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Method of preparing chitobiose/chitotriose monomer on large scale

A technology of chitotriose and chitobiose, which is applied in the field of large-scale preparation of chitobiose/chitotriose monomers, can solve the problems of small sample loading, high filler cost, difficult regeneration, etc., and achieves stable production process and operation. low cost effect

Inactive Publication Date: 2017-06-23
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of the filler in the above-mentioned patent is relatively high, it is not easy to regenerate, and the loading amount is relatively small, so it is not suitable for large-scale production to prepare chitosan oligosaccharide monomer

Method used

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  • Method of preparing chitobiose/chitotriose monomer on large scale
  • Method of preparing chitobiose/chitotriose monomer on large scale
  • Method of preparing chitobiose/chitotriose monomer on large scale

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] (1) The synthesis of strongly acidic cation exchange resin is made by cross-linking styrene and divinylbenzene to form copolymer beads as the skeleton, and then introducing sulfonic acid groups through the sulfonation of concentrated sulfuric acid strong oxidant. The specific process is as follows:

[0061] (a) Preparation of water phase raw materials

[0062] Weigh deionized water: ethylenediamine: sodium chloride: sodium persulfate: polyvinyl alcohol according to the ratio of parts by weight 1000:30:85:1.5:75, adjust the pH of the system to be neutral, and control the temperature to 45 ° C ~ 55 ℃, stirring speed 120rmp / min, react for 24h to obtain the water phase raw material;

[0063] (b) Preparation of oil phase raw materials

[0064] Weigh benzoyl peroxide in parts by weight: azobisisobutyronitrile: styrene: ferrocene: divinylbenzene=1.5:3:900:25:50, mix, with a heating rate of 0.5°C / min Raise the temperature to 78-80°C, keep the temperature constant for 5-6 hou...

Embodiment 2

[0070] The synthesis of strongly acidic cation exchange resin is made by cross-linking styrene and divinylbenzene to form copolymer beads as the skeleton, and then introducing sulfonic acid groups through the sulfonation of concentrated sulfuric acid strong oxidant. The specific process is as follows:

[0071] (a) Preparation of water phase raw materials

[0072] Weigh deionized water: ethylenediamine: sodium chloride: sodium persulfate: polyvinyl alcohol according to the weight ratio of 1040g: 33g: 87g: 2g: 80g, adjust the pH of the system to be neutral, and control the temperature to 45 ° C ~ 55 ℃, stirring speed 120rmp / min, react for 24h to obtain the water phase raw material;

[0073] (b) Preparation of oil phase raw materials

[0074] Weigh benzoyl peroxide in parts by weight: azobisisobutyronitrile: styrene: ferrocene: divinylbenzene=2.0g: 3.5g: 920g: 30g: 53g, mix, at 0.5 ℃ / min Heating rate: raise the temperature to 78-80°C, keep the temperature for 5-6 hours, then c...

Embodiment 3

[0080] (a) Preparation of water phase raw materials

[0081] Weigh deionized water: ethylenediamine: sodium chloride: sodium persulfate: polyvinyl alcohol according to the ratio of parts by weight 1080g: 36g: 90g: 2.5g: 90g, adjust the pH of the system to be neutral, and control the temperature to 45 ° C ~ 55°C, stirring speed 120rmp / min, react for 24h to obtain the water phase raw material;

[0082] (b) Preparation of oil phase raw materials

[0083] Weigh benzoyl peroxide in parts by weight: azobisisobutyronitrile: styrene: ferrocene: divinylbenzene=2.5g: 4.5g: 940g: 35g: 60g, mix, at 0.5 ℃ / min Heating rate: raise the temperature to 78-80°C, keep the temperature for 5-6 hours, then continue to gradually raise the temperature to 93-95°C, keep the temperature for 5-6 hours to obtain the intermediate product A, then add the water-phase raw materials obtained in step (a) to mix, and The temperature is controlled to 65-67°C, and the suspension polymerization is carried out for ...

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Abstract

The invention relates to a method for the large-scale preparation of chitobiose / chitotriose monomers, comprising the following steps: (1) dissolving chitooligosaccharide components in water to form a solution, decolorizing, filtering, and pumping into a strong acid cation exchange The column starts to load the sample, elutes with hydrochloric acid solution, and collects a tube at the same time; (2) each tube takes a sample to detect the sugar components in the collected solution, and merges the same sugar components; (3) the combined chitobiose and The two components of chitotriose are rotary evaporated to dryness, and hydrochloric acid is removed to obtain chitobiose monomer solid and chitotriose monomer solid respectively. Compared with the prior art, the process of the present invention is simple and convenient, and the yield is high, and high-purity chitobiose and chitotriose monomers and the like can be realized on a kilogram-level preparation scale.

Description

technical field [0001] The invention relates to the field of separation and purification of functional marine amino oligosaccharides, in particular to a method for large-scale preparation of chitobiose / chitotriose monomers. Background technique [0002] Oligochitosan is the only positively charged basic oligosaccharide in nature with a degree of polymerization of 2 to 10 and a molecular weight of less than 3000 Da. Its structure is formed by connecting D-glucosamine and N-acetyl-D-glucosamine through β-1,4-glucosidic bonds. Oligochitosan contains hydroxyl and amino active groups in its own structure and has various physiological activities. Such as antibacterial, anti-oxidant, anti-tumor, anti-cancer activities, lowering cholesterol and improving immunity, etc. Because of its small molecule, good water solubility, good tissue compatibility, natural non-toxic and other characteristics, it is often used in the fields of biomedicine, health food, agriculture and animal husban...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F257/02C08F212/08C08F212/36C08F2/20C08F8/36B01J39/20
CPCC08F257/02B01J39/20C08F2/20C08F8/36C08F212/08C08F212/36
Inventor 赵黎明徐庆秦臻陈启明邱勇隽
Owner EAST CHINA UNIV OF SCI & TECH
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