Preparation method of high-purity iridium trichloride

A technology of pure iridium trichloride and ammonium chloride, which is applied in chemical instruments and methods, inorganic chemistry, ruthenium/rhodium/palladium/osmium/iridium/platinum halides, etc., can solve the difficulty of iridium trichloride purification and production Low efficiency, cumbersome process and other problems, to achieve the effect of high yield, high production efficiency and simple process

Pending Publication Date: 2022-03-01
英特派铂业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this application is to solve the problems of difficult purification and mass production of high-purity iridium trichloride, especially the existing technical process, cumbersome process, low production efficiency and other problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1, alkali fusion. Mix the iridium powder with sodium peroxide, sodium hydroxide, and sodium carbonate evenly and put it into an iron crucible. The mass ratio of iridium powder: sodium peroxide: sodium hydroxide: sodium carbonate is 1:1:3:1, and melt at high temperature , The melting temperature is 610°C, the melting time is 3h, and the cooled molten salt is taken out.

[0030] Step 2, slowly dissolve the molten salt with dilute hydrochloric acid, and adjust the pH<1, then add aqua regia to boil, filter off the insoluble residue, add ammonium chloride to the filtrate, keep the concentration of ammonium chloride at about 17%, boil, and filter to obtain Ammonium chloroiridate as a black solid.

[0031] Step 3, pre-purification. Add hydrazine hydrochloride to the black solid ammonium chloroiridate, the dosage of hydrazine hydrochloride is hydrazine hydrochloride: iridium powder = 1:2.13, heat and stir to dissolve the solid slowly, and filter again to obtain ammonium ...

Embodiment 2

[0037] Step 1, alkali fusion. Mix iridium powder with sodium peroxide, sodium hydroxide, and sodium carbonate evenly and put them into a melting crucible. The mass ratio of iridium powder: sodium peroxide: sodium hydroxide: sodium carbonate is 1:0.8:5:1.5, and melt at high temperature , The melting temperature is 550°C, the melting time is 2h, and the cooled molten salt is taken out.

[0038] Step 2, slowly dissolve the molten salt with dilute hydrochloric acid, and adjust the pH to be acidic, then add aqua regia to boil, filter off the insoluble residue, add ammonium chloride to the filtrate, keep the concentration of ammonium chloride at about 10%, boil, and filter to obtain Ammonium chloroiridate as a black solid.

[0039] Step 3, add hydrazine hydrochloride to the black solid ammonium chloroiridate, the dosage of hydrazine hydrochloride is hydrazine hydrochloride: iridium powder = 1:2.13, heat and stir to dissolve the solid slowly, and filter again to obtain ammonium chlo...

Embodiment 3

[0045] Step 1, alkali fusion. Mix iridium powder with sodium peroxide, sodium hydroxide, and sodium carbonate evenly and put them into an iron crucible. The mass ratio of iridium powder: sodium peroxide: sodium hydroxide: sodium carbonate is 1:1:4:1, and melt at high temperature , The melting temperature is 500°C, the melting time is 4h, and the cooled molten salt is taken out.

[0046] Step 2, slowly dissolve the molten salt with dilute hydrochloric acid, and adjust the pH to be acidic, then add aqua regia to boil, filter off the insoluble residue, add ammonium chloride to the filtrate, the concentration of ammonium chloride is 20% of the total concentration of the solution, boil, Ammonium chloroiridate was obtained by filtration as a black solid.

[0047] Step 3, add hydrazine hydrochloride to the black solid ammonium chloroiridate, the dosage of hydrazine hydrochloride is hydrazine hydrochloride: iridium powder = 1:2.13, heat and stir to dissolve the solid slowly, and filt...

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PUM

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Abstract

The invention discloses a method for preparing high-purity iridium trichloride. Iridium powder is used as a raw material to be subjected to alkali fusion under the mixing action of sodium peroxide, sodium hydroxide and sodium carbonate; dissolving the alkali fusion solid with aqua regia, adding ammonium chloride into the filtered solution to form precipitated ammonium chloroiridate, reacting the ammonium chloroiridate with hydrazine hydrochloride to form ammonium chloroiridate, further removing impurities by sodium sulfide and ammonium sulfide, filtering, oxidizing the filtrate by hydrochloric acid / hydrogen peroxide, and precipitating by an ammonium chloride solution to obtain ammonium chloroiridate with higher purity; the preparation method comprises the following steps: removing nitrate from ammonium chloroiridate by using an aqua regia solution, adding sodium nitrite / potassium chloride into the obtained chloroiridate solution, boiling to obtain a potassium hexanitroso iridate solid, filtering, adding hydrochloric acid into the solid, boiling, dissolving, removing nitrate, adding a proper amount of hydrazine hydrochloride, and carrying out rotary evaporation and vacuum calcination on the solution to obtain an iridium trichloride solid with the purity of more than 99.995%.

Description

technical field [0001] The application relates to the technical field of precious metal fine chemicals, in particular to a method for preparing high-purity iridium trichloride. Background technique [0002] Iridium trichloride is an important chemical catalyst and a raw material for preparing other iridium reagents. Iridium trichloride is a very important precursor compound in the field of noble metal catalysis and high-temperature anti-oxidation coating. Iridium-containing compounds and catalysts are widely used in petrochemical, organic catalysis and organic synthesis fields. In addition, iridium trichloride hydrate is also an indispensable and important chemical raw material in the fields of hydrogenation catalysts, polymerization catalysts, and organic synthesis. [0003] A very critical step in the preparation of iridium trichloride hydrate and other iridium compounds is to dissolve chemically stable iridium powder in a solution. However, iridium is one of the most st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
CPCC01G55/005
Inventor 秦喜超王来兵陆凯凯屈新鑫杭云
Owner 英特派铂业股份有限公司
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