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Improved method for acetylation of alkali lignin

A technology of alkali lignin and acetylation, applied in the improvement field of alkali lignin acetylation, can solve the problems of high price, difficult biodegradation, high toxicity of pyridine, etc., and achieve the effect of cost saving, simple process and environmental friendliness

Inactive Publication Date: 2020-06-26
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, pyridine is highly toxic, expensive and difficult to biodegrade, and ether is not a cheap drug

Method used

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  • Improved method for acetylation of alkali lignin
  • Improved method for acetylation of alkali lignin
  • Improved method for acetylation of alkali lignin

Examples

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Embodiment 1

[0034] Carry out the acetylation of alkali lignin with the improved method of a kind of alkali lignin acetylation described in the present invention, the process is as follows: a, lactic acid: choline chloride 1: 1 (molar ratio) is mixed in the beaker, 30 ℃ water bath heating and stirring (stirring speed 200r / min) for 1 hour to prepare a deep eutectic solvent (DES), and put it into a reagent bottle for storage at room temperature. b. Dissolve 100 mg of purified alkali lignin in 8 ml of DES / acetic anhydride (2:1V:V) mixed solution prepared in step a. At the same time, nitrogen gas is passed into the container and sealed. Stir at room temperature for 12 hours under dark conditions. , stop the reaction, wherein the purification conditions of alkali lignin are: first dissolve the crude alkali lignin in acetic acid / water (6:1V:V) solution, then centrifuge to remove the precipitate, obtain an extract, and then add it to the extract Add water to make the alkali lignin precipitate, ta...

Embodiment 2

[0036]Carry out the acetylation of alkali lignin with the improved method of a kind of alkali lignin acetylation of the present invention, the process is as follows: a, lactic acid: choline chloride 2: 1 (molar ratio) is mixed in the beaker, 60 Heat and stir in a water bath at ℃ (stirring speed 300r / min) until the solution is clear and transparent to prepare a deep eutectic solvent (DES), and store it in a reagent bottle at room temperature. b. Dissolve 200 mg of purified alkali lignin in 8 ml of the DES / acetic anhydride (1:1V:V) mixed solution prepared in step a. At the same time, nitrogen gas is introduced into the container and sealed. Stir at room temperature for 24 hours under dark conditions. , stop the reaction, wherein the purification conditions of alkali lignin are: first dissolve the crude alkali lignin in acetic acid / water (9:1V:V) solution, then centrifuge to remove the precipitate, obtain an extract, and then add it to the extract Add water to make the alkali lig...

Embodiment 3

[0038] Carry out the acetylation of alkali lignin with the improved method of a kind of alkali lignin acetylation of the present invention, the process is as follows: a, lactic acid: choline chloride 3: 1 (molar ratio) is mixed in the beaker, 80 Heat and stir in a water bath at ℃ (stirring speed 500r / min) until the solution is clear and transparent to prepare a deep eutectic solvent (DES), and store it in a reagent bottle at room temperature. b. Take 300 mg of purified alkali lignin and dissolve it in 8 ml of DES / acetic anhydride (1:2V:V) mixed solution prepared in step a. At the same time, nitrogen gas is passed into the container and sealed. Stir at room temperature for 36 hours under dark conditions. , stop the reaction, wherein the purification conditions of alkali lignin are: first dissolve the crude alkali lignin in acetic acid / water (10:1V:V) solution, then centrifuge to remove the precipitate, obtain an extract, and then add it to the extract Add water to make the alka...

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Abstract

The invention discloses an improved method for acetylation of alkali lignin. The method comprises the following steps: a, mixing lactic acid and choline chloride, putting the mixture into a beaker, heating and stirring in a water bath until the solution is clear and transparent to prepare a deep eutectic solvent (DES), putting the deep eutectic solvent into a reagent bottle, and carrying out normal-temperature storage; b, dissolving a certain amount of purified alkali lignin into the DES / acetic anhydride mixed solution prepared in the step a, introducing nitrogen into the container, sealing, stirring for a period of time at normal temperature under a dark condition, and stopping reaction; and c, adding a certain volume of acid water into the reaction container in the step b, carrying out standing precipitation, centrifugally separating precipitates, washing the precipitates with deionized water and ethanol, and carrying out freeze drying to obtain the acetylated lignin. The acetylationmethod is simple in step, and compared with the traditional acetylation solvent pyridine and the anti-solvent diethyl ether for precipitating lignin, the reagent used in the method has the advantagesof being non-toxic, environmentally friendly, low in cost and the like, and the acetylation yield is high.

Description

technical field [0001] The invention belongs to the field of utilization of biomass resources, and in particular relates to an improved method for acetylation of alkali lignin. Background technique [0002] Lignocellulosic biomass is the most abundant renewable biomass resource in nature, and the separation and utilization of lignin, one of the three main components of lignocellulosic biomass, is an important strategy to promote the development of biomass resource utilization. major issues. In terms of lignin separation, many biomass pretreatment methods have been developed, such as chemical methods, physical methods, biological methods, and physical and chemical methods. In recent years, deep eutectic solvents have been applied to biomass pretreatment to separate lignin, which has great potential. Deep eutectic solvents (DES) are new green solvents designed with hydrogen bond donors and hydrogen bond acceptors. Among them, DES, which uses organic acids as hydrogen bond d...

Claims

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Application Information

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IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 刘壮李友明侯轶
Owner SOUTH CHINA UNIV OF TECH
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