CN102453046A - Preparation method of di-tert-butoxy diacetoxy silane - Google Patents
Preparation method of di-tert-butoxy diacetoxy silane Download PDFInfo
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- CN102453046A CN102453046A CN2010105158884A CN201010515888A CN102453046A CN 102453046 A CN102453046 A CN 102453046A CN 2010105158884 A CN2010105158884 A CN 2010105158884A CN 201010515888 A CN201010515888 A CN 201010515888A CN 102453046 A CN102453046 A CN 102453046A
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Abstract
The invention discloses a preparation method of di-tert-butoxy diacetoxy silane. The preparation method which is a two-step dropping synthesis method comprises steps of acylation and esterification. According to the acylation reaction, silicon tetrachloride is slowly added to acetic anhydride in a kettle drop by drop and undergoes a reaction under certain temperature conditions, iron ions generated in the reaction process are bad for the product quality, the content of the iron ions can be reduced by discharging partial acetic anhydride from the kettle bottom, and then the kettle is heated to evaporate a byproduct acetyl chloride, so an intermediate product tetraacetoxy silane is remained in the kettle. According to the esterification reaction, t-butyl alcohol which is slowly adding to the intermediate product in the kettle drop by drop undergoes a reaction for a certain time at a certain temperature, a byproduct acetate is evaporated under vacuum conditions, and di-tert-butoxy diacetoxy silane is remained. The preparation method has the advantages of easily operated technology, high yield and high purity of the target product, and relatively low production cost. Di-tert-butoxy diacetoxy silane is a room temperature curing crosslinking agent for the production of deacidification organosilicon sealants.
Description
Technical field
The present invention relates to a kind of preparation method of organosilicon sealant self-vulcanizing linking agent.
Background technology
Ditert-butyldiacetyl oxygen-base silane is a kind of self-vulcanizing linking agent that is mainly used in production depickling type organosilicon sealant, and this type sealer is the maximum organosilicon sealant of market consumption.The main ingredient of ditert-butyldiacetyl oxygen-base silane is aceticanhydride, the trimethyl carbinol and silicon tetrachloride, and existing preparation method is an one-step synthesis, i.e. acidylate, esterification carried out simultaneously; This synthesis method technology poor operability; Raw materials quality requires high, and object yield and purity are low, and production cost is also higher.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, provide a kind of technological operation easy, the preparation method of the ditert-butyldiacetyl oxygen-base silane that object yield and purity are high.
For realizing above-mentioned target, the preparation method of ditert-butyldiacetyl oxygen-base silane of the present invention dripped synthesis method, promptly first acidylate, back esterification in two steps.
Reaction equation is:
SiCl
4+4(CH
3CO)
2O→(CH
3COO)
4Si+4CH
3COCL (1)
(CH
3COO)
4Si+2(CH
3)
3COH→[(CH
3)
3CO]
2Si(CH
3COO)
2+2CH
3COOH (2)
Reaction equation (1) is an acylation reaction, and promptly the acylation reaction generation acylation reaction condition through silicon tetrachloride dropping aceticanhydride is following:
Temperature of reaction: 25～45 (℃)
The dropping time: 2～3 (hr)
Feed ratio: silicon tetrachloride: aceticanhydride=1: (4.5～4.6) (mol)
Starting time: 3～4 (hr)
Take off low temperature: 45～70 (℃)
Reaction equation (2) is an esterification, promptly generates the reaction of tetrem acyloxy silane through trimethyl carbinol dropwise reaction equation (1).
The esterification condition is following:
Feed ratio: silicon tetrachloride: the trimethyl carbinol=1: (2.1～2.2) (mol)
Temperature of reaction: 25～40 (℃)
Reaction times: 3～4 (hr)
Take off low temperature: 45～110 (℃)
Cooling temperature:＜45 ℃
Vacuum tightness: >=650～700 (mmHg)
Above-mentioned two steps drip in the synthesis preparation method the acylation reaction condition preferably:
Temperature of reaction: 30～38 (℃)
The dropping time: 2.2～2.5 (hr)
Feed ratio: silicon tetrachloride: aceticanhydride=1: (4.55～4.58) (mol)
Starting time: 3.3～3.7 (hr)
Take off low temperature: 55～65 (℃)
Above-mentioned two steps drip in the synthesis preparation method the esterification condition preferably:
Feed ratio: silicon tetrachloride: the trimethyl carbinol=1: (2.15～2.18) (mol)
Temperature of reaction: 30～36 (℃)
Reaction times: 3.5～3.8 (hr)
Take off low temperature: 55～100 (℃)
Cooling temperature: 20～35 ℃
Vacuum tightness: 680～700 (mmHg)
Embodiment
The main raw material of ditert-butyldiacetyl oxygen-base silane is silicon tetrachloride, aceticanhydride, the trimethyl carbinol.The first step acylation reaction when present embodiment prepares; Press the feed ratio silicon tetrachloride: aceticanhydride=1: 4.55 (mol) metering, be pumped in the exsiccant reaction kettle aceticanhydride is disposable, start whipping appts; Open water coolant; Slowly drip silicon tetrachloride through 2.2～2.5 (hr), this elementary reaction temperature 30～38 (℃), dropwise continued balanced reaction 3.3～3.7 (hr).The iron ion that in above-mentioned reaction process, generates is the catalyzer that generates the sub product Acetyl Chloride 98Min., and the concentration of the high Acetyl Chloride 98Min. that generates of iron ion content just increases, thereby influences yield and purity.Terms of settlement is at the bottom of still, to emit a part of aceticanhydride in the reaction process later stage, reducing iron ion content in the still, and then be warming up to 55～65 (℃) steam the sub product Acetyl Chloride 98Min., remaining intermediates tetrem acyloxy silane in the still.The sub product Acetyl Chloride 98Min. is a kind of industrial chemicals.Second step of present embodiment, press the feed ratio silicon tetrachloride: the trimethyl carbinol=1: (mol) measured (2.15～2.18), and the trimethyl carbinol is extracted in the scale tank to tetrem acyloxy silane esterification; Start whipping appts, open water coolant, slowly in still, drip the trimethyl carbinol through 3.5～3.8 (hr); This elementary reaction temperature 30～36 (℃); Dropwise continued reaction 0.5 (hr), and then be warmed up to 55～100 (℃), under vacuum tightness 680～700 (mmHg), steam sub product acetate; The remaining ditert-butyldiacetyl oxygen-base silane that is in the still, to be cooled to 20～30 (℃) time in still, take out the product ditert-butyldiacetyl oxygen-base silane.The sub product acetate that generates also is a kind of industrial chemicals.
The ditert-butyldiacetyl oxygen-base silane purity that above-mentioned two steps drip the synthesis method preparation reaches more than 90%; Yield reaches 88～92%; Chloride ion content is merely 200 (ppm); The ditert-butyldiacetyl oxygen-base silane purity that drips the synthesis method preparation than one step of prior art is carried more than 5%, and yield improves about 10%, and chloride ion content has reduced more than 1000 (ppm).Because quality product improves, sale price is high, and manufacturing cost reduces relatively.
Claims (2)
1. the preparation method of a ditert-butyldiacetyl oxygen-base silane is characterized in that: said preparation method dripped synthesis method, promptly first acidylate, back esterification in two steps; Reaction equation is:
SiCl
4+4(CH
3CO)
2O→(CH
3COO)
4Si+4CH
3COCL (1)
(CH
3COO)
4Si+2(CH
3)
3COH→[(CH
3)
3CO]
2Si(CH
3COO)
2+2CH
3COOH (2)
(1) the acylation reaction condition is:
Temperature of reaction: 25～45 (℃)
The dropping time: 2～3 (hr)
Feed ratio: silicon tetrachloride: aceticanhydride=1: (4.5～4.6) (mol)
Starting time: 3～4 (hr)
Take off low temperature: 45～70 (℃);
(2) the esterification condition is:
Feed ratio: silicon tetrachloride: the trimethyl carbinol=1: (2.1～2.2) (mol)
Temperature of reaction: 25～40 (℃)
Reaction times: 3～4 (hr)
Take off low temperature: 45～110 (℃)
Cooling temperature:＜45 ℃
Vacuum tightness: >=650～700 (mmHg).
2. the preparation method of ditert-butyldiacetyl oxygen-base silane according to claim 1 is characterized in that said acylation reaction condition is:
Temperature of reaction: 30～38 (℃)
The dropping time: 2.2～2.5 (hr)
Feed ratio: silicon tetrachloride: aceticanhydride=1: (4.55～4.58) (mol)
Starting time: 3.3～3.7 (hr)
Take off low temperature: 55～65 (℃)
The esterification condition is:
Feed ratio: silicon tetrachloride: the trimethyl carbinol=1: (2.15～2.18) (mol)
Temperature of reaction: 30～36 (℃)
Reaction times: 3.5～3.8 (hr)
Take off low temperature: 55～100 (℃)
Cooling temperature: 20～35 (℃)
Vacuum tightness: 680～700 (mmHg).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105158884A CN102453046A (en) | 2010-10-21 | 2010-10-21 | Preparation method of di-tert-butoxy diacetoxy silane |
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|---|---|---|---|
| CN2010105158884A CN102453046A (en) | 2010-10-21 | 2010-10-21 | Preparation method of di-tert-butoxy diacetoxy silane |
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|---|---|
| CN102453046A true CN102453046A (en) | 2012-05-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203443A (en) * | 2016-12-19 | 2018-06-26 | 湖北环宇化工有限公司 | The synthetic method of ditert-butyldiacetyl oxygen-base silane |
-
2010
- 2010-10-21 CN CN2010105158884A patent/CN102453046A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203443A (en) * | 2016-12-19 | 2018-06-26 | 湖北环宇化工有限公司 | The synthetic method of ditert-butyldiacetyl oxygen-base silane |
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Application publication date: 20120516 |