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Catalyst for preparing enol from alkynol through partial hydrogenation, preparation method of the catalyst, and method for preparing enol by using the catalyst

A hydrogenation catalyst and catalyst technology are applied in hydrogenation preparation, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., and can solve the problems of affecting product odor, increasing equipment investment, and difficulty in separation, etc. The quality and odor achieved are not affected, the effect is long-lasting, and the product selectivity is high.

Active Publication Date: 2019-08-16
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Quinoline is usually separated from the product by rectification, which is difficult to separate and remove trace amounts of quinoline, which affects product odor and increases equipment investment

Method used

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  • Catalyst for preparing enol from alkynol through partial hydrogenation, preparation method of the catalyst, and method for preparing enol by using the catalyst
  • Catalyst for preparing enol from alkynol through partial hydrogenation, preparation method of the catalyst, and method for preparing enol by using the catalyst
  • Catalyst for preparing enol from alkynol through partial hydrogenation, preparation method of the catalyst, and method for preparing enol by using the catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] First, 100 g of ethanol, 1.0 g of 5% Pd-5% Pb palladium-calcium carbonate catalyst, and 0.5 g of 1 wt % zinc acetate aqueous solution were added to the autoclave, and the autoclave was sealed and replaced with nitrogen 6 times. Use synthesis gas containing carbon monoxide and hydrogen with a volume ratio of 1:1 to replace 6 times, turn on the stirring paddle, keep the pressure of synthesis gas (absolute pressure) 0.2MPa, and keep the inner temperature of the reactor at 30°C for 12 hours. Stop stirring and vent gas. A catalyst for the partial hydrogenation of acetylenic alcohols to enols is obtained after filtration.

[0051] First, add 294.5 g of dehydroisophytol, 2.0 g of a catalyst for enol preparation by partial hydrogenation of acetylenic alcohols, and 250 g of ethanol to the autoclave, seal the autoclave, replace 6 times with nitrogen, and then replace 6 times with hydrogen, and turn on the stirring paddle. Keep the hydrogen pressure at 2.0 MPa (gauge pressure), k...

Embodiment 2

[0053] First, 100 g of n-hexane, 1.0 g of 5% Pd-5% Pb palladium-calcium carbonate catalyst, 0.5 g of 0.5 wt % triiron dodecacarbonyl ethanol solution were added to the autoclave, and the autoclave was sealed and replaced with nitrogen 6 times. Use synthesis gas containing carbon monoxide and hydrogen with a volume ratio of 1:1 to replace 6 times, turn on the stirring paddle, keep the pressure of synthesis gas (absolute pressure) at 1.0 MPa, and keep the inner temperature of the reactor at 30°C for 12 hours. Stop stirring and vent gas. A catalyst for the partial hydrogenation of acetylenic alcohols to enols is obtained after filtration.

[0054] First, add 184.3 g of dehydrolinalool, 1.0 g of a catalyst for preparing enol by partial hydrogenation of acetylenic alcohol, and 500 g of n-hexane into the autoclave, seal the autoclave, replace 6 times with nitrogen, and then replace 6 times with hydrogen, and turn on the stirring paddle , keep the hydrogen pressure at 1.0MPa (gauge ...

Embodiment 3

[0056] First, 100 g of ethanol, 1.0 g of 5% Pd-0% Pb palladium-calcium carbonate catalyst, and 1.74 g of 1 wt % ferrous acetate aqueous solution were added to the autoclave, and the autoclave was sealed and replaced with nitrogen 6 times. Use synthesis gas containing carbon monoxide and hydrogen with a volume ratio of 6:4 to replace 6 times, turn on the stirring paddle, keep the pressure of synthesis gas (absolute pressure) 0.5MPa, and keep the inner temperature of the reactor at 30°C for 8 hours. Stop stirring and vent gas. A catalyst for the partial hydrogenation of acetylenic alcohols to enols is obtained after filtration.

[0057] First, add 154.1 g of dihydrodehydrolinalool, 3.0 g of a catalyst for preparing enol by partial hydrogenation of acetylenic alcohol, and 450 g of ethanol into the autoclave, seal the autoclave, replace 6 times with nitrogen, and then replace 6 times with hydrogen, and start stirring paddle, keep the hydrogen pressure at 2.0 MPa (gauge pressure),...

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Abstract

The invention provides a catalyst for preparing enol through partial hydrogenation of alkynol, a preparation method of the catalyst and a method for preparing the enol by using the catalyst. A metal salt or a metal carbonyl compound substance is added into a catalyst system, and the catalyst system is moderately poisoned in a synthesis gas atmosphere to prepare the hydrogenation catalyst. The catalyst is poisoned and then used for partial hydrogenation of alkynol to prepare enol. The catalyst has the advantages of mild reaction conditions, high product selectivity and the like.

Description

technical field [0001] The invention relates to a catalyst and preparation method for preparing enol by partial hydrogenation of acetylenic alcohol, and a method for preparing enol by partial hydrogenation of acetylenic alcohol using the catalyst. The product enol is the main intermediate for producing VE and also DV chrysanthemic acid (Pyrethrin intermediate), synthetic vitamin A, vitamin K1, carotenoid intermediate and some spices. Background technique [0002] Partial hydrogenation of acetylene alcohols to prepare corresponding enols is one of the methods for fine chemical industry to produce intermediates and their chemical products. K1, carotenoid intermediates, synthetic rubber monomers and spices. [0003] Its general reaction formula is: [0004] [0005] Among them, R 1 , R 2 For hydrogen or hydrocarbon group. [0006] The catalyst widely used in industry for the selective hydrogenation of acetylenic alcohols is Lindlar catalyst. This type of catalyst is to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C29/17C07C33/02C07C33/025C07C33/03
CPCB01J31/28C07C29/17C07C33/02C07C33/025C07C33/03
Inventor 鲍元野宋军伟宋明焱李金明张永振黎源
Owner WANHUA CHEM GRP CO LTD
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