Method for preparing alpha-acetyl-gamma-butyrolactone

A technology of butyrolactone and acetyl, which is applied in the field of preparation of α-acetyl-γ-butyrolactone, can solve the problems of slow heat dissipation of the reactor, potential safety hazards, and flushing of materials, so as to reduce production costs and avoid safety hazards. Hidden dangers, high catalytic efficiency

Inactive Publication Date: 2008-07-30
WUJIANG XINYI CHEM
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Problems solved by technology

Since ethylene oxide is a first-class flammable and explosive chemical, using ethylene oxide as the reaction raw material has serious safety hazards in the reaction, and it is also difficult to obtain high-purity α-acetyl-γ -butyrolactone: γ-butyrolactone is used as the starting material, and generally γ-butyrolactone is used to directly react intermittently with metallic sodium in an enamelled glass reactor. Because the reaction is too intense, the heat dissipation of the reactor is slow and the temperature Difficult to control and other issues, frequent material punching, burning and explosion incidents in the production process have caused many domestic and foreign companies to stop using th...

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Embodiment Construction

[0013] The specific embodiment of the present invention is described below:

[0014] A preparation method for α-acetyl-γ-butyrolactone, comprising a reaction section, a neutralization section and a distillation section, wherein the reaction section includes the following steps:

[0015] (1), in reactor, drop into 120 kilograms of toluene as solvent, after nitrogen replacement, drop into 28 kilograms of sodium metals, throw and finish, close nitrogen, close manhole cover, be warming up to 105 degrees Celsius, and keep warm at this temperature for 20 minute.

[0016] (2), start stirring, and after 10 minutes, start to drop 260 kilograms of a mixed solution of ethyl acetate and γ-butyrolactone, keep the reaction system at 85 degrees Celsius for 2.5 hours, ethyl acetate and γ-butyrolactone in the mixed solution The mass ratio of butyrolactone is 1.6:1, and the reaction yield is 92%.

[0017] Neutralization section: transfer the above system that has passed through the reaction s...

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Abstract

The invention relates to a preparation method for Alpha-acetyl-Gamma-butyrolactone. Ethyl acetate and Gamma-butyrolactone are used as the initial material, and the preparation method comprises a reaction section, a neutralization section and a distillation section. The reaction section comprises the following steps: firstly, a metallic sodium catalyst is added into a toluene solvent in nitrogen atmosphere, then the temperature is raised to 100 to 110 DEG C, and is maintained for 15 to 30 minutes; secondly, the mixed liquor of the ethyl acetate and the Gamma-butyrolactone is titrated into the toluene solvent after being treated in step one, heat preservation and reaction are performed for 2.5 to 3 hours at 85 to 90 DEG C, wherein, the mass compounding ratio between the ethyl acetate and the Gamma-butyrolactone is 1.55 to 1.70: 1; in the neutralization section, sulfuric acid is adopted for neutralization. Through the preparation method, high-purity Alpha-acetyl-Gamma-butyrolactone can be obtained, in addition, the operation of the method is simple, the production cost is low, and the security is good.

Description

technical field [0001] The invention belongs to the field of chemical product synthesis, in particular to a preparation method of α-acetyl-γ-butyrolactone. Background technique [0002] At present, there are mainly two routes for the preparation of α-acetyl-γ-butyrolactone. One is the process using ethylene oxide as the starting material, and the other is the process using γ-butyrolactone as the starting material. craft. Since ethylene oxide is a first-class flammable and explosive chemical, using ethylene oxide as the reaction raw material has serious safety hazards in the reaction, and it is also difficult to obtain high-purity α-acetyl-γ -butyrolactone: γ-butyrolactone is used as the starting material, and generally γ-butyrolactone is used to directly react intermittently with metallic sodium in an enamelled glass reactor. Because the reaction is too intense, the heat dissipation of the reactor is slow and the temperature Difficult to control and other issues, frequent ...

Claims

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Application Information

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IPC IPC(8): C07D307/33
Inventor 钱其群
Owner WUJIANG XINYI CHEM
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