A kind of method using furfural as raw material to prepare gamma-butyrolactone

A technology of butyrolactone and furfural, which is applied in the field of preparation of γ-butyrolactone, can solve the problems of low selectivity, overcapacity of furfural, slow reaction rate, etc., and achieve the effect of simple process flow, avoiding high pollution and mild operating conditions

Active Publication Date: 2019-03-19
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But unfortunately, most furfural conversion researches are still in the stage of organic synthesis in the laboratory, and the downstream products of furfural in industry are mainly traditional chemical products such as furfuryl alcohol, tetrahydrofurfuryl alcohol, furfur resin, furan, etc., which leads to excess production capacity of furfural, An important reason for the low profit of the industry
[0008] Some studies have reported organic experiments on the oxidation of furfural to 2(5H)-furanone, but there are problems such as slow reaction rate, low selectivity, and difficult separation of main and by-products, and the application of 2(5H)-furanone is limited, mainly Involved in organic synthesis, but has not yet developed a scalable downstream product
[0009] On the one hand, the traditional γ-butyrolactone synthesis process is complex and highly dependent on petrochemical raw materials; on the other hand, furfural has excess production capacity and single downstream products

Method used

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  • A kind of method using furfural as raw material to prepare gamma-butyrolactone
  • A kind of method using furfural as raw material to prepare gamma-butyrolactone

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Furfural oxidation reaction: add 4.0g furfural, 4.0g anhydrous sodium sulfate, 1.5ml formic acid and 1.5ml deionized water to 10ml of 1,2-dichloroethane, inject 10ml of hydrogen peroxide (30%), at 60 The reaction was stirred under normal pressure at ℃ for 2.5 hours. After the reaction, the mixture was allowed to stand for stratification, and the organic phase was distilled under reduced pressure to obtain 60% yield of 2(5H)-furanone and 18% yield of dibasic acid in the aqueous phase.

Embodiment 2

[0042] Furfural oxidation reaction: add 4.0g furfural, 4.0g anhydrous sodium sulfate, 1.5ml formic acid and 1.5ml deionized water to 10ml ethyl acetate, inject 10ml hydrogen peroxide (30%), stir at 60°C under normal pressure The reaction was carried out for 2.5 hours. After the reaction, the mixture was left to stand and separated, and the organic phase was distilled under reduced pressure to obtain 62% yield of 2(5H)-furanone and 15% yield of dibasic acid in the aqueous phase.

Embodiment 3

[0044] Furfural oxidation: add 4.0g furfural, 4.0g anhydrous sodium sulfate, and 1.5ml formic acid to 10ml methanol, inject 10ml hydrogen peroxide (30%), stir and react at 60°C for 2.5 hours under normal pressure, 2(5H)- The yield of furanone is 13%, and the yield of dibasic acid is 48%.

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Abstract

The invention discloses a method for preparing GBL (Gamma-Butyrolactone) by taking furfural as a raw material. The method comprises two steps of oxidizing the furfural to prepare 2(5H)-furanone and hydrogenating the 2(5H)-furanone to prepare the GBL, wherein the 2(5H)-furanone can be synthesized by the furfural by taking homogeneous-phase acid or solid acid as a catalyst and taking hydrogen peroxide as an oxidant under the conditions of mild temperature and pressure. The 2(5H)-furanone is further selectively hydrogenated to obtain the GBL under the effect of a metal catalyst in a hydrogen atmosphere. The GBL can be generated by commonly hydrogenating the 2(5H)-furanone serving as a main product and C4 binary acid serving as a byproduct of the oxidation of the furfural in situ under appropriate conditions. According to the method, high-efficiency conversion from the furfural serving as a biomass raw material to the GBL serving as a fine chemical product is realized; the method has a great application prospect.

Description

technical field [0001] The invention relates to a new method for preparing gamma-butyrolactone, more specifically a new route for preparing gamma-butyrolactone by using furfural as a raw material through catalytic oxidation and catalytic hydrogenation in series. Background technique [0002] γ-butyrolactone, also known as 1,4-butyrolactone, is an important organic intermediate that is widely used in the synthesis of fine chemicals, medicine, pesticides, spices and other fields. It is the raw material for the synthesis of fine chemicals such as α-pyrrolidone, N-methylpyrrolidone, vinylpyrrolidone, acetylbutyrolactone, and cyclopropylamine, and the intermediate for the synthesis of vitamin B1, ciprofloxacin, and other drugs. It is used in the synthesis of chlorophenoxybutyric acid herbicides, herbicides and insecticides. γ-butyrolactone is also a high-boiling point, strong solubility, good conductivity, non-toxic and safe proton-type strong solvent, which can be used as resin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 王铁峰李晓丹蓝晓程吕舒婷
Owner TSINGHUA UNIV
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