CN1955184A - Preparation method of ditert-butyldiacetyl oxygen-base silane - Google Patents
Preparation method of ditert-butyldiacetyl oxygen-base silane Download PDFInfo
- Publication number
- CN1955184A CN1955184A CN 200510095040 CN200510095040A CN1955184A CN 1955184 A CN1955184 A CN 1955184A CN 200510095040 CN200510095040 CN 200510095040 CN 200510095040 A CN200510095040 A CN 200510095040A CN 1955184 A CN1955184 A CN 1955184A
- Authority
- CN
- China
- Prior art keywords
- reaction
- preparation
- caldron
- silicane
- acetoxy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
This invention discloses a preparation of di-tertiary butoxy di-acetoxy silicane. The mentioned preparation is a method of two-step dropping synthesis, the first is acylation, second is esterification. The mentioned acylation reaction is that silicon tetrachloride is slowly dropped into acetic anhydride that is in the caldron, reacting under certain temperature requirement, ferri ion produced in the reaction process is adverse to product quality, ferri ion content that is in the caldron is reduced by the method of releasing some acetic anhydride from caldron bottom, then warming to evaporate by-product that is acetyl chloride, the remained thing in the caldron is intermediate material that is tetro-acetoxy silicane. The mentioned esterification reaction is that tertiary butyl alcohol is slowly dropped into intermediate material which is in caldron, reacting under certain temperature and time, in condition of vacuum by-product that is acetic acid is evaporated out, the remained thing is di-tertiary butoxy di-acetoxy silicane. In this preparation, technology and manipulation is simple, yield and purity of objective product is high, production cost is relatively low. Di- tertiary butoxy di-acetoxy silicane is a cross linking agent of room temperature rigidification which produces depickling type of organosilicon hermetization mastic.
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 class seal gum is the organosilicon sealant of market consumption maximum.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:
Reaction equation (1) is an acylation reaction, and promptly the acylation reaction generation acylation reaction condition by silicon tetrachloride dropping aceticanhydride is as follows:
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 by trimethyl carbinol dropwise reaction equation (1).
The esterification condition is as follows:
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 reactor 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 the back and continue balanced reaction 3.3～3.7 (hr).The iron ion that generates in above-mentioned reaction process is the catalyzer that generates the byproduct 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 to emit a part of aceticanhydride in the reaction process later stage at the bottom of still, reducing iron ion content in the still, and then be warming up to 55～65 (℃) steam the byproduct Acetyl Chloride 98Min., remaining intermediates tetrem acyloxy silane in the still.The byproduct Acetyl Chloride 98Min. is a kind of industrial chemicals.Second step of present embodiment is to tetrem acyloxy silane esterification, press the feed ratio silicon tetrachloride: the trimethyl carbinol=1: (mol) measure (2.15～2.18), the trimethyl carbinol is extracted in the scale tank, 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 the back and continue reaction 0.5 (hr), and then be warmed up to 55～100 (℃), under vacuum tightness 680～700 (mmHg), steam byproduct 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 byproduct 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 only is 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%, yield improves about 10%, and chloride ion content has reduced more than 1000 (ppm).Because quality product improves, the sale price height, manufacturing cost reduces relatively.
Claims (2)
1, a kind of preparation method of ditert-butyldiacetyl oxygen-base silane is characterized in that: described preparation method dripped synthesis method, promptly first acidylate, back esterification in two steps; Reaction equation is:
(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 described 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 |
|---|---|---|---|
| CN 200510095040 CN1955184A (en) | 2005-10-27 | 2005-10-27 | Preparation method of ditert-butyldiacetyl oxygen-base silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510095040 CN1955184A (en) | 2005-10-27 | 2005-10-27 | Preparation method of ditert-butyldiacetyl oxygen-base silane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1955184A true CN1955184A (en) | 2007-05-02 |
Family
ID=38062762
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510095040 Pending CN1955184A (en) | 2005-10-27 | 2005-10-27 | Preparation method of ditert-butyldiacetyl oxygen-base silane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1955184A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387585A (en) * | 2013-07-22 | 2013-11-13 | 荆州市江汉精细化工有限公司 | A synthetic method for a silane acidic cross-linking agent |
| CN114315890A (en) * | 2022-01-05 | 2022-04-12 | 湖北江瀚新材料股份有限公司 | Preparation method of methacryloxypropyl triacetoxysilane |
-
2005
- 2005-10-27 CN CN 200510095040 patent/CN1955184A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387585A (en) * | 2013-07-22 | 2013-11-13 | 荆州市江汉精细化工有限公司 | A synthetic method for a silane acidic cross-linking agent |
| CN103387585B (en) * | 2013-07-22 | 2016-04-20 | 荆州市江汉精细化工有限公司 | A kind of synthetic method of silane acidic crosslinking agent |
| CN114315890A (en) * | 2022-01-05 | 2022-04-12 | 湖北江瀚新材料股份有限公司 | Preparation method of methacryloxypropyl triacetoxysilane |
| CN114315890B (en) * | 2022-01-05 | 2023-11-17 | 湖北江瀚新材料股份有限公司 | Preparation method of methacryloxypropyl triacetoxy silane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7829736B2 (en) | Method for the production of cyclic phosphonic acid anhydrides | |
| CN1955184A (en) | Preparation method of ditert-butyldiacetyl oxygen-base silane | |
| CN103342718B (en) | A kind of 3-(methyl alkoxy phosphoryl) preparation method of propionic acid ester compound | |
| US20170088502A1 (en) | Method for producing carboxylic acid anhydride and method for producing carboxylic acid ester | |
| CN101143815A (en) | Method for preparing felbinac | |
| CN1911941A (en) | Preparation method of 2,10-dihydro-9-oxo-10-phospho hetero phenanthrene | |
| CN1903830A (en) | Preparation method of 2-bromo-2-nitro-1,3-propylene glycol | |
| CN1340507A (en) | Process for preparing glyphosate | |
| EP2928850A1 (en) | Palladium-catalyzed decarbonylation of fatty acid anhydrides for the production of linear alpha olefins | |
| CN102453046A (en) | Preparation method of di-tert-butoxy diacetoxy silane | |
| CN1651374A (en) | Process for preparing alkoxy-pure alkaline earth alkoxides | |
| KR102151747B1 (en) | Method of preparing alkyl carboxylic acid ester and apparatus of preparing alkyl carboxylic acid ester | |
| CN1268593C (en) | Method for isomerizating 1,4-dichloro-2-butylenes from syn form to anti form | |
| JP2006104169A (en) | Method for producing tertiary cycloalkyl (meth)acrylate | |
| CN107216277B (en) | Preparation method of LCZ696 medicine impurity | |
| CN1238316C (en) | Process for preparing phenol derivative | |
| CN1752001A (en) | The preparation method of sodium thiophosphate | |
| CN1473758A (en) | Method for preparing sulfur dichloride | |
| CN1733691A (en) | Industrial synthesis method of 3,5-di tertiary butyl-4-hydroxyl phenyl methyl propionate | |
| CN1218927C (en) | Synthesis of gamma-ethyl bromo-butyrate | |
| JPS5826330B2 (en) | Method for producing stereo-regulated farnesyl acetate | |
| CN101781201A (en) | Improved process for synthesizing 3-alkoxy acrylic ester | |
| CN1560036A (en) | 4-hydroxylic pyridine and production process thereof | |
| CN1207332C (en) | Preparation of methyl thioglycollic acid tin isooctate | |
| CN107827810B (en) | Synthesis method of N-ethoxycarbonyl-4-hydroxypiperidine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |