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Method for preparing iridous chloride hydrate

A technology of iridium trichloride and hydrate, which is applied in the field of preparation of iridium trichloride hydrate IrCl 3H2O, can solve the problems of low purity of iridium trichloride hydrate, increase preparation steps, increase iridium loss, etc. The effect of high iridium yield, high product purity and low preparation cost

Active Publication Date: 2012-04-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high price of iridium, the dissolution process must minimize the loss of iridium, and in order to remove other ions introduced, the preparation steps will be increased to increase the loss of iridium
In addition, the purity of the iridium trichloride hydrate prepared by the above-mentioned existing method is relatively low

Method used

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  • Method for preparing iridous chloride hydrate
  • Method for preparing iridous chloride hydrate
  • Method for preparing iridous chloride hydrate

Examples

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Effect test

preparation example Construction

[0049] The preparation method of iridium trichloride hydrate of the present invention comprises the following steps:

[0050] The first step, electrolysis: add hydrochloric acid solution 4 and iridium powder raw material 5 in U-shaped electrolytic cell 1;

[0051] The U-shaped electrolytic cell 1 is made of acid-resistant material, and the U-shaped electrolytic cell is provided with electrodes 2 of non-metallic conductive materials;

[0052] Control the temperature of hydrochloric acid in the electrolytic cell at 100-115°C, load alternating current with a voltage of 5-80 volts and a current of 2-50 amperes at both ends of the electrodes, and carry out constant-voltage electrolysis until the iridium powder dissolves to generate an aqueous solution of chloroiridic acid ;

[0053] The purity of the hydrochloric acid is top grade pure, and the concentration of the hydrochloric acid is 8 to 12 mol / L; the weight ratio of the hydrochloric acid to the iridium powder is 3: 1 to 100: 1...

Embodiment 1

[0086] figure 1 It is a schematic diagram of a U-shaped electrolytic cell. The diameter of the vertical pipe 1b of the U-shaped quartz electrolytic cell 1 is 50 mm, and the center of the two vertical pipes is 180 mm apart; the diameter of the bottom elbow 1a is 18 mm, and the diameter of the vertical pipe: the diameter of the elbow is 2.78; The length is 25mm; the volume of the electrolytic cell is 800ml; the electrode 2 is a spectrally pure graphite electrode of Φ12mm and a length of 250mm. Cold water condensers are installed on both sides of the U-shaped quartz electrolytic cell 1 through the condenser interface 1c.

[0087] See iridium powder dissolving device figure 2 , wherein: both ends of the graphite electrode are connected to the AC arc generation controller 3, the iridium powder 5 is placed in the elbow 1a at the bottom of the U-shaped electrolytic cell, and the hydrochloric acid solution 4 is added to the electrolytic cell 1 and placed in the circulating cooling ...

Embodiment 2、3

[0090] Change the electrolytic alternating current voltage to 45 volts and 55 volts, respectively, and the current varies from 10 to 40 amps. Other conditions are as shown in Example 1. The dissolution rate of iridium powder is 89.0% and 85.2% respectively. The solution after the electrolysis of Examples 2 and 3 was filtered, the filtrates were combined, and through simple distillation, excess hydrochloric acid was distilled off to obtain 2.1M / L chloroiridic acid H 3 IrCl 6 solution. put H 3 IrCl 6 The concentrated solution was put into a crystallization furnace, and crystallized at 115 ° C for 10 h to obtain 95.9 g of iridium trichloride hydrate (IrCl 3 ·3H 2 O). The weight percent content of Ir was 54.48% by gravimetric analysis. According to the analysis value of iridium content, the yield of iridium is more than 99.9%. According to ICP analysis, the total weight percentage of ten impurity metals such as K, Na, Ca, Si, Rh, Au, Ag, Mg, Pt, and Cu is 0.0094%. Since ...

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Abstract

The invention relates to a method for preparing an iridous chloride hydrate (IrCl3.3H2O). The method comprises the following steps of: adding a hydrochloric acid solution and an iridium powder raw material into a U-shaped electrolytic cell, loading alternating current onto the two ends of an electrode, and directly dissolving the iridium powder into hydrochloric acid to obtain a chloroiridic acid aqueous solution; filtering the chloroiridic acid aqueous solution, and distilling to obtain a chloroiridic acid concentrated solution; and crystallizing the chloroiridic acid concentrated solution in a crystallization furnace to obtain an iridous chloride hydrate. In the preparation method of the iridous chloride hydrate, the iridous powder raw material is directly dissolved into the hydrochloric acid without adding any other reagent, so that the production cost is lowered, and a product is crystalized into the iridous chloride hydrate which is easy to carry, has stable iridium concentration, and is convenient to weigh and use; and when a high-purify iridous powder raw material is adopted, the impurity interference can be prevented, and a high-purity iridous chloride hydrate is prepared.

Description

technical field [0001] The present invention relates to iridium trichloride hydrate IrCl 3 ·3H 2 The technical field of preparation of O, specifically a preparation method of iridium trichloride hydrate. In particular, it refers to the method for preparing iridium trichloride hydrate with metal iridium powder as raw material. Background technique [0002] Iridium trichloride hydrate is one of the most common compounds of iridium Ir, and is often used as the initial raw material for synthesizing other iridium compounds and preparing iridium-containing catalysts. Iridium-containing compounds and catalysts are widely used in petrochemical and organic synthesis fields. For example, methanol carbonylation to acetic acid and acetic anhydride units both use iridium compounds as homogeneous catalysts. In addition, in the fields of hydrogenation catalyst, polymerization catalyst, organic synthesis, etc., iridium trichloride hydrate is also an indispensable important chemical raw ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G55/00
Inventor 吕顺丰刘博秦燕璜李彤王世亮
Owner CHINA PETROLEUM & CHEM CORP
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