Method for improving amination modification efficiency or phenolic hydroxyl group content of alkali lignin

A technology of alkali lignin and lignin amine, which is applied in the field of improving the reactivity of alkali lignin, can solve the problems of increased water pollution treatment pressure, does not conform to green environmental protection, is not green environmental protection, etc., and achieves improved amination efficiency and easy operation. , the effect of increasing the reactivity

Pending Publication Date: 2021-11-26
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of the above chemical reagents has caused an increase in the pressure of water pollution treatment, which is not a green and environmentally friendly method
[0005] On the other hand, there are a variety of chemical connections between the molecular structural units of lignin, presenting a complex and tight three-dimensional network structure, with low reactivity. In order to increase the content of phenolic hydroxyl groups in lignin and increase its reactivity, research Scholars use sulfuric acid to activate lignin
However, the use of the above-mentioned chemical reagents brings great pollution to the environment and does not meet the requirements of green environmental protection.

Method used

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  • Method for improving amination modification efficiency or phenolic hydroxyl group content of alkali lignin

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Get the alkali lignin (purity is 80%, water content is 3%, particle diameter is 100 orders, molecular weight is 4500) that wheat straw caustic soda anthraquinone method pulping black liquor extracts, adds deep eutectic solvent system (choline chloride / urea system) mixed evenly for heat treatment, adjusting the pretreatment temperature, stirring for a period of time, adding deionized water to terminate the reaction, followed by centrifugation and freeze drying to obtain the pretreated alkali lignin. Carry out vacuum distillation recovery deep eutectic solvent system (choline chloride / urea system). The treatment conditions are: the molar ratio of choline chloride and urea in the deep eutectic solvent system is 1:1.9, the purity of choline chloride is 90%, the purity of urea is 90%, and the choline chloride and urea are mixed evenly Then heat treatment, the mass volume ratio of alkali lignin and choline chloride / urea system is 1g:15mL, the pretreatment temperature is 55°C...

Embodiment 2

[0063] Get the alkali lignin (purity is 85%, water content is 2.6%, particle diameter is 120 orders, molecular weight is 4200) that poplar alkaline sulphite pulping black liquor extracts, adds deep eutectic solvent system (chole chloride Alkali / glycerin system) mixed evenly for heat treatment, adjusting the pretreatment temperature, stirring for a period of time, adding deionized water to terminate the reaction, and then centrifuging and freeze drying to obtain the pretreated alkali lignin. Carry out vacuum distillation recovery deep eutectic solvent system (choline chloride / glycerol system). The treatment conditions are: the molar ratio of choline chloride and glycerin in the deep eutectic solvent system is 1:2.5, the purity of choline chloride is 95%, the purity of glycerin is 95%, and the choline chloride and glycerin are mixed evenly Then heat treatment, the mass volume ratio of alkali lignin and choline chloride / glycerin system is 1g:25mL, the pretreatment temperature is ...

Embodiment 3

[0072] Take commercial alkali lignin (purity is 90%, water content is 4%, particle size is 100 mesh, molecular weight is 5000), add deep eutectic solvent system (choline chloride / acetic acid system) and mix evenly and heat treatment, Adjust the pretreatment temperature, stir for a period of time, add deionized water to terminate the reaction, and then perform centrifugation and freeze drying to obtain the pretreated alkali lignin. Carry out vacuum distillation recovery deep eutectic solvent system (choline chloride / acetic acid system). The treatment conditions are: the molar ratio of choline chloride and acetic acid in the deep eutectic solvent system is 1:2.6, the purity of choline chloride is 95%, the purity of acetic acid is 95%, and the choline chloride and acetic acid are mixed evenly Then heat treatment, the mass volume ratio of alkali lignin and choline chloride / acetic acid system is 1g:20mL, the pretreatment temperature is 65°C, the pretreatment time is 60min, the spee...

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Abstract

The invention belongs to the field of improvement of reaction activity of alkali lignin, and discloses a method for improving the amination modification efficiency or phenolic hydroxyl group content of alkali lignin, which comprises the following preparation steps: adding lignin into a deep eutectic solvent system (a choline chloride / urea system, a choline chloride / glycerol system and a choline chloride / acetic acid system), uniformly mixing, carrying out heating treatment, adjusting the pretreatment temperature, adding deionized water to terminate the reaction after stirring treatment is conducted for a period of time, then performing centrifugation and freeze drying to obtain the pretreated alkali lignin, carrying out reduced pressure distillation to recover the deep-eutectic solvent system, or transferring the reaction system treated by the deep-eutectic solvent system into a dilute acid solution, continuing to mechanically stir for a period of time, and then centrifuging and vacuum drying to obtain the pretreated industrial alkali lignin. The solvent used in the pretreatment method is green and environment-friendly, can be recycled, and is free of pollution, and the method is simple in process, is easy to operate, is suitable for industrial production, and has a good application prospect.

Description

technical field [0001] The invention belongs to the field of improving the reaction activity of alkali lignin, and specifically relates to a method for increasing the amination yield or phenolic hydroxyl content of alkali lignin. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Lignin, as one of the most abundant natural polymers on earth, ranks second only to cellulose in reserves. Worldwide, approximately 30 million tons of lignin waste are obtained annually by various chemical pulping methods. As a by-product of the biomass refining process, most lignin is burned as fuel in the alkali recovery process, but the calorific value of lignin is low, and the combustion of a l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 李凤凤杨桂花陈嘉川吉兴香张志礼
Owner QILU UNIV OF TECH
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