Multi-stage crystallisation process and apparatus to purify a compound

Patent metadata

Field	Value
Publication number	US-9597609-B2
Application number	US-201314759990-A
Country	US
Kind code	B2
Filing date	Dec 18, 2013
Priority date	Jan 14, 2013
Publication date	Mar 21, 2017
Grant date	Mar 21, 2017

Abstract

A process to purify a compound comprising a suspension crystallization step and additionally comprises a layer crystallization step and a storage step of an intermediate product obtained from the layer crystallization step before to its further purification in the suspension crystallization step.

First claim

The invention claimed is:

1. A process to purify a compound comprising:
(i) a suspension crystallization step,
(ii) a layer crystallization step,
(iii) a storage step of an intermediate product obtained from the layer crystallization step before its further purification in the suspension crystallization step.

2. The process of claim 1 , wherein the compound is phosphoric acid.

3. The process of claim 1 , wherein the compound contains one or more metallic or metalloid impurities, wherein the concentration of each metal or metalloid impurity in the compound is reduced in the process to less than 1000 ppb.

4. The process of claim 3 , wherein the one or more metallic or metalloid impurities comprise arsenic and/or boron.

5. The process of claim 1 , wherein the process comprises one layer crystallization stage and two or more suspension crystallization stages, wherein the one layer crystallization stage is carried out before the two or more suspension crystallization stages.

6. The process of claim 1 , wherein the process comprises one layer crystallization stage and three suspension crystallization stages, wherein the one layer crystallization stage is carried out before the three suspension crystallization stages.

7. The process of claim 1 , wherein any layer crystallization step or stage present in the process is carried out in a static crystallization unit or a falling film crystallization unit.

8. The process of claim 7 , wherein the process is carried out in a static crystallization unit.

9. The process of claim 1 , wherein any suspension crystallization step or stage present in the process comprises a solid-liquid separation and washing stage, and wherein the solid-liquid separation and washing stage is carried out in a wash column having a melt circuit.

10. The process of claim 9 , wherein the wash column is a packed bed wash column.

11. The process of claim 9 , wherein a solvent is added to the melt circuit.

12. The process of claim 9 , wherein the solvent is water.

13. An apparatus for purifying a compound comprising:
(i) a suspension crystallization unit,
(ii) a layer crystallization unit,
(iii) a storage unit located after the layer crystallization unit and before the suspension crystallization unit.

14. The apparatus of claim 13 , wherein the layer crystallization unit is a falling film crystallization unit.

15. The apparatus of claim 13 , wherein the layer crystallization unit is a static crystallization unit.

16. The apparatus of claim 13 , additionally comprising a wash column for a melt circuit.

17. The apparatus of claim 16 , wherein the wash column is a packed bed wash column.

18. The apparatus of claim 16 , wherein the melt circuit has an inlet for adding a solvent.

19. A method for using the apparatus of claim 13 for the purification of a feed stream comprising a compound containing one or more metallic or metalloid impurities, wherein the concentration of each metal or metalloid impurity in the compound is reduced in the use to less than 1000 ppb, the method comprising the step of introducing the feed stream to the layer crystallization unit.

20. The method use of claim 19 , wherein the method is satisfactory for the production of electronic grade phosphoric acid in accordance with SEMI C36-0301.

21. The apparatus of claim 13 , wherein the apparatus is configured such that a feed flows from the layer crystallization unit into the storage unit and then into the suspension crystallization unit.

Assignees

• Sulzer Chemtech Ag

Inventors

• Jansen Halbe
• Pfeil Mathias

Classifications

• C01P2006/80

  Compositional purity · CPC title

• C01B25/237

  Selective elimination of impurities {(C01B25/2343 takes precedence)} · CPC title

• C01B25/234

  Purification; Stabilisation; Concentration (purification concomitant with preparation C01B25/22; preparation involving solvent-solvent extraction C01B25/46) · CPC title

• B01D9/0059 Primary

  General arrangements of crystallisation plant, e.g. flow sheets · CPC title

• B01D9/0036

  Crystallisation on to a bed of product crystals; Seeding · CPC title