Materials and methods for the selective recovery of multivalent products

Patent metadata

Field	Value
Publication number	US-2016296926-A1
Application number	US-201615094930-A
Country	US
Kind code	A1
Filing date	Apr 8, 2016
Priority date	Apr 8, 2015
Publication date	Oct 13, 2016
Grant date	—

Abstract

Described herein are processes and apparatus for the high purity and high concentration recovery of multivalent products via continuous ion exchange from aqueous solutions for further down-stream purification.

First claim

What is claimed is:

1 . A method of recovering multivalent products from aqueous solutions using continuous ion exchange comprising:
(a) adsorbing the multivalent product principally as divalent specie onto an ion exchange resin; (b) converting the adsorbed multivalent product to principally the monovalent valence state; (c) concentrating the multivalent product through re-adsorption onto the ion exchange resin; and (d) eluting the multivalent product.

2 . The method of claim 1 , wherein the multivalent product is chosen from dicarboxylic acids and diamines.

3 . The method of claim 2 , wherein the dicarboxylic acids are chosen from succinic acid, glutaric acid, adipic acid, and pimelic acid.

4 . The method of claim 2 , wherein the diamines are chosen from putrescine, cadaverine, hexamethylenediamine, and heptamethylenediamine.

5 . The method of claim 1 , wherein (1) impurities are selectively desorbed and (2) the adsorbed multivalent product is converted to principally the monovalent state by feeding a base or an acid at a concentration that allows the pH of the aqueous solution discharged from the resin to be approximately the pK a2 for cationic divalent products and to be approximately the pK a1 for anionic divalent products.

6 . The method of claim 5 , wherein multivalent product at a pH of approximately the first equivalence point is recycled to the ion exchange resin and concentrated through re-adsorption.

7 . The method of claim 1 , wherein (1) impurities are selectively desorbed and (2) the adsorbed multivalent product is converted to principally the monovalent state by recycling multivalent product in principally the zero valence state, concentrating the multivalent product though re-adsorption.

8 . The method of claim 1 , wherein the multivalent product is eluted from the ion exchange resin with a high concentration of ammonia, ammonium bicarbonate and/or ammonium carbonate.

9 . The method of claim 6 or claim 8 , where the eluted multivalent product is fed to a steam stripper, adjusting the pH of the multivalent product to approximately the first equivalence point.

10 . The method of claim 7 or claim 8 , where the eluted multivalent product is fed to a steam stripper, adjusting the pH to where the multivalent product is principally in the zero valence state.

11 . The method of claim 9 or claim 10 , where a fraction of the multivalent product recovered from the steam stripper is recycled to the ion exchange resin and concentrated through re-adsorption.

12 . The method of claim 1 , further comprising at least one wash step after one or more of steps (a), (b), (c), and (d) using an aqueous solution.

13 . An apparatus for recovering multivalent products from aqueous solutions comprising one or more of the below zones;
(a) an adsorption zone comprising an ion exchange resin, for adsorption of the multivalent product as principally a divalent specie; (b) a monovalent strip zone, for desorbing impurities and converting the adsorbed multivalent product to the monovalent state; (c) a monovalent adsorption zone, for adsorbing recycled multivalent product recycled from a steam stripper; and (d) an elution zone, for eluting the multivalent product using a concentrated ammonia, ammonium bicarbonate or ammonium carbonate solution.

14 . The apparatus according to claim 13 , wherein the multivalent product is chosen from dicarboxylic acids and diamines.

15 . The apparatus according to claim 14 , wherein the dicarboxylic acids are chosen from succinic acid, glutaric acid, adipic acid, and pimelic acid.

16 . The apparatus according to claim 14 , wherein the diamines are chosen from putrescine, cadaverine, hexamethylenediamine, and heptamethylenediamine.

17 . The apparatus of claim 13 , which is configured to selectively desorb impurities and (2) to convert the adsorbed multivalent product to principally the monovalent state by feeding a base or an acid at a concentration that allows the pH of the aqueous solution discharged from the resin to be approximately the pK a2 for cationic divalent products and to be approximately the pK a1 for anionic divalent products.

18 . The apparatus of claim 17 , wherein multivalent product at a pH of approximately the first equivalence point is recycled to the ion exchange resin and concentrated through re-adsorption.

19 . The apparatus of claim 13 , wherein (1) impurities are selectively desorbed and (2) the adsorbed multivalent product is converted to principally the monovalent state by recycling multivalent product in principally the zero valence state, concentrating the multivalent product though re-adsorption.

20 . The apparatus of claim 13 , wherein the multivalent product is eluted from the ion exchange resin with a high concentration of ammonia, ammonium bicarbonate and/or ammonium carbonate.

21 . The apparatus of claim 18 or claim 20 , where the eluted multivalent product is fed to a steam stripper, adjusting the pH of the multivalent product to approximately the first equivalence point.

22 . The apparatus of claim 19 or claim 20 , where the eluted multivalent product is fed to a steam stripper, adjusting the pH to where the multivalent product is principally in the zero valence state.

23 . The apparatus of claim 21 or claim 22 , where a fraction of the multivalent product recovered from the steam stripper is recycled to the ion exchange resin and concentrated through re-adsorption.

24 . The apparatus of claim 13 , further comprising at least one elution wash zone after one or more of zones (a), (b), (c), and (d) using an aqueous solution.

25 . The apparatus of claim 13 , wherein the monovalent strip zone and the monovalent adsorption zone are combined.

Assignees

• Invista North America Sarl

Inventors

• Kamionka Mariusz
• Conradie Alex

Classifications

• B01J39/05

  in the strongly acidic form · CPC title

• C02F2101/34

  containing oxygen · CPC title

• C02F1/42

  by ion-exchange (ion-exchange in general B01J) · CPC title

• C02F2101/38

  containing nitrogen · CPC title

• C07C209/86

  Separation · CPC title