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Method for high-selectivity preparation of gamma-GVL by homogeneous catalysis

A homogeneous catalysis and valerolactone technology, applied in organic chemistry and other fields, can solve problems such as time-consuming, hinder large-scale production, and unsatisfactory industrial production, and achieve convenient operation, improved safety and economy, and low equipment requirements Effect

Active Publication Date: 2017-02-22
CHINA AGRI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method has greatly improved the previous explorations, it still cannot be separated from the protection of inert gas, and the reaction time takes 9 hours, which is time-consuming and does not meet the requirements of industrial production.
[0007] Generally speaking, the preparation of gamma-valerolactone by the prior art has the problem of hindering large-scale production

Method used

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  • Method for high-selectivity preparation of gamma-GVL by homogeneous catalysis
  • Method for high-selectivity preparation of gamma-GVL by homogeneous catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 0.5g methyl levulinate, 8g isopropanol, 0.25g aluminum isopropoxide to the glass reaction tube, stir evenly, add a stirrer, put it into the microwave synthesis reactor after installation; set the initial microwave power as 300W, set the temperature at 150°C, and reacted for 30 minutes under constant speed stirring. After the reaction was completed, the system air cooling was used to quickly cool down to 40°C, and then the reaction mixture was taken out. The reaction product was analyzed by gas chromatography-mass spectrometry, and the results were as follows: figure 1 and figure 2 As shown, it is confirmed that the product of this reaction is determined to be γ-valerolactone, and it also proves that the conversion rate of the substrate in this reaction process is high, and almost no side reactions occur, which is beneficial to the separation and purification of later products. It is calculated that the conversion rate of methyl levulinate is 100%, and the yield of...

Embodiment 2

[0027] Add 0.5g ethyl levulinate, 8g isopropanol, 0.25g aluminum isopropoxide to the glass reaction tube, stir evenly, add a stirrer, put it into the microwave synthesis reactor after installation; set the initial microwave power as 300W, set the temperature at 160°C, and carried out the reaction for 40 minutes under constant stirring. After the reaction was completed, the system air cooling was used to quickly cool down to 40°C, and then the reaction mixture was taken out. Calculated by gas chromatography analysis, the conversion rate of ethyl levulinate was 100%, and the yield of GVL was 88.14%.

Embodiment 3

[0029] Add 0.5g butyl levulinate, 8g isopropanol, 0.25g aluminum isopropoxide to the glass reaction tube, stir evenly, add a stirrer, put it into the microwave synthesis reactor after installation; set the initial microwave power as 300W, set the temperature at 160°C, keep the reaction conditions for 40min, and carry out the reaction under constant speed stirring. Calculated by gas chromatography analysis, the conversion rate of butyl levulinate was 100%, and the yield of GVL was 94.09%.

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Abstract

The invention relates to a method for preparing gamma-GVL by homogeneous catalysis. According to the method, levulinic acid esters are taken as raw materials, secondary alcohols are taken as hydrogen sources and solvents, and in the catalysis of aluminium isopropoxide, hydrogen transfer and lactonization are carried out to obtain the gamma-GVL. The method for the high-selectivity preparation of the gamma-GVL by the homogeneous catalysis has the advantages of short reaction time, fast substrate conversion, high conversion rate, high product selectivity and almost no side reaction. The method does not require high-pressure hydrogen in the reaction process, thereby not needing to isolate air; used catalysts are non-noble metal catalysts, so that the prices are low; harsh reaction conditions of requirements on high temperature and high pressure, protection of inert gases and use of noble metal catalysts are avoided in the existing preparation process, and the method disclosed by the invention is mild in reaction conditions, low in equipment requirements, simple in process and convenient to operate. The secondary alcohols in the method can be recycled. The safety and economy of the preparation method are improved.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation, in particular to a method for preparing gamma-valerolactone with homogeneous catalysis and high selectivity. Background technique [0002] With the depletion of fossil resources required for human survival and development, it is imminent to find new alternative resources. Biomass is the most ubiquitous substance on the earth, with wide distribution, large output, no pollution, and also the only recyclable carbon resource, so it is considered to be a new type of energy that is most likely to replace fossil resources. So at present, the use of biomass to produce chemical products and new fuels has received more and more attention. [0003] γ-valerolactone (abbreviated as GVL) is an excellent fuel additive, but also a green solvent and food additive. In the field of medicine, it is widely used as an anti-cancer pharmaceutical intermediate. Its characteristics of low melting po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 肖卫华赵婷婷韩鲁佳
Owner CHINA AGRI UNIV
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