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Preparation method of iridium catalyst

A catalyst and compound technology, applied in the field of preparation of [IrCl]2, can solve the problems of long reaction time, low product purity, and large amount of raw materials, and achieve the effects of short reaction time, high yield and high product purity

Active Publication Date: 2019-08-02
JIANGSU SINOCOMPOUND CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the invention is to solve the existing [IrCl (C 8 h 12 )] 2 The ubiquitous long reaction time in the preparation method leads to low product purity, large amount of raw materials used, cannot be recycled, high production cost, and the process is not environmentally friendly.

Method used

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  • Preparation method of iridium catalyst
  • Preparation method of iridium catalyst
  • Preparation method of iridium catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Dissolve iridium chloride in anaerobic water to obtain a solution with 10% iridium content, add cyclooctadiene with a molar ratio of 2 times, add hydrazine hydrate dropwise under anaerobic conditions and vigorous stirring, the reaction temperature is 90 °C, and add dropwise to no Precipitation is generated, filtered, and the filter cake is washed with anaerobic water, evaporated and crystallized to obtain cyclooctadiene iridium chloride [IrCl(C 8 h 12 )] 2 . After the filtrate was separated, the cyclooctadiene was continued to be used. Yield 99.5%, mass purity 99%, iridium content: 56.71%, elemental analysis carbon content: 28.35%, nuclear magnetic H-NMR see attached figure 2 .

Embodiment 2

[0029] Dissolve chloroiridic acid in anaerobic water to obtain a solution with 10% iridium content, add cyclooctadiene with a molar ratio of 2 times, add sodium borohydride dropwise under anaerobic conditions and vigorous stirring, the reaction temperature is 80 ° C, dropwise to No precipitation is generated, filter, wash the filter cake with anaerobic water, evaporate and crystallize to obtain cyclooctadiene iridium chloride [IrCl(C 8 h 12 )] 2 . After the filtrate was separated, the cyclooctadiene was continued to be used. Yield 99.5%, mass purity 99%, iridium content: 56.77%, elemental analysis carbon content: 28.38%, nuclear magnetic H-NMR see attached image 3 .

Embodiment 3

[0031] Dissolve sodium chloroiridate in anaerobic water to obtain a solution with 10% iridium content, add cyclooctadiene with a molar ratio of 2 times, add hydrazine hydrate dropwise under anaerobic conditions and vigorous stirring, the reaction temperature is 90 °C, and add dropwise to No precipitation is generated, filter, wash the filter cake with anaerobic water, evaporate and crystallize to obtain cyclooctadiene iridium chloride [IrCl(C 8 h 12 )] 2 . After the filtrate was separated, the cyclooctadiene was continued to be used. Yield 99.5%, mass purity 99%, iridium content: 56.66%, elemental analysis carbon content: 28.32%, nuclear magnetic H-NMR see attached Figure 4 .

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Abstract

The invention discloses a preparation method of an iridium catalyst [IrCl(C8H12)]2. The preparation method comprises following steps: a compound containing iridium and chlorine is dissolved in water in an oxygen-free environment, and an iridium solution is prepared; cyclooctadiene is added to the iridium solution, a reducing agent is slowly dropwise added for a reduction reaction, and the reducingagent is dropwise added until no precipitates are produced; the solution is filtered, evaporative crystallization is performed after solids are washed with water, and [IrCl(C8H12)]2 is obtained. According to the method, the reaction time is short, and the product is high in purity and yield.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to the field of synthesis of noble metal homogeneous catalysts, in particular to a [IrCl(C 8 h 12 )] 2 method of preparation. Background technique [0002] [IrCl(C 8 h 12 )] 2 As a noble metal homogeneous catalyst, it is also the precursor of various iridium catalysts, and is widely used in the chemical industry. Especially in the industrial production of the herbicide metolachlor, [IrCl(C 8 h 12 )] 2 It is a catalyst precursor for an important asymmetric hydrogenation reaction in the synthesis process. [0003] Herde, J, L (Inorganic syntheses, 1974, 15, 18) first reported the synthesis of 1,5 cyclooctadiene iridium chloride dimer. The reaction process was the reaction of iridium chloride and ethanol under anaerobic reflux conditions. More than 24 hours. [0004] In the preparation method of cyclooctadiene iridium chloride disclosed in JP2006045089A, the molar ...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/0033
Inventor 孙明明倪自林李娟祁义军
Owner JIANGSU SINOCOMPOUND CATALYST
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