Method for producing 3-(triphenylphosphine )-carbonyl hydrogenation Rh

A technology of rhodium carbonyl hydride and triphenylphosphine, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of large consumption of raw materials such as solvents, complex processes, and overall The yield is not high, and the effect of good homogeneous catalytic activity for olefin hydroformylation is achieved

Active Publication Date: 2008-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material trans-RhCl(CO)(TPP) 2 Still need to use RhCl 3 ·xH 2 O is produced by the reaction of triphenylphosphine. The preparation process is carried out in two steps. The process is complicated, the total yield is not high, and the consumption of raw materials such as solvents is large.

Method used

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  • Method for producing 3-(triphenylphosphine )-carbonyl hydrogenation Rh
  • Method for producing 3-(triphenylphosphine )-carbonyl hydrogenation Rh

Examples

Experimental program
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Effect test

Embodiment 1

[0050] In the 500ml three-necked reaction flask, add 250ml mass percentage composition and be 95% ethanol aqueous solution, and 15.7 grams triphenylphosphine (TPP), after sufficient nitrogen replacement, under nitrogen protection (atmospheric pressure) stir and be heated to 80°C. After TPP is completely dissolved, add dropwise 10ml containing 1.77g RhCl 3 ·xH 2 O (the mass percentage of rhodium is 39.5%) ethanol solution. After staying for 30 minutes, 6ml of 40% formaldehyde aqueous solution was added dropwise, and the reaction temperature should be kept at 80°C during the addition. After adding the formaldehyde, the stirring reaction was continued for 60 minutes. Then, nitrogen was replaced by hydrogen (atmospheric pressure), and 30 ml of an ethanol solution containing 0.93 g of sodium borohydride and 1.4 g of KOH was added dropwise. After continuing to react at 80° C. for 60 minutes, the reaction was stopped and cooled to below 20° C. under a hydrogen atmosphere. The so...

Embodiment 2

[0052] In a 500ml three-necked reaction flask, add 250ml of 90% ethanol aqueous solution and 18.0 grams of triphenylphosphine. After sufficient hydrogen replacement, stir and heat to 80°C under hydrogen protection (atmospheric pressure). After TPP is completely dissolved, add dropwise 10ml containing 1.77g RhCl 3 ·xH 2 O (the mass percentage of rhodium is 39.5%) ethanol solution. After staying for 20 minutes, add 8 ml of 40% formaldehyde aqueous solution, and the reaction temperature should be kept at 80° C. during the addition. After the addition of formaldehyde, the stirring reaction was continued for 50 minutes. Then, 30 ml of an ethanol solution containing 1.13 g of sodium borohydride and 0.56 g of KOH was added dropwise. After continuing to react at 80°C for 50 minutes, the reaction was stopped and cooled to below 20°C under a hydrogen atmosphere. The solvent was removed by filtration under reduced pressure, washed with 95% ethanol, water, 95% ethanol, and n-hexane re...

Embodiment 3

[0054] In a 500ml three-necked reaction flask, add 250ml of 95% ethanol aqueous solution and 17.0 grams of triphenylphosphine. After sufficient hydrogen replacement, stir (normal pressure) under hydrogen protection and heat to 80°C. After TPP is completely dissolved, add dropwise 10ml containing 1.76g RhCl 3 ·xH 2 O (the mass percentage of rhodium is 39.5%) ethanol solution. After staying for 20 minutes, 11 ml of 40% formaldehyde aqueous solution was added, and the reaction temperature should be kept at 80° C. during the addition. After adding the formaldehyde, the stirring reaction was continued for 60 minutes. Then, 30 ml of an ethanol solution containing 1.50 g of sodium borohydride and 1.0 g of KOH was added dropwise. After continuing to react at 80° C. for 60 minutes, the reaction was stopped and cooled to below 20° C. under a hydrogen atmosphere. The solvent was removed by filtration under reduced pressure, washed with 95% ethanol, water, 95% ethanol, and n-hexane re...

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Abstract

The invention relates to a preparation method of olefin hydrogen formylated homogeneous phase complex catalyst, in particular to the method of using rhodium chloride hydrate as raw material for preparing tri-(triphenyl phosphine) carbonyl hydrogenation rhodium. In the hydrogen atmosphere, alcohol-water component solvent is adopted, and rhodium chloride hydrate is adopted as raw material, and alkali metal hydrated oxide and borohydride mixture are adopted as deoxidizer to directly compose the objective product. Compared with the traditional method, the invention solves the problems of having low obtaining rate and big rhodium loss. The synthesis obtaining rate of tri-(triphenyl phosphine) carbonyl hydrogenation rhodium reaches more than 99 percent measured by rhodium content, and the toxical impurity content of element Cl is less than 0.02 percent. The homogeneous phase catalyst used for propylene hydrogen formylation aldehyde making reaction has good catalytic activity. The invention is applied to the organic chemical industry field.

Description

technical field [0001] The invention relates to a preparation method of a homogeneous complex catalyst for olefin hydroformylation, in particular to a method for preparing tris(triphenylphosphine)rhodium carbonyl hydride by using rhodium trichloride hydrate as a raw material. Background technique [0002] Tris(triphenylphosphine)rhodium carbonyl hydride RhH(CO)(TPP) 3 are α-olefins and syngas (CO and H 2 A good catalyst for the hydroformylation reaction to generate normal and isomeric aldehydes. For example, propylene and syngas in RhH(CO)(TPP) 3 In the presence of a homogeneous catalyst, n-butyraldehyde and isobutyraldehyde are produced. [0003] Rhodium is an extremely expensive rare metal, mass-produced RhH(CO)(TPP) 3 The key technology is to improve the synthesis yield and reduce rhodium loss. In addition, RhH(CO)(TPP) 3 The use as a homogeneous complexation catalyst for olefin hydroformylation also requires that the content of harmful impurities such as Cl is smal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J31/24B01J31/30
Inventor 吕顺丰彭斌
Owner CHINA PETROLEUM & CHEM CORP
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