Method for synthesizing ruthenium acetylacetonate (III)

A technology of ruthenium acetylacetonate and a synthesis method, applied in chemical instruments and methods, ruthenium organic compounds, platinum group organic compounds, etc., can solve the problems such as unfavorable acquisition of reaction raw materials, unfavorable amplification of microwave reaction, etc., and achieves reduced content and high yield. rate, the effect of low chloride ion content

Active Publication Date: 2018-05-18
浙江微通催化新材料有限公司
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Problems solved by technology

[0004] The document Indian Journal of Chemistry, Section A: Inorganic, Bio-inorganic, Physical, Theoretical & Analytical Chemistry, 39A (4), 457-460 reports that potassium chlororuthenate hydrate or potassium ruthenium sulfate hydrate and Hacac are used as reaction substrates, and KOH or KHCO 3 Neutralization, ruthenium (Ⅲ) acetylacetonate is obtained with a yield of 82-87%, but the reaction raw material is not suitable for obtaining
In the document Russian Chemical Bulletin, 61(12), 2236-2242, microwave is used as heating method, and the reaction can be completed in ten minutes, with a yield of 85%. Although the reaction time is short, microwave reaction is not conducive to large-scale production

Method used

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  • Method for synthesizing ruthenium acetylacetonate (III)
  • Method for synthesizing ruthenium acetylacetonate (III)
  • Method for synthesizing ruthenium acetylacetonate (III)

Examples

Experimental program
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Embodiment 1

[0034] Add 10.5g (40mmol) ruthenium trichloride hydrate to 200mL water, stir and dissolve at room temperature, add 30mL of 4mol / L sodium hydroxide solution, a large amount of black precipitate is formed, continue to stir for 1 hour, filter, wash with deionized water, wash with 0.1mol / L silver nitrate solution to measure the content of chloride ions in the washing solution until there is no white turbidity. Transfer the black precipitate to a beaker, add 40mL of 3mol / L perchloric acid solution, heat to 50°C, stir and dissolve for later use.

[0035] Add 12.0 g (120 mmol) of acetylacetone to 60 mL of 2 mol / L sodium hydroxide solution to react to obtain a sodium acetylacetonate solution. Slowly add the above-mentioned standby ruthenium salt solution to the acetylacetonate solution while stirring, and complete the addition After heating at 90°C for 4 hours, a dark red ruthenium(III) acetylacetonate precipitate was formed, which was extracted with 200mLx3 dichloromethane, the orga...

Embodiment 2

[0037] Replace 3mol / L perchloric acid solution with 2mol / L hexafluorophosphoric acid solution, the addition amount is 60mL, the reaction heating temperature of ruthenium salt and acetylacetonate is 100°C, the feeding amount of other reactants and experimental conditions are the same as in Example 1, and the product yield rate of 85%.

Embodiment 3

[0039] Replace 3mol / L perchloric acid solution with 2mol / L tetrafluoroboric acid solution, the addition amount is 60mL, the reaction heating temperature of ruthenium salt and acetylacetonate is 80°C, the feeding amount of other reactants and experimental conditions are the same as in Example 1, and the product yield The rate is 83%.

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Abstract

The invention discloses a method for synthesizing ruthenium acetylacetonate (III). The synthesizing method comprises the following steps: a, dissolving ruthenium trichloride hydrate into water to react with alkali to generate ruthenium hydroxide and dissolving by strong acid after washing to remove chlorine ions to obtain a ruthenium salt solution; b, reacting acyl acetone with alkali to obtain acetylacetonate; c, reacting the ruthenium salt solution with the acetylacetonate solution, generating deep red ruthenium acetylacetonate (III) precipitate under the heating condition and purifying by dichloromethane, wherein a yield is 80 to 90%, and a chlorine ion content is smaller than 50ppm. A total reaction equation is shown in a following image, wherein HL is non-coordinating anion strong acid, acac is acetylacetone acid radial which is shown in a following image, and the M is Na or K. The method disclosed by the invention has the advantages that a high yield of the ruthenium acetylacetonate (III) is ensured, a content of impurity chlorine ions is reduced at the same time, product quality is improved and is favorable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing ruthenium (III) acetylacetonate, belonging to the technical field of chemical catalyst preparation. Background technique [0002] Catalytic reactions involving noble metals are of great significance to the chemical and pharmaceutical industries. Noble metal ruthenium catalysts have excellent characteristics such as high electron transfer capability, high Lewis acidity, and low redox potential, and have been widely used in oxidation reactions, hydrogenation reactions, and hydrogen transfer. reaction. Due to the excellent catalytic performance of ruthenium catalysts and its low price compared with other noble metals, it has developed rapidly in recent years, and research in this field has gradually become a hot spot. Ruthenium(Ⅲ) acetylacetonate is generally used as a catalyst precursor for the synthesis of homogeneous catalysts and heterogeneous catalysts. It can catalyze the hydrogenation of dimethyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
CPCC07F15/0046
Inventor 刘斌潘剑明马银标沈炯黄鹏王惟
Owner 浙江微通催化新材料有限公司
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