CN102718791A - Preparation process of trimethylethoxysilane - Google Patents
Preparation process of trimethylethoxysilane Download PDFInfo
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- CN102718791A CN102718791A CN2012101871871A CN201210187187A CN102718791A CN 102718791 A CN102718791 A CN 102718791A CN 2012101871871 A CN2012101871871 A CN 2012101871871A CN 201210187187 A CN201210187187 A CN 201210187187A CN 102718791 A CN102718791 A CN 102718791A
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- trimethylethoxysilane
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Abstract
The invention discloses a preparation process of trimethylethoxysilane, which comprises the following specific steps of: (1) reaction: firstly adding 14 parts of trimethylchlorosilane and 9 parts of urea in a stirring kettle, mixing and agitating; then dropwise adding 8-9 parts of ethanol into the stirring kettle, finishing adding within 2 hours, stop agitating after reaction, standing and layering for 20-60 minutes, discharging bottom acid liquid and introducing an upper coarse product into a neutralization kettle; (2) neutralization: terminating the neutralization reaction when a system is neutral or alkalescent; standing and settling after reaction, rectifying supernatant liquor, uniformly filtering a lower sediment after accumulation, rectifying generated liquid and recovering solid residues; (3) rectification: adding the supernatant liquor into a rectifying tower kettle to produce the trimethylethoxysilane. The preparation method has the beneficial effects that the reaction can be carried out at a normal temperature, so that the concentration of the hydrogen chloride in the system is reduced, and the generation of secondary reaction is avoided; and the rectification yield is greatly improved, and the production cost is reduced.
Description
Technical field
The present invention relates to the preparation technology of trimethylethoxysilane.
Background technology
Traditional trimethylethoxysilane preparation technology adopts direct alcoholysis fat method, and promptly under the heating evaporation conditions, ethanol and trimethylchlorosilane direct reaction (or adopt double tower fatization; Promptly adopt second-stage reaction, carry out under the different fat temperature), after the product condensation; Add neutralizing agent again and remove wherein hydrogenchloride; Make unreacted continue completely to react completely simultaneously, filter cleaner, liquid go rectifying to obtain product.
The greatest problem of traditional preparation process technology is in reaction process, to have side reaction, and side reaction produces water again after taking place, and makes raw material (or product) hydrolysis, generates the wire organo-siloxane.Owing to exist a large amount of hydrogenchloride to be difficult for removing in the system, promote the generation of side reaction again at a certain temperature simultaneously, caused vicious cycle.In addition since system to contain the hydrogenchloride amount bigger, cause the neutralizing agent add-on to increase, produce the waste residue amount and also increase, the result makes that operation is wayward, technical process is long, product yield significantly reduces, by product and waste residue increase.
Summary of the invention
The present invention is directed to the shortcoming in the background technology, developed the preparation technology of trimethylethoxysilane, in technology, added chlorine hydride absorbent, reduce hydrogen cloride concentration, prevent the generation of side reaction and the vicious cycle that side reaction causes.
Technical solution of the present invention:
The preparation technology of trimethylethoxysilane, concrete steps are:
1, reaction: at first in stirring tank, drop into 14 parts of trimethylchlorosilanes and 9 parts of urea, mix and stir; In stirring tank, drip 8～9 parts of ethanol then, be added dropwise to complete in two hours, be reflected at-200mm～carry out under the 0mm mercury column, temperature is controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 20～60 minutes is emitted the acid liquid in bottom, during the upper strata crude product is imported and still; The hydrogen chloride gas with urea reaction is not absorbed the agent absorption through the hydrogen chloride absorption device;
2, neutralization: before neutralization, analyze wherein trimethylethoxysilane and hydrogen chloride content, in order to confirm the add-on of neutralizing agent, the neutralizing agent add-on requires excessive more than 5%; When system was neutrality or meta-alkalescence, neutralization reaction finished; Reaction finishes the back quiescent settling, supernatant liquid rectifying, and the lower sediment thing is unified the filtration after accumulating, the liquid distillation of generation, solid residue reclaims;
3, rectifying: clear liquid is dropped in the rectifying tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction ethanol (78.4 ℃ of cat head temperature) and middle distillate, extraction trimethylethoxysilane (114 ℃ of cat head temperature) again, interior a little high boiling product that remains of last tower still; Can stay in the tower still, accumulation reaches emits after a certain amount of.
Said hydrogen chloride absorption device is a falling-film absorber.
Said chlorine hydride absorbent is ammonia, amine nitrogenous compound or earth alkali metal.
Said neutralizing agent is potassium alcoholate, sodium alkoxide or earth alkali metal.
Said rectifying tower is a batch fractionating tower.
Said stirring tank is 1m
3The enamel stirring tank.
The control of said step (1) temperature is lowered the temperature with rate of addition or chuck cold water and is realized.
Neutralizing agent is a sodium ethylate during said step (2) neutralization reaction, and the sodium ethylate add-on is 0.12～0.5 part.
Said ethanol recycles after rectifying.
Said middle distillate recycles.
The reaction formula that trimethylethoxysilane prepares in the process is:
1, main reaction:
2, side reaction:
3, neutralization reaction:
Beneficial effect of the present invention:
1. being reflected at normal temperature can carry out, and the hydrogen cloride concentration in the system is reduced, and has avoided the generation of secondary reaction, thereby has made reaction process shorten, and investment reduces; Neutralization reaction is easy to control, and process cost reduces; The rectifying yield significantly improves, and reduces production costs.
2. absorption agent becomes a kind of liquid behind absorbing hydrogen chloride, and does not dissolve each other with crude product, separates so be easy to layering, has prevented that the solid by-product bag from dissolving thick product, and promptly easy handling can improve the yield of crude product again.
3. adopt potassium alcoholate, sodium alkoxide etc. not to produce the neutralizing agent of water in the N-process of the present invention, reaction is easy to thoroughly, and the deposition of generation can be accumulated the after-filtration slagging-off.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Embodiment one: as shown in the figure, the step of preparation process of trimethylethoxysilane is:
1, reaction: at first to 1m
3Drop into trimethylchlorosilane 700kg in the enamel stirring tank, urea 450kg mixes and stirs; In stirring tank, drip ethanol 400kg then, be added dropwise to complete in two hours, be reflected at-carry out under 200～0mm mercury column, temperature is controlled at below 60 ℃ with rate of addition or chuck cold water temperature reduction way; The hydrogen chloride gas with urea reaction is not absorbed by water through falling-film absorber; Stop after reaction finishes stirring, static layering 20 minutes is emitted the acid liquid in bottom, during the upper strata crude product is imported and still.
2, neutralization: before neutralization, analyze wherein trimethylethoxysilane and hydrogen chloride content; In order to confirm the add-on of neutralizing agent, neutralizing agent is potassium alcoholate, sodium alkoxide or earth alkali metal, and add-on is excessive more than 5%; In this process in order to improve speed of response; Add adequate amount of ethanol and improve reactant concn, when system was neutrality or meta-alkalescence, neutralization reaction finished; Reaction finishes the back quiescent settling, supernatant liquid rectifying, and the lower sediment thing is unified the filtration after accumulating, liquid distillation, solid residue reclaims.
3, rectifying: clear liquid is dropped in the batch fractionating tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction trimethylethoxysilane (75.7 ℃ of cat head temperature) and middle distillate, extraction ethanol (78.3 ℃ of cat head temperature) again, interior a little high boiling product that remains of last tower still; Can stay in the tower still, accumulation reaches emits after a certain amount of.
Above-mentioned technology can prepare trimethylethoxysilane 690.2kg, and yield is 51.1%.
Embodiment two: as shown in the figure, the step of preparation process of trimethylethoxysilane is:
1, reaction: at first to 1m
3Drop into trimethylchlorosilane 700kg in the enamel stirring tank, urea 450kg mixes and stirs; In stirring tank, drip ethanol 410kg then, be added dropwise to complete in two hours, be reflected at-carry out under 200～0mm mercury column, temperature is controlled at below 60 ℃, and temperature is controlled at below 60 ℃ with rate of addition or chuck cold water temperature reduction way; The hydrogen chloride gas with urea reaction is not absorbed by water through falling-film absorber; Stop after reaction finishes stirring, static layering 60 minutes is emitted the acid liquid in bottom, during the upper strata crude product is imported and still.
2, neutralization: before neutralization, analyze wherein trimethylethoxysilane and hydrogen chloride content; In order to confirm the add-on of neutralizing agent, neutralizing agent is potassium alcoholate, sodium alkoxide or earth alkali metal, and add-on is excessive more than 5%; In this process in order to improve speed of response; Add adequate amount of ethanol and improve reactant concn, when system was neutrality or meta-alkalescence, neutralization reaction finished; Reaction finishes the back quiescent settling, supernatant liquid rectifying, and the lower sediment thing is unified the filtration after accumulating, liquid distillation, solid residue reclaims.
3, rectifying: clear liquid is dropped in the batch fractionating tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction trimethylethoxysilane (75.7 ℃ of cat head temperature) and middle distillate, extraction ethanol (78.3 ℃ of cat head temperature) again, interior a little high boiling product that remains of last tower still; Can stay in the tower still, accumulation reaches emits after a certain amount of.
Above-mentioned technology can prepare trimethylethoxysilane 700.3kg, and yield is 51.7%.
Embodiment three: as shown in the figure, the step of preparation process of trimethylethoxysilane is:
1, reaction: at first to 1m
3Drop into trimethylchlorosilane 700kg in the enamel stirring tank, urea 450kg mixes and stirs; In stirring tank, drip ethanol 430kg then, be added dropwise to complete in two hours, be reflected at-carry out under 200～0mm mercury column, temperature is controlled at below 60 ℃, and temperature is controlled at below 60 ℃ with rate of addition or chuck cold water temperature reduction way; The hydrogen chloride gas with urea reaction is not absorbed by water through falling-film absorber; Stop after reaction finishes stirring, static layering 45 minutes is emitted the acid liquid in bottom, during the upper strata crude product is imported and still.
2, neutralization: before neutralization, analyze wherein trimethylethoxysilane and hydrogen chloride content; In order to confirm the add-on of neutralizing agent, neutralizing agent is potassium alcoholate, sodium alkoxide or earth alkali metal, and add-on is excessive more than 5%; In this process in order to improve speed of response; Add adequate amount of ethanol and improve reactant concn, when system was neutrality or meta-alkalescence, neutralization reaction finished; Reaction finishes the back quiescent settling, supernatant liquid rectifying, and the lower sediment thing is unified the filtration after accumulating, liquid distillation, solid residue reclaims.
3, rectifying: clear liquid is dropped in the batch fractionating tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction trimethylethoxysilane (75.7 ℃ of cat head temperature) and middle distillate, extraction ethanol (78.3 ℃ of cat head temperature) again, interior a little high boiling product that remains of last tower still; Can stay in the tower still, accumulation reaches emits after a certain amount of.
Above-mentioned technology can prepare trimethylethoxysilane 716.4kg, and yield is 52.5%.
Claims (10)
1. the preparation technology of trimethylethoxysilane, concrete steps are:
(1) reaction: at first in stirring tank, drop into 14 parts of trimethylchlorosilanes and 9 parts of urea, mix and stir; In stirring tank, drip 8～9 parts of ethanol then, be added dropwise to complete in two hours, be reflected at-200mm～carry out under the 0mm mercury column, temperature is controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 20～60 minutes is emitted the acid liquid in bottom, during the upper strata crude product is imported and still; The hydrogen chloride gas with urea reaction is not absorbed the agent absorption through the hydrogen chloride absorption device;
(2) neutralization: before neutralization, analyze wherein trimethylethoxysilane and hydrogen chloride content, in order to confirm the add-on of neutralizing agent, the neutralizing agent add-on requires excessive more than 5%; When system was neutrality or meta-alkalescence, neutralization reaction finished; Reaction finishes the back quiescent settling, supernatant liquid rectifying, and the lower sediment thing is unified the filtration after accumulating, the liquid distillation of generation, solid residue reclaims;
(3) rectifying: clear liquid is dropped in the rectifying tower still, in stage number 6～12 following varying reflux ratio operations, intermittently extraction ethanol and middle distillate; Extraction trimethylethoxysilane again; A little high boiling product of residue can be stayed in the tower still in the last tower still, and accumulation reaches emits after a certain amount of.
2. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: said hydrogen chloride absorption device is a falling-film absorber.
3. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: said chlorine hydride absorbent is ammonia, amine nitrogenous compound or earth alkali metal.
4. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: said neutralizing agent is potassium alcoholate, sodium alkoxide or earth alkali metal.
5. like the preparation technology of the described trimethylethoxysilane of claim 1, it is characterized in that: said rectifying tower is a batch fractionating tower.
6. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: said stirring tank is 1m
3The enamel stirring tank.
7. the preparation technology of trimethylethoxysilane as claimed in claim 1 is characterized in that: the control of said step (1) temperature is lowered the temperature with rate of addition or chuck cold water and is realized.
8. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: neutralizing agent is a sodium ethylate during said step (2) neutralization reaction, and the sodium ethylate add-on is 0.12～0.5 part.
9. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: said ethanol recycles after rectifying.
10. the preparation technology of trimethylethoxysilane as claimed in claim 1, it is characterized in that: said middle distillate recycles.
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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 |
| CN115490239A (en) * | 2022-10-12 | 2022-12-20 | 天津市建筑材料科学研究院有限公司 | Organic silicon hydrophobic modifier, preparation method and application thereof, and preparation method of silicon dioxide aerogel |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4380660A (en) * | 1982-07-01 | 1983-04-19 | Allied Corporation | Producing alkoxysilanes and alkoxy-oximinosilanes |
| 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 |
| CN101712691A (en) * | 2009-12-17 | 2010-05-26 | 吉林新亚强生物化工有限公司 | Preparation method of dimethyl dimethoxy triacetoxy |
| CN102432633A (en) * | 2011-12-07 | 2012-05-02 | 诺贝尔（九江）高新材料有限公司 | Alcoholysis process of chloropropyltriethoxysilane |
-
2012
- 2012-06-08 CN CN2012101871871A patent/CN102718791A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4380660A (en) * | 1982-07-01 | 1983-04-19 | Allied Corporation | Producing alkoxysilanes and alkoxy-oximinosilanes |
| 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 |
| CN101712691A (en) * | 2009-12-17 | 2010-05-26 | 吉林新亚强生物化工有限公司 | Preparation method of dimethyl dimethoxy triacetoxy |
| CN102432633A (en) * | 2011-12-07 | 2012-05-02 | 诺贝尔（九江）高新材料有限公司 | Alcoholysis process of chloropropyltriethoxysilane |
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 |
| CN115490239A (en) * | 2022-10-12 | 2022-12-20 | 天津市建筑材料科学研究院有限公司 | Organic silicon hydrophobic modifier, preparation method and application thereof, and preparation method of silicon dioxide aerogel |
| CN115490239B (en) * | 2022-10-12 | 2023-10-13 | 天津市建筑材料科学研究院有限公司 | Organosilicon hydrophobic modifier, preparation method and application thereof, and preparation method of silica aerogel |
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Application publication date: 20121010 |