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Microwave synthesis method for disproportionated rosin amine quaternary ammonium type cation cassava starch

A technology of rosin amine-based quaternary ammonium and disproportionated rosin amine, which is applied in the field of preparation of hydrophobic modified starch, can solve the problems that the synthesis method has not been reported at home and abroad, and achieve the effects of low price, low production cost and improved solubility

Inactive Publication Date: 2009-04-15
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Disproportionated rosin-based quaternary ammonium cationic tapioca starch is a new type of hydrophobic cationic starch. The substance and its synthesis method have not been reported at home and abroad so far.

Method used

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  • Microwave synthesis method for disproportionated rosin amine quaternary ammonium type cation cassava starch
  • Microwave synthesis method for disproportionated rosin amine quaternary ammonium type cation cassava starch
  • Microwave synthesis method for disproportionated rosin amine quaternary ammonium type cation cassava starch

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Embodiment 1

[0048] The microwave synthesis method of the disproportionated rosin amino group quaternary ammonium type cationic tapioca starch of the present invention comprises the following steps:

[0049] (1) Synthesis of N, N-dimethyl disproportionated rosin amine

[0050] In a three-necked flask, add 40 g of disproportionated abietamine and 52 mL of absolute ethanol, and dropwise add 32 mL of 88% (mass percent) formic acid, and control the reaction temperature below 40° C., and drop it in about 15 minutes. Maintaining the temperature, 32 mL of 38.5% (mass percent) formaldehyde was added dropwise, and the drop was completed in about 20 minutes. Raise the temperature, stir and reflux at 65-70°C for 3 hours, at this time, the reaction liquid is proved to be free of primary amines through qualitative detection. Reclaim ethanol after heating up to 80 ℃ of reflux reaction 1h again, after completion of reaction, adjust pH to 13 with 30mL 30% (mass percentage) NaOH solution, then reactant is...

Embodiment 2

[0057] (1) Synthetic N, N-dimethyl disproportionated abietamine with embodiment 1 (1)

[0058] (2) Synthesis of cationic etherification agent dimethylglycidyl disproportionated abietyl ammonium chloride

[0059] The N,N-dimethyl disproportionated rosin amine prepared above and epichlorohydrin are fed into a weight / volume ratio of 1:2, heated and stirred, and refluxed for 8 hours, and the excess epichlorohydrin was removed by distillation under reduced pressure. Petroleum ether was washed three times (30mL×3) to obtain a brown viscous novel cationic etherification agent, dimethylglycidyl disproportionated abietyl ammonium chloride, with a yield of 96.6%.

[0060] (3) Microwave synthesis of disproportionated rosin-based quaternary ammonium cationic tapioca starch

[0061] Dry tapioca starch and isopropanol are fed in a weight / volume ratio of 1:16, and magnetic stirring is used to disperse the starch evenly. Then slowly add 12.5mL of NaOH solution (the content of NaOH is 0.4g) ...

Embodiment 3

[0064] (1) Synthetic N, N-dimethyl disproportionated abietamine with embodiment 1 (1)

[0065] (2) Synthesis of cationic etherification agent dimethylglycidyl disproportionated abietyl ammonium chloride

[0066] The N,N-dimethyl disproportionated rosin amine and epichlorohydrin prepared above are fed in a weight / volume ratio of 1:2, heated and stirred, and refluxed for 16 hours, and the excess epichlorohydrin was removed by distillation under reduced pressure. Petroleum ether was washed three times (30mL×3) to obtain a brown viscous novel cationic etherification agent dimethylglycidyl disproportionated abietyl ammonium chloride with a yield of 97.3%.

[0067] (3) Microwave synthesis of disproportionated rosin-based quaternary ammonium cationic tapioca starch

[0068] Dry tapioca starch and isopropanol are fed in a weight / volume ratio of 1:16, and magnetic stirring is used to disperse the starch evenly. Then slowly add 10 mL of NaOH solution (NaOH content is 0.8 g) under stir...

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Abstract

The invention relates to a microwave synthesis method of disproportionation abietyl amine quaternary ammonium type positive ion tapioca, which uses disproportionation abietyl amine and tapioca as raw materials, and N, N- dimethyl disproportionation abietyl amine is obtained by the disproportionation abietyl amine through using a formaldehyde-formic acid method, and then reaction with epichlorohydrin is carried out for producing intermediate positive ion etherifying agent chloridization dimethyl glycydyl disproportionation abietyl amine, and under the microwave radiation, by using the mixed solution of isopropyl alcohol and water as a reaction solvent, the disproportionation abietyl amine quaternary ammonium type positive ion tapioca can be obtained by carrying out the etherification reaction with the tapioca. Compared with the existing positive ion starch, the novel positive ion starch prepared by the method enhances the hydrophobic property and lipophilicity, thus expanding the application range of the positive ion starch.

Description

technical field [0001] The invention relates to a preparation method of hydrophobic modified starch, in particular to a microwave synthesis method of disproportionated rosin-based quaternary ammonium cationic tapioca starch. Background technique [0002] Starch is a polysaccharide with D-glucose as the basic unit. The molecule contains a large number of active hydroxyl groups. It can be chemically modified by esterification, etherification, carboxylation and graft copolymerization to prepare a variety of Starch derivatives. The preparation of these derivatives can improve the solubility of starch on the one hand, and more importantly, the introduction of different substituents can endow starch with more functions and make it more widely used in the national economy. Cationic starch is a very important class of starch ether derivatives, which are prepared by reacting starch with cationic etherifying agents under certain conditions. Cationic starch is used as wet cloth addit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B31/12
Inventor 段文贵方华祥许苒妮岑波
Owner GUANGXI UNIV
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