A kind of carbonylation reaction catalyst composition and method for preparing neopentyl glycol

A carbonylation reaction and neopentyl glycol technology, which is applied in the field of carbonylation reaction catalysts and the preparation of neopentyl glycol, can solve problems such as metal catalyst deactivation, and achieve the effect of increasing yield and improving atom utilization

Active Publication Date: 2022-07-12
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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  • A kind of carbonylation reaction catalyst composition and method for preparing neopentyl glycol
  • A kind of carbonylation reaction catalyst composition and method for preparing neopentyl glycol
  • A kind of carbonylation reaction catalyst composition and method for preparing neopentyl glycol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Add 0.35g palladium acetate, 2.5g triphenylphosphine pyrrole, 1.0g lanthanum trifluoromethanesulfonate to the 1L high-pressure stirring kettle; after replacing the gas phase space of the reaction kettle with nitrogen, pressurize it with nitrogen to 2MPaG, then pass through the reaction kettle Add 350g of propyne liquid, mix evenly; after the mixed liquid in the reaction kettle is heated to 80 ℃, feed H 2 : The synthesis gas with a CO mol ratio of 1:1 reaches a pressure of 5 MPaG, and the reaction is stirred. When the pressure in the reaction kettle drops, the synthesis gas is replenished to 5 MPaG, and the temperature and pressure in the reaction kettle are kept constant, and the reaction is completed for 3h to obtain reaction solution A; Gas chromatography analysis showed that the conversion of propyne was 99.2%, and the selectivity of methacrolein was 98.6%.

[0056] Continue to heat up the reaction solution A to 130°C, feed the synthesis gas to a pressure of 20 MPaG ...

Embodiment 2

[0059] 0.11g of carbonyl rhodium, 2.2g of diphenylphosphine-naphthalenesulfonic acid and 1.1g of boron trifluoride were added to the 1L high-pressure stirred kettle; Pour in 350g of propyne liquid and mix it evenly; after heating the mixed liquid in the reaction kettle to 100°C, pass in H 2 The synthesis gas with a CO molar ratio of 1:1 was 9MPaG to a pressure of 9MPaG, and the reaction was stirred. When the pressure in the reaction kettle dropped, the synthesis gas was replenished, and the temperature and pressure in the reaction kettle were kept constant, and the reaction solution A was obtained after 3.5h of reaction. Through gas chromatography analysis, the conversion rate of propyne was 99.5%; the selectivity of methacrolein was 98.3%.

[0060] Continue to heat up the reaction solution A to 120°C, feed the synthesis gas to a pressure of 16 MPaG, and start the reaction. When the pressure in the reaction kettle drops, replenish the synthesis gas, and react for 12 h to obtai...

Embodiment 3

[0063] Add 0.4 rhodium acetylacetonate, 1.85 g triphenylphosphine-naphthalene sulfonic acid, 0.65 g copper bromide to the 1L high-pressure stirred kettle; after replacing the gas phase space of the reactor with nitrogen, pressurize it to 2MPaG with nitrogen, then pass through the reactor Add 350g of propyne liquid and mix evenly; after the mixed liquid in the reaction kettle is heated to 65°C, add H 2 The synthesis gas with a CO molar ratio of 1:1 reaches a pressure of 6 MPaG, and the reaction is stirred. When the pressure in the reaction kettle drops, the synthesis gas is replenished, and the temperature and pressure in the reaction kettle are kept constant, and the reaction solution A is obtained after the reaction is completed for 2 h. Through gas chromatography analysis, the conversion rate of propyne was 99.3%; the selectivity of methacrolein was 98.8%.

[0064] Continue to heat up the reaction solution A to 145°C, feed the synthesis gas to a pressure of 22 MPaG to start ...

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Abstract

The invention provides a carbonylation reaction catalyst composition and a method for preparing neopentyl glycol. The catalyst composition includes: a compound containing palladium or rhodium, one or more of diphenylphosphine pyrrole, triphenylphosphine pyrrole, diphenylphosphine-naphthalenesulfonic acid, and triphenylphosphine-naphthalenesulfonic acid one or more of copper bromide, p-toluenesulfonic acid, boron trifluoride, and lanthanum trifluoromethanesulfonate. The method for preparing neopentyl glycol includes the following steps: (1) carbonylation of propyne to prepare methacrolein; (2) under the action of a catalyst composition, carbonylation of methacrolein to prepare dimethylpropane Dialdehyde; (3) Hydrogenation to prepare neopentyl glycol. The catalyst composition can efficiently catalyze the carbonylation reaction of α,β-unsaturated carbonyl compounds. The method for preparing neopentyl glycol has good atom economy, low cost of raw materials, no waste water generation, and good yield.

Description

technical field [0001] The invention belongs to the technical field of fine chemical synthesis, in particular to a carbonylation reaction, and more particularly to a carbonylation reaction catalyst and a method for preparing neopentyl glycol. Background technique [0002] Neopentyl glycol (ie 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 lubricant oil additives, etc., and also used in the pharmaceutical industry. [0003] At present, the commonly used production processes for preparing neopentyl glycol include disproportionation method and condensation hydrogenation method: disproportionation method is that under the catalysis of inorganic strong...

Claims

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Application Information

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Patent Type & Authority Patents(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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