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Direct transformation process of ethyl levulinate by hydrolysis of cellulose materials

A technology of ethyl levulinate and cellulose, applied in the field of ethyl levulinate preparation, can solve the problems of many by-products, low yield of ethyl levulinate, etc., to reduce the generation of by-products and prevent further The effect of reducing and increasing productivity

Active Publication Date: 2013-09-04
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The reaction process can be carried out under the condition of mixing and heating cellulose with acid and ethanol, but due to the deficiency of the reaction system, there are more by-products, and the yield of ethyl levulinate is relatively low.

Method used

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  • Direct transformation process of ethyl levulinate by hydrolysis of cellulose materials
  • Direct transformation process of ethyl levulinate by hydrolysis of cellulose materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 5g of crushed straw with 50g of the reaction system, the reaction system is composed of ethanol, hydrochloric acid and carbon tetrachloride with a mass ratio of 40:1:20, react at 200°C for 10min, cool down after the reaction, and filter the reaction hydrolyzate. The filtrate was extracted and purified to obtain 1.2 g of ethyl levulinate.

Embodiment 2

[0023] Mix 10g of crushed straw with 200g of the reaction system, the reaction system is composed of ethanol, TiO 2 / SO 4 2- Composition with methyl isobutyl ketone, react at 180°C for 20 minutes, cool down after the reaction, filter the reaction hydrolyzate, extract and refine the filtrate to obtain 2.5 g of ethyl levulinate.

Embodiment 3

[0025] Mix 15g of crushed straw with 100g of the reaction system, the reaction system is composed of ethanol, MCM-41 and toluene with a mass ratio of 70:10:60, react at 150°C for 60min, cool down after the reaction, filter the reaction hydrolyzate, and the filtrate After extraction and purification, 4.5 g of ethyl levulinate was obtained.

[0026] The product of embodiment 1-3 adopts infrared spectrum qualitative, as figure 1 Shown: Main group: 1740cm -1 Carbonyl C=O stretching vibration absorption peak of ester, 2950cm -1 For the C-H stretching vibration of alkanes, the product is ethyl levulinate.

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Abstract

The invention belongs to the technical field of preparing ethyl levulinate, in particular to a direct transformation process of ethyl levulinate by hydrolysis of cellulose materials. The process comprises the following steps: adding the cellulose materials into a reaction system comprising ethanol, liquid acid catalyst / solid acid catalyst, and cosolvent, hydrolyzing for 2 to 60 minutes at the temperature of 150 to 230 DEG C to obtain hydrolyzate containing the ethyl levulinate, and purifying the hydrolyzate to obtain the ethyl levulinate. In the invention, the cosolvent is added into the hydrolysis system of the cellulose materials, and the intermediate products such as hydromethyl furfural, the levulinic acid and the like generated during the hydrolysis of the cellulose materials can be extracted into an organic phase containing the cosolvent in the presence of the cosolvent, thereby preventing the further reduction of the intermediate products, facilitating the reduction of by-products and facilitating the yield increase of ethyl levulinate.

Description

technical field [0001] The invention belongs to the technical field of preparation of ethyl levulinate, and in particular relates to a process for directly converting cellulose substances into ethyl levulinate through hydrolysis. Background technique [0002] Ethyl levulinate is an important chemical product. In addition to being used as a spice and fruit fresh-keeping agent, it can also be used as a diesel oxygenator with good performance. It is mixed with diesel at a ratio of 20%. The mixed diesel has It has the advantages of clean combustion, good lubricity, and reduced sulfur content, and meets the American ASTM D-975 diesel standard. [0003] At present, the production of ethyl levulinate is mostly based on levulinic acid as the starting material, which is obtained by esterification reaction with ethanol through the catalysis of acid catalyst. Due to the high price of levulinic acid itself, the price of ethyl levulinate is high. Therefore, reducing production costs is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/716C07C67/00
Inventor 常春马晓建姜孝先方书起李洪亮陈俊英韩秀丽
Owner ZHENGZHOU UNIV
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