Preparation method of ethyl cellulose nano micelle with UCST (upper critical solution temperature)

A technology of ethyl cellulose and nano micelles, which is applied in the fields of polymer materials and biomedical engineering, can solve problems such as single function and poor solubility, and achieve the effects of wide sources and simple and easy synthesis methods.

Inactive Publication Date: 2015-09-02
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethyl cellulose (EC) is a cellulose derivative in which the unresponsible hydroxyl group in cellulose is replaced by an ethoxy group. It is one of the most widely used water-insoluble cellulose derivatives, but its function is relatively simple and its solubility is relatively low. Poor, so in order to meet higher application requirements, it needs to be modified by physical and chemical methods to expand its function in the biomedical field

Method used

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  • Preparation method of ethyl cellulose nano micelle with UCST (upper critical solution temperature)
  • Preparation method of ethyl cellulose nano micelle with UCST (upper critical solution temperature)
  • Preparation method of ethyl cellulose nano micelle with UCST (upper critical solution temperature)

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Experimental program
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Effect test

Embodiment 1

[0030] Weigh 1.214 grams of ethyl cellulose in a round-bottomed flask, disperse and dissolve it with fresh anhydrous xylene, add 12.16 grams of ε-caprolactone, and then add 132 μL of stannous isooctanoate, and vacuum-fill with nitrogen 3 times, and reacted in an oil bath at 60°C for 12 hours under the protection of nitrogen, dissolved the obtained product in an appropriate amount of dichloromethane, then precipitated, filtered with suction, and dried in vacuum to obtain a macromolecular polymer whose main chain is ethyl cellulose substance (EC- g -PCL). Weigh the macromolecular polymer (EC- g -PCL) 3 g was dissolved in dichloromethane distilled to remove water, added 0.5 g of triethylamine distilled to remove water, the mixture was placed in an ice-water bath, 1.14 g of 2-bromoisobutyryl bromide was added dropwise to the mixture, and After that, the reaction was stirred at room temperature for 24h, and the products were respectively washed with saturated NaHCO 3 Aqueous sol...

Embodiment 2

[0032] Weigh 1.214 grams of ethyl cellulose in a round-bottomed flask, disperse and dissolve it with newly prepared anhydrous toluene, add 18.24 grams of ε-caprolactone, and then add 140 μl of stannous octoate. And under the protection of nitrogen, it was reacted in an oil bath at 80°C for 24 hours, and the obtained product was dissolved in an appropriate amount of chloroform, and then precipitated, filtered by suction, and dried in vacuum to obtain a macromolecular polymer (EC - g -PCL). Weigh the macromolecular polymer (EC- g -PCL) 3 g was dissolved in dichloromethane distilled to remove water, added 0.5 g of triethylamine distilled to remove water, the mixture was placed in an ice-water bath, 1.14 g of 2-bromoisobutyryl bromide was added dropwise to the mixture, and After that, the reaction was stirred at room temperature for 24h, and the products were respectively washed with saturated NaHCO 3 Aqueous solution and distilled water washing, carry out concentration again, ...

Embodiment 3

[0034] Weigh 1.214 grams of ethyl cellulose in a round-bottomed flask, disperse and dissolve it with newly prepared anhydrous dimethyl sulfoxide, add 12.16 grams of ε-caprolactone, and then add 156 μL of hydrogen chloride ether solution, and vacuum-fill Nitrogen process was carried out 3 times, and reacted in an oil bath at 100°C for 32 hours under the protection of nitrogen. The obtained product was dissolved in an appropriate amount of 1,2-dichloroethane, and then precipitated, filtered by suction, and dried in vacuum to obtain the main chain as B Cellulose-based macromolecular polymers (EC- g -PCL). Weigh the macromolecular polymer (EC- g -PCL) 3 g was dissolved in dichloromethane distilled to remove water, added 0.5 g of triethylamine distilled to remove water, the mixture was placed in an ice-water bath, 1.14 g of 2-bromoisobutyryl bromide was added dropwise to the mixture, and After that, the reaction was stirred at room temperature for 24h, and the products were respe...

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Abstract

The invention relates to a preparation method of an ethyl cellulose nano micelle with UCST (upper critical solution temperature). The preparation method comprises the following steps: in an inert gas protective atmosphere, carrying out ring-opening polymerization on the hydroxy group in the ethyl cellulose main chain and caprolactone to obtain a high-molecular graft copolymer, carrying out bromination reaction on the high-molecular polymer to obtain an atom transfer free-radical polymerization high-molecular initiator, carrying out atom transfer free-radical polymerization on N,N-dimethylaminoethyl methacrylate under the initiation action of cuprous bromide, carrying out complete quaterization reaction on the obtained polymer to obtain a graft-block copolymer with UCST temperature responsiveness by using ethyl cellulose as the main chain, and dissolving the graft-block copolymer in water to form the stable nano micelle with UCST temperature responsiveness. The ethyl cellulose nano micelle is biocompatible, bioactive and temperature-responsive, and can be widely used in the fields of drug controlled release carriers, biological intelligent switches, biosensors and the like. The preparation method is simple and easy to implement, can implement industrial production on the raw materials, and has favorable popularization and application value.

Description

technical field [0001] The invention belongs to the fields of polymer materials and biomedical engineering, and in particular relates to a preparation method of ethyl cellulose nano micelles with UCST. Background technique [0002] Ethyl cellulose is one of the most abundant natural biopolymer materials with the most abundant reserves in nature. It has excellent biocompatibility, biodegradability and renewability. The modification of cellulose and its graft copolymerization derivatives can effectively change the physical and chemical properties of cellulose. Ethyl cellulose (EC) is a cellulose derivative in which the unresponsible hydroxyl group in cellulose is replaced by an ethoxy group. It is one of the most widely used water-insoluble cellulose derivatives, but its function is relatively simple and its solubility is relatively low. Therefore, in order to meet higher application requirements, it is necessary to modify it by physical and chemical methods to expand its fun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/02C08F220/34
Inventor 迟海袁伟忠
Owner TONGJI UNIV
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