Acid/salt separation

Patent metadata

Field	Value
Publication number	US-9550712-B2
Application number	US-201214238686-A
Country	US
Kind code	B2
Filing date	Aug 16, 2012
Priority date	Aug 16, 2011
Publication date	Jan 24, 2017
Grant date	Jan 24, 2017

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 preparing 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;
acidifying the magnesium carboxylate with hydrogen chloride (HCl), thereby obtaining a solution comprising carboxylic acid and magnesium chloride (MgCl 2 );
concentrating the solution comprising carboxylic acid and MgCl 2 ; and
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, wherein
the carboxylic acid is selected from the group consisting of adipic acid, itaconic acid, 2,5-furandicarboxylic acid, fumaric acid, maleic acid, glutaric acid, malonic acid, oxalic acid and fatty acids having more than 10 carbon atoms,
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.

2. 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.

3. The method according to claim 2 , wherein thermal decomposition is conducted using a spray roaster.

4. The method according to claim 2 , wherein the thermal decomposition is conducted at a pressure of ranging from 0.1-10 bar.

5. The method according to claim 2 , wherein the thermal decomposition is conducted at a temperature ranging from 300-450° C.

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

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

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

9. 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.

10. The method according to claim 9 , wherein the second precipitation is conducted by cooling and/or concentrating the MgCl 2 solution.

11. The method according to claim 9 , wherein additional MgCl 2 is added to the MgCl 2 solution prior to the second precipitation.

12. 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 .

13. The method according to claim 1 , wherein the carboxylic acid has a solubility in water of less than 60 g/100 g water at 20° C.

14. 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.

15. The method according to claim 1 , wherein magnesium carboxylate is acidified with an HCl solution.

16. The method according to claim 1 , wherein the magnesium carboxylate is provided in dissolved form, as part of an aqueous solution or as part of an aqueous suspension.

17. The method according to claim 1 , wherein the magnesium carboxylate is obtained in a fermentation process, which process comprises a purification step, wherein magnesium carboxylate is crystallized from the fermentation broth and then optionally dissolved in water to form an aqueous solution.

18. The method according to claim 1 , wherein the magnesium carboxylate is obtained in a fermentation process in dissolved form, which process comprises a purification step, wherein the carboxylic acid is neutralized by adding a magnesium base, during which step magnesium carboxylate remains in dissolved form.

19. A method for preparing a carboxylic acid, comprising:
providing magnesium carboxylate, in dissolved form, as part of an aqueous solution or suspension, 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 hydrogen chloride (HCl), thereby obtaining a solution comprising carboxylic acid and magnesium chloride (MgCl 2 );
concentrating the solution comprising carboxylic acid and MgCl 2 to a carboxylic acid concentration that is equal or up to 10 g/L lower than the saturation point of the carboxylic acid; and
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.

20. The method according to claim 19 , 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.

Assignees

• De Haan André Banier
• Van Breugel Jan
• Van Der Weide Paulus Loduvicus Johannes
• Jansen Peter Paul
• Vidal Lancis José María
• Cerdà Baró Augustín
• Purac Biochem Bv

Inventors

• De Haan André Banier
• Van Breugel Jan
• Van Der Weide Paulus Loduvicus Johannes
• Jansen Peter Paul
• Vidal Lancis José María
• Cerdà Baró Augustín

Classifications

• C01F5/30

  Chlorides · CPC title

• C07C51/42

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

• C07C51/02 Primary

  from salts of carboxylic acids · CPC title

• C01F5/06

  by thermal decomposition of magnesium compounds (calcining magnesite or dolomite C04B2/10) · CPC title

• C07C51/43

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