Acid/salt separation

Patent metadata

Field	Value
Publication number	US-10071948-B2
Application number	US-201615378888-A
Country	US
Kind code	B2
Filing date	Dec 14, 2016
Priority date	Aug 16, 2011
Publication date	Sep 11, 2018
Grant date	Sep 11, 2018

Abstract

The invention provides a method for preparing a carboxylic acid, which method includes the steps of providing magnesium carboxylate, wherein the carboxylic acid corresponding with the carboxylate has a solubility in water at 20° C. of 80 g/100 g water or less; acidifying the magnesium carboxylate with HCl, thereby obtaining a solution comprising carboxylic acid and magnesium chloride (MgCl 2 ); optionally a concentration step, wherein the solution comprising carboxylic acid and MgCl 2 is concentrated; precipitating the carboxylic acid from the solution comprising the carboxylic acid and MgCl 2 , thereby obtaining a carboxylic acid precipitate and a MgCl 2 solution.

First claim

The invention claimed is:

1. A method for the recovery of a carboxylic acid, comprising:
providing an aqueous solution or suspension of magnesium carboxylate, wherein the carboxylic acid corresponding with the carboxylate has a solubility in water at 20° C. of 80 g/100 g water or less;
obtaining solid magnesium carboxylate from the solution or suspension, dissolving the solid magnesium carboxylate in water to create an aqueous solution, and acidifying the obtained aqueous solution of magnesium carboxylate with a solution of hydrogen chloride (HCl), thereby obtaining a solution comprising carboxylic acid and magnesium chloride (MgCl 2 );
optionally a concentration step, wherein the solution comprising carboxylic acid and MgCl 2 is concentrated; and,
precipitating carboxylic acid from the solution comprising carboxylic acid and MgCl 2 , thereby obtaining a carboxylic acid precipitate and a MgCl 2 solution.

2. The method according to claim 1 , wherein the carboxylic acid has a solubility in water at 20° C. that is lower than that of MgCl 2 .

3. The method according to claim 1 , wherein the carboxylic acid has a solubility in water of less than 30 g/100 g water.

4. The method of claim 1 , wherein the carboxylic acid is selected from the group consisting of adipic acid, itaconic acid, 2,5-furandicarboxylic acid, fumaric acid, oxalic acid, maleic acid, glutaric acid, malonic acid, and fatty acids having more than 10 carbon atoms.

5. The method according to claim 1 , wherein:
the aqueous solution or aqueous suspension comprises at least 10 wt. % magnesium carboxylate, based on the total weight of the solution or suspension; and,
the solution comprising the carboxylic acid and MgCl 2 comprises at least 5 wt. % of magnesium chloride based on the total weight of the solution comprising carboxylic acid.

6. The method according to claim 1 , wherein magnesium carboxylate is provided in dissolved form, as part of an aqueous solution obtained in a fermentation process or as part of an aqueous suspension obtained in a fermentation process.

7. The method according to claim 6 , wherein the magnesium carboxylate is provided in dissolved form as part of an aqueous suspension obtained in a fermentation process by neutralization of carboxylic acid with a magnesium base and wherein, in the aqueous suspension, at least 95 wt. % of the magnesium carboxylate is in dissolved form.

8. The method according to claim 7 , wherein the aqueous suspension consists of dissolved magnesium carboxylate and insoluble biomass.

9. The method according to claim 1 , wherein the aqueous solution or suspension of magnesium carboxylate provided in the providing step is concentrated by evaporation to obtain the solid magnesium carboxylate.

10. The method according to claim 9 , wherein, in the obtaining solid magnesium carboxylate from the solution or suspension step, the concentrated solution or suspension of magnesium carboxylate is subjected to solid-liquid separation.

11. The method according to claim 1 , wherein acidifying the magnesium carboxylate and precipitating the carboxylic acid thus formed are conducted in one step.

12. The method according to claim 1 , wherein the MgCl 2 solution or concentrated MgCl 2 solution is subjected to a second precipitation step to recover at least part of the carboxylic acid remaining in the MgCl 2 solution obtained in the first precipitation step.

13. The method according to claim 12 , wherein the second precipitation is conducted by cooling and/or concentrating the MgCl 2 solution.

14. The method according to claim 12 , wherein additional MgCl 2 is added to the MgCl 2 solution prior to the second precipitation.

15. The method according to claim 1 , wherein the solution comprising the carboxylic acid and MgCl 2 is concentrated to a carboxylic acid concentration that is equal or up to 10 g/L lower than the saturation point of the carboxylic acid.

16. The method according to claim 1 , wherein the solution comprising the carboxylic acid and MgCl 2 is concentrated to a carboxylic acid concentration that is equal or up to 5 g/L lower than the saturation point of the carboxylic acid.

17. The method according to claim 1 , further comprising:
subjecting the MgCl 2 solution to a thermal decomposition step at temperatures of at least 300° C., thereby decomposing the MgCl 2 to magnesium oxide (MgO) and HCl;
dissolving the HCl formed in the thermal decomposition step in water, thereby obtaining a HCl solution; and
bringing the MgO in contact with water, thereby obtaining Mg(OH) 2 , which Mg(OH) 2 is optionally recycled for use in a fermentation process.

18. The method according to claim 17 , wherein thermal decomposition is conducted using a spray roaster.

19. The method according to claim 17 , wherein the thermal decomposition is conducted at a pressure in a range of from 0.1-10 bar.

20. The method according to claim 17 , wherein the thermal decomposition is conducted at a temperature ranging from 300-450° C.

21. The method according to claim 17 , wherein Mg(OH) 2 is converted to MgCO 3 , which is then used as a neutralizing agent in a fermentation process.

22. The method according to claim 17 , wherein thermal decomposition is conducted by spraying the MgCl 2 solution into contact with a stream of hot gas.

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

24. The method according to claim 23 , wherein the HCl obtained in the thermal decomposition step is used in the acidifying step either as HCl gas or as an aqueous HCl solution, the solution being obtained through dissolving the HCl formed in the thermal decomposition step in water.

25. The method according to claim 23 , wherein at least a part of the MgO is recycled for use in a fermentation process.

26. The method according to claim 23 , further comprising bringing at least a part of the MgO in contact with water, thereby obtaining Mg(OH) 2 .

27. The method according to claim 26 , wherein at least a part of the Mg(OH) 2 is recycled for use in a fermentation process.

28. The method according to claim 23 , further comprising
bringing at least a part of the MgO in contact with water, thereby obtaining Mg(OH) 2 ; and,
converting at least a part of the Mg(OH) 2 to MgCO 3 , which is then used as a neutralizing agent in a fermentation process.

29. The method according to claim 6 , wherein the aqueous solution obtained in the fermentation process or suspension obtained in the fermentation process further comprises the carboxylic acid.

30. The method according to claim 6 , wherein the magnesium carboxylate is provided in dissolved form as part of an aqueous suspension obtained in a fermentation process by neutralization of carboxylic acid with a magnesium base, and wherein the aqueous suspension comprises up to 10 wt. % solids.

Assignees

• Purac Biochem Bv

Inventors

• De Haan André Banier
• Van Breugel Jan
• Van Der Weide Paulus Loduvicus Johannes
• Jansen Peter Paul
• VIDAL LANCIS José Maria
• Cerdà Baró Agustín

Classifications

• C07D307/60

  Two oxygen atoms, e.g. succinic anhydride · CPC title

• C01F5/10

  by thermal decomposition of magnesium chloride with water vapour · CPC title

• C01B7/035

  Preparation of hydrogen chloride from chlorides · CPC title

• C01F5/16

  by treating magnesia, e.g. calcined dolomite, with water or solutions of salts not containing magnesium · CPC title

• C07C51/42

  Separation; Purification; Stabilisation; Use of additives · CPC title