Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF2 Cites 8 Cited by
  • 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 iodide exists and reacts in a gaseous state during the reaction, but the product propionic acid is not in a gaseous state, that is, the generated propionic acid flows out of the fixed-bed reactor in liquid form, which will inevitably cause erosion and dissolution loss of the surface active species of the catalyst
[0004] In short, the low-pressure gas-phase methanol carbonylation of acetic acid has not formed an industrial production process after decades of research and development, and the research on the more complicated gas-phase reaction process of ethanol carbonylation to propionic acid obviously still has a longer way to go

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products