Method and system for extracting long chain dicarboxylic acid

Patent metadata

Field	Value
Publication number	US-11999689-B2
Application number	US-202117551333-A
Country	US
Kind code	B2
Filing date	Dec 15, 2021
Priority date	Dec 19, 2019
Publication date	Jun 4, 2024
Grant date	Jun 4, 2024

Abstract

The present disclosure provides a method for extracting long chain dicarboxylic acid, the method comprising: (1) subjecting a long chain dicarboxylic acid fermentation broth to a primary membrane filtration treatment to give a first filtrate; subjecting the first filtrate to decolorization, crystallization, and solid-liquid separation to give a first solid; (2) redissolving the first solid in water to form a solution; subjecting the solution to decolorization, crystallization by acidification, and solid-liquid separation to give a second solid. By the method, the resulted long chain dicarboxylic acid product has a high purity and no residual organic solvent.

First claim

The invention claimed is:

1. A method for extracting long chain dicarboxylic acid, comprising:
(1) subjecting a long chain dicarboxylic acid fermentation broth to a primary membrane filtration treatment to give a first filtrate; subjecting the first filtrate to decolorization, crystallization, and solid-liquid separation to give a first solid;
(2) redissolving the first solid in water to form a solution;
(3) subjecting the solution to a secondary membrane filtration treatment to form a second filtrate;
(4) subjecting the second filtrate to decolorization, crystallization by acidification, and solid-liquid separation to give a second solid,
wherein the secondary membrane filtration is microfiltration membrane filtration using a micromembrane with a pore size of the microfiltration membrane of 0.01-1 μm or ultrafiltration membrane filtration using an ultrafiltration membrane with a cut-off molecular weight of 2000-50000 Da; and the concentration of the filtrate after the secondary membrane filtration is controlled to be 2 to 10 wt % calculated as the long chain dicarboxylic acid.

2. The method according to claim 1 , further comprising step (5) of mixing the second solid and water to form a mixture, subjecting the mixture to a thermostatic treatment at a temperature of 80 to 150° C., preferably 95 to 150° C., more preferably 105 to 150° C., followed by cooling for crystallization, and solid-liquid separation.

3. The method according to claim 1 , wherein the crystallization in step (1) is selected from any one of crystallization by acidification, cooling for crystallization, and evaporation for crystallization.

4. The method according to claim 3 , wherein the pH value of the solution to be crystallized is adjusted to 2 to 5.5, preferably 2.5 to 4 during the crystallization by acidification; and/or
the final temperature of the cooling for crystallization is 25 to 65° C., preferably 25 to 48° C.

5. The method according to claim 1 , wherein in step (1), prior to the primary membrane filtration, the pH of the long-chain dicarboxylic acid fermentation broth is controlled to be 6.0 to 12; and/or
the primary membrane filtration in step (1) is microfiltration membrane filtration or ultrafiltration membrane filtration; and/or
the filtration membrane for primary membrane filtration in step (1) includes a ceramic membrane, polypropylene membrane, polysulfone membrane, polyether sulfone membrane; and/or
the temperature for the primary membrane filtration in step (1) is 50 to 100° C., and the pressure difference across the membrane is 0.05 to 0.6 MPa; and/or
the concentration of the filtrate after the primary membrane filtration in step (1) is controlled to be 2 to 10 wt %; and/or,
in step (1) and step (2), the temperature for the decolorization is 50 to 100° C.; and/or,
in step (1) and step (2), the solid-liquid separation may be centrifugal separation, filtration separation; and/or,
in step (2), a base may be added to promote the dissolution of the first solid during the process of redissolving the first solid in water to form a solution; and/or,
in step (2), the pH value of the solution to be crystallized is adjusted to 2 to 5.5, preferably 2.5 to 4, during the crystallization by acidification.

6. The method according to claim 1 , wherein, in step (2), subjecting said second filtrate to a tertiary membrane filtration prior to said decolorization to form a third filtrate, said third filtrate is used to perform decolorization in step (2); and/or
in step (2), a tertiary membrane filtration is carried out after the decolorization and before the crystallization by acidification to form a third filtrate, said third filtrate is used to perform the crystallization by acidification.

7. The method according to claim 1 , wherein the temperature for the secondary membrane filtration is 20 to 100° C.

8. The method according to claim 6 , wherein the tertiary membrane filtration is microfiltration membrane filtration or ultrafiltration membrane filtration; and/or,
the temperature for the tertiary membrane filtration is 20 to 100° C., preferably 20 to 45° C.; and/or
the concentration of the filtrate after the tertiary membrane filtration is controlled to be 2 to 10 wt %.

9. The method according to claim 2 , wherein, in step (5), the mass ratio of the second solid to water is 1:(2 to 10), preferably 1:(3 to 15), more preferably 1:(3 to 10); and/or
in step (5), the temperature for the thermostatic treatment is 120 to 140° C.; and/or
the final temperature of the cooling for crystallization is 25 to 65° C.

10. The method according to claim 1 , wherein, in step (5), after the thermostatic treatment, the mixture is first cooled to 97 to 115° C., the average cooling rate is 0.5 to 12° C./h, preferably 0.5 to 8° C./h; cooled further to 85 to 95° C., the average cooling rate is 2 to 15° C./h, preferably 2 to 8° C./h; and then cooled to the final temperature.

11. The method according to claim 9 , wherein, in step (5), after the thermostatic treatment, the mixture is first cooled to 97 to 115° C., the average cooling rate is 0.5 to 12° C./h, preferably 0.5 to 8° C./h; cooled further to 85 to 95° C., the average cooling rate is 2 to 15° C./h, preferably 2 to 8° C./h; and then cooled to the final temperature.

12. The method according to claim 6 , comprising a fourth membrane filtration after the tertiary membrane filtration, the fourth membrane filtration is microfiltration membrane filtration or ultrafiltration membrane filtration.

13. The method according to claim 1 , wherein the long-chain dicarboxylic acid is a C 9 -C 18 dicarboxylic acid.

14. A long-chain dicarboxylic acid product, extracted by the method according to claim 1 .

Assignees

• Cathay Biotech Inc
• Cibt America Inc
• Cathay Jinxiang Biomaterial Co Ltd

Inventors

• Yang Chen
• Zhang Shuhua
• Yang Yufeng
• Liu Xiucai

Classifications

• C07C51/43 Primary

  by change of the physical state, e.g. crystallisation · CPC title

• C07C55/02

  Dicarboxylic acids · CPC title

• C07B2200/13

  Crystalline forms, e.g. polymorphs · CPC title

• C07C51/47

  by solid-liquid treatment; by chemisorption · CPC title