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Method for preparing ethyl levulinate by using straw-type biomass

A technology of ethyl levulinate and biomass, which is applied in the directions of lignin derivatives, chemical instruments and methods, reaction preparation of ester groups and hydroxyl groups, etc., can solve the problems of many by-products, low product concentration, and high production costs, and achieves The reaction time is short, the product concentration is high, and the utilization rate is improved.

Active Publication Date: 2012-09-12
ZHENGZHOU UNIV
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  • Abstract
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AI Technical Summary

Problems solved by technology

The first synthetic route is to use levulinic acid as a raw material to obtain ethyl levulinate through esterification with ethanol; this synthetic route requires high purity of raw material levulinic acid, so the production cost is relatively high
The second synthetic route is the furfuryl alcohol conversion method, which uses furfuryl alcohol and ethanol as raw materials to generate ethyl levulinate through hydrolysis, ring opening and rearrangement reactions under acidic conditions; High, the reaction medium, catalyst and reaction conditions have a greater impact on the yield of the product, and the total production cost is high
The third synthetic route is obtained from cellulosic biomass raw materials, which are obtained by alcoholysis under high temperature and high pressure using a "one-pot method"; this synthetic route has the advantages of wide sources of raw materials and simple process, but due to the Diverse, and contains unreactable lignin components, so there are many by-products, low yield, low product concentration, etc.

Method used

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  • Method for preparing ethyl levulinate by using straw-type biomass
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  • Method for preparing ethyl levulinate by using straw-type biomass

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) In the autoclave, add 7g of wheat straw (containing 39.46% cellulose) and 70ml of 85% ethanol, maintain the pressure at 1.0Mpa, and the reaction time is 3h. After the reaction, perform vacuum filtration for solid-liquid separation to obtain the filtrate and 5g of filter residue; (2) After the filtrate is distilled, ethanol is recovered, and the recovered ethanol can be recycled for the pretreatment of straw and the next reaction, and the filtrate after recovery of ethanol is concentrated and dried to obtain ethanol lignin; (3) The filter residue is In the still, add 50ml of sulfuric acid ethanol solution, the volume concentration of sulfuric acid in the sulfuric acid ethanol solution is 5%, and react at 170°C for 60min to obtain a hydrolyzate containing ethyl levulinate. The GC-MS spectrum and GC spectrum of the hydrolyzate are as follows: figure 1 , 2 Shown, utilize GC-MS qualitative hydrolyzate main product to be ethyl levulinate (19.58min), chromatographic quant...

Embodiment 2

[0023] (1) In the autoclave, add 7.5g of corn stalks (containing 35.20% cellulose) and 150ml of 90% ethanol, maintain the pressure at 1.5Mpa, and the reaction time is 2.5h. After the reaction, perform solid-liquid separation by pressure filtration to obtain Filtrate and 5.6g filter residue; (2) After the filtrate is distilled, ethanol is recovered, and the recovered ethanol can be recycled for the pretreatment of straw and the next reaction, and the filtrate after recovering ethanol is concentrated and dried to obtain ethanol lignin; (3) Filter residue In the autoclave, add 84ml ethanol solution of hydrochloric acid, the volume concentration of hydrochloric acid in the ethanol solution of hydrochloric acid is 2.5%, and react at 190°C for 30min to obtain a hydrolyzate containing ethyl levulinate. Utilize GC-MS qualitative hydrolyzate main product to be ethyl levulinate, chromatographic quantitative analysis shows that the quality of ethyl levulinate is 1.23g, and the productive ...

Embodiment 3

[0025] (1) In the autoclave, add 6g of sorghum straw (containing 32.50% cellulose) and 180ml of 95% ethanol, maintain the pressure at 2.0 Mpa, and the reaction time is 1.0 h. After the reaction is completed, perform solid-liquid separation by pressure filtration to obtain the filtrate and 5.85g of filter residue; (2) After the filtrate is distilled, ethanol is recovered, and the recovered ethanol can be recycled for the pretreatment of straw and the next reaction, and the filtrate after recovery of ethanol is concentrated and dried to obtain ethanol lignin; (3) The filter residue is in In the autoclave, add 117ml of phosphoric acid ethanol solution, the volume concentration of phosphoric acid in the phosphoric acid ethanol solution is 1.0%, and react at 220°C for 10 minutes to obtain a hydrolyzate containing ethyl levulinate. Utilize GC-MS qualitative hydrolyzate main product to be ethyl levulinate, chromatographic quantitative analysis, the quality of ethyl levulinate 0.9g, th...

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Abstract

The invention belongs to the technical field of preparation of ethyl levulinate and particularly relates to a method for preparing ethyl levulinate by using straw-type biomass. According to the method, lignin in cellulose biomass is removed by ethanol extraction, alcoholysis esterification is performed, and both ethanol lignin and ethyl levulinate are obtained, so the utilization rate of raw materials is improved. Moreover, the method has the advantages of short reaction time, less side reaction and high product concentration.

Description

technical field [0001] The invention belongs to the technical field of ethyl levulinate preparation, and in particular relates to a method for preparing ethyl levulinate by utilizing straw-like biomass. Background technique [0002] Straw biomass resource is a kind of biomass resource with wide sources, huge quantity and renewable. However, the degree of utilization of straw biomass resources is relatively low at present, and the development of straw biomass resources into important chemical products has become an important research topic in the field of biomass chemical technology. [0003] As a bulk chemical product, ethyl levulinate has a wide range of uses and can be used in chemical, pharmaceutical, fragrance, new energy and other fields. [0004] At present, the production method of ethyl levulinate reported mainly contains three approaches. The first synthetic route is to use levulinic acid as a raw material to obtain ethyl levulinate through esterification with eth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/03C08H7/00C07G1/00
Inventor 常春徐桂转姜孝先马晓建李洪亮方书起
Owner ZHENGZHOU UNIV
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