Method for processing magnesium chloride solutions and method for manufacturing carboxylic acids

Patent metadata

Field	Value
Publication number	US-10850990-B2
Application number	US-201716068989-A
Country	US
Kind code	B2
Filing date	Jan 19, 2017
Priority date	Jan 19, 2016
Publication date	Dec 1, 2020
Grant date	Dec 1, 2020

Abstract

Magnesium chloride solutions including providing aqueous magnesium chloride solution with magnesium chloride concentration of 10-30 wt. % to concentration step where water is evaporated, resulting in concentrated magnesium chloride solution with magnesium chloride concentration of 30-50 wt. %, wherein concentration step is carried out in one or more stages, wherein at least one of the stages is conducted at elevated pressure, withdrawing concentrated magnesium chloride solution from concentration step, and providing it to thermohydrolysis reactor of at least 300° C., withdrawing MgO from thermohydrolysis reactor in solid form, and withdrawing a HCl containing gas stream of at least 300° C. from thermohydrolysis reactor, providing the HCl-containing gas stream of at least 300° C. to cooling step, where HCl-containing gas stream is contacted with cooling liquid, withdrawing HCl-containing gas stream below 150° C. from cooling step, circulating cooling liquid through heat exchanger where energy is transferred to heating liquid which circulates from heat exchanger to concentration step.

First claim

The invention claimed is:

1. Method for processing magnesium chloride solutions comprising the steps of
providing an aqueous magnesium chloride solution having a magnesium chloride concentration of 10-30 wt. % to a concentration step where water is evaporated with use of energy from a heating liquid, resulting in a concentrated magnesium chloride solution having a magnesium chloride concentration of 30-50 wt. %, wherein the concentration step is carried out in one or more stages, wherein at least one of the stages is conducted at elevated pressure,
withdrawing the concentrated magnesium chloride solution from the concentration step, and providing it 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 having a temperature of at least 300° C. from the thermohydrolysis reactor,
providing the HCl-containing gas stream having a temperature of at least 300° C. to a cooling step, where the HC1-containing gas stream is contacted with a cooling liquid,
withdrawing a HCl-containing gas stream having a temperature below 150° C. from the cooling step,
circulating the cooling liquid through a heat exchanger where energy from the cooling liquid is transferred to the heating liquid, which heating liquid then circulates from the heat exchanger to provide the energy to the concentration step.

2. Method according to claim 1 , wherein the concentration step is carried out in one or more stages, wherein at least one of the stages is conducted at a pressure of at least 1.1 bara and at most 10 bara.

3. Method according to claim 1 wherein the concentration step is carried out in multiple stages.

4. Method according to claim 3 wherein steam is withdrawn from a first concentration stage and provided as heating liquid to a further concentration stage.

5. Method according to claim 3 wherein the multiple stage concentration is carried out in a multiple-effect evaporator.

6. Method according to claim 1 wherein vapor-compression evaporation is used in the concentration step.

7. Method according to claim 1 wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a concentration of 30-48 wt. % and a temperature of 100-170° C.

8. Method according to claim 1 , wherein a temperature of the cooling liquid leaving the cooling step and before entering the heat exchanger is in the range of 90−150° C.

9. Method according to claim 1 wherein a temperature of the cooling liquid leaving the heat exchanger is at least 2° C. below the temperature of the cooling liquid entering the heat exchanger.

10. Method according to claim 1 wherein a temperature of the heating liquid entering the heat exchanger is in the range of 70−95° C.

11. Method according to claim 1 wherein a temperature of the heating liquid exiting the heat exchanger is at least 2° C. above the temperature of the heating liquid entering the heat exchanger.

12. Method according to claim 1 wherein the energy from the heating liquid is indirectly provided to the concentration step by circulating the heating liquid from the heat exchanger through a flash vessel, and the flash vessel supplies steam to at least one stage of the concentration step.

13. Method according to claim 7 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a concentration of 35-48 wt. %.

14. Method according to claim 13 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a concentration of 40-48 wt. %.

15. Method according to claim 14 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a concentration of 45-48 wt. %.

16. Method according to claim 7 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a temperature of 120-170° C.

17. Method according to claim 16 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a temperature of 130-170° C.

18. Method according to claim 17 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a temperature of 140-170° C.

19. Method according to claim 18 , wherein the magnesium chloride solution provided to the thermohydrolysis reactor has a temperature of 145-170° C.

20. Method according to claim 9 , wherein the temperature of the cooling liquid leaving the heat exchanger is at least 5° C. below the temperature of the cooling liquid entering the heat exchanger.

21. Method according to claim 20 , wherein the temperature of the cooling liquid leaving the heat exchanger is at least 10° C. below the temperature of the cooling liquid entering the heat exchanger.

22. Method according to claim 11 , wherein the temperature of the heating liquid exiting the heat exchanger is at least 5° C. above the temperature of the heating liquid entering the heat exchanger.

23. Method according to claim 22 , wherein the temperature of the heating liquid exiting the heat exchanger is at least 10° C. above the temperature of the heating liquid entering the heat exchanger.

24. Method for manufacture of carboxylic acid comprising the steps of
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 the group consisting of magnesium oxide, magnesium hydroxide, and a combination thereof, 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 an effluent comprising carboxylic acid and an aqueous magnesium chloride solution,
providing the aqueous magnesium chloride solution, having a magnesium chloride concentration of 10-30 wt. % to a concentration step where water is evaporated with use of energy from a heating liquid, resulting in a concentrated magnesium chloride solution having a magnesium chloride concentration of 30-50 wt. %, wherein the concentration step is carried out in one or more stages, wherein at least one of the stages is conducted at elevated pressure,
withdrawing the concentrated magnesium chloride solution from the concentration step, and providing it 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 having a temperature of at least 300° C. from the thermohydrolysis reactor,
providing the HCl-containing gas stream having a temperature of at least 300° C. to a cooling step, where the HCl-containing gas stream is contacted with a cooling liquid,
withdrawing a HCl-containing gas stream having a temperature below 150° C. from the cooling step,
circulating the cooling liquid through a heat exchanger where energy from the cooling liquid is transferred to the heating liquid, which heating liquid then circulates from the heat exchanger to provide the energy to the concentration step.

25. Method according to claim

Assignees

• Purac Biochem Bv

Inventors

• De Vries Johannes Jeichienus
• Frediansyah Raymon

Classifications

• C12P17/04

  containing a five-membered hetero ring, e.g. griseofulvin {, vitamin C} · CPC title

• C12P7/56

  Lactic acid · CPC title

• C12P7/52

  Propionic acid; Butyric acids · CPC title

• C12P7/48

  Tricarboxylic acids, e.g. citric acid · CPC title

• C12P7/46

  Dicarboxylic acids having four or less carbon atoms, e.g. fumaric acid, maleic acid · CPC title