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Production method of chitooligosaccharide

A technology of chitosan oligosaccharide and production method, which is applied in the field of chitosan oxidized by hydrogen peroxide as an oxidant to produce chitosan oligosaccharide to achieve the effect of low molecular weight

Inactive Publication Date: 2011-09-14
DALIAN XINDIEHONGXIANG CHITINS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the solubility is as high as 80g, there is no such high solubility product reported at home and abroad

Method used

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  • Production method of chitooligosaccharide
  • Production method of chitooligosaccharide

Examples

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Effect test

Embodiment 1

[0029] Add 200kg of deionized water to a 500L enamel reaction kettle with a stirring, jacket and temperature measuring device, start stirring, add 20kg of 100-mesh chitosan while stirring, and continue stirring for 10 minutes after adding. Then 20 kg of hydrogen peroxide with a mass fraction of 27.5% was added thereto at one time, and stirred for 10 min. The mass fraction of hydrogen peroxide added in this reaction is 27.5%. The jacket is supplied with steam to raise the temperature, and the temperature in the reactor is raised to 60°C to start timing, and the reaction solution is kept at 60°C to 70°C for 2 hours. Then, 20 kg of hydrogen peroxide is added therein, and the reaction solution is reacted at 60° C. to 70° C. Add 5kg chitosan after hydrogen peroxide has been added. Continue to flow and add 20kg hydrogen peroxide, add 5kg chitosan again after adding. Feed the remaining 20kg of hydrogen peroxide, and control the rate of hydrogen peroxide addition at 0.1kg to 0.5kg / ...

Embodiment 2

[0031]Add 250kg of deionized water to a 500L enamel reaction kettle with a stirring, jacket and temperature measuring device, start stirring, add 25kg of 100-mesh chitosan while stirring, and continue stirring for 10 minutes after adding. Then add 25kg of hydrogen peroxide to it at one time, and stir for 10min. The mass fraction of hydrogen peroxide added in this reaction is 27.5%. The jacket is supplied with steam to raise the temperature, and the temperature in the reactor is raised to 60°C to start timing, and the reaction solution is kept at 70°C to 80°C for 2 hours. Then, 25 kg of hydrogen peroxide was added therein, and the reaction solution was reacted at 70° C. to 80° C. Add 6.25kg chitosan after hydrogen peroxide has been added. Continue to flow and add 25kg hydrogen peroxide, add 6.25kg chitosan again after adding. Feed the remaining 20kg of hydrogen peroxide, and control the rate of hydrogen peroxide addition at 0.1kg to 0.5kg / min, to ensure that the reaction tem...

Embodiment 3

[0033] Add 500kg of deionized water to a 1000L enamel reaction kettle with stirring, jacket and temperature measuring device, start stirring, add 40kg of 100 mesh chitosan while stirring, and continue stirring for 10 minutes after adding. Then add 40kg of hydrogen peroxide to it all at once, and stir for 10min. The jacket is supplied with steam to raise the temperature, and the temperature in the reactor is raised to 60°C to start timing, and the reaction solution is kept at 60°C to 70°C for 2 hours. Then, 40 kg of hydrogen peroxide was added therein, and the reaction solution was reacted at 60° C. to 70° C. Add 10kg chitosan after adding hydrogen peroxide. Continue to add 40kg of hydrogen peroxide, and then add 10kg of chitosan after adding. Feed the remaining 40kg of hydrogen peroxide, and control the addition rate of hydrogen peroxide at 0.1kg-0.5kg / min, to ensure that the reaction temperature is between 60°C and 70°C and there is no phenomenon of pot boiling. After addi...

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Abstract

The invention provides a production method of chitooligosaccharide, belongs to the technical field of fine chemical industry. The method is characterized in that hydrogen peroxide is utilized as an oxidizer for oxidizing chitosan to produce the chitooligosaccharide, wherein, mass fraction of the chitosan is 5%-35%; when a reaction end point is reached, the ratio of n (the hydrogen peroxide) to n (the chitooligosaccharide) is 1.3-5.5, and reaction temperature is 50-90 DEG C; the obtained reaction liquid is cooled to 0-10 DEG C, and materials are separated out with ethanol with volume fraction of 95% at minus 30-0 DEG C, wherein, the ratio of w (the ethanol) to w (the reaction liquid) is 1-4; and the obtained filter cake is washed with ethanol with volume fraction of 99% at minus 30-10 DEG C for 1-5 times, and then the filter cake is dried at the temperature of 40-60 DEG C for 2-8 hours. The production method has the beneficial effects that molecular weight of the chitooligosaccharide is low, and the solubility thereof can reach up to 80g per 100g of water; degradation is performed in a neutral medium, thus the obtained product contains no inorganic salts; the reducing substance is added to the reaction liquid so as to completely eliminate the remaining peroxide; and three wastes are avoided during the production process. The obtained chitooligosaccharide product has the advantages of high yield and bioactivity and improved color, and a toxicology test proves that the product belongs to a non-toxic substance.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for chemically oxidizing chitosan to produce chitosan-oligosaccharide and its extraction method, in particular to a method for producing chitosan-oligosaccharide by oxidizing chitosan with hydrogen peroxide as an oxidant . Background technique [0002] The preparation methods of chitosan oligosaccharide mainly include degradation method, synthesis method and fermentation method. At present, the synthesis method and the fermentation method have not been industrialized due to many technical difficulties. The degradation is divided into acid hydrolysis, oxidative degradation and enzymatic degradation. [0003] The acid hydrolysis reaction is often violent, difficult to control, and poor in selectivity. The resulting product has a low degree of polymerization and is even degraded into monosaccharides. At the same time, separation and purification are difficult, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 张勇
Owner DALIAN XINDIEHONGXIANG CHITINS
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