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Process for synthesizing 3-hexyne-2,5-diol through slurry bed based on low pressure method

A technology of slurry bed and low-pressure method, which is applied in the technical field of synthesizing 3-hexyne-2,5-diol by slurry bed low-pressure method, and can solve the problems of being unsuitable for industrial production, low safety and complex process, etc. Achieve the effects of low cost, high safety, and reduced raw material consumption

Active Publication Date: 2013-01-16
LONGCHANG TIANKANG FINE CHEM CO LTD
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  • Abstract
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Problems solved by technology

[0003] The patent application No. 201110152117.8 discloses a synthesis method of 3-hexyne-2,5-diol, the reaction is carried out in an activation kettle, the process is complicated, the safety is low, the yield is low, the cost is high, and it is not suitable for in industrial production

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Embodiment 3

[0021] The preparation method of the present embodiment 3-hexyne-2,5-diol is as follows:

[0022] ① Preparation of catalyst

[0023] Dissolve 75g of copper nitrate (content ≥99%) in 600ml of soft water at 60°C and stir to dissolve it; dissolve 13.5g of bismuth nitrate (content ≥98%) in 180 ml of soft water at 80°C and stir to make it Dissolve; dissolve 75g of sodium carbonate (content ≥ 98%) in 750ml of soft water at 60°C, stir to dissolve; slowly add copper nitrate and bismuth nitrate solution to the sodium carbonate solution at the same time, continue stirring for 20 -25 minutes, then use nitric acid with a mass fraction of 65% to adjust the pH value of the solution to 7-8, keep the reaction at 50-60°C for 4 hours, vacuum filter the prepared reaction solution, and use 60°C soft water Rinse the filter cake repeatedly until neutral. The obtained filter cake was placed in a constant temperature drying oven and dried at 95±2° C. for 5 hours to obtain 42.6 g of dry catalyst (a ...

Embodiment 2

[0028] ① Preparation of catalyst

[0029] Dissolve 75g copper nitrate (content ≥99%) in 600ml soft water at 60°C and stir to dissolve it; dissolve 12.5g bismuth nitrate (content ≥98%) in 170ml soft water at 80°C and stir to dissolve it ; Dissolve 75g of sodium carbonate (content ≥ 98%) in 750ml of soft water at 60°C, stir to dissolve it; slowly add copper nitrate and bismuth nitrate solution to the sodium carbonate solution at the same time, continue stirring for 20- 25 minutes, then use nitric acid with a mass fraction of 65% to adjust the pH value of the solution to 7-8, keep the reaction at 50-60°C for 4.5 hours, vacuum filter the prepared reaction solution, and repeat it with 60°C soft water Rinse the filter cake to neutral.

[0030] The obtained filter cake was placed in a constant temperature drying oven, and dried at 95±2° C. for 5 hours to obtain 42 g of dry catalyst (a mixture of bismuth subcarbonate and copper subcarbonate). The dry catalyst prepared twice was plac...

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Abstract

The invention discloses a process for synthesizing 3-hexyne-2,5-diol through a slurry bed based on a low pressure method, which is characterized by comprising the following steps: mixing an acetaldehyde water solution and a catalyst in a reaction kettle of the slurry bed, and stirring to obtain a slurry solution; introducing acetylene into the slurry system from the lower part of the slurry solution, and reacting; and concentrating, separating, and performing reduced pressure distillation to obtain the 3-hexyne-2,5-diol. The method has the advantages of simple process, good safety, high yield and high purity of the prepared product, and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a preparation method of 3-hexyne-2,5-diol, in particular to a process for synthesizing 3-hexyne-2,5-diol by a slurry bed low-pressure method. Background technique [0002] 3-Hexyn-2,5-diol (3-Hexyn-2,5-diol, HD) is an important raw material for a new type of electroplating brightener and an important chemical raw material for new medicines. Among them, 80% of HD is mainly used in the electroplating industry, and ≥95% of HD is mainly used in new pharmaceutical raw materials and other organic synthesis. At present, BASF in Germany is the main manufacturer of HD in the world, and there is no domestic manufacturer for the time being; BASF mainly develops and produces HD products with a concentration of 80%, which is mainly used as raw materials for new electroplating brighteners. The notch is larger. [0003] The patent application No. 201110152117.8 discloses a synthesis method of 3-hexyne-2,5-diol, the reaction is carried out i...

Claims

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Application Information

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IPC IPC(8): C07C33/044C07C29/42B01J23/843
Inventor 董立瀛古苇唐伟
Owner LONGCHANG TIANKANG FINE CHEM CO LTD
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