A kind of preparation method of trimethylsilyl starch ether

A technology of trimethylsilyl and starch ether, which is applied in the field of preparation of trimethylsilyl starch ether, and achieves the effects of simple operation process, mild reaction conditions and good solubility

Active Publication Date: 2018-11-09
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And take copper salt as catalyst to catalyze starch and hexamethyldisilazane generation etherification reaction to prepare the method for silicon-etherified starch no report

Method used

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  • A kind of preparation method of trimethylsilyl starch ether
  • A kind of preparation method of trimethylsilyl starch ether
  • A kind of preparation method of trimethylsilyl starch ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Get the waxy corn starch of 10g, add the DMF of 100ml as solvent, according to n(Cu(NO 3 ) 2 ·3H 2 O):n(HMDS)=2.1:100, add Cu(NO 3 ) 2 ·3H 2 O as a catalyst, 50W ultrasonic dispersion into a homogeneous system, at 50°C, add HMDS dropwise according to n(HMDS):n(AGU)=3:1, stir magnetically, sample the gas phase every half an hour to analyze the HMDS content, gas phase The end point of the reaction was determined by chromatography. After 7 hours of reaction, the conversion rate of HMDS was 100%. After the reaction, the product was cooled to room temperature, the upper solvent was poured out, and ethanol and deionized water were poured into the lower product to precipitate the product, then suction filtered, and vacuum-dried at 90°C to obtain the crude product of trimethylsilyl starch ether . Grinding the crude product of trimethylsilyl starch, dissolving it in acetone, centrifuging to obtain a supernatant, concentrating the supernatant, adding a large amount of deion...

Embodiment 2

[0033] Get the waxy corn starch of 10g, add the DMF of 100ml as solvent, according to n(Cu(NO 3 ) 2 ·3H 2 O): n(HMDS)=2.1% add Cu(NO 3 ) 2 ·3H 2O as a catalyst, 50W ultrasonic dispersion into a homogeneous system, at 80 ° C, according to n (HMDS) and n (AGU) = 3:1, add HMDS dropwise, magnetic stirring, sampling the gas phase every half an hour to analyze the HMDS content, gas phase The end point of the reaction was determined by chromatography. After 2 hours of reaction, the conversion rate of HMDS was 100%. After the reaction, the product was cooled to room temperature, the upper layer solvent was poured out, and a large amount of ethanol and deionized water were poured into the lower layer product to precipitate the product, which was then filtered by suction and vacuum-dried at 90°C to obtain crude trimethylsilyl starch ether. product. After grinding the crude product of trimethylsilyl starch, dissolve it in acetone, centrifuge to obtain a supernatant, concentrate the...

Embodiment 3～4

[0038] Add HMDS dropwise according to the ratio of n(HMDS) and n(AGU)=1:1 and 2:1, other conditions are consistent with Example 1, and the products with degrees of substitution of 0.84 and 1.63 are obtained, and the yields are 84% and 81.5% respectively. %.

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Abstract

Provided is a method for preparing trimethyl silica-based starch ether. Copper salt is adopted as a catalyst. 1,1,1,3,3,3-hexamethyldisilazane is adopted as an organosilicone etherifying agent. Silica-based hydrophobization modification of starch is carried out in an organic solvent, and the substitution degree of obtained trimethyl silica-based starch ether ranges from 0.83 to 2.68. According to the method, reaction conditions are mild, the operation process is simple, the substitution degree is controllable, the obtained product has very good solubleness in the organic solvent, and high hydrophobicity is achieved.

Description

technical field [0001] The invention relates to a preparation method of trimethylsilyl starch ether. Background technique [0002] Starch has attracted increasing attention due to its advantages of wide sources, low price, non-toxicity and good biodegradability. Hydrophobic modification of starch can destroy the intermolecular hydrogen bonds between the crystalline and non-crystalline regions of starch, making it change from hydrophilic to hydrophobic, greatly improving its stability in THF, acetone, CHCl 3 Solubility in. The usual starch hydrophobizing modification groups use various halogenated hydrocarbon groups. The carbon atoms connected to the halogen atoms are easy to undergo substitution reactions with hydroxyl groups, and hydrocarbon groups connected by ether bonds are introduced into the starch molecules. The reaction conditions of starch hydroxyl groups and halogenated hydrocarbons are relatively high, and the reaction efficiency is low; its hydrophobicity is af...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/00
CPCC08B31/00
Inventor 张淑芬唐炳涛具本植武素丽牛文斌
Owner DALIAN UNIV OF TECH
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