Preparation method of catalyst for synthesizing propionic acid by ethanol carbonylation, and application thereof

A catalyst and chemical synthesis technology, applied in the field of ethanol carbonylation reaction to prepare propionic acid, can solve the problems of surface active species scouring, active species loss, affecting catalyst life and performance, etc.

Inactive Publication Date: 2012-11-28
JIANGSU SOPO GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although theoretically speaking, the gas phase reaction device is simple, convenient for product separation, and less corrosive to equipment, but for the reaction of ethanol carbonylation of propionic acid, there are considerable limitations: (1) The loss of active species of the catalyst , the carbon on the surface of this type of strong exothermic reaction catalyst, etc., all directly affect the life and performance of the catalyst; (2) the dew point of the product propionic acid in the reaction system, according to literature reports, the reaction pressure and temperature can meet the requirements of ethanol and Ethyl io

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation method of the copolymer rhodium catalyst of ethanol carbonylation propionic acid, the steps are as follows:

[0016] (1) Preparation of catalyst ligand

[0017] Weigh 0.2mol of 2-vinylpyridine monomer and 0.05mol of acrolein methyl ester monomer and mix with 1.19g of azobisisobutyronitrile, add to 70ml of benzene solvent, and react at 60°C for 24 hours under stirring , cooled to room temperature, and precipitated with petroleum ether to obtain the copolymer ligand PVA-1.

[0018] (2) Preparation of catalyst

[0019] The PVA-1 copolymer that takes 1 weight part is dissolved in the acetic acid of 50 weight parts, after stirring and dissolving, add dichlorotetracarbonyl dirhodium, the addition is 3% of multipolymer by rhodium weight, reacts after 30 minutes, Ethanol was added to dissolve the sodium tetraphenylborate solution equimolar to rhodium, and the stirring was continued for 10 minutes. Precipitated with ether, and the catalyst obtained by f...

Embodiment 2

[0022] (1) Preparation of catalyst ligand

[0023] Weigh 0.2mol of 2-vinylpyridine monomer and 0.02mol of acrolein methyl ester monomer and mix with 0.23g of azobisisobutyronitrile, add to 70ml of benzene solvent, and react at 70°C for 10 hours under stirring , cooled to room temperature, and precipitated with petroleum ether to obtain the copolymer ligand PVA-2.

[0024] (2) Preparation of catalyst

[0025] The PVA-2 multipolymer that takes 1 weight part is dissolved in the acetic acid of 50 weight parts, after stirring and dissolving, add dichlorotetracarbonyl dirhodium, the addition is 5% of multipolymer by rhodium weight, reacts after 30 minutes, Ethanol was added to dissolve the sodium tetraphenylborate solution equimolar to rhodium, and the stirring was continued for 10 minutes. Precipitation with ether, and the catalyst obtained by filtration were marked as PVA-2-Rh.

[0026] To prepare propionic acid by catalyzing the carbonylation reaction of ethanol, put 45ml o...

Embodiment 3

[0028] (1) Preparation of catalyst ligand

[0029] Weigh 0.2mol of 2-vinylpyridine monomer and 0.10mol of acrolein methyl ester monomer and mix with 0.75g of azobisisobutyronitrile, add to 70ml of benzene solvent, and react at 65°C for 18 hours under stirring , cooled to room temperature, and precipitated with petroleum ether to obtain the copolymer ligand PVA-3.

[0030] (2) Preparation of catalyst

[0031] The PVA-3 multipolymer that takes 1 weight part is dissolved in the acetic acid of 50 weight parts, after stirring and dissolving, add dichlorotetracarbonyl dirhodium, the addition is 10% of multipolymer by rhodium weight, reacts after 30 minutes, Ethanol was added to dissolve the sodium tetraphenylborate solution equimolar to rhodium, and the stirring was continued for 20 minutes, and the catalyst was precipitated with ether, and the catalyst obtained by filtration was marked as PVA-3-Rh.

[0032] To prepare propionic acid by catalyzing the carbonylation reaction of eth...

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PUM

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Abstract

The invention relates to a preparation method of a catalyst for synthesizing propionic acid by ethanol carbonylation, and an application of the catalyst. The catalyst is prepared by the following steps of: taking 2-vinyl pyridine and acraldehyde as monomers, benzene as a solvent and azodiisobutyronitrile as an initiator; adopting a free-radical solution polymerization method, and using petroleum ether for precipitation; carrying out vacuum drying to be at constant weight at the temperature of 60-80 DEG C to obtain a catalyst ligand; dissolving the obtained catalyst ligand in acetic acid, adding dichloro-tetracarbonyl-dirhodium, and carrying out reaction for 10-30min; and adding a precipitator (sodium tetraphenylborate), and continuously stirring for 5-20min to obtain a copolymer rhodium catalyst. The catalyst can be used for catalyzing ethanol carbonylation to synthesize the propionic acid with high selectivity.

Description

technical field [0001] The invention belongs to the field of preparing propionic acid by carbonylation reaction of ethanol, and in particular relates to a catalyst and a preparation method thereof. Background technique [0002] Propionic acid is an important basic chemical raw material. Propionic acid and its ester derivatives are widely used in industrial organic synthesis, food and feed preservation, pesticides, spices, cosmetics and medicine. [0003] The main processes for industrial production of propionic acid include Repa method, propionaldehyde oxidation method and light hydrocarbon oxidation method. While these methods are successfully applied to industrial production, they also show obvious shortcomings, such as high temperature requirements (250-320°C); high pressure (10-30MPa) requirements; cumbersome process flow; complex reaction liquid composition, requiring special purification devices Wait. In order to solve the shortcomings of the current industrial p...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C53/122C07C51/12
Inventor 宋勤华袁国卿邵守言闫芳凌晨夏景峰
Owner JIANGSU SOPO GRP
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