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Industrial preparation method of O-carboxymethyl chitosan

A technology of carboxymethyl chitosan and chitosan, which is applied in the field of industrialized preparation of O-carboxymethyl chitosan, can solve problems such as toxic organic compounds, and achieve the effects of preventing oxidation, ensuring quality and ensuring yield

Active Publication Date: 2017-02-01
浙江澳兴生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] At present, there are no relevant patents for the large-scale industrial production of carboxymethyl chitosan. The existing carboxymethyl chitosan patents are only in the relevant small-scale test stage, and the substitution position is basically at the N position, or at the N position and the O position. In addition, toxic organic compounds are used in the reaction

Method used

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  • Industrial preparation method of O-carboxymethyl chitosan
  • Industrial preparation method of O-carboxymethyl chitosan

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preparation example Construction

[0038] The preparation method that the embodiment of the present invention provides comprises the following steps:

[0039] S101, adding chitosan to the alkaline solution below 30°C to form a wet material.

[0040] Wherein, the added chitosan is preferably chitosan made from crab shells with a fineness exceeding 40 mesh after crushing.

[0041] The proportion of chitosan in the wet material is 25% to 35%.

[0042] Of course, before adding chitosan, the configuration of lye should be carried out first. In this example, water and caustic soda are mixed according to the mass ratio of 1:0.7 to 1:2, and stirred to dissolve the alkali to obtain lye, and cool the lye to below 30°C.

[0043] S102, put the wet material into the tank mixer, stir evenly to make the chitosan swell, put it into a double-layer inner membrane bag, tie the mouth of the bag, and let it stand for 5 to 10 hours.

[0044] S103, put the double-layer inner film bag into the cold storage, and freeze for 24 hours ...

Embodiment 1

[0073] 1) Mix 100kg of caustic soda and 100kg of purified water into a 1:1 lye, and when the temperature of the lye drops to 30°C, add 100kg of chitosan into the lye, and mix it fully with a tank mixer. Then pass through a 40-mesh sieve, put it into a double-layer inner film bag, tie the mouth of the bag, leave it for 6 hours, and then put it into a freezer at -18°C for 48 hours.

[0074] 2) Put the frozen material into the reactor, add 800kg of isopropanol and vacuum pump it into the reactor, soak for 4 hours.

[0075] 3) Stir the soaked feed liquid for 30 minutes. During the stirring process, start the cooling system at the same time to ensure that the temperature in the kettle does not exceed 20°C.

[0076] 4) 120kg of chloroacetic acid and 40kg of ethanol above 95% are formulated into a chloroacetic acid ethanol solution, which is pumped into a metering tank.

[0077] 5) Slowly add the ethanol solution of chloroacetic acid in the metering tank dropwise to the reaction ket...

Embodiment 2

[0085] 1) Prepare 100kg of caustic soda and 110kg of purified water to make a 1:1.1 lye, when the temperature of the lye drops to 30°C, add 100kg of chitosan into the lye, fully stir and mix with the tank mixer, Then pass through a 40-mesh sieve, put it into a double-layer inner film bag, and tie the mouth of the bag; after standing for 7 hours, put it into a freezer at -18°C for 60 hours.

[0086] 2) Put the frozen material into the reactor, add 800kg of isopropanol and vacuum pump it into the reactor, soak for 5 hours.

[0087] 3) Stir the soaked feed liquid for 30 minutes, and start the cooling system at the same time to ensure that the temperature in the kettle does not exceed 20°C.

[0088] 4) 120kg of chloroacetic acid and 40kg of ethanol above 95% are formulated into a chloroacetic acid ethanol solution, which is pumped into a metering tank.

[0089] 5) Slowly add the ethanol solution of chloroacetic acid in the metering tank dropwise to the reaction kettle, control th...

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Abstract

The embodiment of the invention relate to an industrial preparation method of O-carboxymethyl chitosan. Chitosan is added into alkali liquor of the temperature below 30 DEG C, wet materials are formed, and refrigeration is carried out for 24-72 hours; isopropyl alcohol with the mass 2.5-3.5 times that of the wet materials is added, soaking is carried out for 4-6 hours, and stirring is carried out for 30 minutes; a chloroacetic acid and ethanol solution is dropwise added into the material liquid, and the temperature is controlled to be not larger than 50 DEG C; after all the chloroacetic acid and ethanol solution is dropwise added, the material liquid in a reaction still is subjected to heat preservation; the material liquid obtained after heat preservation is centrifugalized for 30 minutes and then put into the reaction still, ethanol with the mass three times that of the materials is added, and stirring is carried out; a 3%-8% hydrochloric acid solution is added, the pH is adjusted to range from 7.0 to 7.7, and centrifugalization is carried out for 30 minutes; ethanol is added, and soaking, stirring and centrifugalizing are carried out; the materials obtained after centrifugalization are put into the reaction still again, ethanol is added, and soaking, stirring and centrifugalizing are carried out; the materials obtained after centrifugalization are dried, smashed and screened, and O-carboxymethyl chitosan is obtained.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical processing technology, in particular to an industrial preparation method of O-carboxymethyl chitosan. Background technique [0002] O-carboxymethyl chitosan, also known as O-carboxymethyl chitosan sodium, English name Carboxymethyl Chitosan, molecular structure formula is: [0003] [0004] O-carboxymethyl chitosan is a water-soluble chitosan derivative, which is the product of carboxymethylated chitosan. Because it not only retains the advantages of chitosan, but also greatly improves the water solubility, it is of great significance in medicine, chemical industry, environmental protection, and health care products. And its stable properties and pharmacological effects such as antibacterial and anti-infection, lipid-lowering and prevention and treatment of arteriosclerosis will make it play a greater role in the daily life of human beings in the future. [0005] Carboxymethyl chitosan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
CPCC08B37/003
Inventor 詹小远张福明金仙花
Owner 浙江澳兴生物科技有限公司
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