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Method for synthesis of acetyl propionate through microwave assisted liquefaction of biomass straw

A technology of biomass straw and levulinate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problem of low solid catalyst recycling rate, high reaction temperature, and difficult product separation. and other problems, to achieve the effect of optimizing biomass resource utilization technology, easy control of process conditions and simple production process

Inactive Publication Date: 2014-11-26
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Chinese patent application CN102659594A discloses a method for preparing ethyl levulinate from straw-like biomass. The method uses straw-like biomass as a raw material, and first uses ethanol extraction to remove lignin from cellulosic biomass, and then uses Add the ethanol solution of acid to carry out the alcoholysis esterification reaction, although the utilization rate of raw materials can be improved, and the by-products of the reaction are few, but the amount of solvent consumed is large, the reaction time is long, and the yield of ethyl levulinate is 15.0%-17.9%
To a certain extent, it can overcome the disadvantages of inorganic acid as a catalyst for equipment corrosion and environmental pollution, but the solid catalyst has a low reuse rate and is difficult to separate from the product. At the same time, the price of furfuryl alcohol as a raw material is high, which increases the production of ethyl levulinate accordingly. cost
[0010] Chinese patent application CN103360255A discloses a method for preparing ethyl levulinate from furfural slag. Using furfural waste slag, liquid acid and solid acid are used as composite catalysts to prepare ethyl levulinate, which can solve the problem of low catalytic effect of solid acid to a certain extent. The disadvantage of easy deactivation, but the temperature required for the reaction is higher, the energy consumption is larger, and the yield of ethyl levulinate obtained is 14.56%-16.10%

Method used

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  • Method for synthesis of acetyl propionate through microwave assisted liquefaction of biomass straw
  • Method for synthesis of acetyl propionate through microwave assisted liquefaction of biomass straw
  • Method for synthesis of acetyl propionate through microwave assisted liquefaction of biomass straw

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Effect test

Embodiment 1

[0031] Add 5g of corn stalks, 25g of methanol, and 0.5g of concentrated sulfuric acid to the PTFE tube, stir evenly, add a stirrer, and put it into the microwave reaction chamber after installation; set the temperature at 160°C, and microwave power at 600w. Put a temperature sensor in it, keep the reaction conditions for 35min, and carry out the reaction under constant stirring. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of methyl levulinate was 39.22mol%.

Embodiment 2

[0033] Add 5g of corn stalks, 30g of ethanol, and 0.9g of concentrated sulfuric acid into the PTFE tube, stir evenly, add a stirrer, and put it into the microwave reaction chamber after installation; set the temperature at 180°C, and microwave power at 600w. Put a temperature sensor in it, keep the reaction conditions for 30min, and carry out the reaction under constant stirring. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of ethyl levulinate was 40.06mol%.

Embodiment 3

[0035] Add 4g of corn stalks, 28g of n-butanol, and 1.12g of concentrated sulfuric acid into the PTFE tube, stir evenly, add a stirrer, and put it into the microwave reaction chamber after installation; set the temperature at 200°C, and microwave power at 600w. A temperature sensor was placed in the controlled tank, and the reaction conditions were maintained for 25 minutes, and the reaction was carried out under constant stirring. After the reaction was completed, the reaction mixture was taken out after rapid cooling by air cooling. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of butyl levulinate was 32.93mol%.

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Abstract

The invention provides a method for synthesis of acetyl propionate through microwave assisted liquefaction of biomass straw. The method includes the steps: (1) adding the biomass straw, a liquefaction agent and an acid catalyst in a reaction vessel (a polytetrafluoroethylene tube), adding a stirring bar, and after installation, putting into a microwave reaction chamber; and (2) carrying out a microwave assisted reaction to synthesize the acetyl propionate, and after completion of the reaction, naturally cooling, and taking out the reaction product from the microwave reaction chamber, wherein the liquefaction agent is selected from at least one of methanol, ethanol and n-butanol.

Description

technical field [0001] The invention relates to the technical field of preparation of levulinic acid esters, in particular to a method for synthesizing levulinic acid esters by microwave-assisted liquefaction of biomass straws. Background technique [0002] Biomass is the most ubiquitous substance on the earth. It is a natural renewable resource that can replace the increasingly depleted fossil energy and has great potential for development. my country is a large agricultural country and also has abundant biomass resources. Currently, the biomass resources that can be developed and utilized are mainly renewable and recycled biomass waste, such as crop straw, animal manure, industrial and urban waste, etc. The main components of crop straw are cellulose, hemicellulose and lignin. Due to the high degree of lignification of plant straw, it is necessary to convert solid macromolecular organic polymers into liquid small molecular substances through physical, chemical or biologica...

Claims

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Application Information

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IPC IPC(8): C07C69/716C07C67/00
CPCC07C67/00C07C69/716
Inventor 肖卫华韩鲁佳刘欢王雪张宇轩陈雪礼
Owner CHINA AGRI UNIV