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Preparation method of carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch

A technology of tapioca starch and carboxylic acid anhydride ester is applied in the field of polymer materials, which can solve the problems of poor solubility, long wet production cycle, and insufficient uniformity of the system, and achieves good water solubility and stability, good physical and chemical activity, and monomer conversion. high rate effect

Inactive Publication Date: 2018-01-05
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the wet process is simple and mature, and has been widely used in industrial production, such as the preparation of acetylated starch esters with acetic anhydride and propylene oxide, but the wet process has long production cycles, high energy consumption, more post-processing, and waste liquid. big pollution
Amphoteric starch prepared by dry method of phosphate and hydroxypropyl starch can be used as stabilizer and thickener, but the dry reaction system is usually not uniform enough, the product particle size is large, and the solubility is poor
Studies have found that the functional groups of phthalic anhydride and 3-chloro-2-hydroxypropyltrimethylammonium chloride (3-Chloro-2-Hydroxy-Propyl-Trimethyl AmmouniumChloride, CHPTMA) have strong ionicity and are , emulsification, and shear resistance, etc., and the research on the preparation of amphoteric starch by esterification with acid anhydride in anion modification is rarely reported in the literature.

Method used

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  • Preparation method of carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch
  • Preparation method of carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch
  • Preparation method of carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Dry 6.0 g of tapioca starch in a vacuum oven at 50° C. for 24 hours to constant weight to obtain tapioca starch on a dry basis.

[0035] (2) Weigh 5 g of tapioca starch obtained in step (1) on a dry basis and add 15 mL of distilled water into a 250 mL four-necked flask, and stir evenly for 10 to 20 minutes to form a starch emulsion with a mass fraction of 25%.

[0036] (3) measure 10mL mass fraction and be 15% sodium hydroxide solution, join in the starch emulsion of step (2) gained in 20 minutes, be warming up to 35 ℃ and activate 25 minutes, obtain activated tapioca starch emulsion.

[0037] (4) Weigh 2.4g trimethylamine and 1.5g epichlorohydrin in a 50mL beaker, stir evenly, add 6mL hydrochloric acid solution with a mass fraction of 35%, and react at room temperature for 2 hours to obtain etherifying agent CHPTMA solution.

[0038] (5) Transfer the etherification agent CHPTMA solution obtained in step (4) to a constant pressure dropping funnel, and drop it into t...

Embodiment 2

[0044] (1) Dry 12.0 g of tapioca starch in a vacuum oven at 50° C. for 24 hours to constant weight to obtain tapioca starch on a dry basis.

[0045] (2) Weigh 10.77g of dry base tapioca starch obtained in step (1) and 20mL of distilled water into a 250mL four-necked flask, and stir evenly for 20 minutes to form a starch emulsion with a mass fraction of 35%.

[0046](3) measure 15mL mass fraction and be 15% sodium hydroxide solution, join in step (2) gained starch emulsion in 20 minutes, be warming up to 40 ℃ and activate 25 minutes, obtain activated tapioca starch emulsion.

[0047] (4) Weigh 7.2g of trimethylamine and 4.2g of epichlorohydrin in a 250mL four-necked flask, stir well, add 10mL of hydrochloric acid solution with a mass fraction of 35%, and react at room temperature for 3 hours to obtain the etherification agent CHPTMA solution.

[0048] (5) Transfer the etherification agent CHPTMA solution obtained in step (4) to a constant pressure dropping funnel, and drop it ...

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Abstract

The invention discloses a preparation method of carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch. Cassava starch is used as a main raw material, 3-chloro-2-hydroxy-propyl-trimethyl ammonium chloride produced by a reaction of trimethylamine and epichlorohydrin in the condition that water is used as solvent is used as cationic reagent, phthalic anhydride is used as anionic reagent, cationization and anionization reactions are carried out by means of a one-pot reaction under the catalysis of ZSM-5 molecular sieve, and then the carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch is synthesized through the steps of extraction filtration, washing, drying and the like. According to the method, the technological reactionconditions are mild, the reaction efficiency is high, and it is unnecessary to separate and purify intermediate products. The product is high in substitution degree, good in water solubility and goodin stability, has various good properties of cationization and esterification starch, and has high application value in the fields of environmental protection, paper making, functional materials and the like.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of carboxylic acid anhydride esterification-CHPTMA etherification amphoteric cassava starch. Background technique [0002] Starch is a renewable biomass resource in nature and a raw material with superior performance. With the rapid development of industrial technology, starch derivative products with multiple functions have emerged. For example, amphoteric starch is a starch derivative obtained from raw starch through physical, chemical or enzymatic methods. It has anion, cationic starch and high Multiple properties of molecular polymers. [0003] At present, in related research and technology at home and abroad, dry or wet processes are often used to introduce anion and cationic groups into the starch skeleton through esterification and etherification for compound modification. Among them, the wet process is simple and mature, and has been widel...

Claims

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Application Information

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IPC IPC(8): C08B31/16
Inventor 李和平胡英相张淑芬冯璇龚俊张俊杨莹莹左凯钱敬侠杨世军
Owner GUILIN UNIVERSITY OF TECHNOLOGY