# US 4,391,766 A · Extraction of poly(.beta.-hydroxybutyric acid)

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- Number: US 4,391,766 A
- Document ID: US4391766A
- Status: Granted
- Kind: A
- Application number: 06/348,325
- Filed: 1982-02-12
- Granted: 1983-07-05
- Earliest claimed: 1979-08-13
- Assignees: Imperial Chemical Industries PLC
- Inventors: Peter J. Barham; Alan Selwood
- Web page: https://patentgrep.com/patent/US4391766A

## CPC

- C08G 63/06: derived from hydroxycarboxylic acids
- C08F 6/12: Separation of polymers from solutions
- C08G 63/88: Post-polymerisation treatment
- C12P 7/625: Polyesters of hydroxy carboxylic acids
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C12P: FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE {(brewing of beer C12C; producing vinegar C12J; producing specific peptides or proteins C07K; producing enzymes C12N9/00; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification C12N15/00; measuring or testing processes involving enzymes or microorganisms C12Q; measuring or testing processes involving nucleic acid amplification reactions C12Q1/6844; fermentation processes to form a food composition, A21 or A23; compounds in general, see the relevant compound class, e.g. C01, C07)}

## Abstract

.beta.-Hydroxybutyric acid polymers are extracted from micro-organism cells by contact with a solvent, such as 1,2-dichloroethane which is a poor solvent for the polymer once it has been precipitated. The solution obtained by extraction is caused to gel and then solvent is expelled by subjecting the gel to a deformation process. Expelled solvent is recovered for extraction of polymer from a further quantity of cells.

## Claims

### Claim 1

A process for the separation of a polymer containing at least 50 mole % of .beta.-hydroxybutyric acid residues in the polymer chain from micro-organism cells comprising
(a) extracting the polymer from the cells by contacting the polymer-containing cells with a solvent in which the polymer is soluble at the extraction temperature but in which extracted polymer, which has been freshly precipitated and not heated to above 40.degree. C., is not soluble at temperatures below 25.degree. C.,
(b) separating the solution of the polymer in said solvent from the micro-organism cell residue,
(c) causing said solution to gel,
(d) subjecting said gel to a non-random deformation process whereby the bulk of the solvent is expelled from said gel, and
(e) using at least the bulk of said expelled solvent for extraction of polymer from a further quantity of the polymer-containing cells.

### Claim 2 (depends on 1)

A process according to claim 1 wherein the amount of solvent used to extract the polymer is such that the resultant solution contains 0.5 to 10% by weight of the polymer.

### Claim 3 (depends on 2)

A process according to claim 2 wherein the amount of solvent used to extract the polymer is such that the resultant solution contains at least 1.5% by weight of the polymer.

### Claim 4 (depends on 1, 2, 3)

A process according to any one of claims 1 to 3 wherein gelation is effected by allowing the solution to stand at a temperature between 10.degree. C. and 30.degree. C., optionally with one or more of the following preliminary steps:
(i) cooling to below 0.degree. C.
(ii) shearing, and
(iii) seeding with a preformed gel of the polymer.

### Claim 5 (depends on 1)

A process according to claim 1 wherein the gel is deformed while in contact with at least one porous member.

### Claim 6 (depends on 1)

A process according to claim 1 wherein the deformed gel is extruded.

### Claim 7 (depends on 6)

A process according to claim 6 wherein at least some of the solvent in the deformed gel is volatilised and removed during the extrusion step.

### Claim 8 (depends on 6, 7)

A process according to claim 6 or claim 7 wherein a solution of an additive in the solvent is added to the deformed gel before, or during, the extrusion step.

### Claim 9 (depends on 1)

A process according to claim 1 wherein the solvent used for the extraction of the polymer from a further quantity of the polymer-containing cells comprises (a) the bulk of the solvent expelled during the deformation step together with (b) at least one of
(i) solvent expelled by syneresis during gel formation,
(ii) solvent recovered during further processing of the deformed gel, or
(iii) fresh solvent.

### Claim 10 (depends on 1)

A process according to claim 1 wherein the solvent used for the extraction of the polymer from a further quantity of the polymer containing cells comprises
(a) recovered solvent alone or together with
(b) fresh solvent, said recovered solvent consisting of
(i) the bulk of the solvent expelled during the deformation step, alone or together with at least one of
(ii) solvent expelled by syneresis during gel formation and
(iii) solvent separated during further processing of the deformed gel, and at least part of said recovered solvent is purified prior to its use for said extraction or polymer from the further quantity of polymer-containing cells.
