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Method for synthesizing iridium (III) triacetylacetonate

A synthesis method and technology of acetylacetone, applied in the synthesis field of triacetylacetonate (iridium (iridium)), can solve problems such as complex process and low yield, and achieve the effects of promoting development, high social and economic benefits, and improving yield

Inactive Publication Date: 2004-11-17
KUNMING INST OF PRECIOUS METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Among the above synthetic methods, the first two processes are complex and have low yields, while the latter one uses the highly toxic solvent benzene, although the latter has a higher yield, and its application is limited to a certain extent.

Method used

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  • Method for synthesizing iridium (III) triacetylacetonate
  • Method for synthesizing iridium (III) triacetylacetonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 10g of iridium(III) chloride trihydrate in 150mL of hot distilled water at 50°C, add 17.5mL of acetylacetone and 2.0g of ascorbic acid, stir and heat until boiling (boiling temperature is 96°C to 100°C), and reflux for 1 hour Slowly add saturated sodium bicarbonate solution (containing 6.8 g of sodium bicarbonate) dropwise, then reflux for 1.5 h, stop heating, cool, and filter with suction to obtain an orange-yellow product, namely iridium(III) triacetylacetonate, which is washed with water two to three times. Pour the filtrate back into the reactor, add 9.0 mL of acetylacetone, continue to stir and heat to reflux for 1 h, then slowly add saturated sodium bicarbonate solution (containing 3.5 g of sodium bicarbonate) dropwise, reflux for 1 h, cool, and suction filter to obtain the second batch of three Iridium(III) acetylacetonate, washed with water two to three times.

[0021] The iridium(III) triacetylacetonate obtained in the above steps was combined, purifie...

Embodiment 2

[0023] Dissolve 10g of iridium(III) chloride trihydrate in 150mL of hot distilled water at 50°C, add 17.5mL of acetylacetone, stir and start flowing hydrogen, then heat until boiling (boiling temperature is 92°C to 96°C), and reflux for 1.5h Then slowly add saturated sodium bicarbonate solution (containing 6.8 g of sodium bicarbonate) dropwise, then reflux for 1.5 h, stop heating until the reaction solution is cooled, then stop the hydrogen flow, and suction filter to obtain an orange-yellow product that is iridium triacetylacetonate ( III), wash with water two to three times. Pour the filtrate back into the reactor, ventilate with hydrogen, add 9.0mL of acetylacetone, continue to stir and heat to reflux for 1.5h, then slowly add saturated sodium bicarbonate solution (containing 3.5g of sodium bicarbonate) dropwise, reflux for 1h, cool down, stop the hydrogenation , Suction filtration to obtain the second batch of triacetylacetonate iridium (III), washed with water two to thre...

Embodiment 3

[0026]Dissolve 10g of iridium(III) chloride trihydrate in 150mL of hot distilled water at 45°C, add 17.5mL of acetylacetone and 2.0g of ascorbic acid, stir and start flowing hydrogen, then heat until boiling (boiling temperature is 92°C to 97°C) , after reflux for 2 hours, slowly add saturated sodium bicarbonate solution (containing 6.8 g of sodium bicarbonate), reflux for another 2 hours, stop heating until the reaction solution is cooled, then stop the hydrogen flow, and filter with suction to obtain an orange-yellow product that is triacetylacetonate Iridium(III), washed two to three times with water. Pour the filtrate back into the reactor, ventilate with hydrogen, add 9.0mL of acetylacetone, continue to stir and heat to reflux for 1.5h, then slowly add saturated sodium bicarbonate solution (containing 3.5g of sodium bicarbonate) dropwise, reflux for 1h, cool down, stop the hydrogenation , Suction filtration to obtain the second batch of triacetylacetonate iridium (III), w...

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Abstract

The invention relates to a method for synthesizing iridium (III) acetylacetonate which comprises, dissolving iridium (III) chloride trihydrated into thermal distillation water, charing acetylacetone when agitating and letting in hydrogen gas, backflow, dropping saturated sodium bicarbonate solution, backflow, stopping hydrogen gas, filtering to obtain the end product.

Description

technical field [0001] The invention relates to a synthesis method of iridium (III) triacetylacetonate (tris(2,4-pentanedione) iridium (III)). Background technique [0002] Among platinum group metal elements (ruthenium, rhodium, palladium, osmium, iridium, platinum), iridium has its own unique properties, such as the highest melting point (2443°C), high density (22.6g / cm 3 ), high chemical inertness, good performance in preventing the diffusion of oxygen, and its oxide also has excellent conductivity. These characteristics make iridium thin films or coatings have superior performance than many existing alloy materials, oxide coatings and other noble metal coatings, thus arousing people's greater interest. [0003] Iridium resources are very scarce and expensive. The preparation of iridium low-dimensional materials such as films or coatings by chemical vapor deposition (Chemical Vapor Deposition, CVD) technology is the main means to save and efficiently utilize iridium res...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 闫革新刘伟平普绍平高文桂梁广
Owner KUNMING INST OF PRECIOUS METALS
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