Process for the production of high purity iridium(III)chloride hydrate

Patent metadata

Field	Value
Publication number	US-11111156-B2
Application number	US-201716474304-A
Country	US
Kind code	B2
Filing date	Dec 4, 2017
Priority date	Jan 25, 2017
Publication date	Sep 7, 2021
Grant date	Sep 7, 2021

Abstract

Process for the production of high purity iridium(III) chloride hydrate, comprising the steps of:(1) providing at least one material selected from the group consisting of solid H2[IrCl6] hydrate, aqueous, at least 1 wt. % H2[IrCl6] solution, and solid IrCl4 hydrate;(2) adding, to the at least one material provided in step (1), at least one monohydroxy compound selected from the group consisting of monohydroxy compounds that are miscible with water at any ratio, primary monoalcohols comprising 4 to 6 carbon atoms, and secondary monoalcohols comprising 4 to 6 carbon atoms at a molar ratio of Ir(IV):monohydroxy compound=1:0.6 to 1000, and allowing to react for 0.2 to 48 hours in a temperature range from 20 to 120° C., followed by removing volatile components from the reaction mixture thus formed.

First claim

The invention claimed is:

1. A process for the production of high purity iridium(III) chloride hydrate having the formula IrCl 3 ·×H 2 O·yHCl, wherein x=1.5 to 5 and y=0 to 1, the process comprising:
(1) providing at least one material selected from the group consisting of solid H2[IrC16] hydrate, aqueous, at least 1 wt. % H 2 [IrCl 6 ] solution, and solid IrCl 4 hydrate;
(2) adding, to the at least one material provided in step (1), at least one monohydroxy compound selected from the group consisting of monohydroxy compounds that are miscible with water at any ratio, primary monoalcohols comprising 4 to 6 carbon atoms, and secondary monoalcohols comprising 4 to 6 carbon atoms at a molar ratio of Ir(IV): monohydroxy compound from 1: 0.6 to 1_1000, and allowing to react for 0.2 to 48 hours in a temperature range from 20 to 120° C., followed by removing volatile components from the reaction mixture thus formed.

2. The process of claim 1 , whereby the at least one monohydroxy compound is selected from the group consisting of methanol, ethanol, and isopropanol.

3. The process of claim 1 , whereby the molar ratio of Ir(IV): monohydroxy compound(s) is from 1: 0.6 to 1:100.

4. The process of claim 1 , whereby the reaction temperature is 50 to 100° C.

5. The process of claim 1 , whereby the reaction time is in the range of 0.5 to 6 hours.

6. The process of claim 1 , whereby step (2) is terminated, before a formation of metallic iridium commences.

7. The process of claim 1 , whereby the course of the reaction and/or completion of the reaction is/are monitored by ESR spectroscopy.

8. The process of claim 1 , whereby selection of chemical and physical parameters of the process takes place specifically through the application of ESR spectroscopy, such that step (2) ends or can be terminated, before a formation of metallic iridium commences.

9. The process of claim 1 , whereby the volatile components are removed by distillation or evaporation.

10. The process of claim 9 , whereby the distillation or evaporation takes place at temperatures in the range of 30 to 120° C. acting from outside on the container containing the reaction mixture thus formed.

11. The process of claim 9 , whereby the distillation or evaporation takes place supported by a vacuum.

Assignees

• Heraeus Deutschland Gmbh & Co Kg

Inventors

• Walter Richard
• Fuchs Alameda Jörg
• Imgrund Christian
• Neumann Christian

Classifications

• C01G55/005 Primary

  Halides · CPC title

• B01D3/10

  Vacuum distillation (B01D3/12 takes precedence) · CPC title

• C01P2006/80

  Compositional purity · CPC title