Method of producing of metal iridium powder from (trifluorophosphine) iridium hydride tetrakis

FIELD: process engineering.

SUBSTANCE: invention relates to method of producing iridium from (trifluorophosphine) iridium hydride tetrakis and may be used for production of high-purity metal iridium powder. Proposed method comprises ammonolysis of volatile complex compound of (trifluorophosphine) iridium hydride tetrakis Hlr(PF3)4 with conversion into nonvolatile iridium metallamine by water solution of ammonium. Then, iridium metallamine is dissolved in concentrated hydrogen nitrate and solution is evaporated. Evaporation over, residue is decomposed to sponge-structure metal iridium. Now, the latter is triturated, reduced in hydrogen flow and purified to high-purity iridium.

EFFECT: high-purity iridium powder.

1 ex

 

The invention relates to a method for iridium from tetrakis(triptorelin)of iridium hydride and may be used to produce powder metal iridium.

The objective of the invention is to obtain iridium metal powder of high purity.

A method of obtaining pure iridium, where as the original substances using the concentrate of platinum group metals, in which iridium is in the form of metallic iridium. The method consists in the oxidation of iridium by fusing it with potassium nitrate, dissolved in Aqua Regia, then deposition in the form of hexachloroiridate ammonium. The residue purified by re-crystallization, mainly for the separation of platinum. After separation in a fairly pure state Sol calcined. Thus obtained metal iridium contains some amount of oxide, which restores when heated in a current of hydrogen. [1]

The difference of the proposed method of obtaining powder of iridium is that the original substance is tetrakis(triptorelin)iridium hydride.

The proposed method is the ammonolysis reaction of tetrakis(triptorelin)of iridium hydride followed by a chemical treatment, comprising the following steps:

1. The ammonolysis and evaporation of the solution;

2. Oxidation of the obtained emmakate nitrogen KIS the Auteuil and evaporation of the resulting solution;

3. Thermal decomposition;

4. The refinement.

The method is as follows.

The ammonolysis is carried out in a closed volume, capacity, lined with Teflon. In the capacity of the pre-fill water solution of ammonia in a molar ratio HIr(PF3)4:NH3=1:(19,425). Tetrakis(triptorelin)iridium hydride from the tank supply precondensed in the capacity of ammonolysis, then defrost and stand capacity to fully interact tetrakis(triptorelin)of iridium hydride with an aqueous solution of ammonia. The resulting solution was evaporated in Teflon cookware at a temperature of 100200C to plastic yellow-orange mass.

Obtained after evaporation of ammicht iridium in the form of a yellow-orange plastic mass is dissolved in concentrated nitric acid in a molar ratio HIr(PF3)4:HNO3=1:(4050). The solution is evaporated until dry in a dark blue residue.

Dark blue residue chopped, placed in a quartz boat and disposed in a vacuum at a constant pumping at a temperature of 7001000C. thus Obtained metallic iridium sponge-like structure to a flat surface and hold dopostavleno in a stream of hydrogen at a temperature of 600C.

Refining is carried out by a method based on obtaining soluble compounds of iridium, hexachloroiridate sodium, followed the by the dissolution and precipitation in the form of hexachloroiridate ammonium. Then hexachloroiridate ammonium restore in hydrogen to metallic iridium. [2]

Example 1. Using this method redesigned to 21.74 g of tetrakis(triptorelin)of iridium hydride. Received iridium metal powder with a yield of at least 99.9% of theoretical. Obtained by this method iridium low chemical purity predominantly contaminated with silicon, the material of construction of boats and classified according to GOST 13867-68 "products of the chemical. Denote purity" as iridium technical.

After refining the yield of the target product was 7,046 g, or 91,64% of theoretical. Iridium obtained by this method, the purity correspond brand I,9 GOST 13099-2006 "Iridium. Brand".

Literature

1. Handbook of rare metals. Ed. Vaitlusega. - M.: Mir, 1965.

2. Gbauer, Glemser, Globe and other inorganic synthesis Manual: 6 so V.5: TRANS. with it. Ed. Gbauer. - M.: Mir, 1982.

A method of producing powder metal iridium from tetrakis(triptorelin)of iridium hydride, including the ammonolysis of volatile complex compound tetrakis(triptorelin)of iridium hydride HIr(PF3)4with conversion in the non-volatile ammicht iridium aqueous solution of ammonia, dissolving emmakate iridium in concentrated nitric acid, evaporation of the solution, decomposition of the remainder of the metal is wow iridium sponge-like structure, his rubbing, dopostavleno in the stream of hydrogen and cleaned to high purity iridium.



 

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