Tris[tris(m-sodium sulfonate phenyl)phosphine]rhodium chloride catalyst preparation method

A sodium sulfonate and rhodium chloride technology, which is applied in the field of preparation of tri[triphosphine] rhodium chloride catalyst, can solve the problems of long reaction time, many steps, complicated separation operation, etc.

Active Publication Date: 2016-06-01
PETROCHINA CO LTD
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Problems solved by technology

The invention relates to a preparation method of tris[tris(m-sulfonate phenyl)phosphine]rhodium chloride catalyst, which mainly solves the large amount of raw material tris(m-sulfo

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  • Tris[tris(m-sodium sulfonate phenyl)phosphine]rhodium chloride catalyst preparation method

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preparation example Construction

[0039] The concrete steps of the preparation method of three [three (inter-sodium sulfonate phenyl) phosphine] rhodium chloride catalysts involved in the present invention are as follows:

[0040] The first step: pass inert gas into the container for protection;

[0041] The second step: configure TPPS solution;

[0042] The third step: heating;

[0043] The fourth step: add ascorbate and rhodium chloride mixed solution to the container;

[0044] The fifth step: heat preservation;

[0045] Step 6: Precipitate, separate, and dry to obtain the product.

Embodiment 1

[0047] To 150 milliliters, electromagnetic stirrer is equipped with, and thermometer, reflux cold tube and three-neck round-bottomed flask of constant pressure dropping funnel are led to protect with nitrogen;

[0048] Add a solution prepared by dissolving 7.0g TPPTS in 10ml pure water into a three-necked round bottom flask and heat to 90°C;

[0049] Then, 0.5 g of RhCl 3 ·3H 2 O (chemically pure, rhodium content 41.72%) and 0.15 gram of ascorbic acid (sodium salt) are dissolved in the solution of 10 milliliters of dehydrated alcohols and add in the round bottom flask through the constant pressure dropping funnel, keep temperature 90 ℃;

[0050] Reflux for 1 hour, the solution turns brownish red, stop heating;

[0051] About 50 ml of absolute ethanol was added dropwise, and a brown-red precipitate was precipitated, filtered, and the filter cake was washed with ethanol to obtain a brown-red solid;

[0052] The solid catalyst was placed in a vacuum oven at 70° C. and dried un...

Embodiment 2

[0054] To 150 milliliters, electromagnetic stirrer is equipped with, and thermometer, reflux cold tube and three-neck round-bottomed flask of constant pressure dropping funnel are led to protect with nitrogen;

[0055] Add a solution prepared by dissolving 7.0g TPPTS in 10ml pure water into a three-necked round bottom flask and heat to 82°C;

[0056] Then, 0.5 g of RhCl 3 ·3H 2 O (chemically pure, rhodium content 41.72%) and 0.15 gram of ascorbic acid (sodium salt) are dissolved in the solution of 10 milliliters of dehydrated alcohols and add in the round bottom flask through the constant pressure dropping funnel, keep temperature 82 ℃;

[0057] Reflux for 1 hour, the solution turns brownish red, stop heating;

[0058] About 50 ml of absolute ethanol was added dropwise, and a brown-red precipitate was precipitated, filtered, and the filter cake was washed with ethanol to obtain a brown-red solid;

[0059] The solid catalyst was placed in a vacuum oven at 70° C. and dried un...

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Abstract

The present invention belongs to the technical field of catalyst preparation, and relates to a tris[tris(m-sodium sulfonate phenyl)phosphine]rhodium chloride catalyst preparation method, which comprises: under nitrogen protection, dissolving an ascorbate and rhodium chloride in an anhydrous alcohol in a mixed manner, adding to a tris(m-sodium sulfonate phenyl)phosphine aqueous solution at a temperature of 60-100 DEG C, carrying out a reaction for 0.5-2 h, adding an alcohol to the reaction solution after completing the reaction, precipitating, and separating and recovering the target catalyst tris[tris(m-sodium sulfonate phenyl)phosphine]rhodium chloride. According to the present invention, the method has advantages of easily available raw materials, less ligand tris(m-sodium sulfonate phenyl)phosphine consumption, simple preparation process, high product yield, and good quality; and the catalyst can be used for hydroformylation reactions, hydrogenation reactions, and carbon-carbon coupling reactions.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation and relates to a method for preparing a tris[tris(m-sulfonate phenyl)phosphine]rhodium chloride catalyst. The invention is not only applied to the water-organic two-phase olefin hydroformylation reaction In addition, it is also suitable for water-organic two-phase hydrogenation reaction and carbon-carbon coupling reaction. technical background [0002] Olefin hydroformylation is a reaction in which olefins and synthesis gas are catalyzed by a catalyst to generate aldehydes with one more carbon. The resulting aldehydes are condensed and hydrogenated to produce alcohols, which are widely used in the field of plasticizers. Aqueous-organic biphasic olefin hydroformylation (B. Cornils, W.A. Herrmann (Eds.), Aqueous-Phase Organometallic Catalysis, 2nded., Wiley-VCH, Weinheim, 2004) can solve catalyst-containing The separation of the aqueous phase of the product and the organic phase of the...

Claims

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Application Information

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IPC IPC(8): B01J31/24
Inventor 肖海成袁茂林白玉洁王斯晗李贤均褚洪岭王桂芝陈华杨春基曾群英关伟宏杜海张宝军贺德福徐显明戴俊源李文鹏李群英孟祥军刘剑汪涵崔锡红辛虹邴淑秋包静严陈丽晶徐群郭桂悦梁立伟赵晶莹
Owner PETROCHINA CO LTD
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