A method for preparing formate, acetate and levulinate by utilizing straw biomass

A technology of levulinic acid ester and biomass, which is applied in the field of formate, acetate, and levulinic acid ester preparation. It can solve the problems of accumulation, large by-products, and difficulty in removing levulinic acid, so as to improve the utilization rate , Lighten the detoxification process route and overcome the effect of massive accumulation of by-products

Active Publication Date: 2017-11-14
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing formate, acetate, and levulinate by using straw biomass, which solves the problem of the accumulation of by-products after dilute acid hydrolysis of cellulosic biomass. Difficulty in removing acetic acid and levulinic acid

Method used

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  • A method for preparing formate, acetate and levulinate by utilizing straw biomass
  • A method for preparing formate, acetate and levulinate by utilizing straw biomass
  • A method for preparing formate, acetate and levulinate by utilizing straw biomass

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Effect test

Embodiment 1

[0016] (1) In a 5L electric heating reactor with a stirring device, add 300g of wheat straw (the mass fraction of cellulose is 40.21%) and 3000mL of ethanol sulfuric acid solution (the liquid-solid ratio of straw to alkyd aqueous solution is 10mL / g ), the ethanol concentration is 25wt%, the sulfuric acid concentration is 3.0wt%, the stirring rate is 60r / min, the reaction temperature is 80-200°C, and the reaction time is 180min. After reaction finishes, be cooled to room temperature, carry out distillation, the distillate that obtains is the mixture of ethyl formate, ethyl acetate and ethanol (the GC collection of illustrative plates of distillate is as figure 1 shown), the mixture at the bottom of the still is still liquid and hydrolysis slag;

[0017] (2) The bottom mixture was subjected to vacuum filtration for solid-liquid separation to obtain filtrate and 185 g of filter residue respectively. The resulting filtrate is a hydrolyzate mainly containing glucose, xylose, arabi...

Embodiment 2

[0019] (1) In a 5L electric heating reactor with a stirring device, add 500g of wheat straw (the mass fraction of cellulose is 40.21%) and 3000ml of methanolic hydrochloric acid solution (the liquid-solid ratio of straw to alkyd aqueous solution is 6mL / g ), the concentration of methanol is 30wt%, the concentration of hydrochloric acid is 3.5wt%, the stirring speed is 80r / min, the reaction temperature is 80~200°C, and the reaction time is 90min. After the reaction is finished, cool to room temperature and carry out distillation. The distillate obtained is a mixture of methyl formate, methyl acetate and methanol, and the mixture at the bottom of the still is still liquid and hydrolysis residue;

[0020] (2) The mixture at the bottom of the still was subjected to vacuum filtration for solid-liquid separation to obtain filtrate and 460 g of filter residue respectively. The resulting filtrate is a hydrolyzate mainly containing glucose, xylose, arabinose and methyl levulinate.

[0...

Embodiment 3

[0023] (1) In a 5L electric heating reactor with a stirring device, add 600g corn stalks (the mass fraction of cellulose is 32.22%) and 3000ml ethanol phosphoric acid solution (the liquid-solid ratio of straw to alkyd aqueous solution is 5mL / g ), the ethanol concentration is 1.0wt%, the phosphoric acid concentration is 1.5wt%, the stirring rate is 80r / min, the reaction temperature is 80-200°C, and the reaction time is 120min. After the reaction is finished, cool to room temperature and distill, the distillate obtained is a mixture of ethyl formate, ethyl acetate and ethanol, and the mixture at the bottom of the still is still liquid and hydrolysis residue;

[0024] (2) The bottom mixture was subjected to vacuum filtration for solid-liquid separation to obtain filtrate and 536 g of filter residue respectively. The resulting filtrate is a hydrolyzate mainly containing glucose, xylose, arabinose and ethyl levulinate.

[0025] Referring to Table 1, it is known that the main subst...

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Abstract

The invention discloses a method for preparing formate, acetate and levulinate from straw-like biomass. Biomass and alcohol are used as reaction raw materials, and acid is used as a catalyst for dilute acid hydrolysis of cellulose biomass. At the same time, as a catalyst for the esterification reaction, the cellulose and hemicellulose in the biomass are hydrolyzed into glucose, xylose, arabinose and organic acids. At the same time, the secondary degradation products of monosaccharides in the hydrolysis process are formic acid, acetic acid and acetyl The esterification reaction of propionic acid not only overcomes the accumulation of by-products after dilute acid hydrolysis of cellulose biomass, but also the difficulty in removing formic acid, acetic acid, and levulinic acid during the detoxification process, which is conducive to obtaining a hydrolyzate suitable for subsequent microbial fermentation. It is also possible to obtain a hydrolyzate mainly containing monosaccharides such as glucose, xylose, and arabinose, and at the same time obtain formate, acetate, and levulinic acid ester, which improves the utilization rate of raw materials and provides opportunities for comprehensive utilization of straw. a realistic approach.

Description

Technical field: [0001] The invention relates to a method for preparing formate, acetate and levulinate, in particular to a method for preparing formate, acetate and levulinate from straw biomass. Background technique: [0002] For a long time, my country, as a large agricultural country, has a wide range of straw biomass resources and a huge amount. The traditional method of using straw biomass in vast rural areas is direct burning, which not only has low utilization efficiency, but also pollutes the environment and endangers human health. It has become an important research topic in the field of biomass chemical technology to develop and utilize straw biomass resources into important chemical products and improve utilization efficiency. Generally, microorganisms can use glucose and other monosaccharides as culture medium to ferment and produce products that people need, such as microbial oil, ethanol, biogas, bacterial cellulose, etc. However, the high cost of traditional...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H3/02C07H1/00C07C67/08C07C69/06C07C69/14C07C69/716
Inventor 陈新德陈雪芳熊莲王璨黄超齐高相
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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