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Modified lignin as well as preparation method and application thereof in rubber composite material

A lignin modification technology, applied in the field of rubber composite materials, can solve problems such as poor reinforcement effect, limited lignin application, and weak binding effect, so as to improve compatibility and affinity, inhibit self-aggregation tendency, The effect of reducing the polarity of molecules

Active Publication Date: 2021-05-25
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Lignin is a natural polymer compound with a three-dimensional network structure. Its content in nature is second only to cellulose. However, as a by-product of the paper industry, lignin is usually burned as fuel, resulting in waste of resources and environmental pollution.
The lignin molecule has a rigid aromatic structure, which has the potential to replace carbon black as a rubber reinforcing agent. However, rubber represented by natural rubber is mostly a non-polar polymer. Due to the presence of polar functional groups such as hydroxyl and carboxyl in lignin, There are problems of poor compatibility and dispersion in the natural rubber matrix, and the reinforcing effect is not good, which limits the application of lignin in rubber
[0003] Reducing the polarity of lignin through chemical modification is an important way to improve the reinforcing effect of lignin. At present, the chemical modification methods of lignin mainly include hydroxymethylation, sulfonation, etc., and the modified lignin still has hydroxyl groups. , sulfonic acid groups and other polar groups, can not effectively improve the compatibility of lignin and natural rubber, can not effectively participate in the rubber vulcanization reaction, it is difficult to form a covalent connection with the rubber molecular chain, the binding effect is relatively weak weak

Method used

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  • Modified lignin as well as preparation method and application thereof in rubber composite material
  • Modified lignin as well as preparation method and application thereof in rubber composite material
  • Modified lignin as well as preparation method and application thereof in rubber composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Add alkali lignin and propioyl chloride into DMSO at a mass ratio of 100:18, the mass concentration of alkali lignin is 0.2g / mL, react at 60°C for 6 hours, cool to room temperature and add appropriate amount of deionized water to obtain Alkynylated lignin is precipitated, washed with deionized water until neutral, and vacuum-dried at 90°C for 24 hours to obtain alkynylated lignin;

[0049] (2) the alkynylated lignin obtained in step (1) is ground to d by a jet mill 50 About 2.2μm;

[0050] (3) Accurately weigh 6.0g of the alkynylated lignin obtained in step (2), add 40.0g of natural rubber, 14.0g of carbon black N330, 2.0g of zinc oxide, and 1.2g of stearic acid into the internal mixer successively, and heat at 100°C 15 minutes of banburying under the same conditions;

[0051] (4) Put the mixed rubber obtained in the step (3) into the rolling mill, add 1.0 g of sulfur and 0.24 g of benzothiazole disulfide in turn, mix for 10 minutes at 20 ° C, and pass through 5 t...

Embodiment 2

[0053] (1) Add alkali lignin and propioyl chloride into DMSO at a mass ratio of 100:36, the mass concentration of alkali lignin is 0.2g / mL, react at 60°C for 6 hours, cool to room temperature and add appropriate amount of deionized water to obtain Alkynylated lignin is completely precipitated, washed with deionized water until neutral, and vacuum-dried at 90°C for 24 hours to obtain alkynylated lignin;

[0054] (2) the alkynylated lignin obtained in step (1) is ground to d by a jet mill 50 About 2.2μm;

[0055] (3) Accurately weigh 6.0g of the alkynylated lignin obtained in step (2), add 40.0g of natural rubber, 14.0g of carbon black N330, 2.0g of zinc oxide, and 1.2g of stearic acid into the internal mixer successively, and heat at 100°C 15 minutes of banburying under the same conditions;

[0056] (4) Put the mixed rubber obtained in the step (3) into the rolling mill, add 1.0 g of sulfur and 0.24 g of benzothiazole disulfide in turn, mix for 10 minutes at 20 ° C, and pass ...

Embodiment 3

[0058] (1) Add alkali lignin and propioyl chloride into DMSO at a mass ratio of 100:54, the mass concentration of alkali lignin is 0.2g / mL, react at 60°C for 6 hours, cool to room temperature and add appropriate amount of deionized water until Alkynylated lignin is precipitated, washed with deionized water until neutral, and vacuum-dried at 90°C for 24 hours to obtain alkynylated lignin;

[0059] (2) the alkynylated lignin obtained in step (1) is ground to d by jet milling 50 About 2.2μm;

[0060] (3) Accurately weigh 6.0g of the alkynylated lignin obtained in step (2), add 40.0g of natural rubber, 14.0g of carbon black N330, 2.0g of zinc oxide, and 1.2g of stearic acid into the internal mixer successively, and heat at 100°C 15 minutes of banburying under the same conditions;

[0061] (4) Put the mixed rubber obtained in the step (3) into the rolling mill, add 1.0 g of sulfur and 0.24 g of benzothiazole disulfide in turn, mix for 10 minutes at 20 ° C, and pass through 5 time...

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Abstract

The invention discloses modified lignin, a preparation method thereof and application of the modified lignin in a rubber composite material. Lignin and alkynyl compounds react in an organic solvent to obtain a reaction solution containing the modified lignin. The modified lignin has the following advantages: (1) the structure of the alkynylation reagent contains an acyl chloride functional group, and the acyl chloride functional group is easily subjected to esterification reaction with an alcoholic hydroxyl group and a phenolic hydroxyl group in lignin molecules to generate the modified lignin grafted with an unsaturated alkynyl functional group; (2) through alkynylation modification, the content of hydroxyl in lignin molecules is reduced, the molecular polarity is reduced, the self-aggregation tendency of lignin caused by hydrogen bonds is inhibited, lignin powder with relatively low particle size is obtained through grinding, the compatibility and affinity of lignin and non-polar natural rubber are improved, and the dispersion of the lignin in a natural rubber matrix is promoted.

Description

technical field [0001] The invention belongs to the technical field of rubber composite materials, and in particular relates to a modified lignin, a preparation method thereof and an application in rubber composite materials. Background technique [0002] Lignin is a natural polymer compound with a three-dimensional network structure. Its content in nature is second only to cellulose. However, lignin, as a by-product of the paper industry, is usually burned as fuel, resulting in waste of resources and environmental pollution. The lignin molecule has a rigid aromatic structure, which has the potential to replace carbon black as a rubber reinforcing agent. However, rubber represented by natural rubber is mostly a non-polar polymer. Due to the presence of polar functional groups such as hydroxyl and carboxyl in lignin, In the natural rubber matrix, there are problems of poor compatibility and dispersion, and poor reinforcing effect, which limits the application of lignin in rub...

Claims

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Application Information

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IPC IPC(8): C08H7/00C08L7/00C08L97/00
CPCC08H6/00C08L7/00C08L97/005
Inventor 应汉杰徐新建朱浬玮凌峰李明朱晨杰庄伟沈涛沈建农欧阳平凯
Owner NANJING UNIV OF TECH
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