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A kind of catalyst for the semihydrogenation of acetylenic alcohol to enol and its preparation method

A catalyst and semi-hydrogenation technology, applied in the direction of hydrogenation preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as unsuitable for industrialization and adverse environmental effects, and achieve high product selectivity and yield, The effect of long service life and high reaction conversion rate

Active Publication Date: 2018-08-28
重庆建峰新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Patent CN1966480A discloses a kind of Pd / C poisoned by lead as a catalyst for the semi-hydrogenation of 1,4-butynediol, and synthesizes 1,4-butynediol at 35-45°C and 0.6-1.7MPa , this catalyst contains heavy metal lead, which has adverse effects on the environment and is not suitable for industrialization

Method used

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  • A kind of catalyst for the semihydrogenation of acetylenic alcohol to enol and its preparation method
  • A kind of catalyst for the semihydrogenation of acetylenic alcohol to enol and its preparation method
  • A kind of catalyst for the semihydrogenation of acetylenic alcohol to enol and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Add 400mL of concentrated hydrochloric acid with a concentration of 37% to 0.45kg of palladium chloride powder and heat to 60°C to dissolve to form solution A; add 10L of deionized water to 5kg of calcium carbonate with a particle size of 200 mesh and stir for 30min to form a milky white milky cloud Solution B; Dissolve 375g of anhydrous sodium carbonate with 7.5L of deionized water at room temperature and slowly add 305mL of formic acid dropwise until no gas is released (at this time the temperature is about 60°C) to form solution C; then add solution A to In emulsion B, after stirring for 5 minutes, heat up to 80°C and keep warm for 10 minutes to obtain brownish-yellow emulsion AB; then quickly add solution C with a temperature of about 60°C to emulsion AB at one time, and heat up to 85°C , then keep warm and stir for 30min until no gas is released, filter while hot, and wash the filter cake 3 times with deionized water until there is no Cl - , dried and weighed to ob...

Embodiment 2

[0056] Add 400mL of concentrated hydrochloric acid with a concentration of 37% to 0.45kg of palladium chloride powder and heat to 60°C to dissolve to form solution A; add 10L of deionized water to 5kg of calcium carbonate with a particle size of 200 mesh and stir for 30min to form a milky white milky cloud Solution B; Dissolve 375g of anhydrous sodium carbonate with 7.5L of deionized water at room temperature and slowly add 305mL of formic acid dropwise until no gas is released (at this time the temperature is about 60°C) to form solution C; then add solution A to In emulsion B, after stirring for 5 minutes, heat up to 80°C and keep warm for 10 minutes to obtain brownish-yellow emulsion AB; then quickly add solution C with a temperature of about 60°C to emulsion AB at one time, and heat up to 85°C , then keep warm and stir for 30min until no gas is released, filter while hot, and wash the filter cake 3 times with deionized water until there is no Cl - , dried and weighed to ob...

Embodiment 3

[0058] Add 400mL of concentrated hydrochloric acid with a concentration of 37% to 0.45kg of palladium chloride powder and heat to 60°C to dissolve to form solution A; add 10L of deionized water to 5kg of calcium carbonate with a particle size of 200 mesh and stir for 30min to form a milky white milky cloud Solution B; Dissolve 375g of anhydrous sodium carbonate with 7.5L of deionized water at room temperature and slowly add 305mL of formic acid dropwise until no gas is released (at this time the temperature is about 60°C) to form solution C; then add solution A to In emulsion B, after stirring for 5 minutes, heat up to 80°C and keep warm for 10 minutes to obtain brownish-yellow emulsion AB; then quickly add solution C with a temperature of about 60°C to emulsion AB at one time, and heat up to 85°C , then keep warm and stir for 30min until no gas is released, filter while hot, and wash the filter cake 3 times with deionized water until there is no Cl - , dried and weighed to ob...

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Abstract

The invention discloses a catalyst for preparation of enol through alkynol semi-hydrogenation and a preparation method of the catalyst. The preparation method is characterized in that Pd is taken as an active component, CaCO3 is taken as a carrier, acetate of Fe, Mg, Ca and Zn is taken as an additive, the mass content of the active component is 1%-10%, the content of the additive is 3%-7%, and the catalyst is prepared with a thermal filtration method. The catalyst shows higher reaction conversion rate as well as high product selectivity and yield in reactions for preparation of enol through alkynol semi-hydrogenation such as preparation of 1,4-butylene glycol from 1,4-butynediol, preparation of methyl butenol from methyl butynol, preparation of vinyl isopropanol from acetenyl isopropanol and the like, the catalyst has longer service life, particularly shows better catalytic performance in the reaction for preparation of 1,4-butylene glycol through 1,4-butynediol semi-hydrogenation and has high industrial application value.

Description

technical field [0001] The invention belongs to the field of fine chemical catalysts and new chemical materials, and in particular relates to a catalyst for the semihydrogenation of highly unsaturated acetylenic alcohols to enols and a preparation method thereof. Background technique [0002] Enols, as important intermediates in chemical synthesis, are widely used in the fields of medicine, pesticides and new materials. Due to the instability of enol substances and the unclear understanding of their structural relationships, the synthesis and development of enol compounds has been severely restricted. Until the middle of the 20th century, Fuson et al. discovered that a series of enols substituted with large sterically hindered aryl groups could exist stably. In such reactions, catalysts played a decisive role. How to prepare synthetic stable Enol catalysts have become one of the important hotspots in the study of alcohol compounds. Among them, the semi-hydrogenation of ace...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/232C07C29/17C07C33/035
CPCB01J27/232C07C29/17C07C33/035
Inventor 郝小兰张伟池华春杨清毛涛联王利敏高瑞刘月
Owner 重庆建峰新材料有限责任公司
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