Method for promoting extraction of lignin in straw and catalytically preparing levulinic acid and ethyl ester thereof by using ammonium-based Brownst acidic ionic liquid

An acidic ionic liquid, catalytic preparation technology, applied in the direction of carboxylate preparation, carboxylate preparation, lignin derivatives, etc., can solve the problems of low yield of lignin extraction, complicated operation process, waste of resources and environment, and achieve Low cost, less dosage, and the effect of reducing pollution

Active Publication Date: 2022-02-01
CHINA UNIV OF MINING & TECH
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  • Abstract
  • Description
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Problems solved by technology

[0009] The purpose of the present invention is to provide a kind of ammonium-based Bronster acidic ionic liquid to promote the extraction of lignin in straw and catalyze the method for preparing levulinic acid and ethyl levulinate thereof, so as to solve the problem of low yield of lignin extraction, High cost, complex operation process, and waste generated during the reaction process cause waste of resources and environmental pollution

Method used

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  • Method for promoting extraction of lignin in straw and catalytically preparing levulinic acid and ethyl ester thereof by using ammonium-based Brownst acidic ionic liquid
  • Method for promoting extraction of lignin in straw and catalytically preparing levulinic acid and ethyl ester thereof by using ammonium-based Brownst acidic ionic liquid
  • Method for promoting extraction of lignin in straw and catalytically preparing levulinic acid and ethyl ester thereof by using ammonium-based Brownst acidic ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Such as figure 2 As shown, take 9g pretreated straw powder, 6mmol ammonium-based Acidic ionic liquid and 150mL aqueous ethanol (V C2H5OH / V H2O ; 4: 1) placed in the reaction kettle, fed with nitrogen protection, the initial pressure is 1MPa, the set speed is 300r / min, the reaction temperature is 200°C, and the reaction time is 30min. After the reaction, the reaction product is taken out, cooled to room temperature rapidly, and filtered 1. Wash (deionized water, 3×30mL), then add 500mL deionized water and let stand for 24h. Finally, the resulting mixture was filtered, washed, dried and ground to obtain a brown solid powder, ie lignin, which was sealed and stored in a dry place, and the yield of lignin was 23.73%.

[0044] image 3 For pretreated straw, without adding ionic liquid and adding [BSTEA]HSO 4 Fourier transform infrared spectrum of extracted lignin (TEAILL). image 3 Medium 3450-3300cm -1 、2935cm -1 and 2841cm -1 The peak at is attributed to -OH, -O...

Embodiment 2

[0057] Such as figure 2 As shown, take 0.5g of the residue CRR of the rich fiber component obtained by filtering after the heating reaction in Example 1, 30wt.% (based on CRR) ammonium-based type Acidic ionic liquid and 20mL of absolute ethanol are placed in a reaction kettle, the rotation speed is set at 600r / min, the reaction temperature is 200°C, and the reaction time is 60min. Ethanol was removed by rotary evaporation and vacuum drying, the conversion rate of the residue was 9.78%, the yield of ethyl levulinate was 0.18%, and the process efficiency was 0.63%.

[0058] The waste liquid obtained after filtering the mixture obtained in Example 1 to remove lignin was subjected to vacuum rotary evaporation and vacuum drying to remove water to obtain a carbohydrate-rich liquid CRL, which was placed in a reaction kettle with 50mL of absolute ethanol, and the rotation speed was set at 600r / min, reaction temperature 200°C, reaction time 60min. After the reaction, the reaction pr...

Embodiment 3

[0066] The recovered ionic liquid [BSTEA]HSO 4 Dry overnight at 80°C, and then directly use it in the next lignin extraction reaction, the results are as follows Figure 6 shown. [BSTEA] HSO 4 After 5 cycles, the activity did not decrease significantly, and the yield of lignin was 19.90%, indicating that [BSTEA]HSO 4 better stability.

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Abstract

The invention discloses a method for promoting extraction of lignin in straw and catalytically preparing levulinic acid and ethyl ester thereof by using ammonium-based Bronsted acidic ionic liquid. The method comprises the following steps: 1) by using pretreated straw powder as a raw material, adopting an organic solvent method and using the ammonium-based acidic ionic liquid as an accelerant, extracting lignin from the straw under proper reaction conditions; and 2) preparing levulinic acid and ethyl levulinate from cellulose-rich residue CRR and waste liquid CRL, which are generated after lignin is extracted from the straw, by using an ammonium-based acidic ionic liquid as a catalyst. The preparation method is simple and effective, low in cost, low in reaction temperature and low in toxicity, and the defects of complex process, high cost, high toxicity, high energy consumption, low product yield and the like in the prior art are overcome; and meanwhile, the ionic liquid has a very good effect on preparation of levulinic acid and ethyl levulinate through lignin extraction and catalytic degradation of carbohydrates.

Description

technical field [0001] The invention relates to the technical field of transformation and reuse of crop straw waste, in particular to a method for promoting the extraction of lignin from straw and catalyzing the preparation of levulinic acid and its ethyl ester by an ammonium-based Bronster acidic ionic liquid. Background technique [0002] China's straw resources are very rich, but long-term single-component resource utilization or low-value utilization leads to the destruction and discarding of other components during processing, resulting in a huge waste of straw resources. As fossil resources are decreasing day by day, as an important way to solve the shortage of energy, materials and chemicals in the future, the high-value utilization technology of all components of straw has attracted great attention and attention from researchers at home and abroad. [0003] From the perspective of raw materials, the fiber components contained in straw have short fibers and poor stren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G1/00C07C67/00C07C69/716C07C51/00C07C59/185B01J31/02
CPCC07G1/00B01J31/0279B01J31/0285C07C51/00C07C67/00C07C59/185C07C69/716
Inventor 赵炜王仃凯刘序堂蒋志杰崔明昱梁冲董林阳王飞
Owner CHINA UNIV OF MINING & TECH
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