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Preparation of carboxymethyl chitosan quaternary ammonium p-toluenesulfonate

A technology of quaternary amine methylbenzenesulfonate and carboxymethyl chitosan is applied in the field of preparation of carboxymethyl chitosan p-toluenesulfonic acid quaternary amine salt, and can solve the problems of non-regeneration, decreased adsorption performance and the like , to achieve the effect of stable scale-up production, reduced risk and toxicity, and easy scale-up production

Inactive Publication Date: 2009-08-12
STATE GRID CORP OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of preparation method of carboxymethyl chitosan p-toluenesulfonic acid quaternary ammonium salt, this preparation method has gentle reaction, simple condition, stable and easy to enlarge production, solves the problem of adsorption due to degradation in water Degraded performance and non-reproducible issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] 1. Construction of reaction system

[0011] Under the protection of nitrogen, 8.53 grams of potassium carbonate and 90 grams of industrial acetonitrile were added to a 0.5-liter clean and water-free four-necked bottle. After stirring for 5 minutes, 12.56 grams of liquid methyl p-toluenesulfonate was added, and 10 grams of acetonitrile Wash the mouth of the bottle. Stir for 5 minutes and control the temperature to 15°C.

[0012] 2. The process of the reaction

[0013] Add dropwise the mixed solution of acetonitrile containing 3.7 g of carboxymethyl chitosan (approximately 0.5 hour). Stir for another 5 minutes, raise the temperature to 83° C. and reflux vigorously to react, turn off the nitrogen gas when reflux occurs, and react for 22 hours.

[0014] 3. Extraction and purification of carboxymethyl chitosan p-toluenesulfonate

[0015] After the reaction is completed, cool down to 10°C, and then perform suction filtration. The filter cake is beaten with 50 grams of ace...

Embodiment 2

[0017] 1. Construction of reaction system

[0018] Under the protection of nitrogen, 17.06 grams of potassium carbonate and 180 grams of industrial acetonitrile were added to a 1-liter clean and water-free four-necked bottle. After stirring for 5 minutes, 25.12 grams of liquid methyl p-toluenesulfonate was added, and 20 grams of acetonitrile Wash the mouth of the bottle. Stir for 5 minutes and control the temperature to 18°C.

[0019] 2. The process of the reaction

[0020] Add dropwise the mixed solution of acetonitrile containing 7.4 g of carboxymethyl chitosan (approximately 0.5 hour). Stir for another 5 minutes, raise the temperature to 83° C. and reflux vigorously to react, turn off the nitrogen gas when reflux occurs, and react for 22 hours. 3. Extraction and purification of carboxymethyl chitosan p-toluenesulfonate

[0021] After the reaction is completed, cool down to 15°C, and then perform suction filtration. The filter cake is beaten with 100 grams of acetonitril...

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Abstract

The invention relates to a preparation method of p-toluene sulfonic acid quaternary amine of carboxymethyl chitosan, which is characterized by comprising the following steps of: under the protection of nitrogen, adding potassium carbonate, acetonitrile and methyl p-toluene sulfonic acid, controlling the temperature of 15 DEG C+3 DEG C, dripping acetonitrile solution of carboxymethyl chitosan, carrying out mechanical stirring for 5 minutes under room temperature, rising temperature to 83 DEG C, and carrying out violently backflow reaction for about 22 hours. The preparation method has the following advantages of having lower price and easy obtaining for reaction materials, mild reaction, simple condition, stability, easy production on scale and novel synthesis method, avoiding the use of highly toxic reagent of methyl iodide and dimethyl sulfate and the like, cleanness, environmental protection and greatly reducing hazard and toxicity; and the products has obvious leap in the properties of absorption and regeneration.

Description

technical field [0001] The invention relates to a preparation method of carboxymethyl chitosan p-toluenesulfonic acid quaternary ammonium salt. Background technique [0002] At present, researchers at home and abroad are doing a lot of research on the modification of chitosan to improve its water solubility and the application of modified chitosan. Carboxymethyl chitosan and chitosan-based quaternary ammonium salts have been studied more and have important effects on humans. [0003] Carboxymethyl chitosan has a certain water solubility and has important and far-reaching application value, such as using its adsorption properties for metal ions to treat industrial wastewater, using its chelation for ferrous ions to prepare blood supplements, and as an inhibitor Fertilizers with bactericidal functions, etc., but the research on the use of it to adsorb metal ions in industrial wastewater shows that the adsorption conditions are narrow and the adsorption efficiency is not high;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 谢宇胡金刚李明俊
Owner STATE GRID CORP OF CHINA
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