Patent US3891612A successfully refreshed from Google Patents.
US3891612A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Polymerized rosin product and process for the production of same
Assignee: United States Department of Agriculture
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Filing: 1973-03-05
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Granted: 1975-06-24
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Expires: 1993-03-05
Abstract
Abstract Rosin or resin acids are polymerized in reaction mixtures of sulfuric acid, water, and acetic acid in such proportions that the rosin or resin acids are readily soluble and the polymerized rosin or resin acids are of limited solubility separating in a polymer-rich layer which may be removed for isolation of the polymerized rosin. Adding more rosin to the mixture produces more polymer-rich layer and thereby the process is continuous. The fractionation of polymerized rosin or resin acids into a highmelting resin having a molecular weight indicating it to be a dimer and a low melting fraction containing monomer and dimer has also been accomplished through solvent extraction.
Inventors
- 👤 Jr Bernard A Parkin
- 👤 Walter H Schuller
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 10:23
CPC Classifications
C; C09; C09F; C09F1/00; C09F1/04
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
94 words
A PROCESS FOR THE PRODUCTION OF A POLYMERIZED COMPOSITION WHICH PROCESS COMPRISES: DISSLOVING A MATERIAL SELECTED FROM THE GROUP CONSISTING OF ROSIN, RESIN ACIDS AND A RESIN ACID IN A MIXTURE OF ACETIC ACID, SULFUR ACID, AND WATER AND REACTING SAID MATERIAL IN SAID MIXTURE, WHEREIN THE PROPORTIONS OF ACETIC ACID SULFURIC ACID AND WATER IN SAID MIXTURE ARE SUCH THAT THE UNREACTED MATERIAL IS SOLUBLE AND THE POLYMERIZED PRODUCTS OF THE REACTION HAVE ONLY LIMITED SOLUBILITY AND SEPARATE FROM THE MIXTURE IN THE FORM OF A POLYMER-RICH LAYER AS THE RATE REACTION PROCEEDS.
Claim 2
Dependent Claim
94 words
A PROCESS FOR THE PRODUCTION OF A POLYMERIZED COMPOSITION WHICH PROCESS COMPRISES: DISSLOVING A MATERIAL SELECTED FROM THE GROUP CONSISTING OF ROSIN, RESIN ACIDS AND A RESIN ACID IN A MIXTURE OF ACETIC ACID, SULFUR ACID, AND WATER AND REACTING SAID MATERIAL IN SAID MIXTURE, WHEREIN THE PROPORTIONS OF ACETIC ACID SULFURIC ACID AND WATER IN SAID MIXTURE ARE SUCH THAT THE UNREACTED MATERIAL IS SOLUBLE AND THE POLYMERIZED PRODUCTS OF THE REACTION HAVE ONLY LIMITED SOLUBILITY AND SEPARATE FROM THE MIXTURE IN THE FORM OF A POLYMER-RICH LAYER AS THE RATE REACTION PROCEEDS.
Claim 3
Dependent Claim
11 words
The process of claim 1 wherein the selected material is rosin.
Claim 4
Dependent Claim
15 words
The process of claim 1 wherein the selected material is a monomeric abietic-type resin acid.
Claim 5
Dependent Claim
156 words
A process for the production of a polymerized resin composition which process comprises dissolving a material selected from the group consisting of rosin, resin acids and a resin acid in a mixture of aqueous sulfuric acid in the range of from 95% H2SO4 and 5% H2O to 50% H2SO4 and 50% H2O by weight with acetic acid in the range of from one part of the aqueous sulfuric acid and 100 parts of acetic acid by volume to 50 parts of the aqueous sulfuric acid and 100 parts of acetic acid by volume, which permits solution of the material and yields separation of a polymer-rich layer, reacting said material in said mixture at a temperature between 0* C. and 118* C. for sufficient time to allow polymerization of said material and the separation of a polymer-rich layer, separating said layer from said mixture and treating said layer and said mixture to remove acetic and sulfuric acid.
Claim 6
Dependent Claim
156 words
A process for the production of a polymerized resin composition which process comprises dissolving a material selected from the group consisting of rosin, resin acids and a resin acid in a mixture of aqueous sulfuric acid in the range of from 95% H2SO4 and 5% H2O to 50% H2SO4 and 50% H2O by weight with acetic acid in the range of from one part of the aqueous sulfuric acid and 100 parts of acetic acid by volume to 50 parts of the aqueous sulfuric acid and 100 parts of acetic acid by volume, which permits solution of the material and yields separation of a polymer-rich layer, reacting said material in said mixture at a temperature between 0* C. and 118* C. for sufficient time to allow polymerization of said material and the separation of a polymer-rich layer, separating said layer from said mixture and treating said layer and said mixture to remove acetic and sulfuric acid.
Claim 7
Dependent Claim
11 words
The process of claim 4 wherein the selected material is rosin.
Claim 8
Dependent Claim
15 words
The process of claim 4 wherein the selected material is a monomeric abietic-type resin acid.
Claim 9
Dependent Claim
173 words
A process for the production of a high melting polymer which process comprises: a. dissolving a material selected from the group consisting of rosin, resin acids and a resin acid in a mixture of aqueous sulfuric acid in the range from 95% H2SO4 and 5% H2O to 50% H2SO4 and 50% H2O by weight with acetic acid in the range of from one part of the aqueous sulfuric acid and 100 parts of acetic acid to 50 parts of the aqueous sulfuric acid with 100 parts of acetic acid by volume; b. reacting said material in said mixture at a temperature of between 0* C. and 118* C. until polymerization of said material and the separation of a polymer-rich layer begins; c. separating said layer from said mixture; d. treating said layer to remove acetic and sulfuric acids; e. making a concentrated solution of said layer in isooctane; f. diluting said concentrated solution with additional isooctane; g. allowing a high melting polymer to precipitate; and h. isolating the precipitate from said diluted solution.
Claim 10
Dependent Claim
173 words
A process for the production of a high melting polymer which process comprises: a. dissolving a material selected from the group consisting of rosin, resin acids and a resin acid in a mixture of aqueous sulfuric acid in the range from 95% H2SO4 and 5% H2O to 50% H2SO4 and 50% H2O by weight with acetic acid in the range of from one part of the aqueous sulfuric acid and 100 parts of acetic acid to 50 parts of the aqueous sulfuric acid with 100 parts of acetic acid by volume; b. reacting said material in said mixture at a temperature of between 0* C. and 118* C. until polymerization of said material and the separation of a polymer-rich layer begins; c. separating said layer from said mixture; d. treating said layer to remove acetic and sulfuric acids; e. making a concentrated solution of said layer in isooctane; f. diluting said concentrated solution with additional isooctane; g. allowing a high melting polymer to precipitate; and h. isolating the precipitate from said diluted solution.
Claim 11
Dependent Claim
12 words
The high melting, hydrocarbon insoluble product of the process of claim 7.
Claim 12
Dependent Claim
41 words
The process of claim 7 including the further steps of diluting with additional isooctane the solution from which the high melting polymer is isolated in step (h), allowing a low melting polymer to precipitate, and isolating the precipitated low melting polymer.
Claim 13
Dependent Claim
12 words
The lower melting, hydrocarbon soluble product of the process of claim 9.
References Cited (Backward Citations)
US2124675A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-06-23 | 1978-12-23 | 1979-06-24 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-06-23 | 1982-12-23 | 1983-06-24 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-06-23 | 1986-12-23 | 1987-06-24 | $7700.00 | Window Closed / Lapsed |