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A kind of preparation method containing rhodium, ruthenium bimetallic catalyst

A bimetallic catalyst, sodium hexachlororuthenate technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low yield and cumbersome process, and achieve high yield , Less restricted conditions, simple operation

Active Publication Date: 2017-12-19
CHINA PETROLEUM & CHEM CORP +1
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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 overcome the defects of low yield and cumbersome technical process in the prior art, and provide a kind of preparation method containing rhodium and ruthenium bimetallic catalyst

Method used

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Examples

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preparation example Construction

[0018] The invention provides a method for preparing rhodium-containing and ruthenium bimetallic catalysts, wherein the preparation method comprises: mixing sodium / potassium hexachlororhodate, sodium / potassium hexachlororuthenate with organic ligands, and mixing them in the presence of alcohol-water mixture Under the protection of inert gas, and under the ultrasonic power of 100-4000W, preferably 1000-3000w ultrasonic vibration, react at 40-100°C, preferably 60-90°C, to obtain a reaction mixture; cool the reaction mixture After reaching 0-5°C, filter, wash and dry in sequence.

[0019] Among the present invention, sodium hexachlororhodium / potassium refers to sodium hexachlororhodate and / or potassium hexachlororhodium, preferably sodium hexachlororhodium; Sodium hexachlororhodate / potassium refers to hexachlororuthenate Sodium and / or potassium hexachlororuthenate, preferably sodium hexachlororuthenate.

[0020] According to the method of the present invention, the ratio of the ...

Embodiment 1

[0034] This embodiment is used for illustrating and adopts the method of the present invention to prepare rhodium-containing, ruthenium bimetallic catalyst

[0035] (1) After mixing 16.5mmol sodium hexachlororhodate, 16.5mmol sodium hexachlororuthenate and 200mmol triphenylphosphine, under nitrogen protection, add to 1500mL ethanol / water mixed solution (water and absolute ethanol The volume ratio is 0.1:1), heated to 78°C, and reacted with ultrasonic waves (power 1000W) for 1.5 hours to obtain a reaction mixture for use;

[0036] (2) Cool the reaction mixture to 0°C with an ice-water bath, filter, wash the filter cake with 100ml of deionized water, 100ml of absolute ethanol, and 100ml of absolute ether, and dry it in vacuum to obtain the product. The yield in terms of rhodium is 93.1%.

Embodiment 2

[0038] This embodiment is used for illustrating and adopts the method of the present invention to prepare rhodium-containing, ruthenium bimetallic catalyst

[0039] (1) After mixing 25mmol sodium hexachlororhodate, 8mmol sodium hexachlororuthenate and 200mmol triphenylphosphine, under nitrogen protection, add to 1500mL ethanol / water mixed solution (volume ratio of water to absolute ethanol 0.3:1), heated to 60°C, and reacted with ultrasonic waves (power 2000W) for 1 hour to obtain a reaction mixture for use;

[0040] (2) Cool the reaction mixture to 2°C in an ice-water bath, filter, wash the filter cake with 100ml deionized water, 100ml absolute ethanol, and 100ml anhydrous ether, and dry it in vacuum to obtain the product. The yield in terms of rhodium is 91.3%.

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Abstract

The invention provides a preparation method of an organic bimetallic complex compound catalyst containing rhodium and ruthenium. The preparation method uses sodium / potassium hexachlororhodate(III) and sodium / potassium hexachlororuthenate(III) as raw materials instead of rhodium trichloride and ruthenium trichloride which are complicated to prepare, employs a supersonic wave-assisted reaction mode, and takes alcohol and water systems to replace the ethanol as solvents. The required solvent amount is greatly reduced, the usage of a large amount of organic solvent is avoided, and therefore the operation for preparing the organic bimetallic catalyst containing the rhodium and the ruthenium according to the invention method is simple, and the production cost is greatly reduced. Meanwhile reactant can reach high yield in a short time, and the method has less controlled conditions, and facilitates industrial scaling-up.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a method for preparing a bimetallic catalyst containing rhodium and ruthenium. Background technique [0002] The selective hydrogenation of carbon-carbon double bonds (C=C) in polymers has always been a hot research area of ​​concern to chemists. Rhodium metal organic complex catalysts have the characteristics of high hydrogenation efficiency and high selectivity, but the abundance of this element is small, expensive, and the application cost is high. To further expand the selective hydrogenation of carbon-carbon double bonds (C=C) in polymers, new alternative catalysts have been continuously tried. Patent ZL97110896.X used Rh and Ru bimetallic catalysts to selectively hydrogenate carbon-carbon double bonds (C=C), and achieved good results. The synthesized Rh and Ru bimetallic catalysts all use rhodium trichloride and ruthenium trichloride and various organic ligan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00B01J31/22B01J37/34
CPCB01J31/2404B01J37/34B01J2531/821B01J2531/822C07F15/008
Inventor 毕海鹏李传清李建成刘天鹤
Owner CHINA PETROLEUM & CHEM CORP
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