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Humus acid polyethylene glycol grafted copolymer and preparation method thereof

A technology of polyethylene glycol grafting and polyethylene glycol, applied in the field of humic acid polyethylene glycol graft copolymer and its preparation, can solve the problems of poor water solubility of humic acid and inapplicability, and reduce equipment The effects of input and production energy consumption, improvement of water solubility, and high reaction efficiency

Active Publication Date: 2019-10-08
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the above technical problems, the object of the present invention is to provide humic acid polyethylene glycol graft copolymer and preparation method thereof, the water-soluble polyethylene glycol polymer segment is keyed into the humic acid in the form of covalent bond In the structure, it overcomes the disadvantage that humic acid has poor water solubility and cannot be used in acidic and neutral environments.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Disperse 5 g of dried humic acid powder in 20 mL of anhydrous dichloromethane, add 1 g of triethylamine to the system, and lower the temperature of the system to 0°C. After the temperature stabilized, 1 g of acryloyl chloride was slowly added dropwise to the reaction system, and the dropwise addition continued for 0.5 hours. After the dropwise addition, the reaction system was warmed up to room temperature, and the reaction was continued for 24 hours. After the reaction is finished, filter with suction, and wash the filter residue with water until it is neutral, and obtain acrylated humic acid after drying.

[0021] (2) Disperse 5g of acrylated humic acid in water, use sodium hydroxide to adjust the pH value of the dispersion system to 9-10, fully dissolve the acrylated humic acid, and add 0.5g of aminopolyethylene glycol Methyl ether (molecular weight: 200 g / mol) was added to the system at one time, and reacted at 60° C. for 8 hours to obtain an aqueous solution o...

Embodiment 2

[0024] (1) Disperse 5 g of dried humic acid powder in 20 mL of anhydrous dichloromethane, add 3.43 g of triethylamine to the system, and lower the temperature of the system to 0°C. After the temperature stabilized, 3.07 g of acryloyl chloride was slowly added dropwise to the reaction system, and the dropwise addition continued for 0.5 hours. After the dropwise addition, the reaction system was warmed up to room temperature, and the reaction was continued for 24 hours. After the reaction is finished, filter with suction, and wash the filter residue with water until it is neutral, and obtain acrylated humic acid after drying.

[0025] (2) Disperse 5g of acrylated humic acid in water, use sodium hydroxide to adjust the pH value of the dispersion system to 9-10, fully dissolve the acrylated humic acid, and dissolve 11.3g of aminopolyethylene glycol Methyl ether (molecular weight: 1000g / mol) was added to the system at one time, and reacted at 60° C. for 8 hours to obtain an aqueou...

Embodiment 3

[0028] (1) Disperse 5 g of dried humic acid powder in 20 mL of anhydrous dichloromethane, add 5.72 g of triethylamine to the system, and lower the temperature of the system to 0°C. After the temperature stabilized, 5.11 g of acryloyl chloride was slowly added dropwise to the reaction system for 0.5 hours. After the dropwise addition, the reaction system was warmed up to room temperature, and the reaction was continued for 24 hours. After the reaction is finished, filter with suction, and wash the filter residue with water until it is neutral, and obtain acrylated humic acid after drying.

[0029] (2) Disperse 5g of acrylated humic acid in water, use sodium hydroxide to adjust the pH value of the dispersion system to 9-10, fully dissolve the acrylated humic acid, and dissolve 22.6g of aminopolyethylene glycol Methyl ether (molecular weight: 2000g / mol) was added to the system at one time, and reacted at 60° C. for 12 hours to obtain an aqueous solution of the crude humic acid p...

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Abstract

The invention relates to a humus acid polyethylene glycol grafted copolymer and a preparation method thereof, and belongs to the field of modification of natural polymers. A humus acid molecule servesas a skeleton structure, peg polymer segments are covalently bonded to the side chain of the humus acid. The preparation method of the grafted copolymer comprises the steps that firstly acrylic acidesterified humus acid is prepared through acylation reaction of the humus acid and acryloyl chloride under condition of trimethylamine existing; secondly, the humus acid was esterified by acrylic acid, Michael reaction is conducted with aminopolyethylene glycol monomethyl ether to prepare a humus acid polyethylene glycol grafted copolymer coarse product; and finally, a dialysis technology is usedfor removing unreacted amino polyethylene glycol monomethyl ether and sodium hydroxide in the coarse product, a final product is obtained after drying. The humus acid polyethylene glycol grafted copolymer and the preparation method thereof have the beneficial effects that a water-soluble and non-toxic polyethylene glycol chain segment is introduced in the humus acid structure to overcome the performance defect of the poor water solubility, the product has good solubility in water, the preparation method is high in efficiency, the reaction condition is mild, using of organic solvent is avoided,and green production is easy to achieve.

Description

technical field [0001] The invention relates to the technical field of modification of natural polymers, in particular to a humic acid polyethylene glycol graft copolymer and a preparation method thereof. Background technique [0002] Humic acid is a kind of natural renewable resource with abundant reserves, which widely exists in lignite, soil, and rivers, and plays an important role in the process of global carbon cycle. Lignite resources account for 16% of my country's total coal reserves, and globally, lignite accounts for 40%. However, due to its high water content, high volatile matter, low combustion calorific value, rich pores and other deficiencies, it cannot be effectively utilized. However, lignite contains a large amount of humic acid organic matter. Therefore, extracting lignite humic acid and realizing efficient utilization is an effective way to increase the added value of lignite, which has attracted widespread attention and has important promotion prospects...

Claims

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Application Information

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IPC IPC(8): C08G81/00
CPCC08G81/00
Inventor 张万斌张光华罗杰
Owner SHAANXI UNIV OF SCI & TECH
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