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US4904516A Expired / Lapsed US ⏱️ 0.0 years remaining

Phenol-formaldehyde resin solution containing water soluble alkaline earth metal salt

Assignee: Certainteed LLC
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Filing: 1988-01-12
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Granted: 1990-02-27
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Expires: 2008-01-12
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Abstract

Abstract A process for preparing a water soluble phenol-formaldehyde resole resin having improved storage stability employs a calcium compound to catalyze the condensation reaction which occurs under basic conditions. Sulfamic acid is used to neutralize the resole solution, yielding a soluble calcium salt which will not settle out of the solution or clog transfer lines or spray nozzles as may a calcium salt precipitated during the neutralization. Glass fiber insulation produced using a binder prepared with the aqueous resole solution shows enhanced thickness recovery and lower odor potential.

Inventors

  • 👤 Albert W. Creamer

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 03:56
CPC Classifications
C; C08; C08G; C08G8/00; C08G8/28; C04; C04B; C04B26/00; C04B26/02; C04B26/10; C04B26/12; C04B26/122; C04B41/00; C04B41/45; C04B41/46; C04B41/48; C04B41/4823; C08G8/04; C08G8/08; C08G8/10; C08K; C08K5/00; C08K5/36; C08K5/43

Claims Analysis

Total Claims: 20
Claim 1
Independent Claim 157 words
A process for preparing a urea-free aqueous solution of a water soluble resole resin having improved storage stability for subsequent use in preparing a binder for mineral fibers, the process comprising: (a) preparing an aqueous mixture of at least one aldehyde and at least one phenol, the molar ratio of aldehyde to phenol being from about 1.5: 1 to 5.0 : 1; (b) adding an alkaline earth metal compound to the aqueous mixture in an amount effective to catalyze the reaction between the aldehyde and the phenol; (c) reacting the aldehyde and the phenol under basic conditions in the absence of urea and in the presence of the alkaline earth metal compound to form a urea-free aqueous solution of a resole resin; and (d) adding sulfamic acid to the urea-free aqueous solution prepared in step (c) to provide a resin solution having improved stability in an amount sufficient to provide a pH from about 1 to 8.
Claim 2
Dependent Claim 157 words
A process for preparing a urea-free aqueous solution of a water soluble resole resin having improved storage stability for subsequent use in preparing a binder for mineral fibers, the process comprising: (a) preparing an aqueous mixture of at least one aldehyde and at least one phenol, the molar ratio of aldehyde to phenol being from about 1.5: 1 to 5.0 : 1; (b) adding an alkaline earth metal compound to the aqueous mixture in an amount effective to catalyze the reaction between the aldehyde and the phenol; (c) reacting the aldehyde and the phenol under basic conditions in the absence of urea and in the presence of the alkaline earth metal compound to form a urea-free aqueous solution of a resole resin; and (d) adding sulfamic acid to the urea-free aqueous solution prepared in step (c) to provide a resin solution having improved stability in an amount sufficient to provide a pH from about 1 to 8.
Claim 3
Dependent Claim 20 words
A process according to claim 1 wherein at least one phenol is phenol and at least one aldehyde is formaldehyde.
Claim 4
Dependent Claim 17 words
A process according to claim 2 wherein the alkaline earth metal is selected from calcium and barium.
Claim 5
Dependent Claim 13 words
A process according to claim 3 wherein the alkaline earth metal is calcium.
Claim 6
Dependent Claim 18 words
A process according to claim 4 wherein the calcium compound is selected from calcium oxide and calcium hydroxide.
Claim 7
Dependent Claim 24 words
A process according to claim 4 wherein the molar ratio of formaldehyde to phenol is from about 3.2 : 1 to 3.8 : 1.
Claim 8
Dependent Claim 31 words
A process according to claim 4 wherein the calcium compound is added in an amount from about 1% to 10% by weight, calculated as calcium oxide on the weight of phenol.
Claim 9
Dependent Claim 31 words
A process according to claim 7 wherein the calcium compound is added in an amount from about 3% to 6% by weight, calculated as calcium oxide on the weight of phenol.
Claim 10
Dependent Claim 32 words
A process according to claim 4 wherein the sulfamic acid is added in an amount sufficient to adjust the acidity of the solution to a pH of from about 6.0 to 7.0
Claim 11
Dependent Claim 31 words
A process according to claim 1 wherein the sulfamic acid is added to the resin solution to provide an acidic solution, the solution being subsequently neutralized by addition of a base.
Claim 12
Dependent Claim 29 words
A process according to claim 10 wherein the base is selected from monoethanolamine, diethanolamine and triethanolamine, the resin solution being neutralized to a pH of about 7 or greater.
Claim 13
Dependent Claim 80 words
A process according to claim 5 wherein the temperature of the aqueous mixture of formaldehyde and phenol is maintained at a first temperature of from about 40° C. to 50° C. as the catalyst is added, the temperature then being adjusted to rise to a second temperature of from about 60° C. to 80° C. within about 30 minutes and maintained until the free formaldehyde content declines to a level of about 10% by weight of the reaction mixture solids.
Claim 14
Dependent Claim 35 words
A process according to claim 12 wherein the reaction mixture is neutralized with solid sulfamic acid, the reaction mixture being cooled to between about 30° C. and 40° C. before addition of the sulfamic acid.
Claim 15
Dependent Claim 13 words
An aqueous solution of phenol-formaldehyde resin prepared according to process of claim 4.
Claim 16
Dependent Claim 190 words
A process for preparing a binder for mineral fibers, the process comprising preparing an aqueous solution of a water soluble urea-free resole resin having improved storage stability, the binder being prepared by a process comprising: (a) preparing an aqueous mixture of at least one aldehyde and at least one phenol, the molar ratio of the aldehyde to the phenol being from about 1.5 : 1 to 5.0: 1; (b) adding an alkaline earth metal compound to the aqueous mixture in an amount effective to catalyze the reaction between the aldehyde and the phenol; (c) reacting the aldehyde and the phenol under basic conditions in the absence of urea and in the presence of the alkaline earth metal compound to form a urea-free aqueous solution of a resole resin; (d) adding sulfamic acid to the urea-free aqueous solution prepared in step (c) to provide a resin solution having improved stability in an amount sufficient to provide a pH from about 1 to 8, and (e) subsequently adding at least one nitrogenous reactant selected from urea, ammonia, ammonium salts, dicyandiamide, meladine, and aminoplast resins to the urea-free aqueous solution including sulfamic acid.
Claim 17
Dependent Claim 190 words
A process for preparing a binder for mineral fibers, the process comprising preparing an aqueous solution of a water soluble urea-free resole resin having improved storage stability, the binder being prepared by a process comprising: (a) preparing an aqueous mixture of at least one aldehyde and at least one phenol, the molar ratio of the aldehyde to the phenol being from about 1.5 : 1 to 5.0: 1; (b) adding an alkaline earth metal compound to the aqueous mixture in an amount effective to catalyze the reaction between the aldehyde and the phenol; (c) reacting the aldehyde and the phenol under basic conditions in the absence of urea and in the presence of the alkaline earth metal compound to form a urea-free aqueous solution of a resole resin; (d) adding sulfamic acid to the urea-free aqueous solution prepared in step (c) to provide a resin solution having improved stability in an amount sufficient to provide a pH from about 1 to 8, and (e) subsequently adding at least one nitrogenous reactant selected from urea, ammonia, ammonium salts, dicyandiamide, meladine, and aminoplast resins to the urea-free aqueous solution including sulfamic acid.
Claim 18
Dependent Claim 12 words
A process according to claim 15 wherein the nitrogenous reactant is urea.
Claim 19
Dependent Claim 28 words
A process according to claim 15 wherein the nitrogenous reactant is added in an amount sufficient to react with substantially all residual formaldehyde in the aqueous resole solution.
Claim 20
Dependent Claim 28 words
A process according to claim 17 wherein the nitrogenous reactant is added in an amount up to about 75% by weight based on the weight of total solids.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1993-02-26 1993-08-28 1994-02-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1997-02-26 1997-08-28 1998-02-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2001-02-26 2001-08-28 2002-02-27 $7700.00 Window Closed / Lapsed

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