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Method for microwave-assisted synthesis of iridium acetate

A microwave-assisted, iridium acetate technology, applied in the field of microwave-assisted synthesis of iridium acetate, can solve the problems of difficult mass production, low product purity, unstable process, etc., and achieve short reaction time, simple process flow, and easy process control Effect

Pending Publication Date: 2019-02-01
CHENZHOU GAOXIN PLATINUM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this process is long, the process is unstable, and the purity of the product is not high, the yield is low, and it is difficult to produce in batches
[0004] In summary, there is not high product purity in the synthetic method of iridium acetate at present, and yield is low, problems such as process instability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 5 g of iridium trichloride hydrate in 50 mL of deionized water, add dropwise sodium hydroxide solution with a mass fraction of 10% under stirring to adjust the pH to 9, equilibrate for 10 min, separate the precipitate by suction filtration, and wash with deionized water until chlorine-free ions, stir and disperse the resulting precipitate in 150mL of glacial acetic acid, add 3g of formic acid, place in a microwave reaction device, start stirring and microwave irradiation (microwave frequency is 2450MHz, power is 150w), the reaction is refluxed for 2h, and the microwave reaction device, the reaction solution was evaporated at 90°C to remove the solvent under reduced pressure until it became a sticky paste, and dried in vacuum at 80°C for 4 hours to obtain 5.82g of green crystal iridium acetate with a product yield of 96.3% and a purity of 99.2%.

Embodiment 2

[0025] Dissolve 5 g of iridium trichloride hydrate in 50 mL of deionized water, add dropwise sodium hydroxide solution with a mass fraction of 20% under stirring to adjust the pH to 9, equilibrate for 10 min, separate the precipitate by suction filtration, and wash with deionized water until chlorine-free ions, stir and disperse the obtained precipitate in 150mL glacial acetic acid, add 4g of absolute ethanol, place it in a microwave reaction device, start stirring and microwave irradiation (microwave frequency is 2450MHz, power is 150w), the reaction is refluxed for 3h, and removed Microwave reaction device, the reaction solution was evaporated under reduced pressure at 90°C to remove the solvent to a sticky paste, and dried in vacuum at 80°C for 4 hours to obtain 5.74g of green crystal iridium acetate with a product yield of 94.7% and a purity of 99.0%.

Embodiment 3

[0027] Dissolve 25g of iridium trichloride hydrate in 50mL of deionized water, add dropwise sodium hydroxide solution with a mass fraction of 10% under stirring to adjust the pH to 8, equilibrate for 10min, separate the precipitate by suction filtration, wash with deionized water until chlorine-free ions, stir and disperse the obtained precipitate in 600mL glacial acetic acid, add 12g of formic acid, place in a microwave reaction device, start stirring and microwave irradiation (microwave frequency is 2450MHz, power is 350w), the reaction is refluxed for 2h, and the microwave reaction device, the reaction solution was distilled off the solvent at 90°C under reduced pressure until it became a sticky paste, and dried in vacuum at 80°C for 4 hours to obtain 29.43g of green crystal iridium acetate with a product yield of 97.4% and a purity of 99.3%.

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PUM

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Abstract

The invention discloses a method for microwave-assisted synthesis of iridium acetate. The method comprises the following steps: (1) adding alkali liquor into a iridium trichloride solution while stirring so as to form a precipitate, and filtering, and dechlorinating the precipitate by filtering and washing to obtain an iridium hydroxide wet product; and (2) pulpifying the iridium hydroxide wet product with glacial acetic acid, adding a reducing agent while stirring, starting microwave irradiation, conducting a reflux reaction until solids are dissolved, removing a solvent by reduced pressure distillation, and drying to obtain iridium acetate. The synthesis process is simple and has high conversion rate and yield. The product has good purity, and the synthesis process is easy to control. The synthesis process is green and environment-friendly and is suitable for industrial promotion.

Description

technical field [0001] The invention belongs to the field of organometallic catalysts, and in particular relates to a microwave-assisted method for synthesizing iridium acetate. Background technique [0002] Acetic acid is an important organic chemical raw material with a wide range of applications. At present, the domestic production process of acetic acid is mainly methanol carbonylation method, with RhI 3 as a catalyst. Rhodium catalysts are expensive and have limited applications. Iridium acetate has the same excellent catalytic performance as rhodium catalyst in methanol carbonylation reaction, and its price is relatively cheap, making it an ideal substitute. As the new domestic acetic acid production process uses iridium acetate as the catalyst, the demand for iridium acetate products in the market is also increasing. In addition, iridium acetate is also used in reactions such as hydroformylation, coupling, hydrogenation, and hydrosilylation, or in electroplating a...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41
CPCC07C51/412C07C53/10
Inventor 雷婧欧阳文兵杨拥军雷涤尘杨静
Owner CHENZHOU GAOXIN PLATINUM
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