New method for preparing solid lignin quaternary ammonium salt and application of solid lignin quaternary ammonium salt

A quaternary ammonium salt and lignin technology, applied in the field of lignin, can solve the problems of large amount of solvent used, many reaction steps, and reduced water solubility, etc., and achieve the effect of short reaction route, mild reaction conditions, and easy control

Active Publication Date: 2014-09-24
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method has the following disadvantages: there are many reaction steps, the amount of solvent used is relatively large, strong acid catalysis is required, and the alkylation reagent part in the raw material is highly toxic.
But the shortcoming of this method is: it is to prepare lignin quaternary ammonium salt solution under strong alkali condition, and the product obtained after concentrating is lignin quaternary ammonium salt viscous liquid (mainly containing: epoxypropyl quaternary ammonium salt middle body, sodium hydroxide, lignin quaternary ammonium salt)
In this method, because the quaternary ammonium salt is continued to be cross-linked by increasing the reaction steps, it takes a lot of time and the method is cumbersome, and some physical and chemical properties of the quaternary ammonium salt after cross-linking have also changed, resulting in a significant reduction in its water solubility.

Method used

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  • New method for preparing solid lignin quaternary ammonium salt and application of solid lignin quaternary ammonium salt
  • New method for preparing solid lignin quaternary ammonium salt and application of solid lignin quaternary ammonium salt
  • New method for preparing solid lignin quaternary ammonium salt and application of solid lignin quaternary ammonium salt

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] 1) Weigh 4.6g of 33% trimethylamine aqueous solution into a single-necked flask, stir for 15min under an ice-salt bath at -5°C, then weigh 2.0g of epichlorohydrin, and gradually add it dropwise to trimethylamine aqueous solution . After the dropwise addition, continue to stir for 30 min, then place in a water bath at 40° C., stir and react for 2 h to obtain a pale yellow glycidyl quaternary ammonium salt intermediate. The molar ratio of trimethylamine and epichlorohydrin is 1.24:1.

[0051] 2) Weigh 2.5g of alkali lignin into a three-necked flask, add 8mL of distilled water, add 0.05g of ammonium persulfate after heating up to 50°C, stir for a while, then add the prepared epoxypropyl quaternary ammonium salt intermediate, and stir to react After 3.5h, a black lignin quaternary ammonium salt solution was obtained. Wherein the molar ratio of the quaternary ammonium salt intermediate to the alkali lignin is 1.45:1, and the amount of the catalyst is 2.0% of the mass of th...

Embodiment 2

[0061] Weigh 0.7 g of triethylamine liquid into a single-necked flask, stir for 10 min in an ice-salt bath at 0° C., then weigh 1.0 g of epichlorohydrin, and gradually add it dropwise into triethylamine. Continue to stir for 30 min after the dropwise addition, and then place it at room temperature, stir and react for 3 h to obtain a pale yellow glycidyl quaternary ammonium salt intermediate. The molar ratio of triethylamine and epichlorohydrin is 1.11:1.

[0062] Weigh 1.2g of alkali lignin into a three-necked flask, add 5mL of distilled water, add 0.02g of potassium persulfate after heating up to 60°C, stir for a while, then add the prepared epoxypropyl quaternary ammonium salt intermediate, and stir for 3 hours , to obtain black lignin quaternary ammonium salt solution. The molar ratio of the quaternary ammonium salt intermediate to the alkali lignin is 1.74:1, and the amount of the catalyst is 1.6% of the mass of the alkali lignin.

[0063] The prepared lignin quaternary ...

Embodiment 3

[0066] Weigh 8.1 g of 33% trimethylamine aqueous solution into a single-necked flask, stir for 15 min under an ice-salt bath at -10°C, then weigh 3.0 g of epichlorohydrin, and gradually add it dropwise to the trimethylamine aqueous solution. Continue to stir for 30 min after the dropwise addition, then place in a water bath at 35° C., and stir for 3 h to obtain a light yellow glycidyl quaternary ammonium salt intermediate. The molar ratio of triethylamine and epichlorohydrin is 1.41:1.

[0067] Weigh 3.0g of alkali lignin into a three-necked flask, add 10mL of distilled water, add 0.15g of cerium ammonium nitrate after heating up to 70°C, stir for a while, then add the prepared epoxypropyl quaternary ammonium salt intermediate, and stir for 4 hours , to obtain black lignin quaternary ammonium salt solution. The molar ratio of the quaternary ammonium salt intermediate to the alkali lignin is 1.81:1, and the amount of the catalyst is 5% of the mass of the alkali lignin.

[006...

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Abstract

The invention discloses a new method for preparing solid lignin quaternary ammonium salt. Epichlorohydrin is added into tertiary amine, and a glycidyl quaternary ammonium salt intermediate is obtained after a reaction; on the condition that an initiating agent exists, the intermediate reacts with alkali lignin; then a reactant is added into a polarity organic solvent, and a precipitate is the solid lignin quaternary ammonium salt. According to the new method for preparing the solid lignin quaternary ammonium salt, the raw materials and reagents are easy to obtain, the reaction path is short, the reaction condition is moderate, and postprocessing is simple. The invention further discloses the application of the solid lignin quaternary ammonium salt obtained through the method.

Description

technical field [0001] The present invention relates to the field of lignin. More specifically, it relates to a new method for preparing solid lignin quaternary ammonium salt and the application of the solid lignin quaternary ammonium salt. Background technique [0002] As one of the most abundant renewable resources on earth, lignin widely exists in seed plants, and forms the basic skeleton of plants together with cellulose and hemicellulose. The amount of lignin in nature is very large, and it is estimated that 150 billion tons of lignin can be produced by plant growth in the world every year. Industrial lignin is the only aromatic compound that can be obtained from renewable resources, including 30 million tons of industrial lignin produced in the pulp and paper industry. [0003] Lignin is a complex phenolic polymer formed from three alcohol monomers (p-coumaryl alcohol, coniferyl alcohol, and sinapyl alcohol). Due to different structural units, lignin can be divided ...

Claims

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Application Information

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IPC IPC(8): C08H7/00A24D3/14
Inventor 朱龙杰庄亚东李朝建廖恵云石怀彬曹毅王晨辉
Owner CHINA TOBACCO JIANGSU INDAL
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