A kind of method for mechanically activating solid phase reaction to prepare lignin ester

A solid-phase reaction and mechanical activation technology is applied in the field of preparation of lignin esters, which can solve the problems of difficulty in solvent recovery, difficulty in direct modification and utilization, and high equipment cost, and achieves a time-saving and simple recovery process, and is easy to realize industrialized production. , Solve the effect of high equipment cost

Active Publication Date: 2018-04-06
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the problems that lignin has low reactivity, is difficult to directly modify and utilize, and the synthesis of lignin ester is difficult to realize industrial production.
At the same time, it also solves the above-mentioned chemical modification methods that require a large amount of solvent, difficult solvent recovery, environmental pollution, catalyst residue, complex process and high cost, long time for acylation of lignin, time-consuming and locked-in equipment for recovery of modified lignin Problems of high cost, insufficient mixing of reaction materials and complicated operation

Method used

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  • A kind of method for mechanically activating solid phase reaction to prepare lignin ester

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Experimental program
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Effect test

Embodiment 1

[0030] Preparation of Lignin Acetate

[0031] Weigh the reaction material according to the ratio of organic lignin: acetic anhydride: 4,4-dimethylaminopyridine = 15g: 43.1g (0.42mol): 0.3g, and put the volume of the reaction material and the grinding medium according to the ratio of 100g: 150mL In the ball mill, the grinding balls are zirconia balls with a diameter of 6 mm. Stirring at a low speed of 150 r / min in a constant temperature water bath at 90 ° C for 2 h, stop heating and stirring, and cool rapidly to obtain crude lignin esters, and mix lignin The crude ester is separated from the grinding balls, the grinding balls and the crude lignin ester are cleaned with deionized water respectively; the crude lignin is left to stand for 15 minutes in deionized water to precipitate solids, and the solids are separated by filtration, and the filter cake is washed with deionized water Until the filtrate is neutral, lignin acetate is obtained.

[0032] The obtained lignin acetate w...

Embodiment ２

[0034] Preparation of Lignin Propionate

[0035]Weigh the reaction material according to the ratio of sodium lignosulfonate: propionic anhydride: 4,4-dimethylaminopyridine=15g:30g (0.23mol):0.3g, and stack the volume of the reaction material and the grinding medium according to the ratio of 100g:200mL Put it in a ball mill, the balls are zirconia balls with a diameter of 6mm, and carry out the acylation reaction at 100r / min at a low speed in a constant temperature water bath at 80°C for 3h, stop heating and stirring, and cool quickly to obtain crude lignin ester, and The crude vegan ester is separated from the grinding ball, and the grinding ball and the crude lignin ester are cleaned with deionized water; the solid is precipitated after standing in ether for 0.5 h, and the solid is separated by filtration, and the filter cake is washed 3 times with ether, each time 50 mL , to obtain lignin propionate.

[0036] The obtained lignin propionate was measured by an ultraviolet spe...

Embodiment ３

[0038] Preparation of lignin butyrate

[0039] Weigh the reaction material according to the ratio of unactivated alkali lignin: butyric anhydride: pyridine=15g:30g (0.19mol):0.5g, put the reaction material and the volume of the grinding medium in the ball mill according to the ratio of 100g:300mL, and grind the ball It is a zirconia ball with a diameter of 6mm. Stir at a low speed of 200r / min in a constant temperature water bath at 50°C for acylation reaction for 4 hours, stop heating and stirring, and cool quickly to obtain crude lignin ester, and separate the crude lignin ester from the balls , the grinding ball and the crude lignin ester were cleaned with an ethanol-water solution with a volume ratio of 1:1; the crude lignin ester was left to stand for 1 hour in an ethanol-water solution with a volume ratio of 1:1 to precipitate a solid, and the solid was separated by filtration. Wash the filter cake with deionized water until the filtrate is neutral to obtain lignin butyra...

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Abstract

The invention discloses a method for preparing lignin ester by mechanical activation-solid reaction. The method comprises the following steps of weighing reaction materials according to the ratio of lignin to an acylating agent to a catalyst is 15g: 0.08-0.6mol: 0.15-6.7g; placing the reaction material in a ball mill; performing thermostatic waterbath at the temperature of 50-90 DEG C; stirring at the low rotating speed of 100-500 r / min and performing acylation for 0.5-4 hours to obtain crude products of the lignin ester; separating the crude products from pellets; placing the crude products of the lignin ester in solvent and standing to separate out solid; separating the solid from the solvent by filtering; and removing the acylating agent and the catalyst by using a solvent repeated washing and filtering method or an extraction method to obtain lignin ester products. The lignin ester is synthesized by mechanical activation-solid synthesis, the shortcoming that activity of chemical reaction of lignin is low is overcome, and problems existing in preparation of the lignin ester by the traditional liquid-phase method are solved. The method has the advantages that the method is pollution-free and low in cost; reaction materials are mixed fully; equipment cost is low; energy consumption is low; reaction time is short; modified lignin is easy to recycle; a producing and preparing technology is simplified; and the method is easy and convenient to operate.

Description

technical field [0001] The invention relates to a method for preparing lignin esters, in particular to a method for preparing lignin esters by mechanically activating solid phase reaction. Background technique [0002] Lignin is an amorphous, aromatic polymer containing oxyphenylpropanol or its derivatives in its molecular structure widely present in plants. Lignin is the only renewable aryl compound that nature can provide, and its content in land plants is second only to cellulose. According to statistics, at present, the global annual lignin production is about 6×10 5 billion tons, and lignin is regenerated at a rate of about 50 billion tons per year. Although lignin has many characteristics such as wide sources, rich active groups, biorenewability and degradation, non-toxic weather resistance, thermoplasticity, glass transition, etc., the current utilization rate of industrial lignin is less than 20%, and most of lignin is used as waste Emissions, waste of resources, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00
Inventor 赵小红黄祖强张燕娟胡华宇冯振飞杨梅黄爱民覃杏珍覃宇奔沈芳
Owner GUANGXI UNIV
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