IP Library Granted Patent US 10,807,937
Granted Patent B2
US 10,807,937 · App. 16/339,756 · Granted Oct 20, 2020

Solid-solid separation process for long chain dicarboxylic acids

Inventors: Bingbing Qin (Shanghai, CN); Yufeng Yang (Shanghai, CN); Xiucai Liu (Shanghai, CN)
Assignees: CATHAY BIOTECH INC.; CIBT AMERICA INC.
C07C51/43C07C51/02C07C51/347C07C51/42C07C55/21C12P7/44C12P7/6409
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Quick Facts
Patent No.
US 10,807,937
App. No.
16/339,756
Granted
Oct 20, 2020
Kind
B2
Abstract

The present disclosure provides a method for isolating a long chain dicarboxylic acid from fermentation broth containing microbial cells. Also provided is a substantially pure long chain dicarboxylic acid isolated by the method.

Claims (29)

1. A method for isolating a long chain dicarboxylic acid from a fermentation broth containing microbial cells, the method comprising:

(a) adding an acid to the fermentation broth to produce a demulsified fermentation broth having a pH of 6 or less;

(b) centrifuging the demulsified fermentation broth using a hydraulic cyclone centrifuge, a hydrocyclone centrifuge, a horizontal spiral centrifuge, or any combination thereof to generate a first phase comprising the long chain dicarboxylic acid and a second phase comprising the microbial cells; and

(c) isolating the long chain dicarboxylic acid from the first phase by filtration to recover an isolated long chain dicarboxylic acid product.

2. The method of claim 1 , wherein the first phase is substantially free of the microbial cells.

3. The method of claim 1 or 2 , wherein the second phase is substantially free of the long chain dicarboxylic acid.

4. The method of claim 1 or 2 , wherein the fermentation broth is a sterilized fermentation broth.

5. The method of claim 1 or 2 , further comprising heating the fermentation broth to a temperature from about 90° C. to about 105° C. prior to step (a).

6. The method of claim 1 or 2 , further comprising heating the demulsified fermentation broth to a temperature from about 90° C. to about 105° C. prior to step (b).

7. The method of claim 5 , further comprising cooling the demulsified fermentation broth to a temperature from about 30° C. to about 80° C. after heating.

8. The method of claim 1 or 2 , wherein the acid is selected from the group consisting of sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, trifluoromethane sulfonic acid, and any combination thereof.

9. The method of claim 1 or 2 , wherein the acid is sulfuric acid.

10. The method of claim 1 or 2 , wherein the demulsified fermentation broth has a pH of 2-5.

11. The method of claim 10 , wherein the pH is pH 2.5-4.

12. The method of claim 1 or 2 , wherein the demulsified fermentation broth has a viscosity of about 5 centipoise (cp)-about 200 cp.

13. The method of claim 1 or 2 , wherein centrifuging comprises sequential centrifugation.

14. The method of claim 1 or 2 , further comprising drying the isolated long chain dicarboxylic acid.

15. The method of claim 1 or 2 , wherein the isolated long chain dicarboxylic acid has a purity of at least 95% or higher.

16. The method of claim 15 , wherein the isolated long chain dicarboxylic acid has a purity of at least 97% or higher.

17. The method of claim 1 or 2 , wherein the long chain dicarboxylic acid is a saturated or unsaturated straight chain dicarboxylic acid having 9 to 18 carbon atoms, with a carboxyl group at each of the two ends of the chain.

18. The method of claim 17 , wherein the long chain dicarboxylic acid is a saturated or unsaturated straight chain dicarboxylic acid having 11 to 14 carbon atoms, with a carboxyl group at each of the two ends of the chain.

19. The method of claim 17 , wherein the long chain dicarboxylic acid is selected from the group consisting of a nonanedioic acid, decanedioic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, 9-ene-octadecanedioic acid, and any combination thereof.

20. The method of claim 19 , wherein the long chain dicarboxylic acid is selected from the group consisting of an undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, and any combination thereof.

21. A method for isolating a long chain dicarboxylic acid from a fermentation broth containing microbial cells, the method comprising:

(a) adding sulfuric acid to the fermentation broth to produce a demulsified fermentation broth having a pH of 2.5-4;

(b) heating the demulsified fermentation broth to a temperature from 90° C. to 105° C.;

(c) centrifuging the demulsified fermentation broth using a hydraulic cyclone centrifuge, a hydrocyclone centrifuge, a horizontal spiral centrifuge, or any combination thereof to generate a first phase comprising the long chain dicarboxylic acid and a second phase comprising the microbial cells, wherein the first phase is substantially free of the microbial cells and the second phase is substantially free of the long chain dicarboxylic acid; and

(d) isolating the long chain dicarboxylic acid from the first phase by filtration to recover an isolated long chain dicarboxylic acid.

22. The method of claim 6 , further comprising cooling the demulsified fermentation broth to a temperature from about 30° C. to about 80° C. after heating.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 3, 2020
From: CATHAY R&D CENTER CO., LTD
To: CATHAY BIOTECH INC.
Reel/Frame 054261/0154 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 10, 2019
From: CATHAY R&D CENTER CO., LTD.
To: CATHAY BIOTECH INC.
Reel/Frame 050328/0834 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 10, 2019
From: CATHAY INDUSTRIAL BIOTECH LTD.
To: CIBT AMERICA INC.
Reel/Frame 050329/0008 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 7, 2019
From: QIN, BINGBING; YANG, YUFENG; LIU, XIUCAI
To: CATHAY BIOTECH R&D CENTER LTD.; CATHAY INDUSTRIAL BIOTECH LTD.
Reel/Frame 049099/0326 →
Continuity (1)
Related Publication 20190248726A1 · Aug 15, 2019