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Process for preparing carboxymethyl chitosan and its application

A technology of carboxymethyl chitosan and chitin, which is applied in the direction of pharmaceutical formulations, medical preparations containing active ingredients, digestive system, etc., can solve the problems of large amount of alkali consumption, long reaction time, and many intermediate steps, and achieve Reduce production costs, reduce pollution hazards, and improve product quality

Inactive Publication Date: 2005-06-22
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of these methods are: (1) The raw material chitosan is a product obtained by deacetylating chitin in 40-50% NaOH solution, separating, washing and drying, and carboxymethyl shell is prepared from chitosan Polysaccharides need to be alkalized in concentrated lye to carry out carboxylation reaction
So before and after two times of soaking in alkali, not only the amount of alkali used is large, the operation is troublesome, there are many intermediate steps, the reaction time is long, the pollution of waste water discharge is serious, and the chitosan molecular chain degradation is serious after the concentrated alkali treatment, and the product viscosity is greatly reduced; 2) Isopropanol and n-butanol reaction medium are costly and highly toxic

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Measure 80-100ml of 95% ethanol and pour it into a three-neck bottle with a stopper, add 12.5-17.5g of NaOH and 5g of chitin, stir in a constant temperature water bath at 90°C, reflux for 2 hours, cool to obtain an alkaline chitosan suspension liquid. Then, to prevent overheating, add 10-20g of monochloroacetic acid in 3-5 times, add time at intervals of about 10min each time, stir at 40-50°C, reflux for 3h, centrifuge to separate the solid precipitate after cooling, and use 70-80% ethanol Wash the precipitate until there is no chloride ion in the washing liquid, and dry in vacuum to obtain the crude product of carboxymethyl chitosan. Dissolve the crude product in 100ml of deionized water, filter to remove insoluble matter, concentrate in a rotary evaporator, add 95% ethanol to the concentrated solution to precipitate a white flocculent precipitate, then use absolute ethanol or acetone to completely remove the water, squeeze dry , vacuum dried. The recovery rate of th...

Embodiment 2

[0013] Pour 80-100L of 95% ethanol into a jacketed reactor with a reflux device, add 12.5-17.5kg of NaOH and 5kg of chitin, heat with steam under temperature control, stir, reflux for 2 hours, and cool to obtain an alkaline chitosan suspension , and then add 10-2.kg monochloroacetic acid 5 times to prevent overheating, with an interval of about 10 minutes each time, stir at 40-50°C, reflux for 3 hours, centrifuge to separate the solid precipitate after cooling, and wash the precipitate with 70-80% ethanol , until there is no chloride ion in the washing solution, and vacuum-dried to obtain a crude product of carboxymethyl chitosan. Dissolve the crude product in 100L deionized water, filter to remove insoluble matter, concentrate in a rotary evaporator, add 95% ethanol to the concentrated solution to precipitate a white flocculent precipitate, then use absolute ethanol or acetone to completely remove the water, squeeze dry , vacuum dried. The recovery rate of the product is 110...

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PUM

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Abstract

The invention provides a process for preparing carboxymethyl chitosan which comprises, using chitosan as raw material, 95% of ethanol as medium, immersing into low concentration alkali in one time, keeping constant temperature at 80-95 deg. C, stirring and reversing flow for 1.5-3.0 hrs, charing monochloroacetic acid in 3-7 times, stiring 2-20h at 40-50 deg. C and reversing flow 2-4h, washing, depositing and drying. The preferred weight proportion range of the chitosan, alkali, monochloroacetic acid and ethanol is 1 : 2.5-3.5 : 2-4 : 16-20. The prepared nano nano film has good effect.

Description

technical field [0001] The invention relates to a method for preparing carboxymethyl chitosan and its application in preparing nanofiltration membrane and medicine for treating gastric acid disease. Background technique [0002] Carboxymethyl chitosan is an important water-soluble chitin derivative, which can be used as cosmetic moisturizer, fruit and vegetable fresh-keeping agent, plant growth promoter, flocculant in water treatment and various pharmaceutical adjuvants. Most of the existing methods for preparing carboxymethyl chitosan use chitosan as a raw material, using the glyoxylic acid method, the chloroacetic acid method, and the combined use of chloroacetic acid and glyoxylic acid. The glyoxylic acid method is to dissolve an appropriate amount of chitosan in 10% glyoxylic acid aqueous solution, stir at 60°C for 4 hours to obtain Shiff base, adjust the pH to 6 with 2mol / L NaOH solution, and then add an appropriate amount of Sodium cyanoborohydride (NaCNBH 3 ), stirr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K31/722A61P1/04C08B37/08
Inventor 陈国华刘长霞晋治涛孙明昆高从堦
Owner OCEAN UNIV OF CHINA
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