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Modified carboxymethyl chitosan quaternary ammonium salt and preparation method thereof

A technology of carboxymethyl chitosan and quaternary ammonium salt, which is applied in the field of modified carboxymethyl chitosan quaternary ammonium salt and its preparation, can solve the problem of inaccurate grafting position, variable molecular weight, and variable grafting efficiency To achieve the effect of easy degradation, simple reaction conditions, and increase of adsorption sites

Pending Publication Date: 2022-05-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the research on carboxymethyl chitosan quaternary ammonium salt is very extensive, there are shortcomings such as inappropriate grafting efficiency, incorrect grafting position, and different molecular weight changes before and after grafting.

Method used

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  • Modified carboxymethyl chitosan quaternary ammonium salt and preparation method thereof
  • Modified carboxymethyl chitosan quaternary ammonium salt and preparation method thereof
  • Modified carboxymethyl chitosan quaternary ammonium salt and preparation method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0039] The preparation method of O-carboxymethyl chitosan quaternary ammonium salt is:

[0040]Add 18~21mL of kerosene to the three-necked flask, add 1.4~1.6g of a mixture of span-60 and tween-80 (HLB value 6~7) under stirring, stir for 5~15min, and stir at a rate of 200~400r / min. Add 10~12mL water and 1.0g O-carboxymethyl chitosan to the beaker and stir for 5~15min, then add the solution to the three-necked flask and stir at room temperature for 30~60min at a stirring rate of 200~400r / min. Add 0.006~0.008g of ceric ammonium nitrate, adjust the temperature to 50~70°C, carry out the initiation reaction for 20~30min, and the stirring speed is 200~400r / min. After initiating the reaction, add 8~10mL of an aqueous solution containing 2~4g of trihydroxyethyl allyl quaternary ammonium salt into the three-necked flask, and react at a temperature of 50~70°C for 4~5h, with a stirring rate of 200~400r / min. After the reaction is completed, a mixed solution of 40 to 80 parts by volume is ...

Embodiment 1

[0042] Add 20 mL of kerosene to the three-necked flask, add 1.5 g of a mixture of span-60 and tween-80 under stirring (span-60 to tween-80 ratio is 4:1), stir for 15 min, and stir at a rate of 400 r / min. Add 12 mL of water and 1.0 g of O-carboxymethyl chitosan to the beaker and stir for 10 min, then add the solution to the three-necked flask and stir at room temperature for 40 min at a stirring rate of 400 r / min. 0.006g of cerium ammonium nitrate was added, the temperature was adjusted to 70°C, and the reaction was initiated for 30min, with a stirring speed of 400r / min. After initiating the reaction, 8 mL of an aqueous solution containing 3 g of trihydroxyethyl allyl quaternary ammonium salt was added to the three-necked flask, and the reaction was carried out at a temperature of 70° C. for 4 h with a stirring rate of 400 r / min. After the reaction, 60 ml of a mixed solution with a volume ratio of ethanol and acetone of 1:2 was added, and the mixture was rapidly stirred for dem...

Embodiment 2

[0044] Add 20 mL of kerosene to the three-necked flask, add 1.4 g of a mixture of span-60 and tween-80 under stirring (the ratio of span-60 to tween-80 is 4:1), and stir for 12 min at a stirring rate of 400 r / min. Add 10 mL of water and 1.2 g of O-carboxymethyl chitosan to the beaker and stir for 10 min, then add the solution to the three-necked flask and stir at room temperature for 40 min at a stirring rate of 400 r / min. 0.008 g of cerium ammonium nitrate was added, the temperature was adjusted to 70° C., and the initiation reaction was carried out for 40 min with a stirring rate of 400 r / min. After the reaction was initiated, 10 mL of an aqueous solution containing 4 g of trihydroxyethyl allyl quaternary ammonium salt was added to the three-necked flask, and the reaction was carried out at a temperature of 70° C. for 4 h with a stirring rate of 400 r / min. After the reaction, 60 ml of a mixed solution with a volume ratio of ethanol and acetone of 1:2 was added, and the mixtu...

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Abstract

The invention relates to a modified carboxymethyl chitosan quaternary ammonium salt and a preparation method thereof, the modified carboxymethyl chitosan quaternary ammonium salt takes O-carboxymethyl chitosan and a trihydroxyethyl allyl quaternary ammonium salt as raw materials, and the trihydroxyethyl allyl quaternary ammonium salt grafted carboxymethyl chitosan is prepared through a polymerization reaction by an inverse emulsion polymerization method. The chitosan and the trihydroxyethyl allyl quaternary ammonium salt used in the invention are easy to obtain, easy to degrade, good in biocompatibility and low in cost. According to the inverse emulsion polymerization method adopted by the invention, reaction is carried out under the condition that water and kerosene are respectively used as a water phase system and an oil phase system, and compared with an aqueous solution polymerization method in the prior art, nitrogen is introduced, the reaction condition is simple, the temperature is low, the time is short, and the energy consumption is low. The synthesized modified carboxymethyl chitosan quaternary ammonium salt can generate an electrification neutralization reaction and an adsorption bridging effect with particles in water, so that the particles in a system are destabilized and flocculated to facilitate sedimentation and dehydration, and meanwhile, the modified carboxymethyl chitosan quaternary ammonium salt has certain sterilization and antibacterial properties and moisture retention.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a modified carboxymethyl chitosan quaternary ammonium salt and a preparation method thereof. Background technique [0002] Water is a basic natural resource as well as a strategic economic resource, and an important material basis for the construction of ecological civilization. With the progress of industrialization, the challenges faced by the water environment are becoming more and more severe, and the wastewater to be treated is more complex and difficult to degrade. Therefore, it is of great practical significance to develop new efficient and environmentally friendly flocculant materials. [0003] The modification and derivatization of chitosan and the introduction of functional groups can not only break the tight arrangement of chitosan molecular chains, improve its molecular spatial structure, weaken intermolecular forces, and increase its solubility in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08C02F1/56
CPCC08B37/003C02F1/56Y02W10/37
Inventor 黄新文王林拓夏莎莎蒋安桦周乾鑫叶翔宇张怡蓉
Owner ZHEJIANG UNIV OF TECH
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