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Preparation method of O-hydroxypropyl-N-alkylated chitosan surfactant

A technology of surfactant and chitosan, which is applied in chemical instruments and methods, chemical/physical processes, transportation and packaging, etc., can solve the problems of single product and lack of system, achieve good surface activity and save reaction raw materials and the effect of time

Inactive Publication Date: 2011-05-11
BIOCHEM ENG COLLEGE OF BEIJING UNION UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sui Weiping and others have synthesized derivatives with surface activity by modifying chitosan, but their products are single and lack systematic

Method used

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  • Preparation method of O-hydroxypropyl-N-alkylated chitosan surfactant
  • Preparation method of O-hydroxypropyl-N-alkylated chitosan surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2g of chitosan into 5mL of 33wt% NaOH and soak for 2 hours and then freeze-dry; mix the dried alkaline chitosan with 20mL of isopropanol and stir for 30min, add 1mL of catalyst tetramethylammonium hydroxide and 20mL of propylene oxide After stirring at room temperature for 60 minutes, the temperature was raised to 60°C for 8 hours (the molar ratio of chitosan, catalyst, isopropanol and propylene oxide = 1:0.5:22:24); the precipitation was allowed to settle, the upper solvent was decanted, and 20mL distilled water was added (The molar ratio of chitosan and distilled water = 1:95) Stir until it is completely dissolved, centrifuge at 4000r / min for 10min, take the supernatant and spin-evaporate at 80℃, remove the remaining isopropanol and propylene oxide, and finally get a purer An aqueous solution of alkaline O-hydroxypropyl chitosan. The preparation method of O-hydroxypropyl chitosan in Example 2 is the same as this.

[0020] The aqueous solution of O-hydroxypropyl chi...

Embodiment 2

[0022] According to the method described in Example 1, O-hydroxypropyl chitosan was obtained.

[0023] Stir the aqueous solution of O-hydroxypropyl chitosan at 40°C for 30 minutes, add 5 mL of hexadecyl bromide dropwise and increase the temperature to 80°C, add 0.06 g of cetyltrimethylammonium bromide, and stir for 8 hours. (The molar ratio of chitosan, hexadecane bromide and phase transfer catalyst = 1:1.4:0.014), cool after the reaction, and neutralize with dilute hydrochloric acid to pH 7 under stirring; add 60 mL of acetone to the reactor to cause precipitation After the precipitation no longer increases, suction filter, wash the filter cake with methanol-water (volume ratio 85:15), absolute ethanol, and dry 1.02g of white or yellow solid. The measured HLB value is 5.33, the critical glue The surface tension of the aqueous solution at a beam concentration of 0.18g / L is 24.81mN / m; it is easy to foam and has good foam stability. The infrared spectrum is measured as figure 1 A...

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Abstract

The invention discloses a preparation method of an O-hydroxypropyl-N-alkylated chitosan surfactant, which comprises the following steps: by using chitosan as the raw material, carrying out etherification with propylene oxide to obtain hydrophilic O-hydroxypropyl chitosan; and carrying out alkylation on 2-NH2 by respectively using alkylogens with different lengths of carbon chains to prepare serial O-hydroxypropyl-N-alkylated chitosan derivatives, so that the serial O-hydroxypropyl-N-alkylated chitosan derivatives have basic properties of a surfactant. The invention completes the original two chitosan modification methods by using a one-step method, omits the intermediate steps of neutralization, drying and the like, saves the reaction material and time, and synthesizes the required serial new products without introducing any unnecessary impurity. The product prepared by the method can be used as an emulsifier, wetting agent, washing agent or the like.

Description

Technical field [0001] The invention relates to the field of polymer surfactants, and more specifically, to a preparation method of O-hydroxypropyl-N-alkylated chitosan series surfactants. Background technique [0002] Polymer surfactant refers to the molecular weight reaching a certain level (generally 10 3 ~10 6 ) A polymer compound with surface active function, composed of a hydrophilic part and a hydrophobic part. Compared with low-molecular-weight surfactants, it has the advantages of high solution viscosity and good film-forming properties, but its disadvantage is that it has poor surface tension reduction ability, and its surface activity decreases sharply with the increase in molecular weight. Surface activity, that is, the property of reducing the surface tension of the solution, is the most basic and most important property of surfactants. It is closely related to emulsification, solubilization, foaming, wetting and other functions, and is the basic index for investiga...

Claims

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Application Information

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IPC IPC(8): C08B37/08B01F17/56C09K23/56
Inventor 林强韩永萍王旭颖
Owner BIOCHEM ENG COLLEGE OF BEIJING UNION UNIV
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