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Preparation method and application of alpha-acetyl-gamma-butyrolactone

A technology of butyrolactone and acetyl group, which is applied in the field of preparation of α-acetyl-γ-butyrolactone, can solve the problems of low acylation reaction yield, large rectification loss, low purity and the like, and achieves improved acylation The effect of reaction yield, elimination of inhibition, and elimination of potential safety hazards

Pending Publication Date: 2022-03-18
江苏兄弟维生素有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since the material used in the traditional process is solid sodium methoxide, which is prone to spontaneous combustion and absorbs moisture, and the feeding of solid sodium methoxide is done manually, there is a greater safety risk; at the same time, the sodium methoxide generated during the reaction process Methanol has an inhibitory effect on the main reaction of acylation, so the yield of the acylation reaction is low, and there are more by-products and impurities; The purity of the crude product of -γ-butyrolactone is not high, and high vacuum rectification equipment is required for purification, resulting in high energy consumption and large rectification loss, so the rectification yield is low, resulting in the preparation of α-butyrolactone from solid sodium methoxide. The overall yield of the process of acetyl-γ-butyrolactone is low

Method used

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  • Preparation method and application of alpha-acetyl-gamma-butyrolactone

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preparation example Construction

[0036] According to a first aspect of the present invention, a method for preparing α-acetyl-γ-butyrolactone is provided, comprising the following steps:

[0037] γ-butyrolactone, acylating reagents, alkaline reagents and benzene reagents are mixed for acylation reaction. At the same time of acylation reaction, acylating reagents, benzene reagents and by-products are azeotroped to remove by-products. And obtain α-acetyl-γ-butyrolactone after;

[0038] Wherein, the alkaline reagent includes an alkoxide solution, and the by-product is a by-product generated by the alkaline reagent.

[0039] In the present invention, the alkoxide solution is used instead of the traditional solid alkoxide as the alkaline reagent for the acylation of γ-butyrolactone, thus eliminating the potential safety hazards caused by the use of solid alkaline reagents and enabling closed material transportation and automatic reaction control; and the present invention introduces benzene-based reagents into th...

Embodiment 1

[0060] The preparation method of α-acetyl-γ-butyrolactone, the flow process is as follows figure 1 , including the following steps:

[0061] Continuously press into γ-butyrolactone 5g / min, methyl acetate 12.5g / min, 29% liquid sodium methylate 14.65g / min and xylene 3g / min in the reaction equipment, while reacting solvent distillation, utilize xylene, Methyl acetate and the methyl alcohol three that produce are azeotropic, and the methyl alcohol distillation that suppresses reaction is carried out (its collecting speed is 22.5g / min, and meteorological detection methanol content is 62.2%, xylene content is 12.9%, and methyl acetate content is 24.9%);

[0062] After the above-mentioned continuous feeding for 10 minutes, the reaction product began to be discharged while feeding. After 20 minutes, a total of 253g of materials were collected, and after cooling, they were neutralized with 95g of anhydrous acetic acid to obtain sodium acetate and α-acetyl-γ-butyrolactone Crude produc...

Embodiment 2

[0066] The preparation method of α-acetyl-γ-butyrolactone comprises the following steps:

[0067] Continuously press 5 g / min of gamma-butyrolactone, 12.5 g / min of methyl acetate, 19 g / min of 29% liquid potassium methylate and 3 g / min of xylene in the reaction equipment, distill solvent while reacting, utilize xylene, acetic acid Methyl ester and the methyl alcohol three that produce azeotrope, the methyl alcohol distillation that suppresses reaction is carried out (its collecting speed is 22.5g / min, and meteorological detection methyl alcohol content is 62.2%, xylene content is 12.9%, and methyl acetate content is 24.9% %); ·

[0068] After the above-mentioned continuous feeding for 10 minutes, the reaction product began to be discharged while feeding. After 20 minutes, a total of 340 g of materials were collected, and after cooling, they were neutralized with 95 g of anhydrous acetic acid to obtain sodium acetate and α-acetyl-γ-butyrolactone Crude product, after separation o...

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Abstract

The invention provides a preparation method and application of alpha-acetyl-gamma-butyrolactone, and relates to the technical field of chemical engineering, and the preparation method comprises the following steps: gamma-butyrolactone, an acylation reagent, an alkaline reagent and a benzene reagent are mixed and then subjected to an acylation reaction, during the acylation reaction, the acylation reagent, the benzene reagent and byproducts are azeotropic to remove the byproducts, and the alpha-acetyl-gamma-butyrolactone is obtained. Carrying out acid neutralization to obtain alpha-acetyl-gamma-butyrolactone; wherein the alkaline reagent comprises an alkoxide solution; the by-product is a by-product generated by an alkaline reagent. The preparation method provided by the invention solves the technical problems that a solid alkaline reagent brings potential safety hazards to manual feeding, the acylation reaction yield is low and the product purification operation is complicated, and achieves the technical effects of eliminating the potential safety hazards of solid feeding, improving the acylation reaction yield and being simple in product purification operation.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of α-acetyl-γ-butyrolactone and its application. Background technique [0002] The materials used in the gamma-butyrolactone acylation process in the prior art are solid sodium methylate, methyl acetate and gamma-butyrolactone. After the materials are mixed, they are added to the reactor reaction equipment for reaction, and then neutralized with anhydrous acetic acid to obtain Sodium acetate and α-acetyl-γ-butyrolactone crude product, after separating sodium acetate, the α-acetyl-γ-butyrolactone crude product can be obtained by vacuum distillation to obtain α-acetyl-γ-butyrolactone finished product, but Yield is lower, and concrete reaction formula is as follows: [0003] [0004] Since the material used in the traditional process is solid sodium methoxide, which is prone to spontaneous combustion and absorbs moisture, and the feeding of solid s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/30
CPCC07D307/30
Inventor 陈英明徐晓海严建斌袁龙英段艳文
Owner 江苏兄弟维生素有限公司
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