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Method for preparing high-viscosity chitosan by using chitin

A chitin and chitosan technology, applied in medical science, bandages, absorbent pads, etc., can solve the problems of cumbersome repeated sampling and detection, difficult temperature control, high energy consumption, etc., to shorten the reaction time, shorten the production cycle, energy low consumption effect

Inactive Publication Date: 2012-06-13
MINZU UNIVERSITY OF CHINA +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Among the patents published in recent years, the patent publication number CN101289518A is a method for preparing chitin and a method for preparing chitosan by using chitin. Add 40-45% NaOH solution and heat for 16 hours during the whole process, which has low efficiency and high energy consumption, and it is cumbersome to repeatedly sample and test during the whole process
Publication No. CN101200505A discloses a method for preparing chitosan with high deacetylation degree and high viscosity by using shrimp shells, which is to add chitin into NaOH with a concentration of 45-50% at a ratio of 1:20-30 for microwave treatment for 15-20 minutes. Then add 13-23% NaOH ethanol solution according to the ratio of material to liquid 1: 2-4, reflux at 78°C for 2-3 hours, and finally obtain chitosan by washing, drying and pulverizing. The whole process consumes a lot of alkali, and additional consumption Ethanol, and the temperature is not easy to control during microwave treatment for a long time

Method used

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  • Method for preparing high-viscosity chitosan by using chitin
  • Method for preparing high-viscosity chitosan by using chitin
  • Method for preparing high-viscosity chitosan by using chitin

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Embodiment 1

[0029] Take a certain quality of chitin, soak it in tap water at 60°C for 6 hours, wash it at 60°C by ultrasonic method for 1 hour, then dry it at 105°C for 3 hours, then crush it to 60-80 mesh and repeat the above washing and drying steps. Take 10g of dried powder and add 120g of 30% concentration NaOH solution, so that the mass ratio of NaOH solution to chitin is 12:1, stir at 40°C for 10min, put it into an 800W, 2450MHz microwave reactor and heat for 5min to take it out, and the temperature of the mixture is now 90°C, filter and rinse with 60°C water until the pH value is 7.2-7.5, add the product to 50% NaOH solution, make the mass ratio of NaOH solution to chitin is 12:1, mix well and heat to 90°C, keep the temperature and stir After 50 minutes of reaction, the product was washed with water at 60°C until the pH value was 7.2-7.5, and dried at 105°C for 3 hours to obtain high-viscosity chitosan powder.

[0030] Table 1 shows the changes of deacetylation degree and viscosity...

Embodiment 2

[0044] Take a certain quality of chitin, soak it in tap water at 60°C for 6 hours, wash it at 60°C using ultrasonic method for 1 hour, and then dry it at 105°C for 3 hours, then crush it to 60-80 mesh and repeat the above washing and drying steps. Take 10g of dried powder and add 100g of 30% concentration NaOH solution, so that the mass ratio of NaOH solution to chitin is 10:1, stir at 40°C for 10min, put it into a 800W, 2450MHz microwave reactor and heat for 3min to take it out, at this time the temperature of the mixture is 78°C, filter and rinse with 60°C water until the pH value is 7.2-7.5, add the product to 50% NaOH solution, make the mass ratio of NaOH solution to chitin 10:1, mix well and heat to 90°C, keep the temperature and stir After 50 minutes of reaction, the product was washed with water at 60°C to pH 7.2-7.5 and dried at 105°C for 3 hours to obtain high-viscosity chitosan powder.

[0045] Table 3 shows the changes of deacetylation degree and viscosity every 10 ...

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Abstract

The invention discloses a method for preparing high-viscosity chitosan by using chitin, belongs to the field of biological chemistry and material chemistry, and relates to an industrial production method in which the chitin is pulverized, and then is subject to microwave pretreatment and two-step deacetylation reaction, so as to obtain high-viscosity refined chitosan in a short time. First the chitin is subject to a series of pulverizing, cleaning and drying processes to obtain refined chitin; then the refined chitin is put into a 30% NaOH solution, and reacts for a short time after being preheated and stirred; a product is put into a 50% NaOH solution after being cleaned and is heated for constant-temperature reaction; and finally a product is cleaned and then dried, so as to obtain the high-viscosity chitosan. The production period of the whole process is shorted by 3 to 6 times, the energy consumption is low, the reaction temperature is easy to control, industrial large-scale production is convenient to realized, and the obtained chitosan is 80 to 90 percent in deacetylation degree, 600 to 2000 MPa.s in viscosity and more than 3*106 in viscosity-average molecular weight, and can be used as a medical absorbable hemostatic material.

Description

Technical field [0001] The invention belongs to the fields of biochemistry and material chemistry, and relates to a method for preparing high-viscosity chitosan by using chitin, in particular to a method for deacetylating reaction in two steps by using chitin after pulverization and pretreatment with microwaves, which can be carried out in a short time. A production method for obtaining high-viscosity refined chitosan. Background technique [0002] At present, chitosan is widely used in many industries such as food, medical and textile, and has high economic value and economic growth potential. According to its own viscosity and deacetylation degree, chitosan can be divided into several types with different physical and chemical properties. Properties of materials, such as high-viscosity chitosan, high degree of deacetylation chitosan and water-soluble chitosan, etc., are used in different fields. According to the Chinese aquatic industry standard SC / T3403-2004, the standar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08A61L15/28
Inventor 黄耀江孙雷王进李娜张玉玺慕雷
Owner MINZU UNIVERSITY OF CHINA
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