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US3976675A Expired / Lapsed US ⏱️ 0.0 years remaining

Silicate-based surfactant composition

Assignee: Olin Corp
•
Filing: 1974-11-19
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Granted: 1976-08-24
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Expires: 1994-11-19
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Abstract

Abstract A novel silicate-based surfactant composition is prepared by a selective process involving (1) reaction of silicon tetrahalide with water and alcohol followed by (2) transesterification with a polyether alcohol. The resulting surfactant composition is utilized as a stabilizer in the production of polyurethane foam.

Inventors

  • 👤 Robert N. Scott
  • 👤 Henry F. Lederle
  • 👤 Frank J. Milnes
  • 👤 Maurice A. Raymond

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 21:04
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/0061; C07; C07F; C07F7/00; C07F7/02; C07F7/025; C08G; C08G77/00; C08G77/42; C08G77/46; C08J2375/00; C08J2375/04; C08J2483/00

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 259 words
A process for preparing a silicate-based surfactant composition which comprises: a. reacting together, at a temperature of about 40°-200°C, (1) a silicon tetrahalide selected from the group consisting of silicon tetrachloride, silicon tetrabromide, and silicon tetraiodide, and, per every mole of said silicon tetrahalide (2) about 0.2-2.0 moles of water and (3) at least about one mole of an alcohol represented by the formula R 1 OH wherein R 1 is alkyl of 2-20 carbon atoms or aryl of 6-14 carbon atoms, the reaction yielding a product made up of a volatile portion and a non-volatile portion, and b. at a temperature of about 65°-320°C and in the presence of a transesterification catalyst, reacting the non-volatile portion of the product of step (a) with a polyether alcohol having a molecular weight of about 500-5,000 and represented by the formula R 2 --C n H 2n O-- H wherein R 2 is alkyl of 1-10 carbon atoms and the moiety --C n H 2n O-- represents a polyoxyalkylene chain consisting of from about 10 to 100 percent by weight of oxyethylene units, and, correspondingly, about 90-0 percent of oxypropylene units, oxybutylene units or a mixture of oxypropylene and oxybutylene units, said polyether alcohol being employed in a molar proportion ranging from about 0.006 to about 1.1 moles per every mole of said silicon tetrayalide which is used in step (a), with the proviso that the molar proportion of said polyether alcohol is no more than about 55% of the molar proportion of alcohol consumed in the reaction of step (a).
Claim 2
Dependent Claim 259 words
A process for preparing a silicate-based surfactant composition which comprises: a. reacting together, at a temperature of about 40°-200°C, (1) a silicon tetrahalide selected from the group consisting of silicon tetrachloride, silicon tetrabromide, and silicon tetraiodide, and, per every mole of said silicon tetrahalide (2) about 0.2-2.0 moles of water and (3) at least about one mole of an alcohol represented by the formula R 1 OH wherein R 1 is alkyl of 2-20 carbon atoms or aryl of 6-14 carbon atoms, the reaction yielding a product made up of a volatile portion and a non-volatile portion, and b. at a temperature of about 65°-320°C and in the presence of a transesterification catalyst, reacting the non-volatile portion of the product of step (a) with a polyether alcohol having a molecular weight of about 500-5,000 and represented by the formula R 2 --C n H 2n O-- H wherein R 2 is alkyl of 1-10 carbon atoms and the moiety --C n H 2n O-- represents a polyoxyalkylene chain consisting of from about 10 to 100 percent by weight of oxyethylene units, and, correspondingly, about 90-0 percent of oxypropylene units, oxybutylene units or a mixture of oxypropylene and oxybutylene units, said polyether alcohol being employed in a molar proportion ranging from about 0.006 to about 1.1 moles per every mole of said silicon tetrayalide which is used in step (a), with the proviso that the molar proportion of said polyether alcohol is no more than about 55% of the molar proportion of alcohol consumed in the reaction of step (a).
Claim 3
Dependent Claim 10 words
A surfactant composition prepared by the process of claim 1.
Claim 4
Dependent Claim 32 words
A process as claimed in claim 1 which includes the intermediate step of removing said volatile portion before reacting said non-volatile portion of the product of step (a) with said polyether alcohol.
Claim 5
Dependent Claim 36 words
The process of claim 3 wherein said transesterification catalyst is selected from the group consisting of a Lewis acid, an alkali metal, an alkali metal hydride, an alkaline earth metal, and an alkaline earth metal hydride.
Claim 6
Dependent Claim 15 words
The process of claim 4 wherein said R 1 is alkyl of 2-10 carbon atoms.
Claim 7
Dependent Claim 10 words
A surfactant composition prepared by the process of claim 5.
Claim 8
Dependent Claim 20 words
The process of claim 5 wherein the reaction of step (b) is carried out in the substantial absence of moisture.
Claim 9
Dependent Claim 30 words
A process as claimed in claim 7 which includes the added step of removing alcohol of said formula R 1 OH which is liberated during the reaction of step (b).
Claim 10
Dependent Claim 10 words
A surfactant composition prepared by the process of claim 8.
Claim 11
Dependent Claim 12 words
The process of claim 8 wherein said silicon tetrahalide is silicate tetrachloride.
Claim 12
Dependent Claim 60 words
The process of claim 10 wherein said polyether alcohol has a molecular weight of about 1,500-4,000 and in which said R 2 is alkyl of 1-6 carbon atoms and said --C n H 2n O-- moiety represents a polyoxethylene chain or a polyoxyethylene-oxypropylene chain having a weight ratio of oxyethylene to oxypropylene units ranging from about 2:1 to about 1:2.
Claim 13
Dependent Claim 10 words
A surfactant composition prepared by the process of claim 11.
Claim 14
Dependent Claim 41 words
The process of claim 11 wherein the reaction of step (a) is carried out at about 55°-110°C, under reflux and using, per every mole of said silicon tetrachloride, about 2-12 moles of said alcohol and about 0.4-1.7 moles of said water.
Claim 15
Dependent Claim 40 words
The process of claim 13 wherein the reaction of step (b) is carried out at about 80°-260°C and using about 0.06 -0.8 moles of said polyether alcohol per each mole of said silicon tetrachloride which is used in step (a).
Claim 16
Dependent Claim 10 words
A surfactant composition prepared by the process of claim 14.
Claim 17
Dependent Claim 245 words
A process for preparing a silicate-based surfactant composition which comprises the following steps: a. at a temperature from about -30°C to about 20°C, mixing together silicon tetrachloride and, per every mole of said silicon tetrachloride, about 0.7-1.4 moles of water and about 3-8 moles of isopropyl alcohol, b. allowing said mixture to react at a temperature of about 60°-100°C and under reflux conditions, thereby forming a reaction product made up of hydrochloric acid, unreacted isopropyl alcohol and a non-volatile mixture comprised of silicate-based materials, c. stripping off said hydrochloric acid and unreacted isopropyl alcohol, d. reacting said non-volatile mixture with a polyether alcohol having a molecular weight of about 1,200-1,500 and represented by the formula C 4 H 9 --C n H 2n O-- H wherein the moiety --C n H 2n O-- represents a polyoxyethylene-oxypropylene chain having a weight ratio, of oxyethylene to oxypropylene units, ranging from about 6:4 to about 4:6, the reaction being carried out; 1. using about 0.1-0.7 mole of said polyether alcohol per each mole of said silicon tetrachloride used in step (a), 2. at a temperature of about 140°-220°C, 3. in the substantial absence of moisture, and 4. in the presence of a transesterification catalyst selected from the group consisting of a Lewis acid, an alkali metal and an alkali metal hydride, thereby forming a product comprised of a silicate-based surfactant composition and liberated isopropyl alcohol, and e. removing said liberated isopropyl alcohol and recovering said silicate-based surfactant composition.
Claim 18
Dependent Claim 245 words
A process for preparing a silicate-based surfactant composition which comprises the following steps: a. at a temperature from about -30°C to about 20°C, mixing together silicon tetrachloride and, per every mole of said silicon tetrachloride, about 0.7-1.4 moles of water and about 3-8 moles of isopropyl alcohol, b. allowing said mixture to react at a temperature of about 60°-100°C and under reflux conditions, thereby forming a reaction product made up of hydrochloric acid, unreacted isopropyl alcohol and a non-volatile mixture comprised of silicate-based materials, c. stripping off said hydrochloric acid and unreacted isopropyl alcohol, d. reacting said non-volatile mixture with a polyether alcohol having a molecular weight of about 1,200-1,500 and represented by the formula C 4 H 9 --C n H 2n O-- H wherein the moiety --C n H 2n O-- represents a polyoxyethylene-oxypropylene chain having a weight ratio, of oxyethylene to oxypropylene units, ranging from about 6:4 to about 4:6, the reaction being carried out; 1. using about 0.1-0.7 mole of said polyether alcohol per each mole of said silicon tetrachloride used in step (a), 2. at a temperature of about 140°-220°C, 3. in the substantial absence of moisture, and 4. in the presence of a transesterification catalyst selected from the group consisting of a Lewis acid, an alkali metal and an alkali metal hydride, thereby forming a product comprised of a silicate-based surfactant composition and liberated isopropyl alcohol, and e. removing said liberated isopropyl alcohol and recovering said silicate-based surfactant composition.
Claim 19
Dependent Claim 10 words
A surfactant composition prepared by the process of claim 16.

References Cited (Backward Citations)

US2756212A Cited
US2839558A Cited
US2776307A Cited
US2990377A Cited
US2993871A Cited
US3032439A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-08-24 1980-02-23 1980-08-24 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-08-24 1984-02-23 1984-08-24 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-08-24 1988-02-23 1988-08-24 $7700.00 Window Closed / Lapsed

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