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Method for preparing enol by semi-hydrogenating alkynol

A technology for semi-hydrogenation and alkynol, which is used in hydrogenation preparation, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problems of difficult control of hydrogenation steps and imprecise control of reaction conditions.

Inactive Publication Date: 2017-05-31
CHONGQING JIANFENG INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the hydrogenation of 1,4-butynediol to 1,4-butenediol belongs to the surface reaction on the surface of the catalyst, such as the selective preparation of the catalyst and the inaccurate control of the reaction conditions, it is easy to occur Complete hydrogenation of acetylenic alcohols to produce 1,4-butanediol, the hydrogenation step is not easy to control

Method used

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  • Method for preparing enol by semi-hydrogenating alkynol
  • Method for preparing enol by semi-hydrogenating alkynol
  • Method for preparing enol by semi-hydrogenating alkynol

Examples

Experimental program
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Effect test

preparation example 1

[0073]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 obt...

preparation example 2

[0075] The preparation method of the catalyst was the same as that of the catalyst preparation example 1, except that the auxiliary agent was changed from zinc acetate to 152 g of iron acetate to make catalyst C-2.

preparation example 3

[0077] The preparation method of the catalyst was the same as that of the catalyst preparation example 1, except that the auxiliary agent was changed from zinc acetate to 140 g of magnesium acetate to make catalyst C-3.

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Abstract

The invention provides a method for preparing 1,4-butenediol by semi-hydrogenating 1,4-butynediol. The method comprises the following steps: pre-treating raw materials by utilizing an alkaline solution; and realizing the controllability of a hydrogenating step by adopting a gradient stirring method in the presence of a catalyst. According to the method, the liquid-solid ratio of 1,4-alkynediol to the catalyst is (80-200) to 1, and the operation temperature (30 DEG C-115 DEG C) and the pressure (0.3MP-1MPa) are relatively low; and the conversion ratio of the 1,4-butynediol reaches 99.9% and the selectivity and yield of the 1,4-butenediol reach 98.2% and 95.87%. According to the method provided by the invention, the charge density of the raw material is changed and the controllability of a hydrogenating process is realized in the presence of the catalyst through adjusting a stirring speed by gradient, and a relatively good semi-hydrogenating performance is represented; and the method has a good industrial application value.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemicals, and in particular relates to a method for preparing enol by semihydrogenation of acetylenic alcohol. 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 acetylenic alcohols to enols is an ideal technical route, so the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/035C07C29/17B01J31/26B01J31/04B01J27/232
CPCC07C29/17B01J27/232B01J31/04B01J31/26B01J2231/645
Inventor 郝小兰杨清池华春张伟张宇杨益张强
Owner CHONGQING JIANFENG INDAL GROUP
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