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Method for synthesizing, extracting and purifying 3-hexyne-2, 5-diol

A technology for hexynediol and hexyne, which is applied in the field of safe synthesis and separation and purification of 3-hexyne-2,5-diol, can solve problems such as difficulty in production, and achieve safe production, convenient transportation and storage, The effect of eliminating the explosion hazard

Pending Publication Date: 2021-11-19
四川众邦新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be determined that the rectification of 3-hexyne-2,5-diol in the aqueous phase containing more potassium hydroxide is difficult to achieve in production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Distill paraldehyde through acid-catalyzed depolymerization, and absorb it with n-hexane solvent to make a solution with acetaldehyde content of 40.9%. Take 318g of the solution (equivalent to 130g of acetaldehyde), and seal it for use.

[0044] (2) Put 400g of n-hexane and 210g of potassium hydroxide (industrial grade, purity 94%) into the grinder in turn to grind into a slurry, transfer it to a stainless steel pressure reactor, start stirring, heat to 70°C-80°C and keep 1 hour, then lower the temperature to 18 ℃ ~ 20 ℃ control.

[0045] (3) Introduce acetylene gas and keep the acetylene pressure in the range of 0.08MPa-0.1MPa to react for about 1 hour. Then add the acetaldehyde solution prepared above into the reaction kettle evenly and slowly from the head tank, while keeping the acetylene pressure in the range of 0.08MPa-0.12MPa to react, and gradually increase it at a rate of 2°C-3°C every 10 minutes. Keep it after the high temperature reaches 54℃~56℃. After ...

Embodiment 2

[0053] Operate according to the mode of operation of embodiment 1, wherein:

[0054] The solvent used in the operation step (1) is petroleum ether, and the concentration of the prepared acetaldehyde solution is 38.1%. Weigh 368g of the solution (containing 140g of acetaldehyde) for use.

[0055] In the operation step (2), the feeding materials are 540g of solvent petroleum ether and 217g of catalyst potassium hydroxide.

[0056] In the operation step (3), the acetaldehyde: potassium hydroxide = 1.15: 1 (molar ratio) is controlled, and the acetylene pressure is 0.1MPa~0.12MPa.

[0057] The amount of clean water in the operation step (5) is 750g.

[0058] In the operation step (6), the extraction solvent is fed with 700 g of 2-ethylhexanol.

[0059] Rectification yielded 167.2 g of 3-hexyne-2,5-diol with a purity of 98.4%.

Embodiment 3

[0061] Operate according to the mode of operation of embodiment 1, wherein:

[0062] The solvent used in the operation step (1) is toluene, and the concentration of the prepared acetaldehyde solution is 42.7%. Weigh 305g of the solution (containing 130g of acetaldehyde) for use.

[0063] In the operation step (2), the feeding materials are 400 g of solvent toluene and 210 g of catalyst potassium hydroxide.

[0064] In the operation step (3), the acetaldehyde: potassium hydroxide = 1.22: 1 (molar ratio) is controlled, and the acetylene pressure is 0.12MPa~0.14MPa.

[0065] The amount of clean water in the operation step (5) is 700g.

[0066] The extraction solvent in the operation step (6) is 650 g of isobutanol.

[0067] Rectification yielded 157.7 g of 3-hexyne-2,5-diol with a purity of 97.8%.

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Abstract

A method for synthesizing, extracting and purifying 3-hexyne-2, 5-diol adopts paraldehyde as an acetaldehyde raw material source and potassium hydroxide as a catalyst to react with acetylene of which the pressure is lower than 0.15 MPa in an aliphatic hydrocarbon or aromatic hydrocarbon organic solvent to generate the 3-hexyne-2, 5-diol. The method comprises the following steps: carrying out two-phase separation and hydrolysis on a reaction endpoint material which is a liquid-liquid two-phase system to obtain an aqueous solution containing a target product and potassium hydroxide, extracting by using an alcohol organic solvent with small water solubility, separating the target product from potassium hydroxide, and rectifying to obtain the target product 3-hexyne-2, 5-diol. The synthesis reaction process is carried out under the safe acetylene pressure of 0.15 MPa, the explosion danger is eliminated, and the method has the characteristics of safe production, high product yield, high product purity and the like.

Description

technical field [0001] The invention relates to a method for safely synthesizing, separating and purifying 3-hexyne-2,5-diol starting from paraldehyde through reaction with acetylene. Background technique [0002] 3-Hexyne-2,5-diol is a chemical intermediate that can be used to prepare surfactants in the chemical industry, used as steel corrosion inhibitors in the steel industry, and used as electroplating brighteners and leveling agents in the electroplating industry Wait. The downstream product 2,5-hexanediol produced by the hydrogenation of 3-hexyne-2,5-diol is also used in the synthesis of antihypertensive drugs captopril, diltiazem and other chiral drugs and other chiral chemicals important raw material. [0003] The method of synthesizing 3-hexyne-2,5-diol was reported in the early stage with a Grignard reagent synthesis method. Because of the need to use Grignard reagents, the production operation is complicated, the equipment requirements are high, and there are ma...

Claims

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Application Information

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IPC IPC(8): C07C29/42C07C29/76C07C29/78C07C29/80C07C29/86C07C29/88C07C33/044
CPCC07C29/42C07C29/76C07C29/78C07C29/80C07C29/86C07C29/88C07C33/044Y02P20/584
Inventor 王南王林生李果
Owner 四川众邦新材料股份有限公司
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