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Process for preparing narrow-distribution chitosan with controllable molecular weight through microwave-H2O2 combined degradation method

A -H2O2, chitosan technology, applied in the field of preparation of water-soluble chitosan, can solve the problems of complex post-processing, difficult acquisition, purification and immobilization, harsh requirements, etc., and achieves clear molecular weight distribution characteristics, effective control of molecular weight distribution, The effect of saving energy and resources

Inactive Publication Date: 2015-05-06
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the degradation process of this method is difficult to control, the molecular weight range of the resulting degradation product is very wide, the stability and repeatability of the reaction are poor, the yield of the product is low, and the environmental pollution caused is more serious; the physical degradation method obeys the dynamics of random degradation Science, simple operation, fast response, low energy consumption, no pollution
However, this method is easy to cause some crosslinking and branching reactions, the post-treatment is complicated, and the yield is too low, resulting in high production costs. It is difficult to apply to industrial production as the main method, but can only be used as an auxiliary means to accelerate the reaction. ;The enzymatic degradation method is carried out under milder conditions, does not require a large amount of reaction reagents, and the molecular weight of the degradation product is easy to control
However, this degradation method has strict requirements for raw enzymes, and different enzymes have different degrees of degradation of chitosan. At the same time, it is difficult to obtain enzymes, purify enzymes, and immobilize enzymes, and the cost is also very high.
There are also combined use of different degradation methods, but it still cannot solve the problems of long operation process, high energy consumption, low yield and complicated process. It is difficult to achieve standardized control of the molecular weight of the final product, and the repeatability is poor.
There are individual methods that can partially achieve molecular weight-controlled degradation, but the product is water-insoluble chitosan with a high molecular weight, and there is no mention of the molecular weight distribution characteristics of the degradation

Method used

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  • Process for preparing narrow-distribution chitosan with controllable molecular weight through microwave-H2O2 combined degradation method
  • Process for preparing narrow-distribution chitosan with controllable molecular weight through microwave-H2O2 combined degradation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 2.00g of chitosan into the reactor, add 30mL of 1% (w / w) acetic acid and stir to dissolve, after standing for 10min, add 6% (w / w) H 2 o 2 30mL was placed in the microwave reactor and equipped with a reflux device, and stirred evenly; set the microwave radiation temperature to 65°C, the radiation anode current to 80mA, and turned on the microwave pulse radiation; start the radiation timing, and control the effective radiation time for 3 minutes. After the reaction, cool to room temperature, adjust the pH to 7~8 with 5% (w / w) sodium hydroxide solution, filter to remove a small amount of residue, precipitate the filtrate with 2.5 times the volume of absolute ethanol, collect the precipitate, and vacuum at 40°C Dry to obtain water-soluble oligomeric chitosan; the measured yield is 55%, the average molecular weight of the product is 7255, and the polydispersity coefficient D is 1.6, which belongs to a narrow distribution product.

[0026] The infrared spectrograms of ...

Embodiment 2

[0034] Weigh 2.00g of chitosan into the reactor, add 30mL of 1% (w / w) acetic acid and stir to dissolve, then add 2% (w / w) H 2 o 2 30mL was placed in a microwave reactor and equipped with a reflux device, and stirred evenly; set the microwave radiation temperature to 50°C, the radiation anode current to 40mA, and turned on microwave pulse radiation; control the effective radiation time for 3 minutes. After the reaction, cool to room temperature, adjust the pH to 7~8 with 5% (w / w) sodium hydroxide solution, remove a small amount of residue by filtration, precipitate the filtrate with 2 times the volume of absolute ethanol, collect the precipitate and dry it under vacuum at 40°C , to obtain water-soluble oligomeric chitosan; the measured yield was 49%, the average molecular weight of the product was 18229, and the polydispersity coefficient D was 1.8, which belonged to narrow distribution products.

[0035] The preparation process of this example was repeated at least five times...

Embodiment 3

[0038] The steps are the same as in Example 2, except that the effective radiation time is controlled for 5 minutes to obtain water-soluble chitosan oligosaccharides; the measured yield is 52%, the average molecular weight of the product is 6560, and the polydispersity coefficient D is 1.8, which belongs to a narrow distribution product .

[0039] The preparation process of this example was repeated at least five times, and the measured yields were all about 52%, the average molecular weight of the products was 6560-8407, and the polydispersity coefficient D was between 1.8-2.0, all of which were narrowly distributed products.

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Abstract

The invention discloses a process for preparing narrow-distribution chitosan with controllable molecular weight through a microwave-H2O2 combined degradation method. The process comprises the following steps of: adding highly polymerized chitosan into a reactor, then stirring and dissolving by using an acetic acid solution, and standing for 10 minutes; adding 2-8 percent of H2O2 into the obtained solution; fixing the reactor in a microwave experimental instrument, simultaneously starting stirring, radiating for 3-8 minutes through a pulse mode to obtain a pale yellow solution; and regulating a pH value to be 7-8 by using an alkaline liquor, filtering, collecting the precipitation, performing vacuum drying to obtain water-soluble oligochitosan. Due to the adoption of the microwave-H2O2 combined degradation method, the narrow-distribution water-soluble oligochitosan is prepared under homogeneous-phase condition, According to the method, the operation is easy, environmental protection is realized, and secondary pollution is avoided; and moreover, the reaction is rapid during synergism of microwave and H2O2, a large quantity of energies and resources are saved, the molecular weight and distribution of the oligochitosan can be effectively controlled, and the repeatability is good.

Description

technical field [0001] The present invention relates to the preparation of water-soluble chitosan, specifically utilizes microwave and H 2 o 2 The chitosan is degraded by synergistic action to obtain oligomeric chitosan products with controllable molecular weight and narrow molecular weight distribution. technical background [0002] Chitosan is the only cationic alkaline polysaccharide that exists in nature. It is a product of high deacetylation of chitin and has good biocompatibility. It is widely used in biomedicine, agriculture, forestry, chemical industry and other fields. As a high polymer, chitosan is composed of glucosamine units linked numerous times, with molecular weights ranging from hundreds of thousands to millions. As the molecular weight increases, the strength, modulus, and toughness of chitosan slow down, and finally tend to a certain limit value. When the molecular weight is very high, that is to say, when the molecular chain is very long, the flow is di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/08
Inventor 张惠欣朱玉超王枫窦倩王冬冬
Owner HEBEI UNIV OF TECH
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