Method for preparing dicarbonyl iridium acetylacetonate (I)

A technology of acetone dicarbonyl iridium and acetylacetone, which is applied in the field of preparation of metal organic iridium compound acetylacetonate dicarbonyl iridium, can solve the problems of high cost and low production yield, and achieve the effect of short reaction time and high yield

Inactive Publication Date: 2014-12-24
KUNMING INST OF PRECIOUS METALS
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0016] These three routes all have the problems of low preparation yield and high cost. Therefore, it is necessary to develop [Ir(CO) 2 (acac)] efficient synthesis technology

Method used

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  • Method for preparing dicarbonyl iridium acetylacetonate (I)
  • Method for preparing dicarbonyl iridium acetylacetonate (I)
  • Method for preparing dicarbonyl iridium acetylacetonate (I)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: IrCl 3 ·3H 2 O (2.0g, 2.84mmol) and 30mL of secondary deionized water, 80mL of ethanol and 20mL of 1,5-cyclooctadiene were placed in a 250mL round-bottom flask, under the control of standard Schlenk vacuum line technology, stirred and heated to reflux for 5h . The reaction was stopped, the reaction solution was concentrated, and most of the solvent was removed, and a solid was precipitated, filtered, and the filter cake was washed with distilled water and methanol. After vacuum drying for 5 hours, 1.81 g was obtained with a yield of 95.2%.

[0022] [Ir(COD)(μ-Cl)] 2 (1.0 g, 1.49 mmol) and 150 mL of tetrahydrofuran (THF) were placed in a 250 mL round bottom flask, and the system was under an argon atmosphere under standard Schlenk vacuum line technology control. Then, CO gas was introduced for 3 minutes, and the solution changed from yellow to blue-black. Under argon atmosphere, quickly add NaHCO 3 (10 g, 119.04 mmol) and 1.5 mL acetylacetone (Hacac). ...

Embodiment 2

[0026] Example 2: IrCl 3 ·3H 2 O (10.0g, 14.2mmol) and 150mL of secondary deionized water, 400mL of ethanol and 100mL of 1,5-cyclooctadiene were placed in a 1000mL round-bottomed flask, under the control of standard Schlenk vacuum line technology, stirred and heated to reflux for 5h . The reaction was stopped, the reaction solution was concentrated, and most of the solvent was removed, and a solid was precipitated, filtered, and the filter cake was washed with distilled water and methanol. After vacuum drying for 5 hours, 9.1 g was obtained with a yield of 95.8%.

[0027] [Ir(COD)(μ-Cl)] 2 (5.0 g, 7.45 mmol) and 750 mL of tetrahydrofuran (THF) were placed in a 1000 mL round bottom flask, and the system was under an argon atmosphere under standard Schlenk vacuum line technology control. Then, CO gas was introduced for 3 minutes, and the solution changed from yellow to blue-black. Under argon atmosphere, quickly add NaHCO 3 (50 g, 595.2 mmol) and 7.5 mL acetylacetone (Haca...

Embodiment 3

[0029] Embodiment 3: the IrCl 3 ·3H 2O (20.0g, 28.4mmol) and 300mL of secondary deionized water, 800mL of ethanol and 200mL of 1,5-cyclooctadiene were placed in a 2000mL round-bottomed flask, under the control of standard Schlenk vacuum line technology, stirred and heated to reflux for 5h . The reaction was stopped, the reaction solution was concentrated, and most of the solvent was removed, and a solid was precipitated, filtered, and the filter cake was washed with distilled water and methanol. After vacuum drying for 5 hours, 18.2 g was obtained with a yield of 95.8%.

[0030] [Ir(COD)(μ-Cl)] 2 (15.0 g, 22.35 mmol) and 2250 mL of tetrahydrofuran (THF) were placed in a 3000 mL round bottom flask, and the system was under an argon atmosphere under standard Schlenk vacuum line technology control. Then, CO gas was introduced for 3 minutes, and the solution changed from yellow to blue-black. Under argon atmosphere, quickly add NaHCO 3 (150 g, 1785.6 mmol) and 22.5 mL acetyl...

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Abstract

The invention discloses a method for preparing dicarbonyl iridium acetylacetonate (I). Dicarbonyl iridium acetylacetonate (I) is a precursor compound for preparing an iridium coating by MOCVD (metal-organic chemical vapor deposition), and is also a common carbonyl addition homogeneous catalyst. The method mainly comprises the following steps: (1) reacting iridous chloride hydrate and 1,5-cyclooctadiene to generate an intermediate (1,5-cyclooctadiene) iridium chloride (I) dimer; and (2) reacting the intermediate and carbon monoxide to introduce carbonyl group, reacting with acetylacetone to obtain the dicarbonyl iridium acetylacetonate (I). The preparation method has the advantages of simple technical process, high yield and high product purity, and is suitable for mass preparation of [Ir(CO)2(acac)].

Description

technical field [0001] The invention relates to a preparation method of metal organic iridium compound acetylacetonate dicarbonyl iridium (I), which belongs to the field of chemistry and chemical industry. Background technique [0002] Metal-organic chemical vapor deposition (MOCVD) is a common method for preparing iridium coating materials. The key to this method is to select the appropriate precursor compound according to the characteristics of the substrate and deposition conditions. Metal-organic compounds that meet the requirements of MOCVD generally have the characteristics of volatilization and sublimation at lower temperatures, and can decompose metals or their oxides at higher temperatures. Currently, the most widely used compounds are β-diketone metal compounds, such as iridium(III) acetylacetonate. However, the sublimation temperature and decomposition temperature of iridium(III) acetylacetonate are relatively high, and the carbon content is high, and carbon co-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
Inventor 晏彩先常桥稳刘伟平赵婧叶青松姜婧余娟
Owner KUNMING INST OF PRECIOUS METALS
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