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Separation method of 2-methyl-3-butyn-2-ol

A separation method and technology of butyne, applied in the separation/purification of hydroxy compounds, chemical instruments and methods, preparation of hydroxy compounds, etc., can solve the problems of product conversion rate and selectivity reduction, high content, etc.

Active Publication Date: 2020-10-23
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0017] In view of the prior art, product conversion rate and selectivity decrease during the preparation and separation of 2-methyl-3-butyn-2-ol, 2,5-dimethyl-3-hexyne-2,5 -The problem of higher diol content, the purpose of the present invention is to provide a method for separating high-purity 2-methyl-3-butyn-2-alcohol, which can effectively control the content of 2-methyl-3 - The content of 2,5-dimethyl-3-hexyne-2,5-diol in the reaction solution of butyn-2-ol ensures the separation effect and membrane service life of the membrane separation treatment in the separation and purification process, Furthermore, effective separation and purification can be achieved, high-purity 2-methyl-3-butyn-2-ol products can be obtained, and the color number and refractive index of 2-methyl-3-butyn-2-ol products can be improved

Method used

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  • Separation method of 2-methyl-3-butyn-2-ol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Embodiment 1: the preparation of 1# reaction solution

[0083] First, replace the 500L autoclave with ammonia gas three times, lower the temperature in the reactor to -20°C, add liquid ammonia (144.5Kg, 8500mol), start stirring, and feed acetylene (16800L, 750mol) at a concentration of 20wt%. Magnesium sulfate aqueous solution 43.5g and concentration are 50wt% potassium hydroxide aqueous solution (1008g, the potassium hydroxide consumption as solute is 3mol% of acetone), be warming up to 10 ℃ and add acetone (17.4Kg, 300mol), control acetone to add The feed rate is completed in about 1h; the reaction temperature is 10°C, and after 2h of reaction, 5Kg of ammonium sulfate aqueous solution with a concentration of 10wt% is added for neutralization to obtain 1# reaction containing 2-methyl-3-butyn-2-ol solution, and sampled to detect the reaction solution by GC.

[0084] The composition of 1# reaction solution: the content of inorganic salt is 2.16wt%, the content of water ...

Embodiment 2

[0085] Embodiment 2: the preparation of 2# reaction solution

[0086] First, replace the 500L autoclave with ammonia gas three times, lower the temperature in the reactor to -20°C, add liquid ammonia (144.5Kg, 8500mol), start stirring, and feed acetylene (16800L, 750mol) at a concentration of 20wt%. Zinc acetate aqueous solution 17.5g, then add concentration and be the potassium hydroxide aqueous solution (1008g of 50wt%, the potassium hydroxide consumption as solute is 3mol% of acetone), be warming up to 10 ℃ and add acetone (17.4Kg, 300mol), control The acetone addition rate is about 1h and the feed is completed; the reaction temperature is 10°C, and after 2 hours of reaction, 5Kg of ammonium sulfate aqueous solution with a concentration of 10wt% is added for neutralization to obtain 2-methyl-3-butyn-2-ol containing 2 #Reaction solution, and take a sample to detect the reaction solution by GC.

[0087] The composition of 2# reaction solution: the content of inorganic salt i...

Embodiment 3

[0088] Embodiment 3: the preparation of 3# reaction solution

[0089] First, replace the 500L autoclave with ammonia gas three times, lower the temperature in the reactor to -20°C, add liquid ammonia (144.5Kg, 8500mol), start stirring, and feed acetylene (16800L, 750mol) at a concentration of 20wt%. Zinc acetate aqueous solution 8.7g, then adding concentration is 50wt% potassium hydroxide aqueous solution (1008g, the potassium hydroxide consumption as solute is 3mol% of acetone), be warming up to 10 ℃ and add acetone (17.4Kg, 300mol), control The acetone addition rate is about 1h, and the feed is completed; the reaction temperature is 10°C, and after 2 hours of reaction, 5Kg of ammonium sulfate aqueous solution with a concentration of 10wt% is added for neutralization to obtain 3-butyn-2-ol containing 2-methyl-3- #Reaction solution, and take a sample to detect the reaction solution by GC.

[0090] The composition of 3# reaction solution: the content of inorganic salt is 2.17w...

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Abstract

The invention belongs to the technical field of acetylene alcohol production, and particularly relates to a separation method of 2-methyl-3-butyn-2-ol, which comprises the following steps: pretreatinga reaction solution containing 2-methyl-3-butyn-2-ol to remove unreacted acetone and contained salt from the reaction solution to obtain a 2-methyl-3-butyn-2-ol crude product, with the content of 2,5-dimethyl-3-hexyn-2,5-diol in the reaction solution containing 2-methyl-3-butyn-2-ol being not higher than 0.1 wt%; separating and purifying the 2-methyl-3-butyn-2-ol crude product by virtue of membrane separation treatment and reduced pressure distillation treatment, so as to obtain a 2-methyl-3-butyn-2-ol product. According to the method disclosed by the invention, water in the product can be removed and the content of the 2,5-dimethyl-3-hexyn-2,5-diol can be reduced under the condition that the investment and the energy consumption are reduced, so that the 2-methyl-3-butyn-2-ol with relatively high purity and conversion rate is obtained.

Description

technical field [0001] The invention belongs to the technical field of production of acetylenic alcohols, in particular to a method for separating high-purity 2-methyl-3-butyn-2-ol. Background technique [0002] 2-Methyl-3-butyn-2-ol is one of the important acetylenic alcohol chemicals, which are mainly used in the fields of corrosion inhibitors, food and medicine, and other chemical products. In terms of corrosion inhibitor application, because 2-methyl-3-butyn-2-ol has both polar groups and non-polar groups in its molecule, it can be used as an adsorption corrosion inhibitor, which can effectively Prevent metal hydrogen embrittlement. [0003] In addition, methyl heptenone, a downstream product of 2-methyl-3-butyn-2-ol, is an important pharmaceutical intermediate and food intermediate, which can further produce linalool, citral and pseudo-violet Ketones, and further preparation of vitamin A, vitamin E, vitamin K1 and various spices and flavors. Moreover, 2-methyl-3-buty...

Claims

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Application Information

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IPC IPC(8): C07C29/76C07C29/80C07C29/42C07C33/042
CPCC07C29/76C07C29/80C07C29/42C07C33/042
Inventor 鲍元野杨颖刘英俊张永振黎源
Owner WANHUA CHEM GRP CO LTD
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