IP Library Granted Patent US 10,017,451
Granted Patent B2
US 10,017,451 · App. 14/366,595 · Granted Jul 10, 2018

Lactic acid extraction

Inventors: André Banier De Haan (Best, NL); Jan Van Krieken (Gorinchem, NL); Tanja Ðekic {hacek over (Z)}ivkovic ('s-Hertogenbosch, NL)
Assignee: PURAC BIOCHEM B.V.
C07C51/48B01D11/04C07C51/412C12P7/56B01D11/0426
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Quick Facts
Patent No.
US 10,017,451
App. No.
14/366,595
Granted
Jul 10, 2018
Kind
B2
Abstract

A method for recovering lactic acid from an aqueous mixture including the steps of: providing an aqueous mixture including lactic acid and at least 5 wt. % dissolved magnesium chloride, based on the total weight of water and dissolved material in the aqueous mixture; extracting the lactic acid from the aqueous mixture into a first organic liquid including an organic solvent selected from the group consisting of C5+ ketones, diethylether and methyl-tertiary-butyl-ether, thereby obtaining an organic lactic acid solution and an aqueous waste liquid including magnesium chloride; and extracting the lactic acid from the organic lactic acid solution into an aqueous liquid, thereby obtaining an aqueous lactic acid solution and a second organic liquid. The method according to the invention allows a combined purification and concentration step for feed solutions of lactic acid.

Claims (32)

1. Method for recovering lactic acid from an aqueous mixture comprising the steps of

providing an aqueous mixture comprising lactic acid and at least 5 wt. % dissolved magnesium chloride, based on the total weight of water and dissolved material in the aqueous mixture,

a first extraction comprising extracting the lactic acid from the aqueous mixture into a first organic liquid comprising at least 90 wt. % of an organic solvent selected from the group consisting of C5+ ketones, diethylether and methyl-tertiary-butyl-ether, thereby obtaining an organic lactic acid solution and an aqueous waste liquid comprising magnesium chloride, and

a second extraction comprising extracting the lactic acid from the organic lactic acid solution into an aqueous liquid, thereby obtaining an aqueous lactic acid solution and a second organic liquid.

2. Method according to claim 1 , wherein the aqueous mixture comprises at least 15 wt. % dissolved magnesium chloride, based on the total weight of water and dissolved material in the aqueous mixture.

3. Method according to claim 1 , wherein the organic solvent is a C5+ ketone.

4. Method according to claim 3 , wherein the solvent is a C5-C8 ketone.

5. Method according to claim 1 , wherein the first extraction is conducted at a temperature of at least 30° C.

6. Method according to claim 1 , wherein the second extraction is conducted at a lower temperature than a temperature at which the first extraction is conducted.

7. Method according to claim 6 , wherein the second extraction is conducted at a temperature 10° C. to 50° C. lower than the temperature at which the first extraction is conducted.

8. Method according to claim 1 , wherein the second extraction is conducted within 10° C. of a temperature at which the first extraction is conducted.

9. Method according to claim 1 , wherein the first organic liquid comprises substantially no extractants.

10. Method according to claim 1 , wherein the first organic liquid is essentially free of amines, ethers, and alcohols, which means that these compounds, if present at all, are each present in an amount of less than 2 wt. %, calculated on the weight of the organic liquid.

11. Method according to claim 1 , wherein the aqueous mixture has a pH of 2 or lower.

12. Method according to claim 1 , which further comprises

subjecting the aqueous waste liquid comprising magnesium chloride to a thermal decomposition step at a temperature of at least 300° C., thereby decomposing the magnesium chloride salt to a magnesium oxide and HCl; and

dissolving the HCl formed in the thermal decomposition step in water, thereby obtaining a HCl solution; and

optionally recycling the magnesium oxide in a fermentation process as a neutralizing agent or precursor thereof.

13. Method according to claim 1 , further comprising a fermentation step to form the lactic acid, which fermentation process comprises the steps of fermenting a carbon source by means of a micro-organism in a fermentation broth to form lactic acid and neutralizing at least part of the lactic acid by adding a magnesium base, thereby obtaining the corresponding lactate.

14. Method according to claim 1 , wherein the method further comprises the step of

preparing an aqueous mixture by acidifying a lactate salt with an acid, thereby obtaining an aqueous mixture.

15. Method according to claim 14 , wherein the lactate salt is acidified with HCl and further comprising the step of concentrating the thus obtained aqueous mixture prior to extraction to a dissolved salt concentration of at least 5 wt. %, based on the total weight of water and dissolved material in the aqueous mixture.

16. Method according to claim 1 , wherein the aqueous mixture comprises at least 20 wt. % dissolved magnesium chloride based on the total weight of water and dissolved material in the aqueous mixture.

17. Method according to claim 1 , wherein the method further comprises a step of preparing the aqueous mixture by acidifying a mixture of lactic acid and magnesium lactate salt with HCl.

18. Method according to claim 1 , further comprising subjecting the magnesium chloride solution to a thermal decomposition step at a temperature of at least 300° C., thereby decomposing the MgCl 2 to magnesium oxide (MgO) and HCl.

19. Method according to claim 18 , wherein the MgO is recycled for use in a fermentation process as a neutralizing agent.

20. Method according to claim 19 , further comprising bringing the MgO into contact with water, thereby obtaining Mg(OH) 2 , which is recycled for use in a fermentation process as a neutralizing agent.

21. Method according to claim 18 , wherein said HCl obtained in the thermal decomposition step is used in an acidifying step either as HCl gas or as an aqueous HCl solution, said solution being obtained through dissolving the HCl formed in the thermal decomposition step in water.

22. Method for recovering lactic acid from an aqueous mixture comprising the steps of

providing an aqueous mixture comprising lactic acid and at least 5 wt. % dissolved magnesium chloride, based on the total weight of water and dissolved material in the aqueous mixture,

a first extraction comprising extracting the lactic acid from the aqueous mixture into a first organic liquid comprising at least 90 wt. % of an organic solvent selected from the group consisting of C5+ ketones, diethylether and methyl-tertiary-butyl-ether, thereby obtaining an organic lactic acid solution and an aqueous waste liquid comprising magnesium chloride, wherein the first extraction is conducted at a temperature of at least 30° C., and

a second extraction comprising extracting the lactic acid from the organic lactic acid solution into an aqueous liquid, thereby obtaining an aqueous lactic acid solution and a second organic liquid, wherein the second extraction is conducted at a temperature 10° C. to 50° C. lower than the temperature at which the first extraction is conducted.

Assignments (3)
CORRECTIVE ASSIGNMENT TO CORRECT THE 3RD INVENTOR'S NAME PREVIOUSLY RECORDED AT REEL: 033256 FRAME: 0540. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Jul 17, 2014
From: DE HAAN, ANDRÉ BANIER; VAN KRIEKEN, JAN; DEKIC ZIVKOVIC, TANJA
To: PURAC BIOCHEM BV
Reel/Frame 033350/0722 →
CORRECTIVE ASSIGNMENT TO CORRECT THE 3RD INVENTOR'S NAME PREVIOUSLY RECORDED AT REEL: 033131 FRAME: 0443. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Jun 30, 2014
From: DE HAAN, ANDRE BANIER; VAN KRIEKEN, JAN; DEKIC ?IVKOVIC, TANJA
To: PURAC BIOCHEM BV
Reel/Frame 033256/0540 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 18, 2014
From: DE HAAN, ANDRÉ BANIER; VAN KRIEKEN, JAN; ÐEKIC ?IVKOVIC, TANJA
To: PURAC BIOCHEM BV
Reel/Frame 033131/0443 →
Priority Claims (1)
EP 11195691 · Dec 23, 2011 · regional
Continuity (2)
Provisional Application 61579730 · Dec 23, 2011
Related Publication 20140335581A1 · Nov 13, 2014
Cited By (1)
US 12,486,212