Patent US4562245A successfully refreshed from Google Patents.
US4562245A
Expired / Lapsed
US
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Extraction process
Assignee: Syngenta Ltd
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Filing: 1984-04-16
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Granted: 1985-12-31
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Expires: 2004-04-16
Abstract
Abstract A continuous process for the extraction of 3-hydroxybutyrate polymers from micro-organism cells wherein a non-solvent is added to the extracted syrup to permit separation of the polymer and, by distillation, the bulk of the extraction liquid, which may be a solvent/non-solvent mixture, is recovered for re-use. Preferably the non-solvent added to the syrup is also recovered in the distillation.
Inventors
- 👤 John F. Stageman
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 16:21
CPC Classifications
C; C12; C12P; C12P7/00; C12P7/62; C12P7/625; C08; C08G; C08G63/00; C08G63/88; C08G63/89; C08G85/00
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
312 words
A continuous, or cyclic batch, process for the extraction of a 3-hydroxybutyrate (HB) polymer from dried, solvent-permeable HB-polymer containing microorganism cells, said process comprising: (a) contacting said cells with an extraction liquid to form a syrup containing HB-polymer dissolved in the extraction liquid, said extraction liquid consisting of a mixture of (i) a solvent for said HB-polymer selected from dichloromethane, chloroform, and 1,2-dichloroethane, and (ii) a non-solvent for said HB polymer selected from methanol and ethanol, with the proviso that the non-solvent is methanol when said solvent is 1,2-dichloroethane, said extraction liquid containing sufficient of said solvent that said extraction liquid dissolves said polymer under the extraction conditions, (b) separating said syrup from the undissolved cell residue, (c) treating said syrup by adding thereto a sufficient quantity of a liquid composition, that is miscible with said syrup so that said syrup is converted to a composition that can be mechanically separated into a solid polymer phase and a liquid phase, and effecting said mechanical separation, said liquid composition A. consisting of (iii) said non-solvent, or a mixture of said non-solvent and said solvent, and optionally (iv) water, the amount, if any, of water in said liquid composition being such that said separated liquid phase contains less than 20% by weight of water, and B. having a lower content of said solvent than said extraction liquid, (d) distilling at least a proportion of said separated liquid phase to recover therefrom the azeotrope formed between said solvent and said non-solvent to leave a residue that is richer in non-solvent than said liquid phase, and (e) recycling at least a proportion of said recovered azeotrope to the syrup forming stage, the proportion of said liquid phase that is subjected to distillation and of said azeotrope that is recycled being such that at least 80% by weight of said extraction liquid consists of said recycled azeotrope.
Claim 2
Dependent Claim
312 words
A continuous, or cyclic batch, process for the extraction of a 3-hydroxybutyrate (HB) polymer from dried, solvent-permeable HB-polymer containing microorganism cells, said process comprising: (a) contacting said cells with an extraction liquid to form a syrup containing HB-polymer dissolved in the extraction liquid, said extraction liquid consisting of a mixture of (i) a solvent for said HB-polymer selected from dichloromethane, chloroform, and 1,2-dichloroethane, and (ii) a non-solvent for said HB polymer selected from methanol and ethanol, with the proviso that the non-solvent is methanol when said solvent is 1,2-dichloroethane, said extraction liquid containing sufficient of said solvent that said extraction liquid dissolves said polymer under the extraction conditions, (b) separating said syrup from the undissolved cell residue, (c) treating said syrup by adding thereto a sufficient quantity of a liquid composition, that is miscible with said syrup so that said syrup is converted to a composition that can be mechanically separated into a solid polymer phase and a liquid phase, and effecting said mechanical separation, said liquid composition A. consisting of (iii) said non-solvent, or a mixture of said non-solvent and said solvent, and optionally (iv) water, the amount, if any, of water in said liquid composition being such that said separated liquid phase contains less than 20% by weight of water, and B. having a lower content of said solvent than said extraction liquid, (d) distilling at least a proportion of said separated liquid phase to recover therefrom the azeotrope formed between said solvent and said non-solvent to leave a residue that is richer in non-solvent than said liquid phase, and (e) recycling at least a proportion of said recovered azeotrope to the syrup forming stage, the proportion of said liquid phase that is subjected to distillation and of said azeotrope that is recycled being such that at least 80% by weight of said extraction liquid consists of said recycled azeotrope.
Claim 3
Dependent Claim
28 words
A process according to claim 1 wherein the extraction liquid has a composition that has a solvent content equal to or greater than that of the solvent/non-solvent azeotrope.
Claim 4
Dependent Claim
22 words
A process according to claim 1 wherein all of the azeotrope is recycled to form at least part of the extraction liquid.
Claim 5
Dependent Claim
32 words
A process according to claim 1 wherein at least part of the residue is recycled, directly or indirectly, for use as at least part of the liquid composition added to the syrup.
Claim 6
Dependent Claim
18 words
A process according to claim 1 wherein all of the separated liquid phase is subjected to said distillation.
Claim 7
Dependent Claim
28 words
A process according to claim 5 wherein lipids are coextracted from the micro-organism cells with the HB polymer and part of the residue is discarded as a purge.
Claim 8
Dependent Claim
48 words
A process according to claim 6 wherein at least part of the residue is subjected to a further distillation to form a lipid-free distillate and a lipid-containing residue and said lipid-containing residue is that part of the residue obtained by distillation of the liquid phase that is discarded.
Claim 9
Dependent Claim
49 words
A process according to claim 1 wherein the separated polymer phase is subjected to a washing step with a liquid rich in said non-solvent, and the wash liquid separated from the washed polymer is recycled for use as at least part of the liquid composition added to the syrup.
Claim 10
Dependent Claim
40 words
A process according to claim 8 wherein at least part of the residue obtained by distillation of the liquid phase is recycled and the liquid used to wash the separated polymer phase comprises at least part of that recycled residue.
Claim 11
Dependent Claim
48 words
A process according to claim 9 wherein, at least part of the residue is subjected to a further distillation, and at least part of the distillate obtained from said further distillation is used as that part of the recycled residue in the liquid used to wash the polymer.
Claim 12
Dependent Claim
19 words
A process according to claim 1 wherein the extraction liquid contains at least 60% by weight of the solvent.
Claim 13
Dependent Claim
49 words
A process according to claim 1 wherein the amount of the liquid of lower solvent content than the extraction liquid that is added to the syrup is such that the mixture of that lower solvent content liquid and the syrup contains at least 60% by weight of the non-solvent.
Claim 14
Dependent Claim
30 words
A process according to claim 2 wherein the extraction liquid consists of the recycled azeotrope together with that quantity of fresh solvent necessary to compensate for losses of the solvent.
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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) | 1988-12-30 | 1989-07-01 | 1989-12-31 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-12-30 | 1993-07-01 | 1993-12-31 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-12-30 | 1997-07-01 | 1997-12-31 | $7700.00 | Window Closed / Lapsed |