Method for synthesizing acetyl propionate by catalyzing alcoholysis of biomass carbohydrate through microwave assistance in presence of phosphotungstic acid and phosphowolframate

A technology of levulinic acid ester and carbohydrate, applied in the field of synthesis and preparation of levulinic acid ester, can solve the problems of unsatisfactory catalytic effect, inability to effectively recycle and reuse the catalyst, long reaction time, etc. The effect of high rate and short response time

Active Publication Date: 2017-09-15
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It shows that this method also has problems such as long reaction time required, unsatisfactory catalytic effect on high polysaccharides such as cellulose, etc., and the catalyst cannot be effectively recycled and reused.

Method used

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  • Method for synthesizing acetyl propionate by catalyzing alcoholysis of biomass carbohydrate through microwave assistance in presence of phosphotungstic acid and phosphowolframate
  • Method for synthesizing acetyl propionate by catalyzing alcoholysis of biomass carbohydrate through microwave assistance in presence of phosphotungstic acid and phosphowolframate
  • Method for synthesizing acetyl propionate by catalyzing alcoholysis of biomass carbohydrate through microwave assistance in presence of phosphotungstic acid and phosphowolframate

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preparation example Construction

[0044] The preparation methods of iron phosphotungstate, indium phosphotungstate and chromium phosphotungstate are basically the same as those of aluminum phosphotungstate.

[0045] In the following examples, the conditions of gas chromatography analysis are as follows:

[0046] Chromatographic column: DB-5 (30m×0.250mm, 0.25μm); hydrogen flame ionization detector (FID); heating program: initial temperature 60°C, keep 3min; increase to 180°C at 6°C / min, keep 3min; Then rise to 270°C at 10°C / min and keep for 15min; the temperature of the injection port is 250°C; the temperature of the detector is 270°C; the injection volume is 1 μL; the carrier gas is nitrogen; ester yield.

Embodiment 1

[0048] Add 2g glucose, 15g methanol (liquid-solid ratio 7.5:1g / g) and 0.4mmol aluminum phosphotungstate to the PTFE tube, add a stirrer, pass in argon gas and put it into the microwave reaction chamber after installation, and use magnetic force The stirrer pre-stirred for 1 min to mix the reactants evenly; set the microwave power to 600W, and raised the temperature to 160°C within 2 min. The temperature was maintained for 30 min under 500W microwave power, and the reaction was carried out under constant stirring; after the reaction was completed, the temperature was rapidly cooled to room temperature using an ice-water bath, and the reaction mixture was taken out. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of methyl levulinate was 64mol%.

Embodiment 2

[0050] Add 1g sucrose, 15g ethanol (liquid-solid ratio 15:1g / g) and 0.3mmol phosphotungstic acid to the PTFE tube, add a stirrer, pass in argon gas, put it into the microwave reaction chamber after installation, and use magnetic stirring Pre-stirrer for 1 min to mix the reactants evenly; set the microwave power to 600W, and raise the temperature to 190°C within 2 min. The temperature was maintained for 30 min under 500W microwave power, and the reaction was carried out under constant stirring; after the reaction was completed, the temperature was rapidly cooled to room temperature using an ice-water bath, and the reaction mixture was taken out. The reaction mixture was taken and analyzed by gas chromatography to calculate that the yield of ethyl levulinate was 45 mol%.

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Abstract

The invention discloses a method for synthesizing acetyl propionate by catalyzing alcoholysis of biomass carbohydrate through microwave assistance in the presence of phosphotungstic acid and phosphowolframate. The method comprises the step of allowing biomass carbohydrate and alcohol to react under the conditions of microwave assistance and a catalyst, so as to obtain acetyl propionate, wherein the catalyst is phosphotungstic acid or a phosphowolframate, phosphowolframate is any one of aluminum phosphowolframate, iron phosphowolframate, indium phosphowolframate and chromium phosphowolframate, and the use amount of the catalyst is 0.1mmol/15g-0.5mmol/15g of alcohol. The method for preparing acetyl propionate by catalyzing biomass carbohydrate through microwave assistance in the presence of phosphotungstic acid and phosphowolframate has the beneficial effects that the process is simple, reaction conditions are mild, the reaction time is short, the energy consumption can be reduced, and the yield of acetyl propionate is high; and the used catalyst is easy to prepare, has wide applicability to the raw materials, can be repeatedly used, and the catalytic activity of the catalyst is not obviously decreased.

Description

technical field [0001] The invention relates to a microwave-assisted method for phosphotungstic acid or its salt to catalyze the alcoholysis of biomass carbohydrates to synthesize levulinate, which belongs to the field of synthesis and preparation of levulinate. Background technique [0002] At present, the depletion of traditional non-renewable fossil resources such as oil, natural gas and coal and the environmental problems caused by their consumption have become two major problems restricting the sustainable and rapid development of human society. Biomass is a renewable resource with abundant reserves, wide distribution, low price and carbon fixation function. It has the potential to replace fossil resources in the production of hydrocarbon fuels and chemical products. In recent years, the efficient conversion and utilization of biomass resources has received more and more attention. Studies have found that biomass such as lignocellulose is mainly composed of cellulose, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/00C07C69/716B01J27/28
CPCB01J27/285C07C67/00C07C69/716Y02P20/584
Inventor 肖卫华张宇轩韩鲁佳吕雪陈雪礼赵广路
Owner CHINA AGRI UNIV
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