Preparation method of gamma-butyrolactone

A technology of butyrolactone and vanadyl, which is applied in the field of preparation of γ-butyrolactone, can solve the problems of harsh reaction conditions and large fluctuations, and achieve mild reaction conditions, abundant sources, and obvious innovative effects

Active Publication Date: 2013-06-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction conditions of these process routes are relatively harsh, and the key raw materials rely on non-renewable fossil resources such as petroleum, coal and natural gas, so they are greatly affected by fluctuations in international energy prices

Method used

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  • Preparation method of gamma-butyrolactone
  • Preparation method of gamma-butyrolactone
  • Preparation method of gamma-butyrolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Add 1.02g of tetrahydrofurfuryl alcohol and 1mol% vanadyl tartrate into a 50mL reaction kettle to close the kettle, fill it with oxygen at a pressure of 1.5MPa, heat up to 100°C under stirring, and run for 8h. If there is oxygen consumption during the period, is supplemented. It was then cooled to room temperature and carefully depressurized to atmospheric pressure. Sampling was used to analyze the product by GC-MS, and the chromatographic retention time of the main components of the product was compared with the γ-butyrolactone and tetrahydrofurfuryl alcohol standards to determine the main product. Product quantitative analysis uses gas chromatography (GC), tetrahydrofurfuryl alcohol transformation rate 96%, gamma-butyrolactone selectivity is 74%, other products such as figure 2 shown

Embodiment 2

[0018] Embodiment 2: Except that the catalyst type, catalyst consumption, reaction time, and oxygen partial pressure are different, other experimental conditions are all the same as in Example 1, and the activity evaluation of different catalysts is carried out according to the steps in Example 1. The catalytic activities of different vanadium-based catalysts are shown in Table 1:

[0019] Table 1: Preparation of γ-butyrolactone by selective oxidation of tetrahydrofurfuryl alcohol

[0020]

Embodiment 3

[0021] Example 3: 5.10 g of tetrahydrofurfuryl alcohol and 0.1 mol% vanadyl sulfate were added to a 50 mL reactor to close the reactor, filled with oxygen at a pressure of 1.0 MPa, heated to 80° C. under stirring, and kept for 15 hours. Then cooled to room temperature, decompressed to normal pressure, sampling analysis, tetrahydrofurfuryl alcohol conversion rate was 79%, gamma-butyrolactone selectivity was 77%.

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Abstract

The invention provides a novel method for preparing gamma-butyrolactone. With the method, molecular oxygen (air or oxygen) is adopted as an oxygen source; a high-efficiency catalyzing method is adopted, and tetrahydrofurfuryl alcohol is directly subjected to liquid-phase selective oxidation, such that gamma-butyrolactone is obtained. The method adopts a reaction raw material of tetrahydrofurfuryl alcohol which can be obtained from biomass raw materials such as corn cob, husk, and downstream product furaldehyde. The material source is rich, and price is low. The method is a gamma-butyrolactone preparation novel technological path which is independent of fossil resources. During the reaction process, no solvent is needed. The reaction condition is mild. The method has important application prospect.

Description

technical field [0001] The invention relates to a new method for preparing gamma-butyrolactone by catalytic selective oxidation of tetrahydrofurfuryl alcohol. The reaction raw material tetrahydrofurfuryl alcohol used in this method can be obtained from bio-based raw materials such as corncobs, rice husks and its downstream products furfural, which has abundant sources and mild oxidation reaction conditions. technical route. Background technique [0002] γ-butyrolactone is an important fine chemical, which is widely used in petrochemical, textile, fragrance, pesticide and pharmaceutical industries. γ-butyrolactone is a solvent with high boiling point, strong solubility, high conductivity and good stability. It is often used as an extractant and absorbent in the petroleum industry and as an electrolyte solution in the battery industry. As a chemical intermediate, γ-butyrolactone is mainly used in the synthesis of N-methylpyrrolidone, polyvinylpyrrolidone, etc., and can also ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
Inventor 杜中田徐杰刘俊霞杨艳良苗虹高进
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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