Method for processing magnesium chloride solutions

Patent metadata

Field	Value
Publication number	US-10106821-B2
Application number	US-201414902374-A
Country	US
Kind code	B2
Filing date	Jul 2, 2014
Priority date	Jul 3, 2013
Publication date	Oct 23, 2018
Grant date	Oct 23, 2018

Abstract

A method for processing MgCl2 solutions including the steps of: providing an aqueous solution including 5-25 wt. % of MgCl2 and optionally organic contaminants to a step, wherein water and present, organic components are evaporated; withdrawing aqueous solution with a MgCl2 concentration of 25-35 wt. % from an evaporation step and providing it to a preconcentrator where it is contacted with a HCl containing gas stream at least 300° C.; providing aqueous solution with a MgCl2 concentration of 35-45 wt. % resulting from the preconcentrator to a thermohydrolysis reactor, being at at least 300° C.; withdrawing MgO from the thermohydrolysis reactor in solid form, and withdrawing a HCl containing gas stream from the thermohydrolysis reactor, said HCl-containing gas stream at least 300° C.; providing the HCl-containing gas stream with at least 300° C. to the preconcentrator; withdrawing a HCl-containing gas stream with a temperature of at most 150° C. from the preconcentrator.

First claim

The invention claimed is:

1. Method for processing magnesium chloride solutions comprising the steps of
providing an aqueous solution comprising 5-25 wt. % of magnesium chloride and organic contaminants to an evaporation step, wherein water and organic components are evaporated, wherein the product resulting from the evaporation step has a total organic compounds (TOC) which is at most 50% of the TOC of the aqueous solution provided to the evaporation step,
withdrawing an aqueous solution with a magnesium chloride concentration of 25-35 wt. % from the evaporation step and providing it to a preconcentrator where it is contacted with a HCl containing gas stream with a temperature of at least 300° C.,
providing an aqueous solution with a magnesium chloride concentration of 35-45 wt. % resulting from the preconcentrator to a thermohydrolysis reactor, the reactor being at a temperature of at least 300° C.,
withdrawing MgO from the thermohydrolysis reactor in solid form, and withdrawing a HCl containing gas stream from the thermohydrolysis reactor, said HCl-containing gas stream having a temperature of at least 300° C.,
providing the HCl-containing gas stream with a temperature of at least 300° C. to the preconcentrator,
withdrawing a HCl-containing gas stream with a temperature of at most 150° C. from the preconcentrator.

2. Method according to claim 1 , wherein the aqueous solution comprising magnesium chloride has a TOC of at least 1000 ppm.

3. Method according to claim 1 , wherein the product resulting from the evaporation step has a TOC which is at most 30% of the TOC of the aqueous solution provided to the evaporation step.

4. Method according to claim 1 , wherein the product resulting from the evaporation step which is provided to the preconcentrator has a TOC of at most 1000 ppm.

5. Method according to claim 1 , wherein the concentration increase effected during the evaporation step before the preconcentrator, defined as [magnesium chloride prec]-[magnesium chloride start], is between 30 and 5 wt. %.

6. Method according to claim 1 , wherein the evaporation step is a single-stage evaporation step.

7. Method according to claim 1 , wherein the evaporation step is a multiple-stage evaporation step.

8. Method according to claim 7 , wherein in a first evaporation stage of the multiple-stage evaporation step, volatile organic compounds are removed, so that the concentrated product from the first evaporation stage has a total volatile organic compounds (VTOC) which is at most 50% of the VTOC of the aqueous solution provided to the first evaporation stage.

9. Method according to claim 7 , wherein steam is withdrawn from the first evaporation stage and provided as heating liquid to a further evaporation stage.

10. Method according to claim 9 , wherein the multiple-stage evaporation is carried out in a multiple-effect evaporator.

11. Method according to claim 1 , wherein vapor-compression evaporation is used in the evaporation step or in one or more stages thereof.

12. Method according to claim 1 , wherein the magnesium chloride solution is derived from a process comprising
subjecting a carbon source to a fermentation step to form a carboxylic acid, which fermentation step comprises the steps of fermenting a carbon source by means of a micro-organism in a fermentation broth to form carboxylic acid and neutralizing at least part of the carboxylic acid by adding a magnesium base selected from magnesium oxide and magnesium hydroxide, thereby obtaining a magnesium carboxylate,
subjecting the magnesium carboxylate to an acidification step wherein the magnesium carboxylate is contacted with HCl in an aqueous environment to form an aqueous mixture comprising carboxylic acid and magnesium chloride,
subjecting the aqueous mixture comprising carboxylic acid and magnesium chloride to a separation step, to form (1) an effluent comprising carboxylic acid and (2) a magnesium chloride solution.

13. Method according to claim 12 further comprising
recycling the organic components evaporated during the evaporation step at least in part to the separation step, and/or
recycling the magnesium oxide withdrawn from the thermohydrolysis reactor at least in part to the fermentation step, and/or
recycling the HCl-containing gas stream derived from the preconcentrator at least in part to the acidification step.

14. Method according to claim 12 , wherein the method further comprises
recycling the organic components evaporated during the evaporation step at least in part to the separation step, and
recycling the magnesium oxide withdrawn from the thermohydrolysis reactor at least in part to the fermentation step, and
recycling the HCl-containing gas stream derived from the preconcentrator at least in part to the acidification step.

15. Method according to claim 12 , wherein the separation step encompasses an extraction step, wherein use is made of an organic extractant.

16. Method for manufacturing a carboxylic acid comprising
subjecting a carbon source to a fermentation step to form a carboxylic acid, which fermentation step comprises the steps of fermenting a carbon source by means of a micro-organism in a fermentation broth to form carboxylic acid and neutralizing at least part of the carboxylic acid by adding a magnesium base selected from magnesium oxide and magnesium hydroxide, thereby obtaining a magnesium carboxylate,
subjecting the magnesium carboxylate to an acidification step wherein the magnesium carboxylate is contacted with HCl in an aqueous environment to form an aqueous mixture comprising carboxylic acid and magnesium chloride,
subjecting the aqueous mixture comprising carboxylic acid and magnesium chloride to a separation step, to form (1) an effluent comprising carboxylic acid and (2) a magnesium chloride solution,
providing an aqueous solution comprising 5-25 wt. % of magnesium chloride and organic contaminants to an evaporation step, wherein water and organic components are evaporated, wherein the product resulting from the evaporation step has a total organic compounds (TOC) which is at most 50% of the TOC of the aqueous solution provided to the evaporation step,
withdrawing an aqueous solution with a magnesium chloride concentration of 25-35 wt. % from the evaporation step and providing it to a preconcentrator where it is contacted with a HCl containing gas stream with a temperature of at least 300° C.,
providing an aqueous solution with a magnesium chloride concentration of 35-45 wt. % resulting from the preconcentrator to a thermohydrolysis reactor, the reactor being at a temperature of at least 300° C.,
withdrawing MgO from the thermohydrolysis reactor in solid form, and withdrawing a HCl containing gas stream from the thermohydrolysis reactor, said HCl-containing gas stream having a temperature of at least 300° C.,
providing the HCl-containing gas stream with a temperature of at least 300° C. to the preconcentrator,
withdrawing a HCl-containing gas stream with a temperature of at most 150° C. from the preconcentrator,
wherein the carboxylic acid is derived from the effluent comprising carboxylic acid.

Assignees

• Purac Biochem Bv

Inventors

• De Vries Johannes Jeichienus
• Frediansyah Raymon
• De Haan André Banier

Classifications

• C07C51/02

  from salts of carboxylic acids · CPC title

• C12P7/40 Primary

  containing a carboxyl group {including Peroxycarboxylic acids} · CPC title

• C01F5/06

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

• C01B13/18

  by thermal decomposition of compounds, e.g. of salts or hydroxides · CPC title

• C07C51/412

  by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part · CPC title