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Water-soluble lignin base chain transferring agent and preparation method thereof

A water-soluble lignin and chain transfer agent technology, which is applied in the field of polymer material science and application, can solve the problems of limited practical application, poor water solubility, and few high-active sites, and achieve good polymerization controllability and harsh reaction conditions , easy operation effect

Inactive Publication Date: 2019-08-02
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the inert network structure of lignin macromolecules, there are problems such as few high-active sites and poor water solubility, which limit its practical application, resulting in a very low recycling rate, even less than 5% that should be recycled.
Except for a small part that is used as fuel for direct combustion, most of the lignin is discharged into rivers, lakes and seas in the form of waste water and waste liquid, which wastes resources and pollutes the environment.

Method used

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  • Water-soluble lignin base chain transferring agent and preparation method thereof
  • Water-soluble lignin base chain transferring agent and preparation method thereof
  • Water-soluble lignin base chain transferring agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 Preparation of water-soluble lignin-based chain transfer agent

[0020] Weigh 1g of lignin and 15mL of chloroform in a reaction flask, stir well, add 1g of chlorosulfonic acid to react for 2h, add NaOH solution to the system to adjust to pH>7, continue to react for 1h, add HCl solution to adjust the system pH to Neutral, the obtained mixed solution was dialyzed for 48 hours, and then freeze-dried to obtain a sulfonated lignin sample.

[0021] Put 1g of the above-obtained sulfonated lignin and 30mL of 1M NaOH solution in the reaction flask, stir to dissolve, and add 1.62g CS dropwise to the flask in an ice water bath 2 After reacting at 30℃ for 4h, add 1.83g methyl bromoacetate dropwise, continue the reaction for 12h, drop the reaction solution into anhydrous ethanol for precipitation, the resulting precipitate is dissolved in deionized water and then dropped into anhydrous ethanol for precipitation, repeat operation 2 ~3 times, the precipitate is dried to a constan...

Embodiment 2

[0022] Example 2 Preparation of water-soluble lignin-based chain transfer agent

[0023] Weigh 1g of lignin and 15mL of chloroform in a reaction flask, stir well, add 2g of chlorosulfonic acid to react for 2h, add NaOH solution to the system to adjust to pH>7, continue the reaction for 1h, add HCl solution to adjust the system pH to Neutral, the obtained mixed solution was dialyzed for 48 hours, and then freeze-dried to obtain a sulfonated lignin sample.

[0024] Put 1g of the above-obtained sulfonated lignin and 30mL of 1M NaOH solution in the reaction flask, stir to dissolve, and add 1.62g CS dropwise to the flask in an ice water bath 2 After reacting at 30℃ for 4h, add 1.83g methyl bromoacetate dropwise, continue the reaction for 12h, drop the reaction solution into anhydrous ethanol for precipitation, the resulting precipitate is dissolved in deionized water and then dropped into anhydrous ethanol for precipitation, repeat operation 2 ~3 times, the precipitate is dried to a con...

Embodiment 3

[0025] Example 3 Preparation of water-soluble lignin-based chain transfer agent

[0026] Weigh 1g of lignin and 15mL of chloroform in a reaction flask, stir well, add 3g of chlorosulfonic acid to react for 3h, add NaOH solution to the system to adjust to pH>7, continue to react for 2h, add HCl solution to adjust the system pH to Neutral, the obtained mixed solution was dialyzed for 48 hours, and then freeze-dried to obtain a sulfonated lignin sample.

[0027] Put 1g of the above-obtained sulfonated lignin and 30mL of 1M NaOH solution in the reaction flask, stir to dissolve, and add 1.62g CS dropwise to the flask in an ice water bath 2 After reacting at 30℃ for 4h, add 1.83g methyl bromoacetate dropwise, continue the reaction for 12h, drop the reaction solution into anhydrous ethanol for precipitation, the resulting precipitate is dissolved in deionized water and then dropped into anhydrous ethanol for precipitation, repeat operation 2 ~3 times, the precipitate is dried to a constan...

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Abstract

The invention relates to a water-soluble lignin base chain transferring agent and a preparation method thereof. The water-soluble lignin base chain transferring agent comprises the following steps: (1) sulfonating lignin by treating trichloromethane as a solvent and chlorosulfonic acid as a sulfonating agent; and (2) feeding sulfonated lignin and an alkaline solution into a reaction bottle to fully solve; dropwise adding CS2 to the bottle; reacting for 4-8h; dropping bromo ester to continuously react for a period of time; precipitating and washing a product; and drying to obtain the water-soluble lignin base chain transferring agent which is high in water soluble performance. According to the method, the problem of low solubility of a lignin product in a water solution can be released; andmoreover, the operation is convenient and easy to carry out; the cost is low; and the prepared water-soluble lignin base chain transferring agent is high in polymerizing controllability in polymerizing reaction.

Description

Technical field [0001] The invention relates to a water-soluble lignin-based chain transfer agent and a preparation method thereof, and relates to the field of polymer material science and application. Background technique [0002] Lignin is an agricultural and forestry biomass resource with great economic value, with huge output and broad application prospects. However, due to the inert network structure of lignin macromolecules, there are problems such as few highly active sites and poor water solubility, which limit its practical application, resulting in extremely low recycling rate, even less than 5% that should be recycled. Except for a small part that is directly burned as fuel, most of the lignin is discharged into rivers, lakes and seas in the form of waste water, which wastes resources and pollutes the environment. Therefore, exploring new ways to realize the high-value utilization of lignin has great practical significance and economic value. Appropriate chemical mod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08F2/38C08F120/56
CPCC08F2/38C08F120/56C08H6/00
Inventor 许玉芝王广彬李宁王春鹏储富祥
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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