US4039567A
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US
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Process for the continuous esterification of chlorosilanes
Assignee: Dynamit Nobel AG
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Filing: 1975-06-05
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Granted: 1977-08-02
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Expires: 1995-06-05
Abstract
Abstract An improvement in a process for the preparation of an alkoxysilane of the formula: R.sub.4.sub.-n.sub.-m Si(OR').sub.n Cl.sub.m wherein R is hydrogen or a saturated or unsaturated, chlorinated or unchlorinated alkyl radical of 1 to 12 carbon atoms; R' is an alkyl radical of 1 to 11 carbon atoms which can contain a hetero atom in the chain; m equals 0 to 3; n equals 1 to 4; n + M is equal to or less than 4; By esterification of a chlorosilane of the formula: R.sub.4.sub.-n SiCl.sub.n wherein R and n have the previously assigned significance with an alcohol, the improvement residing in continuously charging liquid alcohol and liquid chlorosilane from a separate source into a distillative reaction zone having a head portion and a sump portion, maintaining the head portion at a temperature sufficient for said esterification, continuously distilling off gaseous HCl formed during said esterification while maintaining the resultant reaction mixture in the sump at its boiling point and continuously separating liquid alkoxysilane from the sump.
Inventors
- 👤 Hans-Joachim Kotzsch
- 👤 Hans-Joachim Vahlensieck
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 19:09
CPC Classifications
C; C07; C07F; C07F7/00; C07F7/02; C07F7/025; C07F7/08; C07F7/18; C07F7/1804; C07F7/1872; C07F7/188
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
167 words
In a process for the preparation of an alkoxysilane of the formula: R.sub.4.sub.-n.sub.-m Si(OR').sub.n Cl.sub.m wherein R is hydrogen or a saturated or unsaturated, chlorinated or unchlorinated alkyl radical of 1 to 12 carbon atoms; R' is an alkyl radical of 1 to 11 carbon atoms which can contain a hetero atom in the chain; m is 0 to 3; n is 1 to 4; n + m is equal to or less than 4; by esterification of a chlorosilane of the formula: R.sub.4.sub.-n SiCl.sub.n wherein R and n have the previously assigned significance, with an alcohol, the improvement which comprises continuously charging liquid alcohol and liquid chlorosilane simultaneously from separate sources into a distillative reaction zone having a head portion and a sump portion, maintaining the head portion at a temperature sufficient for said esterification, continuously distilling off gaseous HCl formed during said esterification while maintaining the resultant reaction mixture in the sump at its boiling point and continuously separating liquid alkoxy silane from the sump.
Claim 2
Dependent Claim
167 words
In a process for the preparation of an alkoxysilane of the formula: R.sub.4.sub.-n.sub.-m Si(OR').sub.n Cl.sub.m wherein R is hydrogen or a saturated or unsaturated, chlorinated or unchlorinated alkyl radical of 1 to 12 carbon atoms; R' is an alkyl radical of 1 to 11 carbon atoms which can contain a hetero atom in the chain; m is 0 to 3; n is 1 to 4; n + m is equal to or less than 4; by esterification of a chlorosilane of the formula: R.sub.4.sub.-n SiCl.sub.n wherein R and n have the previously assigned significance, with an alcohol, the improvement which comprises continuously charging liquid alcohol and liquid chlorosilane simultaneously from separate sources into a distillative reaction zone having a head portion and a sump portion, maintaining the head portion at a temperature sufficient for said esterification, continuously distilling off gaseous HCl formed during said esterification while maintaining the resultant reaction mixture in the sump at its boiling point and continuously separating liquid alkoxy silane from the sump.
Claim 3
Dependent Claim
27 words
A process according to claim 1 wherein the temperature of the reaction mixture in the sump is maintained at the boiling point of the desired ester product.
Claim 4
Dependent Claim
58 words
A process according to claim 1 wherein a solvent is employed, said solvent is introduced at the head portion of the distillative reaction zone and the temperature of the reaction mixture including solvent in the sump is maintained constantly in the range in which the mixture of the desired silane ester and solvent boils at a constant ratio.
Claim 5
Dependent Claim
28 words
A process according to claim 1 wherein the distillation zone comprises a plurality of distillation column trays and the liquid reactants react on the top most column tray.
Claim 6
Dependent Claim
25 words
A process according to claim 4 wherein liquid alcohol and liquid chlorosilane react within the upper 15% region of the length of the distillation column.
Claim 7
Dependent Claim
31 words
A process according to claim 1 wherein the chlorosilane is selected from the group consisting of trichlorosilane, tetrachlorosilane, methyldichlorosilane, dimethyldichlorosilane, trimethylchorosilane, methyltrichlorosilane, ethyltrichlorosilane, vinyltrichlorosilane, propyltrichlorosilane, allyltrichlorosilane, 3-chloropropyltrichlorosilane, normal butyltrichlorosilane and isobutyltrichlorosilane.
Claim 8
Dependent Claim
29 words
A process according to claim 1 wherein said alcohol is selected from the group consisting of methanol, ethanol, propanol, abutanol, an octanol, 2-methoxyethanol, 2-ethoxyethanol, 2-methoxyethyldiethyleneglycol ether and tetrahydrofurfuryl alcohol.
References Cited (Backward Citations)
US3792071A
Cited
US3801618A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-08-01 | 1981-01-31 | 1981-08-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-08-01 | 1985-01-31 | 1985-08-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-08-01 | 1989-01-31 | 1989-08-02 | $7700.00 | Window Closed / Lapsed |