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Water-soluble phosphorylated chitosan and preparation method thereof

A technology for polymer phosphorylated chitosan and alkalized chitosan, which is applied in the field of water-soluble phosphorylated chitosan and its preparation, can solve the problems of poor complexation performance and selectivity, and achieves a simple and easy preparation method. , the reaction conditions are mild and controllable, and the effect of reducing energy consumption

Pending Publication Date: 2021-11-19
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the water-soluble polymer complexing agents commonly used in this process, such as sodium polyacrylate (PAAS), acrylic acid-maleic acid copolymer (PMA), etc., have poor complexing performance and selectivity for rare earth ions, so it is necessary to design and synthesize new Rare earth complexing agent for complexation – separation of rare earth ions by ultrafiltration concentration

Method used

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  • Water-soluble phosphorylated chitosan and preparation method thereof
  • Water-soluble phosphorylated chitosan and preparation method thereof
  • Water-soluble phosphorylated chitosan and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Slowly add NaOH solution with a mass fraction of 30% into the reactor containing chitosan, wherein the mass ratio of chitosan to NaOH solution is 1:5, stir evenly, freeze for 8 days, and remove by filtration after thawing lye, namely to obtain alkalized chitosan.

[0026] Add the alkalized chitosan to the acetic acid solution with a mass fraction of 1%, stir and dissolve to obtain the acetic acid solution of the chitosan, wherein the mass concentration of the chitosan is 1%; then add dimethyl phosphite under stirring at room temperature , then raise the temperature to 60°C, add formaldehyde solution with a mass fraction of 37% to 40% into the system, wherein the mass ratio of alkalized chitosan, dimethyl phosphite and formaldehyde solution is 1:4:10, after mixing evenly Then add the catalyst p-toluenesulfonic acid, wherein the mass ratio of p-toluenesulfonic acid and alkalized chitosan is 0.1:1, reflux reaction for 5h; after the reaction, the solution is cooled to norma...

Embodiment 2

[0030] Slowly add NaOH solution with a mass fraction of 30% into the reactor containing chitosan, wherein the mass ratio of chitosan to NaOH solution is 1:3, stir evenly, freeze for 5 days, and remove by filtration after thawing lye, namely to obtain alkalized chitosan.

[0031] Add the alkalized chitosan to the acetic acid solution with a mass fraction of 1%, stir and dissolve to obtain the acetic acid solution of chitosan, wherein the mass concentration of chitosan is 0.5%; then add dimethyl phosphite under stirring at room temperature , then heat up to 65°C, add formaldehyde solution with a mass fraction of 37% to 40% into the system, wherein the mass ratio of alkalized chitosan, dimethyl phosphite and formaldehyde solution is 1:4:10, after mixing evenly Then add catalyst p-toluenesulfonic acid, wherein the mass ratio of p-toluenesulfonic acid and alkalized chitosan is 0.1:1, and reflux reaction for 4h; after the reaction, the solution is cooled to normal temperature, and t...

Embodiment 3

[0033] Slowly add NaOH solution with a mass fraction of 30% into the reactor containing chitosan, wherein the mass ratio of chitosan to NaOH solution is 1:4, stir evenly, freeze for 6 days, and remove by filtration after thawing lye, namely to obtain alkalized chitosan.

[0034]Add alkalized chitosan to the acetic acid solution with a mass fraction of 1%, stir and dissolve to obtain the acetic acid solution of chitosan, wherein the mass concentration of chitosan is 0.6%; then add dimethyl phosphite under stirring at room temperature , then heat up to 70°C, add formaldehyde solution with a mass fraction of 37% to 40% into the system, wherein the mass ratio of alkalized chitosan, dimethyl phosphite and formaldehyde solution is 1:4:10, after mixing evenly Then add catalyst p-toluenesulfonic acid, wherein the mass ratio of p-toluenesulfonic acid and alkalized chitosan is 0.1:1, and reflux reaction for 6h; after the reaction, the solution is cooled to normal temperature, and then t...

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Abstract

The invention relates to a water-soluble phosphorylated chitosan and a preparation method thereof. The preparation method comprises the following steps: performing alkalization treatment on chitosan (CS) to obtain alkalized chitosan, performing Kabachnik-Fields reaction on the alkalized chitosan, dimethyl phosphite and formaldehyde under the catalytic action of p-toluenesulfonic acid (TsOH), controlling the reaction temperature to be 60-70 DEG C and the reaction time to be 4-6 hours, cooling, putting into a dialysis bag of which the molecular weight cut-off is 8000-14000 Da, dialyzing for 24-48 hours, and carrying out reduced pressure distillation, precipitation of a mixed solvent, filtration, washing and vacuum drying to obtain a faint yellow solid, namely phosphorylated chitosan (PCS). According to the invention, methylene and phosphoryl groups are introduced to a polymer chitosan skeleton through grafting modification, so that the product phosphorylated chitosan has excellent hydration capability, rare earth complexing performance and selectivity. The preparation process is simple, and the reaction conditions are mild and controllable.

Description

technical field [0001] The invention belongs to the field of polymer modification, and in particular relates to a water-soluble phosphorylated chitosan and a preparation method thereof. Background technique [0002] Chitosan is a natural polymer that can be easily extracted from shells, shrimp shells and other substances. It is non-toxic and harmless and has a wide range of sources. It is used in the field of environmental treatment, especially in water treatment. However, chitosan has defects such as low metal adsorption capacity and poor solubility, which limit its application range. Therefore, the modified chitosan with excellent performance can be obtained through the functional modification of the functional group with the main chain of chitosan as the backbone, which can expand the application range of chitosan. Modified chitosan has made many achievements in the treatment of heavy metal wastewater, but there is no report on the concentration and separation of rare e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
CPCC08B37/003
Inventor 邱运仁陈雨欣陈玉娟
Owner CENT SOUTH UNIV