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Process for synthesis of 3-hexyne- 2, 5-diol by slurry bed acidity control method

An acidity control, slurry bed technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of unsuitability for industrial production, large market gap, low safety, etc., and reduce consumption costs. , The effect of reducing production cost and high production rate

Inactive Publication Date: 2015-11-18
四川隆桥化工集团有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[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; 80% of HD is mainly Used in the electroplating industry, ≥95% HD is mainly used in new pharmaceutical raw materials and other organic synthesis; at present, the world's main manufacturer of HD is BASF in Germany, and there is no domestic manufacturer for the time being; BASF mainly develops and produces 80% concentration The HD products are mainly used as raw materials for new electroplating brighteners, and the production capacity is 200 tons per year, and the market gap is relatively large
[0003] The patent application No. 201110152117.8 discloses a synthesis method of 3-hexyne-2,5-diol, the reaction is carried out in an autoclave, 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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  • Process for synthesis of 3-hexyne- 2, 5-diol by slurry bed acidity control method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The preparation method of 3-hexyne-2,5-diol is as follows:

[0044] (1) Preparation of catalyst: Dissolve 75g of copper nitrate in 600ml of soft water at 60°C and stir to dissolve; dissolve 13.5g of bismuth nitrate in 180ml of soft water at 80°C and stir to dissolve; dissolve 75g of sodium carbonate in Stir to dissolve in 750ml soft water at 60°C; slowly add copper nitrate and bismuth nitrate solutions to the sodium carbonate solution at the same time, continue stirring for 20-25 minutes, and then adjust the pH value of the solution with nitric acid with a mass fraction of 65% to 7~8, heat-preserve and react at 50°C for 4 hours to obtain a product liquid, vacuum filter the prepared liquid, rinse the filter cake repeatedly with soft water at 60°C until neutral, and place the obtained filter cake in Dry in a constant temperature drying oven at 95°C for 5 hours to obtain 42.6g of a catalyst, which is a mixture of basic copper carbonate and bismuth basic carbonate. The prepar...

Embodiment 2

[0053] The preparation method of 3-hexyne-2,5-diol is as follows:

[0054] (1) The preparation and activation of the catalyst are the same as the preparation and activation of the catalyst in Example 1.

[0055] (2) Then add 1100ml of acetaldehyde aqueous solution with a mass fraction of 45% and 80g of catalyst into the slurry bed reactor, replace the reactor with acetylene for 3 to 5 times, start stirring, and slowly raise the temperature to 120°C, and at the same time The compressed 162.5g of acetylene is imported from the lower part of the reactor, and the pressure in the reactor is controlled at 1.3Mpa to carry out the stirring reaction. After 13 hours of reaction, take samples from the sampling valve of the reactor, and take samples every half an hour until the product content is qualified. , to obtain the resulting solution;

[0056] In the reaction process, when the reaction is carried out to 5 / 3 hours, the 25ml sodium hydroxide solution with a mass concentration of 3%...

Embodiment 3

[0061] The preparation method of 3-hexyne-2,5-diol is as follows:

[0062] (1) The preparation and activation of the catalyst are the same as the preparation and activation of the catalyst in Example 1.

[0063] (2) Then add 1100ml of acetaldehyde aqueous solution with a mass fraction of 48% and 88g of catalyst into the slurry bed reactor, replace the reactor with acetylene for 3 to 5 times, start stirring, and slowly raise the temperature to 120°C, and at the same time The compressed 173g of acetylene is introduced from the lower part of the reactor, and the pressure in the reactor is controlled at 1.0Mpa to carry out the stirring reaction. After 10 hours of reaction, take samples from the reactor sampling valve, and take samples every half an hour until the product content is qualified. to obtain the resulting liquid;

[0064] In the reaction process, when the reaction is carried out to 4 / 3 hour, the 20ml sodium hydroxide solution with a mass concentration of 3.0% is pumped...

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Abstract

The invention discloses a process for synthesis of 3-hexyne- 2, 5-diol by slurry bed acidity control method. The process includes: adding an acetaldehyde aqueous solution and a catalyst into a slurry bed reaction kettle and conducting mixing to obtain a slurry solution, then introducing acetylene from the lower part of the slurry solution into a slurry system to carry out reaction, thus obtaining a generated solution; in the reaction process, adding an alkali solution repeatedly to control the pH value of the reaction solution at 5.5-7.0; cooling the generated solution, conducting first standing settlement layering, then conveying the generated solution from standing settlement to a high level settler to carry out second standing settlement layering, and carrying out concentration and separation on the supernatant, and subjecting the remaining concentrated liquid to vacuum distillation, thus obtaining the 3-hexyne- 2, 5-diol. In the synthesis process, the low concentration alkali solution is added to control the pH value of the reaction solution at 5.5-7.0, so that the whole reaction has high selectivity and high production rate, thus being more conducive to 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 acidity control 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; 80% of HD is mainly Used in the electroplating industry, ≥95% HD is mainly used in new pharmaceutical raw materials and other organic synthesis; at present, the world's main manufacturer of HD is BASF in Germany, and there is no domestic manufacturer for the time being; BASF mainly develops and produces 80% concentration HD products are mainly used as raw materials for new electroplating brighteners, with a production capacity of 200 tons per year, and a large market gap. [0003] The patent application No. 201110152117.8 discloses a synthesis method of 3-hexyne-2,5-diol, the reaction is...

Claims

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Application Information

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IPC IPC(8): C07C29/42C07C29/80C07C33/044C07C33/042B01J23/843
CPCB01J23/8437C07C29/42C07C29/80C07C33/044C07C33/042
Inventor 董立瀛古苇唐伟郑恒刚
Owner 四川隆桥化工集团有限公司
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