Green and environment-friendly method for preparing alkaline water-soluble chitosan derivative

A green environmental protection, water-soluble shell technology, applied in the field of preparing alkaline water-soluble chitosan derivatives, can solve the problems of heavy pollution, large consumption of reagents, not in line with the concept of green environmental protection, etc., and achieves mild reaction conditions, good water solubility, The effect of high molecular weight

Inactive Publication Date: 2016-05-25
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reagent consumption of the whole carboxymethylation process is large, and small molecules containing chlorine are produced in the reaction product. A large amount of sodium hydroxide solution is used in the process. Therefore, from the perspective of environmental protection, the current industrialized carboxymethyl chitosan The production process has heavy pollution and does not conform to the concept of green environmental protection
Adopt the method for depolymerization chitosan molecule, the chitosan molecular weight that usually prepares also can't satisfy the needs of industry well

Method used

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  • Green and environment-friendly method for preparing alkaline water-soluble chitosan derivative
  • Green and environment-friendly method for preparing alkaline water-soluble chitosan derivative
  • Green and environment-friendly method for preparing alkaline water-soluble chitosan derivative

Examples

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Effect test

Embodiment 1

[0037] A preparation method of chitosan water-soluble derivatives, comprising the following steps: 1) preparation of chitosan grafted polyacrylic acid

[0038] Using water as a solvent, put it in an oil bath at 60 ° C, and after purging the air with nitrogen, according to the mass ratio of chitosan and acrylic acid monomer is 1:6 (w / w), acrylic acid is passed through constant pressure drop Slowly add the funnel dropwise into the aqueous solution mixing system of reactive chitosan, after fully mixing, slowly add 3.28×10 -3 mol / L cerium ammonium nitrate (Ce 4+ ) as an initiator, after the dropwise addition, continue to deoxidize with nitrogen, maintain the original temperature at 60° C. for 5 h, and stop the reaction. Precipitate with concentrated hydrochloric acid, then filter the solution, wash the solid with 99% ethanol for three times, and then filter under reduced pressure to remove the homopolymer of acrylic acid. After vacuum drying at 50°C, a solid chitosan grafted poly...

Embodiment 2

[0046] A preparation method of chitosan water-soluble derivatives, comprising the following steps:

[0047] 1) Preparation of chitosan grafted polyacrylamide

[0048] Use water as a solvent, put it in an oil bath at 50°C, and after purging the air with nitrogen, pass acrylamide through constant pressure according to the mass ratio of chitosan and acrylamide monomer at a ratio of 1:10 (w / w). The dropping funnel was slowly added dropwise into the aqueous solution mixing system of the reaction chitosan, and after being fully mixed, slowly added 6×10 -3 mol / L cerium ammonium nitrate (Ce 4+ ) as an initiator, after the dropwise addition, continue to deoxidize with nitrogen, maintain the original temperature of 50° C. for 5 hours, and stop the reaction. Precipitate with concentrated hydrochloric acid, then filter the solution, wash the solid with 99% ethanol three times, and then filter under reduced pressure to remove the acrylamide homopolymer. After vacuum drying at 50°C, a sol...

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Abstract

The invention discloses a green and environment-friendly method for preparing an alkaline water-soluble chitosan derivative, and belongs to the technical field of macromolecular synthesis. The method comprises the steps that 1, a chitosan grafted polymer is prepared, wherein chitosan macromolecules are mixed with vinyl monomers with hydrophilic groups, degassing is conducted, an initiator is added, degassing is conducted continuously, the reaction is stopped, sedimentation and filtration are conducted, washing separation and purification are conducted, drying and grinding are conducted, and the chitosan grafted polymer powder is obtained; 2, N-acylation chitosan grafted polymer is obtained, wherein the chitosan grafted polymer powder is completely dissolved in water and added to an acetic acid solution, 1,2-propylene glycol is added, standing and degassing are conducted at room temperature for one day, an N-acylation solution is added to a reaction mixture, and the pH is adjusted to 7-13, evaporative crystallization is conducted, and the alkaline water-soluble chitosan derivative is obtained. The green and environment-friendly method for preparing the alkaline water-soluble chitosan derivative is friendly to environment, the chitosan derivative which is mild in reaction condition, large in molecular weight and good in water solubility and basically accords with industrial application, water solubility can be achieved within the pH range of 7-11, and the solubility reaches up to 10 mg / mL.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a green and environment-friendly method for preparing alkaline water-soluble chitosan derivatives. Background technique [0002] Chitosan (CS) is the deacetylation product of chitin extracted from the shell skeleton of shrimp, crab and insect, and is the only alkaline polysaccharide in nature. It is rich in sources and is a renewable natural polymer material. Chitosan has the characteristics of good biocompatibility, easy degradation, non-toxicity, and environmental friendliness. However, the physical properties of chitosan insoluble in water and alkaline solution limit its application in human life and industry. Generally speaking, chitosan can only be dissolved in water with pH<4. It is reported that under the condition of pH<5, the degradation rate of chitosan will be greatly increased, which may cause the molecular weight of chitosan to decrease...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/00C08F220/06C08F220/56C08F8/10
CPCC08F251/00C08F8/10C08F220/06C08F220/56
Inventor 倪恨美张丽娟时凯吴敏
Owner SOUTHEAST UNIV
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