Method for preparing hyper branched polyrotaxane based on cyclodextrin

A technology of cyclodextrin and polyrotaxane, which is applied in the field of preparation of hyperbranched polyrotaxane, and achieves the effects of simple preparation, high yield and easy structure adjustment

Inactive Publication Date: 2008-03-12
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In polymers, hyperbranched polymers are a new type of important polymers, and polyrotaxanes with hyperbranched structures have not been reported so far

Method used

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  • Method for preparing hyper branched polyrotaxane based on cyclodextrin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step a: Add 20 milliliters of deionized water to a 100 milliliter reaction flask, then add 1.297 grams of gamma-cyclodextrin to dissolve it, then add 0.1292 grams of 1-(2-aminoethyl) piperazine, at 70 degrees Celsius Stirred under conditions for 5 hours, cooled naturally to obtain a light yellow solution.

[0025] Step b: Add 0.1182 g of divinyl sulfone to the small molecule solution obtained above, seal it with an inversion plug, blow nitrogen for 10-15 minutes to remove the air, seal it well, stir at room temperature for 3-5 minutes, and then heat to 40 Stirring was continued for 120 hours at °C.

[0026] Step c: Add 20 ml of petroleum ether into the reaction bottle after the reaction, and continue stirring at room temperature for about 3-5 hours to obtain a cloudy solution. The precipitate was removed by centrifugation to obtain a clear biphasic solution. The upper layer is excess petroleum ether, and the lower layer is light yellow aqueous solution of hyperbranche...

Embodiment 2

[0028] Step a: Add 20 ml of deionized water to a 100 ml reaction flask, then add 0.0045 g of β-cyclodextrin to dissolve it, then add 0.1162 g of hexamethylenediamine, stir at 70 degrees Celsius for 5 hours, and cool naturally to obtain Pale yellow solution.

[0029] Step b: Add 0.1542 g of methylene bisacrylamide to the small molecule solution obtained above, seal it with an inversion plug, blow nitrogen for 10-15 minutes to remove the air, seal it well, stir at room temperature for 3-5 minutes, and then heat Stirring was continued for 120 hours at 40°C.

[0030] Step c: Add 20 ml of petroleum ether into the reaction bottle after the reaction, and continue stirring at room temperature for about 3-5 hours to obtain a cloudy solution. The precipitate was removed by centrifugation to obtain a clear biphasic solution. The upper layer is excess petroleum ether, and the lower layer is light yellow aqueous solution of hyperbranched polyrotaxane. The excess petroleum ether was remo...

Embodiment 3

[0032] Step a: Add 20 ml of deionized water to a 100 ml reaction flask, then add 0.4635 g of α-cyclodextrin, then add 0.1292 g of 1-(2-aminoethyl)piperazine, and stir at 70 degrees Celsius After 5 hours, cool naturally to obtain a light yellow solution.

[0033] Step b: Add 0.1542 g of methylene bisacrylamide to the small molecule solution obtained above, seal it with an inversion plug, blow nitrogen for 10-15 minutes to remove the air, seal it well, stir at room temperature for 3-5 minutes, and then heat Stirring was continued for 120 hours at 40°C.

[0034] Step c: Add 20 ml of petroleum ether into the reaction bottle after the reaction, and continue stirring at room temperature for about 3-5 hours to obtain a cloudy solution. The precipitate was removed by centrifugation to obtain a clear biphasic solution. The upper layer is excess petroleum ether, and the lower layer is light yellow aqueous solution of hyperbranched polyrotaxane. The excess petroleum ether was removed ...

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Abstract

The present invention discloses a preparation method for cyclodextrin-based hyperbranched poly-rotaxane in the chemical technology field. The present invention takes use of a ''composition fist and polymerization after'' approach to combine the main polyamines monomer with the cyclodextrin in the water and then the product is added with Maikeer addition reagent for polymerization. Petroleum ether is added to get rid of deposit generated in the composition process of the free cyclodextrin. And the product is liquid-separated, cooled and dried to get hyperbranched poly-rotaxane. The hyperbranched poly-rotaxane is of a plurality of cyclodextrins. Each cyclodextrin molecule is locked by the branched point of the hyperbranched polymer to prevent the falling off of the cyclodextrin molecule. The proportion of the cyclodextrin on the polymer chain can be controlled through the adjustment of the amount of cyclodextrin. The hyperbranched poly-rotaxane is of a novel hyper-molecular structure, and can be taken as the basis for the design of other hyper-molecular system as the molecular machine. The present invention can be used in drug control release field, biological sensor field and so on.

Description

technical field [0001] The invention relates to a method in the technical field of chemical engineering, in particular to a method for preparing cyclodextrin-based hyperbranched polyrotaxanes. Background technique [0002] Rotaxanes are a kind of interlocking supramolecular system formed by a cyclic molecule wrapped around a dumbbell-shaped linear molecule. If it contains multiple cyclic molecules, it becomes a polyrotaxane. Polyrotaxane is a new type of supramolecular structure, and this kind of supramolecular inclusion complex is an effective model to study the interaction and properties between biological entities. New smart materials and molecular devices developed on this basis also have important application prospects. In addition, this system has also been used in the research of biodegradable materials, drug carriers and release, molecular recognition, chemical sensors, polymer separation and molecular simulation, and has great application prospects. [0003] Acco...

Claims

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Application Information

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IPC IPC(8): C08B37/16C08K5/36C08K5/3462C08K5/17C08K5/20C08K5/10
CPCY02P20/582
Inventor 万会师朱新远陈亮颜德岳
Owner SHANGHAI JIAO TONG UNIV
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