Patent US4054601A successfully refreshed from Google Patents.
US4054601A
Expired / Lapsed
US
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Method of recovering purified glycolic acid from its contaminated aqueous solutions
Assignee: Evonik Operations GmbH
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Filing: 1976-06-22
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Granted: 1977-10-18
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Expires: 1996-06-22
Abstract
Abstract Pure glycolic acid is recovered practically completely from the product obtained by hydrolysis of glycolonitrile containing at least stoichiometrically equivalent amounts of ammonium and sulfate ions by extraction with a mixture of a trialkyl phosphate and a dialkylether, preferably of equal weights of tributyl phosphate and diisopropyl ether, and separation of the glycolic acid from the extraction medium by contact with water.
Inventors
- 👤 Ulrich Metz
- 👤 Horst Michaud
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 20:14
CPC Classifications
C; C07; C07C; C07C51/00; C07C51/42; C07C51/48; C07C51/08
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
116 words
A method of recovering purified glycolic acid from an aqueous solution thereof contaminated with ammonium and sulfate ions in respective amounts at least stoichiometrically equivalent to said glycolic acid which comprises: a. contacting said contaminated solution with an extraction medium consisting essentially of a mixture of a trialkyl phosphate with a dialkyl ether until said glycolic acid is dissolved in said extraction medium, 1. alkyl in said trialkyl phosphate having up to six carbon atoms, 2. alkyl in said dialkyl ether having two to five carbon atoms, 3. each of said trialkyl phosphate and said dialkyl ether constituting at least 10% by weight of said medium; and b. separating said glycolic acid from said extraction medium.
Claim 2
Independent Claim
116 words
A method of recovering purified glycolic acid from an aqueous solution thereof contaminated with ammonium and sulfate ions in respective amounts at least stoichiometrically equivalent to said glycolic acid which comprises: a. contacting said contaminated solution with an extraction medium consisting essentially of a mixture of a trialkyl phosphate with a dialkyl ether until said glycolic acid is dissolved in said extraction medium, 1. alkyl in said trialkyl phosphate having up to six carbon atoms, 2. alkyl in said dialkyl ether having two to five carbon atoms, 3. each of said trialkyl phosphate and said dialkyl ether constituting at least 10% by weight of said medium; and b. separating said glycolic acid from said extraction medium.
Claim 3
Dependent Claim
55 words
A method as set forth in claim 1, wherein said contaminated solution, prior to said contacting is formed by hydrolyzing glycolonitrile in the presence of sulfuric acid, at elevated temperature, said glycolic acid being separated from said extraction medium by contacting said extraction medium with water until said glycolic acid is dissolved in said water.
Claim 4
Dependent Claim
35 words
A method as set forth in claim 2, wherein said elevated temperature is 100° to 150° C, and the amount of said sulfuric acid is approximately one mole for each 2 moles of said glycolonitrile.
Claim 5
Dependent Claim
26 words
A method as set forth in claim 3, wherein said extraction medium is contacted sequentially with said contaminated solution and with said water in counter-current flow.
Claim 6
Dependent Claim
22 words
A method as set forth in claim 2, wherein said trialkyl phosphate is tributyl phosphate, and said dialkyl ether is diisopropyl ether.
Claim 7
Dependent Claim
27 words
A method as set forth in claim 5, wherein each of said tributyl phosphate and diisopropyl ether constitutes at least 35% by weight of said extraction mixture.
Claim 8
Dependent Claim
27 words
A method as set forth in claim 6, wherein said extraction mixture consists essentially of approximately equal weights of said tributyl phosphate and of said diisopropyl ether.
References Cited (Backward Citations)
FR1494958A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-10-17 | 1981-04-18 | 1981-10-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-10-17 | 1985-04-18 | 1985-10-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-10-17 | 1989-04-18 | 1989-10-18 | $7700.00 | Window Closed / Lapsed |