A kind of preparation method of tri[tris (m-sulfosodium phenyl) phosphine] rhodium chloride catalyst

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

Active Publication Date: 2017-11-07
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-sulfonate phenyl)phosphine existing in the existing preparation technology , long reaction time, many steps, low yield and complicated separation operation and other technical problems

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  • A kind of preparation method of tri[tris (m-sulfosodium phenyl) phosphine] rhodium chloride catalyst

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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 invention belongs to the technical field of catalyst preparation, and is a preparation method of tris[tris(m-sodium phenyl sulfonate phenyl)phosphine]rhodium chloride catalyst. The method is as follows: under nitrogen protection, ascorbate and rhodium chloride are mixed Dissolve it in absolute alcohol, and add it into the aqueous solution of tris(m-sodium sulfonate phenyl)phosphine at 60°C to 100°C to react for 0.5 hours to 2 hours. After the reaction was completed, alcohol precipitation was added in the reaction solution, and the target catalyst tris[tris(m-sulfonate phenyl)phosphine]rhodium chloride was separated and recovered. The invention has the advantages that the method has the advantages of easy availability of raw materials, less dosage of ligand tris(m-sodium sulfonate phenyl)phosphine, simple preparation process, high product yield and good quality. Catalysts can be used in hydroformylation reactions, as well as in hydrogenation 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 two-phase olefin hydroformylation (B. Cornils, W.A. Herrmann (Eds.), Aqueous-Phase Organometallic Catalysis, 2nd ed., Wiley-VCH, Weinheim, 2004) can be solved by a simple liquid-liquid separation The separation of the aqueous phase containing the catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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