Recovery of acetic acid from a fermentation broth

• US 4,405,717 A
• Filed: 10/26/1981
• Issued: 09/20/1983
• Est. Priority Date: 10/26/1981
• Status: Expired due to Term

• Current Assignee: Michigan Biotechnology Institute A Michigan Not-Profit Corporation
• Original Assignee: CPC International, Inc. (Unilever PLC)
• Inventors: Urbas, Branko
• Primary Examiner(s): BASCOMB JR, WILBUR
• Application Number:
  US06/314,627
• Time in Patent Office: 694 Days
• Field of Search: 435/140, 435/141, 435/842, 426/17, 562/513, 562/608, 203/16, 203/43, 203/59, 203/38, 203/33, 159/47 R
• US Class Current: 435/140
• CPC Class Codes: C07C 51/487 by treatment giving rise to chemical modification by chemisorption C07C51/47
• CPC Class Codes: C07C 53/08 Acetic acid pyroligneous acid C10C; preparation of vinegar C12J
• CPC Class Codes: Y10S 435/842 Clostridium

Abstract

A process is provided for the recovery of acetic acid from dilute aqueous solutions. The acid in the form of its calcium salt is treated with a tertiary amine carbonate and the resulting trialkylammonium acetate is isolated and heated to give the acetic acid plus a tertiary amine.

Claims

1. A process for the recovery of acetic acid from an aqueous solution of clacium acetate which comprises the steps of:

(a) adding a molar equivalent of a water-soluble tertiary amine carbonate to the calcium acetate solution to form a trialkylammonium acetate solution and a precipitate of calcium carbonate;

(b) concentrating the trialkylammonium acetate solution; and

(c) heating the concentrated trialkylammonium acetate solution to obtain acetic acid and the tertiary amine.

2. The process of claim 1 wherein the tertiary amine is tributylamine.

3. The process of claim 1 wherein the tertiary amine is dicyclohexylmethylamine.

4. The process of claim 1, 2 or 3 wherein the trialkylammonium acetate is concentrated by extraction with a solvent.

5. The process of claim 4 wherein the precipitated calcium carbonate is separated from the solution of trialkylammonium acetate before said acetate is extracted with a solvent.

6. The process of claim 4 wherein the solvent is chloroform.

7. The process of claim 4 wherein the solvent is distilled from the extract of trialkylammonium acetate before the acetate is heated to obtain acetic acid and the tertiary amine.

8. The process of claim 1 wherein the tertiary amine carbonate used in Step (a) is generated in situ by first adding to the calcium acetate solution a molar equivalent of a tertiary amine that forms a water-soluble carbonate and then adding sufficient carbon dioxide to dissolve the amine and to precipitate the calcium as calcium carbonate.

9. The process of claim 1 wherein the tertiary amine obtained in Step (c) is converted to a tertiary amine carbonate and recycled to Step (a).

10. A process for the recovery of acetic acid from a fermentation reaction which comprises:

(a) converting of the acetic acid to calcium acetate;

(b) adding a molar equivalent of a water-soluble tertiary amine carbonate to the calcium acetate solution to form a trialkylammonium acetate solution and a precipitate of calcium carbonate;

(c) concentrating the trialkylammonium acetate solution; and

(d) heating the concentrated trialkylammonium acetate solution to obtain acetic acid and the tertiary amine.

11. The process of claim 10 wherein the tertiary amine carbonate used in Step (b) is generated in situ by first adding to the calcium acetate solution a molar equivalent of a tertiary amine that forms a water-soluble carbonate and then adding sufficient carbon dioxide to dissolve the amine and to precipitate the calcium as calcium carbonate.

12. The process of claim 10 wherein the tertiary amine obtained in Step (d) is converted to a tertiary amine carbonate and recycled to Step (b).

13. The process of claim 10 wherein the calcium carbonate obtained in Step (b) is added to the fermentation reaction to convert the acetic acid to calcium acetate.

14. The process of claim 10 wherein the fermentation broth is one in which is grown a strain of Clostridium thermoaceticum.

15. The process of claim 10 wherein the tertiary amine is tributylamine.

16. The process of claim 10 wherein the tertiary amine is dicyclohexylmethylamine.

17. The process of claim 10, 15 or 16 wherein the trialkylammonium acetate is concentrated by extraction with a solvent.

18. The process of claim 17 wherein the solvent is distilled from the extract of trialkylammonium acetate before the acetate is heated to obtain acetic acid and the tertiary amine.

19. The process of claim 17 wherein the precipitated calcium carbonate is separated from the solution of trialkylammonium acetate before said acetate is extracted with a solvent.

20. The process of claim 17 wherein the solvent is chloroform.