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Method for preparing ethyl levulinate from pennisetum sinese stalks

A technology of ethyl levulinate and Juncao is applied in directions such as carboxylate preparation, chemical instrument and method, preparation of organic compounds, etc., and can solve the problems of low yield of ethyl levulinate, low catalyst efficiency, and low reaction temperature. Advanced problems, to achieve the effect of reducing the requirements of reaction conditions, shortening the reaction time, and low cost

Pending Publication Date: 2021-09-03
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

For example, Jidnyasa Hedal et al. used microporous acidic H-USY zeolite to convert wheat straw into ethyl levulinate, and the yield was only 24.5%, which shows that the yield is inefficient (Microporous and Mesoporous Materials, 2020, 306, 1387-1811 ); and Chang Chun et al. used sulfuric acid as a catalyst to treat wheat straw, and the yield of the ester was slightly increased to 51.0% (Bioresource Technology, 2012, 121, 93-99), and the above reactions were carried out at high temperatures from 180°C to 200°C ; Huan Liu et al. used sulfuric acid to catalyze ball milling of pretreated corn stover under microwave radiation, and the yield of ethyl levulinate was only 44.6% (Fuel Processing Technology, 2018, 174, 53-60), which shows that the preparation of biomass raw materials The yield of ethyl levulinate is low
In short, currently, biomass itself is used as a raw material to prepare ethyl levulinate, the reaction temperature is high and time-consuming, the catalyst efficiency is low, and more importantly, the yield of ethyl levulinate is generally low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: In this embodiment, the method for preparing ethyl levulinate by using the stalk of Jujuncao is as follows:

[0022] (1) Crush and sieve the air-dried stalks of Jujuncao, select 40 mesh to 60 mesh powder raw materials, and then dry at 105°C for 24 hours;

[0023] (2) Mix 5g of giant stalk powder and 100mL NaOH solution (mass concentration 1%) into the Erlenmeyer flask, put it into the rotor and seal it, put it in the water bath, and stir it at a constant speed of 20r / min at 80°C 60min;

[0024] (3) After the reaction is completed, cool and filter the mixture in the Erlenmeyer flask, wash the filter residue with distilled water until the filtrate is neutral, and dry it at 105°C to constant weight to obtain the pretreated giant fungus grass, which is sealed and stored in a dry place for later use;

[0025] The cellulose, hemicellulose and lignin components of the stalks and the pretreated materials of the giant genus were analyzed by the two-step acid hydro...

Embodiment 2

[0030] Embodiment 2: In this embodiment, the method for preparing ethyl levulinate by utilizing the stalk of Jujuncao is as follows:

[0031] (1) Crush and sieve the air-dried stalks of Jujuncao, select 40 mesh to 60 mesh powder raw materials, and then dry at 100°C for 24 hours;

[0032](2) Mix 5g of giant stalk powder and 100mL NaOH solution (mass concentration 1%) into the Erlenmeyer flask, put the rotor into the water bath after sealing it, and stir at a constant speed of 20r / min at 75°C for reaction 60min;

[0033] (3) Cool and filter the mixture in the Erlenmeyer flask after the reaction is completed, wash the filter residue with distilled water until the filtrate is neutral, and dry it at 100°C to constant weight to obtain the pretreated giant Juncao, which is sealed and stored in a dry place for later use;

[0034] (4) Weigh 0.1g and 0.0237g Al(OTf) of the pretreated stalk samples of Jujuncao 3 Add it into a stainless steel autoclave lined with polytetrafluoroethylene...

Embodiment 3

[0036] The method for preparing ethyl levulinate by using the stalks of giant fungus grass described in this example, the specific steps are the same as in Example 1, the difference is that the alcoholysis reaction was carried out at 190°C for 60 minutes to obtain the reaction product ethyl levulinate, which was used Gas chromatography analysis showed that the yield of ethyl levulinate was 72.6%.

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Abstract

The invention provides a method for preparing ethyl levulinate from pennisetum sinese stalks, and belongs to the technical field of biomass energy chemical engineering; the method comprises the following steps: by taking the pennisetum sinese stalks as a raw material, carrying out pretreatment by using a NaOH solution, and then further carrying out alcoholysis on collected solid residues to prepare the ethyl levulinate; in the alcoholysis process, a cosolvent of gamma-valerolactone and ethanol is used as a reaction medium, Al(OTf)3 is used as a catalyst, the reaction is carried out at 170-190 DEG C, and the highest yield of the reaction product ethyl levulinate can reach 72.6%. A biomass fiber raw material is converted into ethyl levulinate through pretreatment and the synergistic effect of gamma-valerolactone and an ethanol system; the ethyl levulinate is directly prepared from the pennisetum sinese stalks, and the method has the advantages of cheap and easily available raw materials, high conversion efficiency and target product yield, economical and efficient preparation process and the like, and has a good industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing ethyl levulinate from the stalks of giant fungus grass, and belongs to the technical field of biomass energy chemical industry. Background technique [0002] As a globally renewable resource, biomass energy is of great significance to transform its high-value utilization into the production of high-grade fuels and chemicals. The current research shows that both cellulose and hemicellulose components in biomass carbohydrates can be used as raw materials for the preparation of levulinate. However, due to the structural complexity of biomass raw materials, the diversity of components, and their insoluble properties in the reaction medium, it is difficult to deconstruct and utilize biomass carbohydrates, resulting in low conversion rates of biomass raw materials and low yields of finished products. Good and other issues. Therefore, seeking efficient and practical pretreatment methods and catalytic systems i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/00C07C69/716
CPCC07C67/00C07C69/716
Inventor 彭林才孔艳萍张俊华宋伟鹏
Owner KUNMING UNIV OF SCI & TECH
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