1:3.0, one end of wireway is passed into
In A below reaction solution liquid level, first is added in the 1000ml there-necked flasks B in the other end dry nitrogen of access of wireway
Base trichlorosilane, heats A to 60 DEG C, opens brine ice cooling water, while B to 65 DEG C of heating, when methyl trichlorine silicon
When alkane seethes with excitement, to dry nitrogen is passed through in B, charging is completed, and A is warming up to 80 DEG C, and backflow 3 as a child stops heating,
After being cooled to normal temperature, it is passed through ammonia and is neutralized to pH=8~9, filter, 143 DEG C of cut, the product for obtaining is collected in distillation
Rate is 98.96%.
Claims (3)
1. a kind of preparation method of methyl trialkoxysilane, it is characterised in that comprise the following steps：
1) toward adding one end of absolute alcohol, wireway to be passed through to reaction vessel A liquid levels in the reaction vessel A equipped with thermometer, mechanical agitator, wireway and condenser, the other end of wireway is accessed in the container B equipped with methyl trichlorosilane；
2) absolute alcohol in heating response container A is to 55-63 DEG C, and turn on agitator is stirred, open condenser, methyl trichlorosilane in heating container B to 62-68 DEG C, when methyl trichlorosilane seethes with excitement, to being passed through N2 in container B, treat that the methyl trichlorosilane in container B is added completely into reaction vessel A, continue to be passed through N2 toward container B, the mixed solution in reaction vessel A is warming up to 75-88 DEG C, flow back and insulation reaction 1-4h；
Flow back and stopping heating after insulation reaction 1-4h, obtain product, product is naturally cooled into normal temperature, be passed through ammonia and be neutralized to pH for 8-9, filtering, distillation, recovery cut liquid obtain methyl trialkoxysilane.
2. the preparation method of methyl trialkoxysilane according to claim 1, it is characterised in that：R is：Methyl, ethyl, propyl group, butyl, isopropyl.
3. the preparation method of methyl trialkoxysilane according to claim 1, it is characterised in that：Methyl trichlorosilane is 1 with the mol ratio of absolute alcohol：2.5-4.0.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232636A (en) * | 2018-10-22 | 2019-01-18 | 浙江衢州正邦有机硅有限公司 | A kind of preparation method of methyltriethoxysilane |
| 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 |
-
2015
- 2015-11-16 CN CN201510789380.6A patent/CN106699800A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109232636A (en) * | 2018-10-22 | 2019-01-18 | 浙江衢州正邦有机硅有限公司 | A kind of preparation method of methyltriethoxysilane |
| 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 |
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