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Quasi-carboxymethyl chitosan and new one-step synthesis process

A technology of pseudo-carboxymethyl chitosan and carboxymethyl chitosan is applied in the field of one-step synthesis of pseudo-carboxymethyl chitosan, which can solve the problem of governance, large amount of waste salt organic water, difficulty in collecting raw materials, etc. It can achieve the effect of excellent water absorption rate and water retention rate, good water absorption and water retention performance, and easy separation and purification.

Active Publication Date: 2021-01-05
XIAMEN UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing production process has difficulties in collecting natural raw materials, high production costs and other constraints, which limit the development of the industry
[0003] The current carboxymethyl chitosan adopts the process route of extracting chitosan from shrimp and crab shells first, and then carrying out carboxymethylation to produce carboxymethyl chitosan. There are difficulties in raw material collection, high production cost, and difficult synthesis process. It is cumbersome and lengthy, high acid and alkali consumption, low yield, large amount of waste acid, waste alkali, waste salt organic water, difficult treatment, difficult collection of raw materials, high production costs and other serious problems that seriously restrict its large-scale application. The current global annual output Less than 100,000 tons
Due to the greater steric hindrance of glycinate than ammonia, stronger nucleophilicity and the repulsion between the secondary ammonia structure of the substitution product and the negative charge, it may be easier to replace than ammonia and more conducive to reducing the polymerization by-product, divalent calcium The attraction of ions and positive ions can help the intermolecular approach of raw materials, and the precipitation of calcium ions and sulfate radicals is beneficial to help the sulfate radicals to leave, but the participation effect of the adjacent groups of glycine may lead to the hydrolysis of bio-based sulfate monoesters and molecular degradation. Response must be suppressed

Method used

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  • Quasi-carboxymethyl chitosan and new one-step synthesis process
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  • Quasi-carboxymethyl chitosan and new one-step synthesis process

Examples

Experimental program
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Effect test

preparation example Construction

[0055] according to figure 1 The preparation process flow chart of pseudo carboxymethyl chitosan shown in , obtains following conclusion through a large amount of experiments and process exploration: the optimized process condition of pseudo carboxymethyl chitosan preparation is: temperature is below 200 ℃, (preferably 80-160°C), the appropriate reaction time is 6-24h, (preferably 8-16h), and can synthesize carboxymethyl chitosan with a degree of substitution DS=0.6 or so and hemicellulose substituted with carboxymethylamino The mixture of this process degradants and by-products are very few.

[0056] The reaction equation of raw material preparation is as follows:

[0057]

[0058] The reaction equation for preparing pseudo carboxymethyl chitosan is as follows:

[0059]

[0060] See Table 1 for related testing and analysis methods.

[0061] Table 1: Analysis content and analysis method of the product

[0062] analysis content Analytical method Degre...

Embodiment 1

[0063] The preparation of embodiment 1 raw material cellulose sulfate monoester salt

[0064] Weigh 0.486g microcrystalline cellulose, add 3.75ml DCE to swell the cellulose, add 1mol / L SO 3 / DCE sulfonation reagent, by cellulose structural unit and SO 3 The molar ratio is 3: 5 feed intake, after stirring in ice bath for 15min, the reaction solution is placed at room temperature and reacted for 2h to obtain cellulose sulfate monoester (this cellulose sulfate monoester is used in Example 12 and Example 13) , add in 10ml water and lime mixed solution, stirring and neutralizing to pH is 7, filters out solid, and filtrate is calcium cellulose sulfonate, obtains 2.66g of solid product through dialysis, concentrating and drying, and product yield is 54.8%, The test sulfonation substitution degree is 1.2, wherein, the infrared spectrogram of cellulose sulfonate see figure 2 , SEM analysis diagram see image 3 . Carboxymethyl chitosan was prepared using calcium cellulose sulfonate...

Embodiment 2

[0073] Yield and degree of substitution of pseudo carboxymethyl chitosan under different reaction times in the water system of embodiment 2

[0074] Add 0.281g calcium cellulose sulfonate (CaCS) into the autoclave, and add an appropriate amount of calcium glycinate to it, change the equivalent ratio of glucose units in calcium glycinate and calcium cellulose sulfonate to 2:1, add 35ml of Deionized water, the reaction temperature is 180°C, and the reaction time is changed. After the reaction, the solid and liquid are separated. The yield of the liquid after dialysis, concentration and drying is the pure product yield, and the degree of substitution is calculated by elemental analysis.

[0075] Table 2: Degree of substitution and yield of pseudocarboxymethyl chitosan with different reaction times in water system

[0076] Reaction time (h) Degree of Substitution (DSN) Degree of Substitution (DSS) Pure product yield (%) 4 0.09 0.45 44.2 8 0.25 0.30 21...

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Abstract

The invention relates to a quasi-carboxymethyl chitosan polymer, a new process for synthesizing the polymer in one step and a composition containing the polymer. The cellulose sulfate monoester salt or bio-based mixed sulfate monoester salt is used as a raw material, a novel method for synthesizing the quasi-carboxymethyl chitosan polymer by one step through a substitution reaction with calcium glycinate in a water or alcohol-water system, in particular to the method for producing quasi-carboxymethyl chitosan with higher conversion rate and higher substitution degree in a shorter time and at lower temperature by using the alcohol-water system, and the process is simple and convenient in synthesis process, few in byproducts, high in substitution degree and suitable for industrial production, and separation and purification are easily carried out. According to the breakthrough technology, low-cost and large-scale production of the quasi-carboxymethyl chitosan becomes possible, and wide application of the quasi-carboxymethyl chitosan polymer with high cost performance in the fields of water-retaining agents, sustained and controlled release fertilizers, liquid foliar fertilizers, adhesives and the like is certainly promoted.

Description

technical field [0001] The invention belongs to the field of biomass deep processing industry, in particular to the field of polysaccharide derivative production, and more specifically relates to the preparation of widely used carboxymethyl chitosan and its carboxymethyl shell containing the sulfonated product of biomass material as raw material Compositions of polysaccharides, and a method for the one-step synthesis of pseudocarboxymethyl chitosan. Background technique [0002] Carboxymethyl chitosan is a derivative of chitosan, which has better film-forming properties, water solubility, flocculation, antibacterial and biocompatibility, and can be widely used in industry, agriculture, environmental protection, medical treatment, etc. industry. However, the existing production process has constraints such as difficulty in collecting natural raw materials and high production costs, which limit the development of the industry. [0003] The current carboxymethyl chitosan adop...

Claims

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Application Information

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IPC IPC(8): C08B15/06C08L1/16C08L1/08C09J101/08C09J125/14C05G3/40C05G3/80C05G5/20C05C11/00C09K17/32
CPCC08B15/06C08L1/16C08L1/08C09J101/08C09J125/14C05G3/40C05G3/80C05G5/20C05C11/00C09K17/32C08L2205/02C08L2205/04C08L25/14
Inventor 尹应武陈思瑞师雪琴吐松叶李艺高玉兴张文军张海双马杜媚
Owner XIAMEN UNIV
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