# US 5,708,121 A · Storage stable melamine-modified phenolic resole resins using an alkaline condensation and polyhydroxyl compound stabilization > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,708,121 A - Document ID: US5708121A - Status: Granted - Kind: A - Application number: 08/813,579 - Filed: 1997-03-07 - Granted: 1998-01-13 - Earliest claimed: 1995-02-22 - Assignees: Georgia-Pacific Resins, Inc. - Inventors: Claude Phillip Parks; Kurt Forrest Anderson - Web page: https://patentgrep.com/patent/US5708121A ## CPC - C08G 14/10: Melamines - C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS ## Abstract This invention relates to an emulsifiable melamine-modified phenolic resole resin composition useful as a binder for glass fibers. The invention is more particularly directed to the process of preparing the resole resin composition using an alkaline condensation in the presence of a polyhydroxyl compound. ## Claims ### Claim 1 A method of preparing a storage stable emulsifiable melamine-modified phenolic resole resin comprising: (a) preparing an alkaline resole resin by reacting formaldehyde and a phenol at a formaldehyde to phenol mole ratio between about 1:1 to 6:1 at a pH between about 8 and 10 in the presence of an effective catalytic amount of a monovalent basic catalyst; followed by (b) adding a polyhydroxy compound and reacting formaldehyde remaining unreacted after the formaldehyde and phenol reaction, with melamine at a pH between about 8 and 10, at an unreacted formaldehyde to melamine mole ratio between about 3:1 to 1:1, wherein the polyhydroxy compound is added in an amount sufficient to prevent premature crystallization of methylolated melamine species; (c) neutralizing the melamine modified, phenolic resole resin to a pH between about 6.5 and 8.5; and (d) adding a protective colloid to the neutralized melamine modified phenolic resole resin. ### Claim 2 (depends on 1) The method of claim 1 wherein the catalyst is selected from the group consisting of NaOH, LiOH, KOH, and mixtures thereof. ### Claim 3 (depends on 2) The method of claim 2 wherein the catalyst is NaOH. ### Claim 4 (depends on 1) The method of claim 1 wherein the polyhydroxy compound is selected from the group consisting of sucrose, sorbitol and triethanolamine. ### Claim 5 (depends on 4) The method of claim 4 wherein the polyhydroxy compound is sorbitol. ### Claim 6 (depends on 1) The method of claim 1 wherein the melamine modified phenolic resole resin is neutralized with sulfamic acid. ### Claim 7 (depends on 1) The method of claim 1 wherein the protective colloid is selected from the group consisting of casein, guar gum, gum arabic, lecithin, soya protein, and mixtures thereof. ### Claim 8 (depends on 7) The method of claim 7 wherein the protective colloid is casein. ### Claim 9 (depends on 1) The method of claim 1 wherein the formaldehyde to phenol ratio is between about 2:1 to 6:1. ### Claim 10 (depends on 1) The method of claim 1 wherein the basic catalyst to phenol mole ratio is between about 0.6:1 to 0.8:1. ### Claim 11 (depends on 1) The method of claim 1 wherein the unreacted formaldehyde to melamine ratio is between about 3.0:1 to 1.5:1. ### Claim 12 (depends on 1) The method of claim 1 wherein the reaction temperature during step (a) is about 55.degree. to 95.degree. C. ### Claim 13 (depends on 1) The method of claim 1, wherein the pH during step (a) is between about 8.5 and 9.5 and the pH during step (b) is between about 8.5 and 9.5. ### Claim 14 (depends on 1) The method of claim 1, wherein the melamine modified phenolic resole resin is neutralized to a pH between about 7 and 8. ### Claim 15 (depends on 1) The method of claim 1 wherein the phenol is phenol (C.sub.6 H.sub.5 OH) or a substituted phenol. ### Claim 16 A storage stable emulsifiable melamine-modified phenolic resole resin comprising: a melamine-modified alkaline resole resin prepared by first reacting formaldehyde and a phenol at a formaldehyde to phenol mole ratio between about 1:1 to 6:1 at a pH of between about 8 and 10 in the presence of an effective catalytic amount of a monovalent basic catalyst; then adding a polyhydroxy compound and reacting formaldehyde remaining unreacted after the formaldehyde and phenol reaction with melamine at a pH between about 8 and 10, at an unreacted formaldehyde to melamine mole ratio between about 3:1 to 1:1, wherein the polyhydroxy compound is added in an amount sufficient to prevent premature crystallization of methylolated melamine species; adding a neutralizing agent to the melamine-modified phenolic resole resin to a pH between about 6.5 and 8.5; and adding a protective colloid to the neutralized melamine modified phenolic resole resin. ### Claim 17 (depends on 16) The resole resin of claim 16 wherein the catalyst is selected from the group consisting of NaOH, LiOH, KOH, and mixtures thereof. ### Claim 18 (depends on 17) The resole resin of claim 17 wherein the catalyst is NaOH. ### Claim 19 (depends on 16) The resole resin of claim 16 wherein the polyhydroxy compound is selected from the group consisting of sucrose, sorbitol, and triethanolamine. ### Claim 20 (depends on 19) The resole resin of claim 19 wherein the polyhydroxy compound is sorbitol. ### Claim 21 (depends on 16) The resole resin of claim 16 wherein the neutralizing agent is sulfamic acid. ### Claim 22 (depends on 16) The resole resin of claim 16 wherein the protective colloid is selected from the group consisting of casein, guar gum, gum arabic, lecithin, soya protein, and mixtures thereof. ### Claim 23 (depends on 22) The resole resin of claim 22 wherein the protective colloid is casein. ### Claim 24 (depends on 16) The resole resin of claim 16 wherein the formaldehyde to phenol ratio is between about 2:1 to 6:1. ### Claim 25 (depends on 16) The resole resin claim 16 wherein the basic catalyst to phenol mole ratio is between about 0.6:1 to 0.8:1. ### Claim 26 (depends on 16) The resole resin of claim 16 wherein the unreacted formaldehyde to melamine ratio is between about 3.0:1 to 1.5:1. ### Claim 27 (depends on 16) The resole resin of claim 16 wherein the phenol is phenol (C.sub.6 H.sub.5 OH) or a substituted phenol.