A preparation method of water-soluble filter paper cellulose micelles with photoresponsive properties

A cellulose and water-soluble technology, which is applied in the fields of polymer materials and biomedical engineering, can solve the problems of high chemical inertness and poor solubility, and achieve the effects of wide application prospects, solubility changes, and excellent stability

Active Publication Date: 2019-09-27
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the presence of a large number of intermolecular and intramolecular hydrogen bonds in the molecular structure of cellulose, it is insoluble in water and general organic solvents at room temperature, and has excellent chemical stability. It is widely used as a laboratory filter material, but it is extremely poor. The solubility and high chemical inertness also affect the application of cellulose in some fields such as biomedicine and chemical analysis.

Method used

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  • A preparation method of water-soluble filter paper cellulose micelles with photoresponsive properties
  • A preparation method of water-soluble filter paper cellulose micelles with photoresponsive properties
  • A preparation method of water-soluble filter paper cellulose micelles with photoresponsive properties

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Experimental program
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Effect test

Embodiment 1

[0019] Break 3g of cellulose filter paper into a pulp in tetrahydrofuran, add carboxyl-containing spiropyran with a mass ratio of 1:4 to the filter paper cellulose, and 4 -Dimethylaminopiperidine, and cooled to 0°C, then dropwise added dicyclohexylcarbodiimide solution dissolved in tetrahydrofuran at a molar ratio of 1.2:1 to carboxyl-containing spiropyran, and stirred at constant temperature for 2 hours, Continue to react for 48 hours at 25°C under the protection of nitrogen to complete; filter and wash; collect all the filtrate and distill under reduced pressure to obtain the crude product; after dissolving and filtering in ethanol, add a large amount of deionized water to the filtrate to filter to remove impurities to obtain a pink solid, after vacuum drying, Dissolve the obtained spiropyran modified filter paper cellulose in ethanol to configure a concentration of 3.8×10 -1 g / L solution, irradiate the prepared solution under 365nm ultraviolet light for 6 minutes. Then in ...

Embodiment 2

[0021] Break 3g of cellulose filter paper into pulp in dichloromethane, add carboxyl-containing spiropyran in a mass ratio of 1:3 to filter paper cellulose, and carboxyl-containing spiropyran in a molar ratio of 1:4 4-dimethylaminopiperidine, and cooled to 5°C, then dropwise added dicyclohexylcarbodiimide solution dissolved in dichloromethane with a molar ratio of 1.1:1 to carboxyl-containing spiropyran, and stirred at constant temperature After 2 hours, continue the reaction at 20°C under the protection of nitrogen for 24 hours; filter and wash; collect all the filtrate and distill under reduced pressure to obtain the crude product; after dissolving and filtering in ethanol, add a large amount of distilled water to the filtrate to filter to remove impurities to obtain a pink solid, and vacuum dry Finally, the obtained spiropyran-modified filter paper cellulose was dissolved in methanol to form a solution with a concentration of 1 g / L, and the prepared solution was irradiated w...

Embodiment 3

[0023] Break 3 g of cellulose filter paper into pulp in chloroform, add carboxyl-containing spiropyran in a mass ratio of 1:3 to filter paper cellulose, and 4 -Dimethylaminopiperidine, and cooled to 10°C, then dropwise added dicyclohexylcarbodiimide solution dissolved in chloroform with a molar ratio of 1.2:1 to carboxyl-containing spiropyran, and stirred at constant temperature for 3 hours, Continue to react for 48 hours at 25°C under the protection of nitrogen to complete; filter and wash; collect all the filtrate and distill under reduced pressure to obtain the crude product; after dissolving and filtering in methanol, add a large amount of distilled water to the filtrate and filter to remove impurities to obtain a pink solid, which will be obtained after vacuum drying. The spiropyran modified filter paper cellulose was dissolved in ethanol to form a concentration of 8×10 -1 g / L solution, irradiate the prepared solution under 365nm ultraviolet light for 8 minutes. Then in ...

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Abstract

The invention relates to a preparation method of a water-soluble filter paper cellulose micelle having photo-responsive characteristics and belongs to the field of high polymer materials and biomedical engineering. The preparation method comprises the steps that under nitrogen protection, a hydroxide radical in a main chain of filter paper and carboxyl containing spiropyrane are utilized to perform esterification reaction so as to synthesize spiropyrane modified filter paper cellulose, and finally the water-soluble filter paper cellulose micelle having the photo-responsive characteristics is obtained through a dialysis method. By the adoption of the preparation method, the solubleness of the filter paper cellulose can be remarkably changed, meanwhile the prepared micelle has the three photo-responsive characteristics of photochromism, fluorescence and light-dependent control particle size change, biocompatibility and biodegradability and is good in stability and excellent in fluorescence property. Therefore, the water-soluble filter paper cellulose micelle has the wide application in the fields of medicine release control, biological fluorescence labeling, chemical sensing, bioimaging and the like. The synthetic method is simple and easy to operate, the raw material filter paper cellulose is wide in source, the price is low, industrial production can be achieved, and the preparation method has a very good 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 water-soluble filter paper cellulose micelles with light response characteristics. Background technique [0002] Cellulose is the most abundant bio-organic raw material on earth. Due to the presence of a large number of intermolecular and intramolecular hydrogen bonds in the molecular structure of cellulose, it is insoluble in water and general organic solvents at room temperature, and has excellent chemical stability. It is widely used as a laboratory filter material, but it is extremely poor. The solubility and high chemical inertness of cellulose also affect the application of cellulose in some fields such as biomedicine and chemical analysis. As a kind of cellulose modification, chemical modification is an effective method to overcome the shortcomings of cellulose, and many researchers have tried to modify the r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21C9/00C08B3/00
Inventor 田进涛玄俊极
Owner OCEAN UNIV OF CHINA
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