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Rhodium catalyst for acetic oxide carbonyl synthesis from methyl acetate and preparation thereof

A technology of oxo synthesis and methyl acetate, which is applied in the direction of carboxylic anhydride preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., which can solve the problem of catalyst stability or/and activity and solubility and other problems, to achieve the effects of reducing flash and evaporation load, improving production efficiency, good stability and solubility

Active Publication Date: 2008-10-08
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of high activity, and have the novel catalyst of methyl acetate carbonylation acetic anhydride with better stability and solubility, to overcome the unsatisfactory problems such as original catalyst stability or / and activity, solubility defect

Method used

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  • Rhodium catalyst for acetic oxide carbonyl synthesis from methyl acetate and preparation thereof
  • Rhodium catalyst for acetic oxide carbonyl synthesis from methyl acetate and preparation thereof
  • Rhodium catalyst for acetic oxide carbonyl synthesis from methyl acetate and preparation thereof

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Embodiment 1

[0028] The rhodium catalyst for the carbonylation of methyl acetate to synthesize acetic anhydride in the present embodiment is a cis-dicarbonylrhodium cationic structure catalyst formed by the action of rhodium carbonyl and a ligand, which has the structure of the following general formula I, and is a chelating type square plane complex, Its cation part is cis-dicarbonyl rhodium cation, and its ligand is acetylmorpholine;

[0029]

[0030] where X is BPh 4 .

[0031] The preparation method of the above-mentioned rhodium catalyst of the present embodiment is as follows:

[0032] Weigh 0.13 g (0.01 mol) of acetylmorpholine, dissolve it in 10 ml of methanol, add 0.21 g (0.0005 mol) of tetrachlorodicarbonyl dirhodium in 20 ml of methanol solution at 40°C, then add 0.15 g (0.0004 mol) of methanol solution. ) 10 ml aqueous solution of sodium tetraphenylborate, filtered, the obtained yellow precipitate was washed twice with water and methanol respectively, and dried under reduc...

Embodiment 2

[0034] The rhodium catalyst for the carbonylation of methyl acetate to synthesize acetic anhydride in the present embodiment is a cis-dicarbonylrhodium cationic structure catalyst formed by the action of rhodium carbonyl and a ligand, which has the structure of the following general formula I, and is a chelating type square plane complex, Its cation part is cis-dicarbonyl rhodium cation, and its ligand is acetylmorpholine;

[0035]

[0036] Wherein, X is Cl.

[0037] The preparation method of the above-mentioned rhodium catalyst of the present embodiment is as follows:

[0038] Weigh 0.26 g (0.002 mol) of acetylmorpholine, dissolve it in 20 ml of acetic acid, add 0.41 g (0.001 mol) of 20 ml of acetic acid solution dissolved in tetrachlorodicarbonyl dirhodium at 50°C, then add 0.05 g (0.0008 mol) of acetic acid solution. ) aqueous solution of 15 ml of sodium chloride, filtered, the obtained yellow precipitate was washed 3 times with water and methanol respectively, and drie...

Embodiment 3

[0040] The rhodium catalyst for the carbonylation of methyl acetate to synthesize acetic anhydride in the present embodiment is a cis-dicarbonylrhodium cationic structure catalyst formed by the action of rhodium carbonyl and a ligand, which has the structure of the following general formula I, and is a chelating type square plane complex, Its cation part is cis-dicarbonyl rhodium cation, and its ligand is acetylmorpholine;

[0041]

[0042] where X is I.

[0043] The preparation method of the above-mentioned rhodium catalyst of the present embodiment is as follows:

[0044] Weigh 0.9 g (0.007 mol) of acetylmorpholine, dissolve it in 50 ml of ethanol, add 0.67 g (0.001 mol) of 15 ml of ethanolic solution containing 0.67 g (0.001 mol) of tetraiododicarbonyl dirhodium at 10°C, then add 0.33 g (0.002 mol of ethanol) ) 20 ml aqueous solution of potassium iodide, filtered, the obtained yellow precipitate was washed with water and methanol once, and dried under reduced pressure a...

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Abstract

The present invention discloses a rhodium catalyst for synthesizing acetic anhydride by acid methyl carbonyl, which is a cis-dicarbonyl rhodium cation structural catalyst formed by carbonyl rhodium and ligand function; the catalyst is a chelate square plane complex; the cation part of the catalyst is cis-dicarbonyl rhodium cation and the ligand is acetyl morpholine. The catalyst not only shows excellent thermal stability, but also keeps excellent catalyzing activity during the reaction of synthesizing acetic anhydride by acid methyl carbonyl; simultaneously the solubility of the catalyst species can also be increased in a reaction system, thus avoiding the addition of acetic acid and / or acetic anhydride as a catalyst solvent in the industrial production, thus effectively reducing the load of flash evaporation and evaporation and improving the manufacture efficiency of acetic anhydride synthesis by acid methyl carbonyl. The present invention also discloses a preparation method of synthesizing acetic anhydride by acid methyl carbonyl by the rhodium catalyst..

Description

Technical field [0001] The invention belongs to the technical field of chemical synthesis, and particularly relates to a catalyst for carbonyl synthesis of acetic anhydride from methyl acetate and a preparation method thereof. Background technique [0002] Acetic anhydride is an important organic chemical raw material, widely used in many fields such as medicine, dyes, pesticides, spices and acid derivatives, and is an important part of the national economy. [0003] The acetic anhydride oxo synthesis method has the advantages of short process, good product quality, low consumption, and low emission of three wastes, etc., and represents the current advanced technology level of production. However, the activation energy of the carbonylation reaction to synthesize acetic anhydride is very high and must be achieved with the help of a catalyst. Therefore, the development of high-performance catalysts has always been a core issue in the oxo synthesis of acetic anhydride. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J23/46C07C51/56C07C53/12
Inventor 张华西曾健王晓东雍永祜廖炯李荣
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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