# US 9,434,667 B2 · Method for isolation of 1,3-propanediol from post-fermentation broth obtained by bioconversion > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,434,667 B2 - Document ID: US9434667B2 - Status: Granted - Kind: B2 - Application number: 14/431,976 - Filed: 2013-09-27 - Published: 2015-09-17 - Granted: 2016-09-06 - Earliest claimed: 2012-09-28 - Assignees: Prochimia Surfaces SP. Z.o.o. - Applicants: Prochimia Surfaces Sp. Z O.O. - Inventors: Agnieszka Lindstaedt; Dariusz Witt; Joanna Puzewicz-Barska; Piotr Barski - Web page: https://patentgrep.com/patent/US9434667B2 ## CPC - C07C 29/76: by physical treatment - B01D 11/04: of solutions which are liquid - C07C 29/80: by distillation - C07C 29/86: by liquid-liquid treatment - C12P 7/18: polyhydric - B01D 2011/007: {Extraction using a solvent in the gas phase} - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) - 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 A method for isolation of 1,3-propanediol from post-fermentation broth is disclosed. The method generally involves the following steps: (1) biomass removal from post-fermentation broth by one of the following methods: ultrafiltration, filtration, centrifugation or sedimentation; (2) 1,3-propanediol extraction with organic solvent mixture containing 2-butanone with high efficiency performed continuously or stepwise; (3) distillation under vacuum to obtain highly pure target product and (4) organic solvent recovery and recycling the solvent back into the process. The method is useful for recovering valuable 1,3-propanediol from aqueous solutions produced by fermentation. ## Claims ### Claim 1 A method for isolation of 1,3-propanediol from the post-fermentation broth comprising: a) removing biomass from post-fermentation broth; and b) extracting 1,3-propanediol using a mixture of organic solvents, wherein the mixture contains 2-butanone. ### Claim 2 (depends on 1) The method according to claim 1, repeating step (b) a plurality of times using the same organic solvent mixture. ### Claim 3 (depends on 1) The method according to claim 1, wherein the said method is carried out stepwise and organic solvent used in the extraction process is used repeatedly. ### Claim 4 (depends on 1) The method according to claim 1, wherein in step (b) the organic solvent mixture comprises at least 10% (v/v) 2-butanone. ### Claim 5 (depends on 1) The method according to claim 1, wherein the volume ratio of the post-fermentation broth, comprising 1,3-propanediol after biomass removal in step (a) to the organic solvent mixture in step (b) is at a minimum 1:3. ### Claim 6 (depends on 1) The method according to claim 1, wherein in step (a) the biomass removal is conducted without salting out or concentrating the post-fermentation broth. ### Claim 7 (depends on 1) The method according to claim 1, and further comprising step (c) subsequent to step (b) distilling the extracted 1,3-propanediol under vacuum to obtain purified 1,3-propanediol. ### Claim 8 (depends on 7) The method according to claim 7, wherein in step (c) the 1,3-propanediol is distilled to at least 99.90% purity. ### Claim 9 (depends on 1) The method according to claim 1, wherein in (a) removing the biomass from post-fermentation broth is carried out using at least one of the following methods: ultrafiltration, filtration, centrifugation and sedimentation. ### Claim 10 (depends on 2) The method according to claim 2, wherein in step (b) the organic solvent mixture comprises at least 10% (v/v) 2-butanone. ### Claim 11 (depends on 2) The method according to claim 2, wherein the volume ratio of the post-fermentation broth, comprising 1,3-propanediol after biomass removal in step (a) to the organic solvent mixture in step (b) is at a minimum 1:3. ### Claim 12 (depends on 2) The method according to claim 2, wherein in step (a) the biomass removal is conducted without salting out or concentrating the post-fermentation broth. ### Claim 13 (depends on 2) The method according to claim 2, and further comprising step (c) subsequent to step (b) distilling the extracted 1,3-propanediol under vacuum to obtain purified 1,3-propanediol. ### Claim 14 (depends on 2) The method according to claim 2, wherein in (a) removing the biomass from post-fermentation broth is carried out using at least one of the following methods: ultrafiltration, filtration, centrifugation and sedimentation. ### Claim 15 (depends on 3) The method according to claim 3, wherein in step (b) the organic solvent mixture comprises at least 10% (v/v) 2-butanone. ### Claim 16 (depends on 3) The method according to claim 3, wherein the volume ratio of the post-fermentation broth, comprising 1,3-propanediol after biomass removal in step (a) to the and organic solvent mixture in step (b) is at a minimum 1:3. ### Claim 17 (depends on 3) The method according to claim 3, wherein in step (a) the biomass removal is conducted without salting out or concentrating the post-fermentation broth. ### Claim 18 (depends on 3) The method according to claim 3, and further comprising step (c) subsequent to step (b) distilling the extracted 1,3-propanediol under vacuum to obtain purified 1,3-propanediol. ### Claim 19 A method for isolation of 1,3-propanediol from the post-fermentation broth comprising: a) removing biomass from post-fermentation broth; and b) extracting, without using back extraction, 1,3-propanediol using a mixture of organic solvents, wherein the mixture contains 2-butanone. ### Claim 20 A method for isolation of 1,3-propanediol from the post-fermentation broth comprising: a) removing biomass from post-fermentation broth; b) extracting, without using back extraction, 1,3-propanediol using a mixture of organic solvents, wherein the mixture contains 2-butanone, c) subsequent to step (b) distilling the extracted 1,3-propanediol under vacuum to obtain purified 1,3-propanediol; wherein in step (c) the 1,3-propanediol is distilled to at least 99.90% purity.