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US4115328A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for making stable solvent-free, aqueous epoxy resin dispersions

Assignee: BASF Corp
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Filing: 1977-01-07
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Granted: 1978-09-19
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Expires: 1997-01-07
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Abstract

Abstract Essentially, solvent-free, stable aqueous dispersions or low solvent emulsions of epoxy resins are made through use of selected nonionic surfactants and selected organic solvents followed by vacuum distillation of most or almost all of the organic medium. The stable aqueous emulsions are useful for making coatings, films and the like.

Inventors

  • 👤 Edward G. Bozzi
  • 👤 Robert C. Nelson

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 07:08
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/02; C08J3/03; C08J3/07; C09; C09D; C09D163/00; C08J2363/00; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31511; Y10T428/31529

Claims Analysis

Total Claims: 31
Claim 1
Independent Claim 345 words
An improved process for preparing a stable aqueous dispersion having no particles large in size than 5 microns or an aqueous, low organic solvent fine particle emulsion of an epoxy resin having a molecular weight from about 4,000 to about 100,000 useful in forming water-dilutable, heat-curable coating compositions with aminoplast or phenoplast curing systems, which comprises dissolving said epoxy resin in an organic solvent to prepare a 40 to 80% by weight solution, said organic solvent containing from 1 to 25% by weight based on the epoxy resin of a nonionic surfactant and said organic solvent having a boiling point below 160° C. and being selected from the group consisting of aromatic hydrocarbons, esters, ethers, alcohols, ketones, halogenated aromatic hydrocarbons and mixtures thereof, adding with stirring sufficient water to give a mixture containing from 30 to 50% by weight water, subjecting the resulting mixture to homogenizing action using a colloid mill, homogenizer or other high speed, high shear mixer, removing essentially all the organic solvent present by vacuum distillation at a temperature under 40° C. and with a pressure of about 5 to 100 mm Hg to give an essentially solvent free aqueous dispersion having from about 40 to 65 weight percent epoxy resin, from about 0.5 to 13 weight percent nonionic surfactant and from about 35 to 60 weight percent water; or removing from 40 to 70 percent of the organic solvent by vacuum distillation under 40° C. and with a pressure of about 5 to 100 mm Hg to give a low organic solvent aqueous emulsion having about 35 to 65 weight percent epoxy resin, from about 0.5 to 13 weight percent nonionic surfactant, from about 8 to 20 weight percent organic solvent and from about 35 to 60 weight percent water, wherein the improvement comprises using as the nonionic surfactant a dispersing agent selected from the group consisting of the polyoxyethylene esters of fatty, rosin and tall oil acids having 8 to 20 carbon atoms in the acid moiety and having from 5 to 50 moles of poly(ethylene oxide) per acid molecule.
Claim 2
Dependent Claim 345 words
An improved process for preparing a stable aqueous dispersion having no particles large in size than 5 microns or an aqueous, low organic solvent fine particle emulsion of an epoxy resin having a molecular weight from about 4,000 to about 100,000 useful in forming water-dilutable, heat-curable coating compositions with aminoplast or phenoplast curing systems, which comprises dissolving said epoxy resin in an organic solvent to prepare a 40 to 80% by weight solution, said organic solvent containing from 1 to 25% by weight based on the epoxy resin of a nonionic surfactant and said organic solvent having a boiling point below 160° C. and being selected from the group consisting of aromatic hydrocarbons, esters, ethers, alcohols, ketones, halogenated aromatic hydrocarbons and mixtures thereof, adding with stirring sufficient water to give a mixture containing from 30 to 50% by weight water, subjecting the resulting mixture to homogenizing action using a colloid mill, homogenizer or other high speed, high shear mixer, removing essentially all the organic solvent present by vacuum distillation at a temperature under 40° C. and with a pressure of about 5 to 100 mm Hg to give an essentially solvent free aqueous dispersion having from about 40 to 65 weight percent epoxy resin, from about 0.5 to 13 weight percent nonionic surfactant and from about 35 to 60 weight percent water; or removing from 40 to 70 percent of the organic solvent by vacuum distillation under 40° C. and with a pressure of about 5 to 100 mm Hg to give a low organic solvent aqueous emulsion having about 35 to 65 weight percent epoxy resin, from about 0.5 to 13 weight percent nonionic surfactant, from about 8 to 20 weight percent organic solvent and from about 35 to 60 weight percent water, wherein the improvement comprises using as the nonionic surfactant a dispersing agent selected from the group consisting of the polyoxyethylene esters of fatty, rosin and tall oil acids having 8 to 20 carbon atoms in the acid moiety and having from 5 to 50 moles of poly(ethylene oxide) per acid molecule.
Claim 3
Dependent Claim 18 words
A process according to claim 1 wherein the epoxy resin is an aromatic polyglycidyl ether derived from 2,2-bis(4-hydroxyphenyl)propane.
Claim 4
Dependent Claim 19 words
A process according to claim 2 wherein the epoxy resin has an average molecular weight between 4,000 and 8,000.
Claim 5
Dependent Claim 28 words
A process according to claim 1 wherein the organic solvent is selected from the group consisting of methyl ethyl ketone, methyl amyl ketone, ethyl acetate and mixtures thereof.
Claim 6
Dependent Claim 14 words
A process according to claim 4 wherein the organic solvent is methyl ethyl ketone.
Claim 7
Dependent Claim 21 words
A process according to claim 1 wherein the nonionic surfactant has 35 to 50 moles of poly(ethylene oxide) per acid molecule.
Claim 8
Dependent Claim 33 words
A process according to claim 6 wherein the nonionic surfactant is an ester of a fatty acid of 12 to 18 carbon atoms with about 50 moles of poly(ethylene oxide) per acid molecule.
Claim 9
Dependent Claim 24 words
A process according to claim 1 wherein from 4 to 8% by weight, based on the epoxy resin, of the nonionic surfactant is used.
Claim 10
Dependent Claim 138 words
A stable aqueous dispersion of an epoxy resin which comprises (a) from about 40 to about 65 weight percent epoxy resin having an average molecular weight from about 4,000 to about 100,000, (b) from 0.5 to 13 weight percent nonionic surfactant selected from the group consisting of the polyoxyethylene esters of a fatty, rosin or tall oil acid having 8 to 20 carbon atoms in the acid moiety and having from 5 to 50 moles of poly(ethylene oxide) per acid molecule, (c) from 2 to 5% by weight of an organic solvent having a boiling point below 160° C. and being selected from the group consisting of aromatic hydrocarbons, esters, ethers, alcohols, ketones, halogenated aromatic hydrocarbons and mixtures thereof, and (d) from about 35 to 60% by weight water with no particles larger in size than 5 microns.
Claim 11
Dependent Claim 138 words
A stable aqueous dispersion of an epoxy resin which comprises (a) from about 40 to about 65 weight percent epoxy resin having an average molecular weight from about 4,000 to about 100,000, (b) from 0.5 to 13 weight percent nonionic surfactant selected from the group consisting of the polyoxyethylene esters of a fatty, rosin or tall oil acid having 8 to 20 carbon atoms in the acid moiety and having from 5 to 50 moles of poly(ethylene oxide) per acid molecule, (c) from 2 to 5% by weight of an organic solvent having a boiling point below 160° C. and being selected from the group consisting of aromatic hydrocarbons, esters, ethers, alcohols, ketones, halogenated aromatic hydrocarbons and mixtures thereof, and (d) from about 35 to 60% by weight water with no particles larger in size than 5 microns.
Claim 12
Dependent Claim 21 words
A dispersion according to claim 9 wherein the epoxy resin has an average molecular weight from about 4,000 to about 8,000.
Claim 13
Dependent Claim 46 words
A dispersion according to claim 10 wherein the nonionic surfactant is selected from the group consisting of the polyoxyethylene esters of a fatty acid having 12 to 18 carbon atoms in the acid moiety and having 35 to 50 moles of poly(ethylene oxide) per acid molecule.
Claim 14
Dependent Claim 28 words
A dispersion according to claim 10 wherein the organic solvent is selected from the group consisting of methyl ethyl ketone, methyl amyl ketone, ethyl acetate and mixtures thereof.
Claim 15
Dependent Claim 14 words
A dispersion according to claim 10 wherein the organic solvent is methyl ethyl ketone.
Claim 16
Dependent Claim 140 words
A low organic solvent, stable aqueous emulsion of an epoxy resin which comprises (a) from about 35 to about 65 weight percent epoxy resin having an average molecular weight from about 4,000 to about 100,000, (b) from 0.5 to 13 weight percent nonionic surfactant selected from the group consisting of the polyoxyethylene esters of a fatty, rosin or tall oil acid having 8 to 20 carbon atoms in the acid moiety and having from 5 to 50 moles of poly(ethylene oxide) per acid molecule, (c) from 8 to 20% by weight of an organic solvent having a boiling point below 160° C. and being selected from the group consisting of aromatic hydrocarbons, esters, ethers, alcohols, ketones, halogenated aromatic hydrocarbons and mixtures thereof and (d) from about 35 to 60% weight water with no particles larger in size than 5 microns.
Claim 17
Dependent Claim 140 words
A low organic solvent, stable aqueous emulsion of an epoxy resin which comprises (a) from about 35 to about 65 weight percent epoxy resin having an average molecular weight from about 4,000 to about 100,000, (b) from 0.5 to 13 weight percent nonionic surfactant selected from the group consisting of the polyoxyethylene esters of a fatty, rosin or tall oil acid having 8 to 20 carbon atoms in the acid moiety and having from 5 to 50 moles of poly(ethylene oxide) per acid molecule, (c) from 8 to 20% by weight of an organic solvent having a boiling point below 160° C. and being selected from the group consisting of aromatic hydrocarbons, esters, ethers, alcohols, ketones, halogenated aromatic hydrocarbons and mixtures thereof and (d) from about 35 to 60% weight water with no particles larger in size than 5 microns.
Claim 18
Dependent Claim 21 words
An emulsion according to claim 14 wherein the epoxy resin has an average molecular weight from about 4,000 to about 8,000.
Claim 19
Dependent Claim 46 words
An emulsion according to claim 14 wherein the nonionic surfactant is selected from the group consisting of the polyoxyethylene esters of a fatty acid having 12 to 18 carbon atoms in the acid moiety and having 35 to 50 moles of poly(ethylene oxide) per acid molecule.
Claim 20
Dependent Claim 28 words
An emulsion according to claim 14 wherein the organic solvent is selected from the group consisting of methyl ethyl ketone, methyl amyl ketone, ethyl acetate and mixtures thereof.
Claim 21
Dependent Claim 14 words
An emulsion according to claim 14 wherein the organic solvent is methyl ethyl ketone.
Claim 22
Dependent Claim 157 words
A process for preparing a water-dilutable, heat-curable coating composition, comprising an epoxy resin, a nonionic surfactant, organic solvent, water and an aminoplast or phenoplast curing agent, which comprises adding to the aqueous dispersion or aqueous, low organic solvent fine particle emulsion prepared according to the process of claim 1, 5 to 50% by weight of solids of an aminoplast or phenoplast curing agent and sufficient water to bring the total percent solids in the range of 10 to 80% by weight, or adding to the epoxy resin dissolved in the organic solvent containing the nonionic surfactant from 5 to 50% by weight of solids of an aminoplast or phenoplast curing agent, the adding water with stirring, subjecting the resulting mixture to homogenizing action, removing the organic solvent by vacuum distillation according to the procedure of claim 1, and finally adding sufficient water to bring the total percent solids in the range of 10 to 80% by weight.
Claim 23
Dependent Claim 21 words
The process according to claim 19 wherein the total percent solids are in the range of 30 to 70% by weight.
Claim 24
Dependent Claim 21 words
The process according to claim 19 wherein the total percent solids are in the range of 40 to 60% by weight.
Claim 25
Dependent Claim 26 words
The process according to claim 19 wherein the aminoplast or phenoplast curing agent is present in the amount of 5 to 40% by weight of solids.
Claim 26
Dependent Claim 26 words
The process according to claim 19 wherein the aminoplast or phenoplast curing agent is present in the amount of 5 to 30% by weight of solids.
Claim 27
Dependent Claim 16 words
The process according to claim 19 wherein the aminoplast curing agent is a methylated urea-formaldehyde resin.
Claim 28
Dependent Claim 17 words
The process according to claim 19 wherein the aminoplast curing agent is a methoxy methyl melamineformaldehyde resin.
Claim 29
Dependent Claim 13 words
The process according to claim 19 wherein the aminoplast curing agent is hexamethyoxymethylmelamine.
Claim 30
Dependent Claim 24 words
The process according to claim 19 wherein the phenoplast curing agent is a phenolic hardener which is an etherified resol resin based on bisphenol-A.
Claim 31
Dependent Claim 18 words
A water-dilutable, heat-curing coating composition consisting essentially of the product obtained according to the process of claim 19.

References Cited (Backward Citations)

US3282863A Cited
FR1575303A Cited
US3879324A Cited
US3772228A Cited
US3888812A Cited
US3905929A Cited
US3935146A Cited
DE2424887A1 Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-09-18 1982-03-20 1982-09-19 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-09-18 1986-03-20 1986-09-19 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-09-18 1990-03-20 1990-09-19 $7700.00 Window Closed / Lapsed

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