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Production method of 4-hydroxy-2-butanone

A production method, technology of methyl ethyl ketone, applied in chemical instruments and methods, separation/purification of carbonyl compounds, preparation of carbonyl compounds, etc., can solve problems such as low yield, achieve reduced production costs, strong resistance to autooxidation, Post-processing for easy effects

Inactive Publication Date: 2019-08-09
GANSU RES INSTION OF CHEM IND GRICI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to provide a kind of production method of 4-hydroxyl-2-butanone, to solve the problem that the productive rate of existing synthetic method is lower

Method used

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  • Production method of 4-hydroxy-2-butanone

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Effect test

Embodiment 1

[0030] Step 1. Add 1,3-butanediol 10,000mol, catalyst sodium molybdate 200mol, additive tetrabutylammonium chloride 200mol, water 50,000mol and water-carrying agent diisopropyl ether 4,000mol into a 3,000-liter reactor, and stir evenly. Form a mixed solution and heat up to 60°C;

[0031] Step 2. While stirring, drop 10,000 mol of hydrogen peroxide with a mass fraction of 30% into the mixed solution, and at the same time divide water by vacuum distillation. ;

[0032] Step 3. When the gas chromatography detects that the content of 1,3-butanediol in the reactor is not higher than 25% of the initial content, stop adding hydrogen peroxide dropwise, continue stirring for 1.5 hours, and control the temperature in the reactor not higher than 60°C , steam the water-carrying agent;

[0033] Step 4: Control the temperature of the system to not be higher than 60°C, and rectify under reduced pressure to obtain 428kg of the final product 4-hydroxy-2-butanone. The gas phase detection puri...

Embodiment 2

[0035] Step 1. Add 1,3-butanediol 10,000mol, catalyst sodium molybdate 240mol, additive tetrabutylammonium chloride 240mol, water 50,000mol and water-carrying agent diisopropyl ether 4,000mol into a 3,000-liter reactor, and stir evenly. Form a mixed solution and heat up to 60°C;

[0036] Step 2. While stirring, drop 10,000 mol of hydrogen peroxide with a mass fraction of 30% into the mixed solution, and at the same time divide water by vacuum distillation. ;

[0037] Step 3. When the gas chromatography detects that the content of 1,3-butanediol in the reactor is not higher than 25% of the initial content, stop adding hydrogen peroxide dropwise, continue stirring for 1.2 hours, and control the temperature in the reactor not higher than 60°C , steam the water-carrying agent;

[0038] Step 4: Control the temperature of the system to not be higher than 60° C., rectify under reduced pressure to obtain 416 kg of the final product 4-hydroxy-2-butanone, and the gas phase detection p...

Embodiment 3

[0040] Step 1. Add 1,3-butanediol 10,000mol, catalyst sodium molybdate 200mol, additive tetrabutylammonium chloride 200mol, water 50,000mol and water-carrying agent diisopropyl ether 5,000mol into a 3,000-liter reactor, and stir evenly. Form a mixed solution and heat up to 60°C;

[0041] Step 2. While stirring, drop 10,000 mol of hydrogen peroxide with a mass fraction of 30% into the mixed solution, and at the same time divide water by vacuum distillation. ;

[0042] Step 3. When the gas chromatography detects that the content of 1,3-butanediol in the reactor is not higher than 25% of the initial content, stop adding hydrogen peroxide dropwise, continue stirring for 1.5 hours, and control the temperature in the reactor not higher than 60°C , steam the water-carrying agent;

[0043] Step 4: Control the temperature of the system to not be higher than 60° C., rectify under reduced pressure to obtain 410 kg of the final product 4-hydroxy-2-butanone, and the purity of the product...

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Abstract

Belonging to the field of fine chemicals, the invention discloses a production method of 4-hydroxy-2-butanone, and solves the problem of low yield of existing synthetic methods. The method provided bythe invention includes the steps of: adding 1, 3-butanediol, a catalyst, an assistant, water and a water-carrying agent into a reaction kettle, and performing heating to 55-60DEGC; adding hydrogen peroxide dropwise into the mixed solution, and conducting reduced pressure distillation of water; stopping adding hydrogen peroxide, and further performing stirring for 1-1.5h to distill the water-carrying agent out; controlling the temperature of the system not higher than 60DEGC, and conducting reduced pressure rectification to obtain the final product 4-hydroxy-2-butanone. By adding the assistant, 1, 3-butanediol can better participate in the reaction, and the conversion rate can be improved. The chemical reaction carried out in the invention is carried out under a negative pressure condition, and the temperature is controlled not higher than 60DEG C, thus avoiding the generation of methyl vinyl ketone; and in a negative pressure system, the reaction can be fully carried out under a low temperature condition, the product is easier to distill, and impurities are not easily produced.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a production method of 4-hydroxy-2-butanone. Background technique [0002] 4-hydroxy-2-butanone, commonly known as butanol, its English name is 4-hydroxy-2-butanone, is an important pharmaceutical intermediate. It can be used to synthesize six-carbon alcohol, which is an important intermediate in the synthesis of vitamin A (Retinol); it can also react with phenol to synthesize a warm-scented raspberry ketone with an elegant and fruity aroma; adding After a suitable catalyst, the important chemical raw material (R)-1,3-butanediol can be synthesized, which can be used to synthesize the optical compound azetidinone, which is a penem antibiotic, pheromone, fragrance and sterilant Intermediate raw material for the synthesis of insecticides; 4-hydroxy-2-butanone can also be synthesized (R)-3-aminobutanol by biological enzymatic method, (R)-3-aminobutanol is synthesized from L...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/17C07C45/00C07C45/82
CPCC07C45/002C07C45/82
Inventor 王永胜刘荣路彬
Owner GANSU RES INSTION OF CHEM IND GRICI
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