US4176216A
Expired / Lapsed
US
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Cellular products derived from phenol/formaldehyde resoles
Assignee: Union Carbide Corp
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Filing: 1978-09-29
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Granted: 1979-11-27
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Expires: 1998-09-29
Abstract
Abstract The present invention provides particular phenol/formaldehyde resoles which are especially useful as foamable resins, and further provides cellular phenolic products having physical properties which are especially attractive for end-use application as construction foam. The resoles are characterized by a particular relationship between their viscosity and water content, expressed as the area bounded by certain points on a plot of resole viscosity on a logarithmic scale, as a function of water content of the resole, the particular area depending upon the mole ratio of formaldehyde-to-phenol at which the resole has been condensed. It has been found that phenol-formaldehyde resoles having the defined viscosity/water relationship are capable of providing phenolic foam having acceptable foam processability, a foam density from about 1.90 to about 3.70 pounds per cubic foot and, within this foam density range, a good balance of friability resistance and compressive strength, that is, a friability of less than 35 percent weight loss and a compressive strength of at least 20 pounds per square inch. Preferred resoles within the invention are foamable to phenolic foam having a reduced tendency to punk as well as the aforementioned desirable combination of foam processability and mechanical properties.
Inventors
- 👤 Wallace G. Reid
- 👤 Rakesh Saini
- 👤 Kenneth E. Atkins
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 19:09
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/04; C08J9/12; C08J9/14; C08G; C08G8/00; C08G8/04; C08G8/08; C08G8/10; C08J2361/00; C08J2361/04; C08J2361/06; C08J2361/08; Y; Y10; Y10S; Y10S521/00; Y10S521/907; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31942
Claims Analysis
Total Claims: 27
Claim 1
Independent Claim
433 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot and, within said density range, a friability of less than about 35 percent weight loss (after 10 minutes) and a compressive strength (parallel) of at least about 20 pounds per square inch, which foam is produced by foaming a reaction mixture containing a phenolic resole, an acidic catalyst, a blowing agent and a surface active agent, wherein the said resole has been produced by the base-catalyzed condensation of formaldehyde and phenol at a formaldehyde-to-phenol mole ratio from about 1.6:1 to about 2.2:1, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (i)-(iv) where points (i)-(iv) are as follows for the indicated formaldehyde-to-phenol mole ratios: (a) at a formaldehyde-to-phenol mole ratio of at least 1.9:1 and no more than about 2.2:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 1.7 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (iii) a viscosity of about 12,000 centipoise at a water content of about 15.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 15.0 weight percent; (b) at a formaldehyde-to-phenol mole ratio of at least 1.7:1 and less than 1.9:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 3.0 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 14.0 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 16.0 weight percent; (c) at a formaldehyde-to-phenol mole ratio of at least about 1.6:1 and less than 1.7:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 6.5 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 12.5 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 3,000 centipoise at a water content of about 16.0 weight percent; wherein the said viscosity values are Brookfield at 25° C.
Claim 2
Dependent Claim
433 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot and, within said density range, a friability of less than about 35 percent weight loss (after 10 minutes) and a compressive strength (parallel) of at least about 20 pounds per square inch, which foam is produced by foaming a reaction mixture containing a phenolic resole, an acidic catalyst, a blowing agent and a surface active agent, wherein the said resole has been produced by the base-catalyzed condensation of formaldehyde and phenol at a formaldehyde-to-phenol mole ratio from about 1.6:1 to about 2.2:1, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (i)-(iv) where points (i)-(iv) are as follows for the indicated formaldehyde-to-phenol mole ratios: (a) at a formaldehyde-to-phenol mole ratio of at least 1.9:1 and no more than about 2.2:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 1.7 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (iii) a viscosity of about 12,000 centipoise at a water content of about 15.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 15.0 weight percent; (b) at a formaldehyde-to-phenol mole ratio of at least 1.7:1 and less than 1.9:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 3.0 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 14.0 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 16.0 weight percent; (c) at a formaldehyde-to-phenol mole ratio of at least about 1.6:1 and less than 1.7:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 6.5 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 12.5 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 3,000 centipoise at a water content of about 16.0 weight percent; wherein the said viscosity values are Brookfield at 25° C.
Claim 3
Dependent Claim
24 words
A phenolic foam as defined in claim 1 wherein the acidic catalyst of the reaction mixture which is foamed comprises an organic sulfonic acid.
Claim 4
Dependent Claim
17 words
A phenolic foam as defined in claim 2 wherein the said reaction mixture additionally contains phosphoric acid.
Claim 5
Dependent Claim
17 words
A phenolic foam as defined in claim 2 wherein the said reaction mixture additionally contains boric acid.
Claim 6
Dependent Claim
279 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot and, within said density range, a friability of less than about 35 percent weight loss (after 10 minutes) and a compressive strength (parallel) of at least about 20 pounds per square inch, which foam is produced by foaming a reaction mixture containing a phenolic resole, an acidic catalyst, a blowing agent and a surface active agent, wherein the said phenolic resole has been produced by the base-catalysed condensation of formaldehyde and phenol as the sole organic reactants fed to the condensation reaction, at a mole ratio of at least 1.9 and no more than about 2.2 moles of formaldehyde per mole of phenol, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (a)-(e) where points (a)-(e) are as follows: (a) a viscosity of about 50,000 centipoise at a water content of about 7.0 weight percent; (b) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (c) a viscosity of about 26,000 centipoise at a water content of about 12.0 weight percent; (d) a viscosity of about 4,000 centipoise at a water content of about 12.0 weight percent; and (e) a viscosity of about 20,000 centipoise at a water content of about 7.0 weight percent; wherein the viscosity values are Brookfield at 25° C.
Claim 7
Dependent Claim
279 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot and, within said density range, a friability of less than about 35 percent weight loss (after 10 minutes) and a compressive strength (parallel) of at least about 20 pounds per square inch, which foam is produced by foaming a reaction mixture containing a phenolic resole, an acidic catalyst, a blowing agent and a surface active agent, wherein the said phenolic resole has been produced by the base-catalysed condensation of formaldehyde and phenol as the sole organic reactants fed to the condensation reaction, at a mole ratio of at least 1.9 and no more than about 2.2 moles of formaldehyde per mole of phenol, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (a)-(e) where points (a)-(e) are as follows: (a) a viscosity of about 50,000 centipoise at a water content of about 7.0 weight percent; (b) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (c) a viscosity of about 26,000 centipoise at a water content of about 12.0 weight percent; (d) a viscosity of about 4,000 centipoise at a water content of about 12.0 weight percent; and (e) a viscosity of about 20,000 centipoise at a water content of about 7.0 weight percent; wherein the viscosity values are Brookfield at 25° C.
Claim 8
Dependent Claim
276 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot and, within said density range, a friability of less than about 35 percent weight loss (after 10 minutes) and a compressive strength (parallel) of at least about 20 pounds per square inch, which foam is produced by foaming a reaction mixture containing a phenolic resole, an acidic catalyst, a blowing agent and a surface active agent, wherein the said resole has been produced by the base-catalyzed condensation of formaldehyde and phenol as the sole organic reactants fed to the condensation reaction, at a mole ratio of at least 1.7 and less than 1.9 moles of formaldehyde per mole of phenol, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (a)-(e) where points (a)-(e) are as follows: (a) a viscosity of about 50,000 centipoise at a water content of about 7.0 weight percent; (b) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (c) a viscosity of about 25,000 centipoise at a water content of about 12.0 weight percent; (d) a viscosity of about 4,200 centipoise at a water content of about 12.0 weight percent; and (e) a viscosity of about 34,000 centipoise at a water content of about 7.0 weight percent; wherein the viscosity values are Brookfield at 25° C.
Claim 9
Dependent Claim
276 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot and, within said density range, a friability of less than about 35 percent weight loss (after 10 minutes) and a compressive strength (parallel) of at least about 20 pounds per square inch, which foam is produced by foaming a reaction mixture containing a phenolic resole, an acidic catalyst, a blowing agent and a surface active agent, wherein the said resole has been produced by the base-catalyzed condensation of formaldehyde and phenol as the sole organic reactants fed to the condensation reaction, at a mole ratio of at least 1.7 and less than 1.9 moles of formaldehyde per mole of phenol, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (a)-(e) where points (a)-(e) are as follows: (a) a viscosity of about 50,000 centipoise at a water content of about 7.0 weight percent; (b) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (c) a viscosity of about 25,000 centipoise at a water content of about 12.0 weight percent; (d) a viscosity of about 4,200 centipoise at a water content of about 12.0 weight percent; and (e) a viscosity of about 34,000 centipoise at a water content of about 7.0 weight percent; wherein the viscosity values are Brookfield at 25° C.
Claim 10
Dependent Claim
427 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot, a compressive strength (parallel) of at least about 20 pounds per square inch and a friability of less than about 35 percent weight loss after 10 minutes, which foam is produced by foaming and reacting a reaction mixture containing a phenol/formaldehyde resole, an acidic catalyst and a blowing agent, wherein the said phenol/formaldehyde resole has been produced by the base-catalyzed condensation of formaldehyde and phenol at a formaldehyde-to-phenol mole ratio from about 1.6:1 to about 2.2:1, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (i)-(iv) where points (i)-(iv) are as follows for the indicated formaldehyde-to-phenol mole ratios: (a) at a formaldehyde-to-phenol mole ratio of at least 1.9:1 and no more than about 2.2:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 1.7 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (iii) a viscosity of about 12,000 centipoise at a water content of about 15.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 15.0 weight percent; (b) at a formaldehyde-to-phenol mole ratio of at least 1.7:1 and less than 1.9:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 3.0 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 14.0 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 16.0 weight percent; (c) at a formaldehyde-to-phenol mole ratio of at least about 1.6:1 and less than 1.7:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 6.5 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 12.5 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 3,000 centipoise at a water content of about 16.0 weight percent, wherein the said viscosity values are Brookfield at 25° C.
Claim 11
Dependent Claim
427 words
A phenolic foam having a density from about 1.90 to about 3.70 pounds per cubic foot, a compressive strength (parallel) of at least about 20 pounds per square inch and a friability of less than about 35 percent weight loss after 10 minutes, which foam is produced by foaming and reacting a reaction mixture containing a phenol/formaldehyde resole, an acidic catalyst and a blowing agent, wherein the said phenol/formaldehyde resole has been produced by the base-catalyzed condensation of formaldehyde and phenol at a formaldehyde-to-phenol mole ratio from about 1.6:1 to about 2.2:1, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (i)-(iv) where points (i)-(iv) are as follows for the indicated formaldehyde-to-phenol mole ratios: (a) at a formaldehyde-to-phenol mole ratio of at least 1.9:1 and no more than about 2.2:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 1.7 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (iii) a viscosity of about 12,000 centipoise at a water content of about 15.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 15.0 weight percent; (b) at a formaldehyde-to-phenol mole ratio of at least 1.7:1 and less than 1.9:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 3.0 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 14.0 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 16.0 weight percent; (c) at a formaldehyde-to-phenol mole ratio of at least about 1.6:1 and less than 1.7:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 6.5 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 12.5 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 3,000 centipoise at a water content of about 16.0 weight percent, wherein the said viscosity values are Brookfield at 25° C.
Claim 12
Dependent Claim
17 words
A phenolic foam as defined in claim 7 wherein the acidic catalyst is an organic sulfonic acid.
Claim 13
Dependent Claim
17 words
A phenolic foam as defined in claim 8 wherein the organic sulfonic acid is phenol sulfonic acid.
Claim 14
Dependent Claim
15 words
A phenolic foam as defined in claim 7 wherein the reaction mixture contains phosphoric acid.
Claim 15
Dependent Claim
15 words
A phenolic foam as defined in claim 7 wherein the reaction mixture contains boric acid.
Claim 16
Dependent Claim
19 words
A phenolic foam as defined in claim 7 wherein the acidic catalyst comprises phenol sulfonic acid and phosphoric acid.
Claim 17
Dependent Claim
24 words
A phenolic foam as defined in claim 7 wherein the acidic catalyst comprises phenol sulfonic acid and the reaction mixture additionally contains boric acid.
Claim 18
Dependent Claim
279 words
A phenolic foam having a density from about 2.0 to about 3.0 pounds per cubic foot, a compressive strength (parallel) of at least 25 pounds per square inch and a friability of less than 25 percent weight loss after 10 minutes, which foam is produced by foaming and reacting a reaction mixture containing a phenol/formaldehyde resole, an acidic catalyst comprising an organic sulfonic acid, a blowing agent, and a surface active agent, wherein the said phenol/formaldehyde resole has been produced by the base-catalyzed condensation of formaldehyde and phenol as the sole organic reactants fed to the condensation reaction, at a mole ratio of at least 1.9 and no more than about 2.2 moles of formaldehyde per mole of phenol, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereof of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (a)-(e) where points (a)-(e) are as follows: (a) a viscosity of about 50,000 centipoise at a water content of about 7.0 weight percent; (b) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (c) a viscosity of about 26,000 centipoise at a water content of about 12.0 weight percent; (d) a viscosity of about 4,000 centipoise at a water content of about 12.0 weight percent; and (e) a viscosity of about 20,000 centipoise at a water content of about 7.0 weight percent; wherein the viscosity values are Brookfield at 25° C.
Claim 19
Dependent Claim
279 words
A phenolic foam having a density from about 2.0 to about 3.0 pounds per cubic foot, a compressive strength (parallel) of at least 25 pounds per square inch and a friability of less than 25 percent weight loss after 10 minutes, which foam is produced by foaming and reacting a reaction mixture containing a phenol/formaldehyde resole, an acidic catalyst comprising an organic sulfonic acid, a blowing agent, and a surface active agent, wherein the said phenol/formaldehyde resole has been produced by the base-catalyzed condensation of formaldehyde and phenol as the sole organic reactants fed to the condensation reaction, at a mole ratio of at least 1.9 and no more than about 2.2 moles of formaldehyde per mole of phenol, the aqueous alkaline condensate having been brought to a pH from about 5.0 to about 7.0 by the addition thereof of a salt-forming acidic compound, which resole is characterized by an average molecular weight such that a plot of log viscosity as a function of water content of the resole falls within the area defined by straight line interconnection in series of points (a)-(e) where points (a)-(e) are as follows: (a) a viscosity of about 50,000 centipoise at a water content of about 7.0 weight percent; (b) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (c) a viscosity of about 26,000 centipoise at a water content of about 12.0 weight percent; (d) a viscosity of about 4,000 centipoise at a water content of about 12.0 weight percent; and (e) a viscosity of about 20,000 centipoise at a water content of about 7.0 weight percent; wherein the viscosity values are Brookfield at 25° C.
Claim 20
Independent Claim
383 words
The method for producing phenolic foam which comprises foaming a reaction mixture containing a phenolic resole, an acidic catalyst and a blowing agent wherein said phenolic resole is produced by the base-catalyzed condensation of phenol and formaldehyde at a formaldehyde-to-phenol mole ratio of from about 1.6:1 to about 2.2:1 and the aqueous alkaline condensate is brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, the base-catalyzed condensation reaction being effected under conditions such that a plot of log viscosity as a function of water content of the resole product falls within the area defined by straight line interconnection in series of points (i)-(iv) where points (i)-(iv) are as follows for the indicated formaldehyde-to-phenol mole ratios: (a) at a formaldehyde-to-phenol mole ratio of at least 1.9:1 and no more than about 2.2:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 1.7 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (iii) a viscosity of about 12,000 centipoise at a water content of about 15.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 15.0 weight percent; (b) at a formaldehyde-to-phenol mole ratio of at least 1.7:1 and less than 1.9:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 3.0 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 14.0 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 16.0 weight percent; (c) at a formaldehyde-to-phenol mole ratio of at least 1.6:1 and less than 1.7:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 6.5 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 12.5 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 3,000 centipoise at a water content of about 16.0 weight percent; wherein the said viscosity values are Brookfield at 25° C.
Claim 21
Independent Claim
383 words
The method for producing phenolic foam which comprises foaming a reaction mixture containing a phenolic resole, an acidic catalyst and a blowing agent wherein said phenolic resole is produced by the base-catalyzed condensation of phenol and formaldehyde at a formaldehyde-to-phenol mole ratio of from about 1.6:1 to about 2.2:1 and the aqueous alkaline condensate is brought to a pH from about 5.0 to about 7.0 by the addition thereto of a salt-forming acidic compound, the base-catalyzed condensation reaction being effected under conditions such that a plot of log viscosity as a function of water content of the resole product falls within the area defined by straight line interconnection in series of points (i)-(iv) where points (i)-(iv) are as follows for the indicated formaldehyde-to-phenol mole ratios: (a) at a formaldehyde-to-phenol mole ratio of at least 1.9:1 and no more than about 2.2:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 1.7 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 9.5 weight percent; (iii) a viscosity of about 12,000 centipoise at a water content of about 15.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 15.0 weight percent; (b) at a formaldehyde-to-phenol mole ratio of at least 1.7:1 and less than 1.9:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 3.0 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 14.0 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 1,000 centipoise at a water content of about 16.0 weight percent; (c) at a formaldehyde-to-phenol mole ratio of at least 1.6:1 and less than 1.7:1, points (i)-(iv) are: (i) a viscosity of about 50,000 centipoise at a water content of about 6.5 weight percent; (ii) a viscosity of about 50,000 centipoise at a water content of about 12.5 weight percent; (iii) a viscosity of about 25,000 centipoise at a water content of about 16.0 weight percent; and (iv) a viscosity of about 3,000 centipoise at a water content of about 16.0 weight percent; wherein the said viscosity values are Brookfield at 25° C.
Claim 22
Dependent Claim
15 words
The method of claim 15 in which said acidic catalyst comprises an organic sulfonic acid.
Claim 23
Dependent Claim
15 words
The method of claim 16 in which the organic sulfonic acid is phenol sulfonic acid.
Claim 24
Dependent Claim
14 words
The method of claim 16 in which said reaction mixture additionally contains phosphoric acid.
Claim 25
Dependent Claim
20 words
The method of claim 15 in which said reaction mixture contains a surface active agent as an additional component thereof.
Claim 26
Dependent Claim
17 words
The method of claim 19 in which the surface active agent is a non ionic organic surfactant.
Claim 27
Dependent Claim
15 words
The method of claim 19 in which the surface active agent is a polysiloxane-poly(oxyalkylene) copolymer.
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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) | 1982-11-26 | 1983-05-28 | 1983-11-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-11-26 | 1987-05-28 | 1987-11-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-11-26 | 1991-05-28 | 1991-11-27 | $7700.00 | Window Closed / Lapsed |