US5049338A
Expired / Lapsed
US
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Method of promoting sol gel siliceous-containing reactions
Assignee: PPG Industries Inc
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Filing: 1989-06-22
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Granted: 1991-09-17
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Expires: 2009-06-22
Abstract
Abstract A sol gel reaction process for forming glassy articles involves the hydrolysis of silicon alkoxides with or without additional dispersions of hydrated silicon oxides, and polymerization including crosslinking. The present process involves forming glassy articles by the sol gel reaction route utilizes coagulation promoters having fatty acid hydrophobic moieties and hydrophilic moieties of primary, secondary, tertiary amines or quaternary ammonium compounds. The coagulation promoter catalyzes either and/or both of the hydrolysis and polymerization reactions. The coagulation promoter can be the only catalyst in forming the sol or can be used in addition to acid or basic catalyst. Additionally or alternatively, the coagulation promoter is added to a coagulation fluid to which shaped hydrolyzate is added. Afterwards the gelled shape precursor is optionally consolidated to form a precursor glass shape and optionally is consolidated to form the glassy shapes of films, coatings, beads, fibers, tubes and monolithic structures.
Inventors
- 👤 Desaraju V. Varaprasad
- 👤 Agaram S. Abhiraman
- 👤 Ernest L. Lawton
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 08:32
CPC Classifications
C; C03; C03C; C03C1/00; C03C1/006; C03C1/008; C03B; C03B19/00; C03B19/12; C03B37/00; C03B37/01; C03B37/011; C08; C08G; C08G77/00; C08G77/02; C09; C09D; C09D183/00; C09D183/02; D; D01; D01F; D01F6/00; D01F6/96
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
178 words
Process of producing at least one siliceous-containing amorphous shape from a sol-gel process, comprising: forming at least one shape from metallic type compounds selected from the group consisting of: silicon alkoxide, dispersion of hydrated siliceous oxides, and mixtures thereof by at least partial hydrolysis in the presence of an organic solvent and water to result in a shapable ungelled polymerizate, where in forming an effective catalytic amount of at least one coagulation promoter is present to catalyze the hydrolysis and polymerization in the coagulation process, and wherein the coagulation promoter is selected from the group consisting of: aliphatic mono-, di-, and polyamines and rosin-derived amines; and reaction products of fatty acids and hydrophilic moieties selected from the group consisting of amino nitrogen moieties, quaternary nitrogen moieties; and amine oxides, polyoxyethylene alkyl-alicyclic-amines, 1-(2-hydroxyethyl)-2 alkyl-2-imidazolines, N,N,N',N'-tetrakis-substituted ethylenediamine derivatives; amines with amide linkages prepared by the condensation of carboxylic acids with a di-, or polyamine; partially amidated polyalkylenimines and acidic solutions thereof; and long chain alkyl amines, long chain alkyl amides, amidated alkyl amines, polyamino alkyl amides, partially amidated polyalkylene amides.
Claim 2
Dependent Claim
178 words
Process of producing at least one siliceous-containing amorphous shape from a sol-gel process, comprising: forming at least one shape from metallic type compounds selected from the group consisting of: silicon alkoxide, dispersion of hydrated siliceous oxides, and mixtures thereof by at least partial hydrolysis in the presence of an organic solvent and water to result in a shapable ungelled polymerizate, where in forming an effective catalytic amount of at least one coagulation promoter is present to catalyze the hydrolysis and polymerization in the coagulation process, and wherein the coagulation promoter is selected from the group consisting of: aliphatic mono-, di-, and polyamines and rosin-derived amines; and reaction products of fatty acids and hydrophilic moieties selected from the group consisting of amino nitrogen moieties, quaternary nitrogen moieties; and amine oxides, polyoxyethylene alkyl-alicyclic-amines, 1-(2-hydroxyethyl)-2 alkyl-2-imidazolines, N,N,N',N'-tetrakis-substituted ethylenediamine derivatives; amines with amide linkages prepared by the condensation of carboxylic acids with a di-, or polyamine; partially amidated polyalkylenimines and acidic solutions thereof; and long chain alkyl amines, long chain alkyl amides, amidated alkyl amines, polyamino alkyl amides, partially amidated polyalkylene amides.
Claim 3
Dependent Claim
21 words
Process of claim 1, wherein the shapes are selected from the group consisting of films, coatings, fibers, tubes and monolithic structures.
Claim 4
Dependent Claim
24 words
Process of claim 1, wherein the coagulation promoter is used with a base to increase the pH of the hydrolyzate up to around 10.
Claim 5
Dependent Claim
26 words
Process of claim 1, wherein the coagulation promoter is present in an amount up to 3 mole percent of the total alkoxides present in the hydrolyzate.
Claim 6
Dependent Claim
38 words
Process of claim 1, which includes furthering coagulation of the shape by placing the shapes in a coagulation solution wherein the coagulation promoter is present in an amount of 0.05 to 1 weight percent of a coagulation solution.
Claim 7
Dependent Claim
22 words
Process of claim 1, wherein the organic solvent is an alkyl alcohol where the alkyl group has one to five carbon atoms.
Claim 8
Dependent Claim
149 words
Process of producing at least one siliceous-containing amorphous shape from a sol-gel process, comprising: a. forming at least a partial hydrolyzate of compounds selected from the group consisting of silicon alkoxide, colloidal dispersions of hydrous siliceous oxides and mixtures thereof by acid catalyzed hydrolysis in the presence of an organic solvent at a temperature in the range of around ambient to elevated temperatures less than 100° C. and with a molar ratio of water to silicon alkoxide in the range of around 1 to 1 up to 4 to 1 so that ungelled polymerization results in a shape-formable viscosity in the range of around 50 to greater than 1000 poise, b. forming the shape from the hydrolyzate, c. contacting at least one shape with a nonsolvent liquid having a coagulation promoter for effective coagulation to produce at least a sticky shape, d. removing the shape from the nonsolvent liquid.
Claim 9
Dependent Claim
149 words
Process of producing at least one siliceous-containing amorphous shape from a sol-gel process, comprising: a. forming at least a partial hydrolyzate of compounds selected from the group consisting of silicon alkoxide, colloidal dispersions of hydrous siliceous oxides and mixtures thereof by acid catalyzed hydrolysis in the presence of an organic solvent at a temperature in the range of around ambient to elevated temperatures less than 100° C. and with a molar ratio of water to silicon alkoxide in the range of around 1 to 1 up to 4 to 1 so that ungelled polymerization results in a shape-formable viscosity in the range of around 50 to greater than 1000 poise, b. forming the shape from the hydrolyzate, c. contacting at least one shape with a nonsolvent liquid having a coagulation promoter for effective coagulation to produce at least a sticky shape, d. removing the shape from the nonsolvent liquid.
Claim 10
Dependent Claim
124 words
Process of producing at least one siliceous-containing amorphous shape from a sol-gel process, comprising: a. forming at least a partial hydrolyzate of compounds selected from the group consisting of silicon alkoxide, colloidal dispersions of hydrous siliceous oxides and mixtures thereof by acid catalyzed hydrolysis in the presence of an organic solvent at a temperature in the range of around ambient to elevated temperatures less than 100° C. and with a ratio of water to silicon alkoxide in the range of around 1 to 1 up to 4 to 1 so that ungelled polymerization results in a shape-formable viscosity in the range of around 50 to greater than 1000 poise, and b. forming the shape from the hydrolyzate in the presence of a coagulation promoter.
Claim 11
Dependent Claim
124 words
Process of producing at least one siliceous-containing amorphous shape from a sol-gel process, comprising: a. forming at least a partial hydrolyzate of compounds selected from the group consisting of silicon alkoxide, colloidal dispersions of hydrous siliceous oxides and mixtures thereof by acid catalyzed hydrolysis in the presence of an organic solvent at a temperature in the range of around ambient to elevated temperatures less than 100° C. and with a ratio of water to silicon alkoxide in the range of around 1 to 1 up to 4 to 1 so that ungelled polymerization results in a shape-formable viscosity in the range of around 50 to greater than 1000 poise, and b. forming the shape from the hydrolyzate in the presence of a coagulation promoter.
Claim 12
Dependent Claim
21 words
Process of claim 8, wherein the organic solvent is alkyl alcohol where the alkyl group has one to five carbon atoms.
Claim 13
Dependent Claim
16 words
Process of claim 8, wherein the organic solvent is ethyl alcohol in an effective solvent amount.
Claim 14
Dependent Claim
15 words
Process of claim 8, wherein the acid is hydrochloric acid in an effective catalytic amount.
Claim 15
Dependent Claim
80 words
Process of claim 8, wherein the shape is a fiber formed by dry jet spinning where the ratio of water to silicon alkoxide is in the range of 1.5 to 1 to around and including 4 to 1 so that ungelled polymerization results in a spinnable viscosity in the range of around 60 to greater than 1000 poise as measured at room temperature and the amount of the coagulation promoter is in the range of 0.2 to 1 weight percent.
Claim 16
Dependent Claim
100 words
Process of claim 8, wherein the coagulation promoter is selected from the group consisting of aliphatic mono-, di-, and polyamines and rosin-derived amines; and reaction products of fatty acids and hydrophilic moieties selected from the group consisting of amino nitrogen moieties, quaternary nitrogen moieties; and amine oxides, polyoxyethylene alkyl-alicyclic-amines, 1-(2-hydroxyethyl)-2 alkyl-2-imidazolines, N,N,N',N'-tetrakis-substituted ethylenediamine derivatives; amines with amide linkages prepared by the condensation of carboxylic acids with a di-, or polyamine; partially amidated polyalkylenimines and acidic solutions thereof; long chain alkyl amines, long chain alkyl amides, amidated alkyl amines, polyamino alkyl amides, partially amidated polyalkylene amides and partially amidated polyalkylene imines.
Claim 17
Dependent Claim
96 words
Process of claim 7, wherein the coagulation promoter is selected from the group consisting of aliphatic mono-, di-, and polyamines and rosin-derived amines; and reaction products of fatty acids and hydrophilic moieties selected from the group consisting of amino nitrogen moieties, quaternary nitrogen moieties; and amine oxides, polyoxyethylene alkyl-alicyclic-amines, 1-(2-hydroxyethyl)-2 alkyl-2-imidazolines, N,N,N',N'-tetrakis-substituted ethylenediamine derivatives; amines with amide linkages prepared by the condensation of carboxylic acids with a di-, or polyamine; partially amidated polyalkylenimines and acidic solutions thereof; and long chain alkyl amines, long chain alkyl amides, amidated alkyl amines, polyamino alkyl amides, partially amidated polyalkylene amides.
References Cited (Backward Citations)
US4396587A
Cited
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