Process for the preparation and/or purification of ruthenium(III) chloride

Patent metadata

Field	Value
Publication number	US-9994458-B2
Application number	US-201515508281-A
Country	US
Kind code	B2
Filing date	Jun 24, 2015
Priority date	Sep 3, 2014
Publication date	Jun 12, 2018
Grant date	Jun 12, 2018

Abstract

The present invention relates to a process for the preparation of ruthenium(III) chloride (RuCl 3 ) as well to a process for the purification of ruthenium(III) chloride (RuCl 3 ) and a use of the process for the preparation or the purification of ruthenium(III) chloride (RuCl 3 ).

First claim

We claim:

1. A process for the preparation of ruthenium(III) chloride (RuCl 3 ), the process comprising at least the steps of:
a) providing a hydrochloric acid solution,
b) providing at least one ruthenium salt:
(X) y [RuCl 6 ] 2− or (X) y [RuCl 6 ] 3−
wherein X is a monovalent, divalent or trivalent cation and y is 1, 2 or 3,

c) combining the hydrochloric acid solution of step a) and the at least one ruthenium salt of step b) and heating the obtained mixture to a temperature T of ≥70° C.,
d) adjusting the pH of the mixture obtained in step c) to a pH from 0 to 2, and
e) passing a mixture obtained in step d) through a cation exchanger to obtain a solution comprising ruthenium(III) chloride (RuCl 3 ).

2. A process for the purification of ruthenium(III) chloride (RuCl 3 ), the process comprising at least the steps of:
a) providing a hydrochloric acid solution,
b) providing ruthenium(III) chloride in dry form or in a form of a solution, wherein the ruthenium(III) chloride comprises impurities,
c) combining the hydrochloric acid solution of step a) and the ruthenium(III) chloride of step b) and heating the obtained mixture to a temperature T of ≥70° C.,
d) adjusting the pH of the mixture obtained in step c) to a pH from 0 to 2, and
e) passing a mixture obtained in step d) through a cation exchanger to obtain a solution comprising ruthenium(III) chloride (RuCl 3 ).

3. The process according to claim 1 , wherein in the at least one ruthenium salt:
i) X is a monovalent cation selected from the group consisting of NH 4 + , Na + , K + , Cu + and mixtures thereof, and y is 2 or 3, or
ii) X is a divalent cation selected from the group consisting of Cd 2+ , Co 2+ , Cu 2+ , Ni 2+ , Pb 2+ , Zn 2+ , Sn 2+ , Fe 2+ , Mg 2+ , Ca 2+ and mixtures thereof, and y is 1, or
iii) X is Fe 3+ and y is 1.

4. The process according to claim 1 , wherein in process step c) the obtained mixture is heated to a temperature T in the range from 70° C. to 110° C.

5. The process according to claim 1 , further comprising concentrating the mixture obtained in step c) before adjusting step d) is performed.

6. The process according to claim 5 , wherein the concentrating is performed such that the total weight of the obtained mixture is reduced by at least 15.0 wt %, based on the total weight of the mixture obtained in step c).

7. The process according to claim 5 , wherein the concentrating is performed by rotary evaporation or distillation.

8. The process according to claim 1 , wherein in step d), the pH is adjusted to a pH from 0 to 1.5.

9. The process according to claim 1 , wherein process step e) is performed within a period of not more than 2 hours after step d).

10. The process according to claim 1 , wherein the process further comprises step f) concentrating the solution obtained in step e).

11. The process according to claim 10 , wherein concentrating step f) is performed until RuCl 3 is crystallized from the solution.

12. The process according to claim 10 , wherein step f) is performed by evaporation.

Assignees

• Heraeus Deutschland Gmbh & Co Kg
• Heraeus South Africa Pty Ltd

Inventors

• Mock Christian
• Fife David
• Van Tonder Waldo
• Joubert Albert
• Lässig Walter

Classifications

• B01J39/05

  in the strongly acidic form · CPC title

• C01G55/001 Primary

  Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange · CPC title

• C01G55/005 Primary

  Halides · CPC title