Direct sulfonation method preparation of sulfonated silk fibroin

A technology of silk fibroin and sulfonated silk fibroin, applied in the field of direct sulfonation method to prepare sulfonated silk fibroin, can solve the problem of low sulfonation efficiency

Inactive Publication Date: 2014-10-15
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] It is known that sulfonated silk fibroin has anticoagulant properties through literature review, bu

Method used

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  • Direct sulfonation method preparation of sulfonated silk fibroin
  • Direct sulfonation method preparation of sulfonated silk fibroin
  • Direct sulfonation method preparation of sulfonated silk fibroin

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Experimental program
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Embodiment Construction

[0004] Process parameters such as temperature, concentration and reaction time of sulfonation reaction are as follows:

[0005]

[0006] Note on concentration ratio: 1g of silk fibroin corresponds to the dosage of 5, 10, and 15ml of chlorosulfonic acid;

[0007] Temperature conditions: 0, 25, 50°C;

[0008] Time conditions: 5, 10, 15hr;

[0009] Weigh 1.20g of degummed and dried silk fibroin fiber with a balance, put it into a 100ml round single-necked flask, press the silk fibroin to the bottom of the bottle with a glass rod, and then add 6ml of chlorosulfur (see orthogonal table) dropwise acid solution, rotate the flask to make the silk fibroin fully infiltrated by chlorosulfonic acid, and then use a vacuum cock to connect the flask to a container containing CaCl 2 The desiccant drying tower is used to remove the water generated by the reaction between serine and tyrosine hydroxyl (-OH) on silk fibroin and chlorosulfonic acid, and placed in an oil bath at 50°C (see orth...

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Abstract

The invention discloses a silk fibroin sulfonation modification method and technical screening of anticoagulant properties of sulfonated silk fibroin, belongs to the field of biological (medical) materials, and mainly relates to the following steps: natural silk is boiled in an alkaline (0.5% (wt%) Na2CO3 water solution) for degumming, and rinsed with distilled water, then silk fibroin fiber is dried at the temperature of 50 DEG C, then the dried silk fibroin is reacted with chlorosulfonic acid, a corresponding sulfonated modified silk fibroin solution is obtained by all steps of a sulfonation process optimized by an orthogonal method, then is neutralized into a neutral solution by use of a sodium hydroxide solution, then cooled to room temperature, transferred into a dialysis bag for dialysis for 72hr, concentrated by rotary evaporation, and frozen and dried to obtain sulfonated modified silk fibroin powder. By the optimized sulfonation process, the use amount of the chlorosulfonic acid can be reduced, the anticoagulant properties of the sulfonated silk fibroin can be improved, the repeatability is good, the product is pure, and the composition is stable.

Description

Technical field: [0001] Silk fibroin and sulfonated silk fibroin belong to the scope of natural polymers and their modified materials, and are also commonly used biological materials. Background technique: [0002] It is known that sulfonated silk fibroin has anticoagulant properties through literature review, but in specific repeated experiments, it is found that the sulfonation efficiency of this process is not high. So try to reduce the pyridine organic solvent to improve the use efficiency of sulfonic acid, and get the optimized process parameters of the direct sulfonation method and a purer sulfonated silk fibroin product. Invention content: [0003] Chlorosulfonic acid has the highest sulfonation efficiency among all inorganic acids. Here, chlorosulfonic acid is used to sulfonate silk fibroin, and the parameters of the sulfonation modification process are optimized by orthogonal method, and a preparation method that can significantly improve the anticoagulant effect...

Claims

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Application Information

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IPC IPC(8): C08H1/00
Inventor 吴建荣
Owner SOUTHWEST JIAOTONG UNIV
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