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Carbonylation reaction catalyst composition and method for preparing neopentyl glycol

A technology of carbonylation reaction and catalyst, which is applied in the field of carbonylation reaction catalyst and preparation of neopentyl glycol, and can solve problems such as metal catalyst deactivation

Active Publication Date: 2020-10-27
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above carbonylation, if the phosphine ligand-modified complex and Bronsted acid are used in a physically mixed manner, the Bronsted acid needs to be in excess, but the excess of the acid often leads to the alkylation of the phosphine ligand, resulting in the deactivation of the metal catalyst.

Method used

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  • Carbonylation reaction catalyst composition and method for preparing neopentyl glycol
  • Carbonylation reaction catalyst composition and method for preparing neopentyl glycol
  • Carbonylation reaction catalyst composition and method for preparing neopentyl glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Add 0.35g of palladium acetate, 2.5g of triphenylphosphinepyrrole, and 1.0g of lanthanum trifluoromethanesulfonate to a 1L high-pressure stirred tank; Add 350g of propyne liquid and mix evenly; after the temperature of the mixed solution in the reactor is raised to 80°C, inject H 2 : CO molar ratio 1:1 syngas to a pressure of 5MPaG, stirring reaction, when the pressure in the reactor is reduced, the synthesis gas is replenished to 5MPaG, keep the temperature and pressure in the reactor constant, and react for 3h to obtain the reaction solution A; According to gas chromatography analysis, the conversion rate of propyne was 99.2%, and the selectivity of methacrolein was 98.6%.

[0056] Continue to raise the temperature of the reaction solution A to 130°C, feed the synthesis gas to a pressure of 20MPaG to start the reaction, and replenish the synthesis gas to 5MPaG when the pressure in the reactor drops, and obtain the reaction solution B after 10 hours of reaction; releas...

Embodiment 2

[0059] Add 0.11g rhodium carbonyl, 2.2g diphenylphosphine-naphthalenesulfonic acid, and 1.1g boron trifluoride to a 1L high-pressure stirred tank; Pass in 350g of propyne liquid and mix evenly; after raising the temperature of the mixed liquid in the reactor to 100°C, pass in H 2 :CO molar ratio of 1:1 synthesis gas to a pressure of 9MPaG, stirring and reacting, when the pressure in the reactor drops, the synthesis gas is replenished, the temperature and pressure in the reactor are kept constant, and the reaction solution A is obtained after 3.5 hours of reaction. According to gas chromatography analysis, the conversion rate of propyne is 99.5%; the selectivity of methacrolein is 98.3%.

[0060] Continue to raise the temperature of the reaction solution A to 120°C, feed the synthesis gas to a pressure of 16MPaG, and start the reaction. When the pressure in the reactor drops, the synthesis gas is replenished, and the reaction solution B is obtained after 12 hours of reaction; a...

Embodiment 3

[0063] Add 0.4 rhodium acetylacetonate, 1.85g triphenylphosphine-naphthalenesulfonic acid, and 0.65g copper bromide to a 1L high-pressure stirred tank; Add 350g of propyne liquid and mix evenly; after the temperature of the mixed solution in the reactor is raised to 65°C, inject H 2 :CO molar ratio of 1:1 synthesis gas to a pressure of 6MPaG, stirring and reacting, when the pressure in the reactor drops, the synthesis gas is replenished, the temperature and pressure in the reactor are kept constant, and the reaction solution A is obtained after 2 hours of reaction. According to gas chromatography analysis, the conversion rate of propyne is 99.3%; the selectivity of methacrolein is 98.8%.

[0064] Continue to raise the temperature of the reaction solution A to 145°C, feed the synthesis gas to the pressure of 22MPaG to start the reaction, and replenish the synthesis gas when the pressure in the reactor drops, and react for 14 hours to obtain the reaction solution B; after the re...

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Abstract

The invention provides a carbonylation reaction catalyst composition and a method for preparing neopentyl glycol. The catalyst composition comprises one or more of a palladium or rhodium-containing compound, diphenylphosphine pyrrole, triphenylphosphine pyrrole, diphenylphosphine-naphthalene sulfonic acid and triphenylphosphine-naphthalene sulfonic acid, and one or more of copper bromide, p-toluenesulfonic acid, boron trifluoride and lanthanum trifluoromethanesulfonate. The method for preparing neopentyl glycol comprises the following steps: (1) carrying out carbonylation on propyne to preparemethylacrolein; (2) under the action of a catalyst composition, methylacrolein is subjected to carbonylation to prepare dimethyl malonaldehyde; and (3) preparing neopentyl glycol by hydrogenation. The catalyst composition can be used for efficiently catalyzing the carbonylation reaction of the alpha, beta-unsaturated carbonyl compound. The method for preparing neopentyl glycol is good in atom economy, low in raw material cost, free of wastewater generation and relatively good in yield.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, and specifically relates to carbonylation reaction, more specifically to a carbonylation reaction catalyst and a method for preparing neopentyl glycol. Background technique [0002] Neopentyl glycol (2,2-dimethyl-1,3-propanediol, Neopentyl glycol, NPG for short) is an important chemical intermediate. It is mainly used in the production of unsaturated resins, polyester powder coatings, oil-free alkyd resins, polyurethane foams, plasticizers for elastomers, synthetic plasticizers, surfactants, insulating materials, printing inks, polymerization inhibitors, Synthetic aviation lubricating oil additives, etc., and is also used in the pharmaceutical industry. [0003] The current production process for preparing neopentyl glycol includes disproportionation method and condensation hydrogenation method: the disproportionation method is catalyzed by an inorganic strong base, formaldehyde ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/20B01J31/22B01J31/24C07C29/141C07C31/20B01J31/30C07C45/50C07C47/22C07C47/21
CPCB01J31/2239B01J31/2234B01J31/20B01J31/2404B01J31/2447B01J31/30C07C45/50C07C29/141B01J2231/321B01J2531/822B01J2531/824B01J2540/32B01J2540/40C07C47/22C07C47/21C07C31/20Y02P20/584
Inventor 王鹏马岩龙孙文龙修维晓张智慧袁帅
Owner WANHUA CHEM GRP CO LTD
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