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Preparation method of silk fibroin nanofiber whiskers

A technology of silk fibroin and nanofibers, applied in the preparation of silk fibroin nanofiber whiskers, using ultrasonic-assisted sulfuric acid to prepare silk fibroin nanofiber whiskers, can solve the complex preparation process and long time-consuming silk fibroin nanofibers , fewer preparation methods, etc., to achieve good repeatability, good product recovery, and short time-consuming effects

Pending Publication Date: 2020-12-11
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to overcome the current time-consuming preparation of silk fibroin nanofibers, the preparation process is relatively complicated, and the preparation methods are less, the purpose of the present invention is to provide a preparation method of silk fibroin nanofiber whiskers

Method used

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  • Preparation method of silk fibroin nanofiber whiskers

Examples

Experimental program
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Embodiment 1

[0023] 1) Cut silkworm cocoons into about 1×1cm 2 For small pieces, use 1000ml of 0.5% (w / w) Na 2 CO 3 The solution was boiled for 30 minutes to degumming, washed with deionized water repeatedly, repeated 3 times, and dried overnight at 60°C to obtain silk fibroin;

[0024] 2) Configure 60wt% H 2 SO 4 After solution, preheat it to 45°C in a constant temperature water bath, transfer it to a 100w ultrasonic reactor, pull apart the more obvious entangled parts of the silk fibroin obtained in step 1), and put it in a preheated well H 2 SO 4 React in the solution for 30min, silk fibroin and H 2 SO 4 The mass ratio of the solution is 1:10, the reaction is terminated by using room temperature deionized water with 5 times the volume of the acid solution, and the acid solution is cleaned to obtain the reactant;

[0025] 3) The reactant obtained in step 2) is diluted with deionized water, neutralized with 0.2wt% NaOH solution, and cleaned with deionized water to desalinize the s...

Embodiment 2

[0029] 1) Cut silkworm cocoons into about 1×1cm 2 For small pieces, use 1000ml of 0.5% (w / w) Na 2 CO 3 The solution was boiled for 30 minutes to degumming, washed with deionized water repeatedly, repeated 3 times, and dried overnight at 60°C to obtain silk fibroin;

[0030] 2) Configure 45wt% H 2 SO 4 After solution, preheat it to 75°C in a constant temperature water bath, transfer it to a 100w ultrasonic reactor, pull apart the more obvious entangled parts of the silk fibroin obtained in step 1), and put it in a preheated well H 2 SO 4 React in the solution for 30min, silk fibroin and H 2 SO 4 The mass ratio of the solution is 1:10, the reaction is terminated by using room temperature deionized water with 5 times the volume of the acid solution, and the acid solution is cleaned to obtain the reactant;

[0031] 3) The reactant obtained in step 2) is diluted with deionized water, neutralized with 0.05wt% NaOH solution, and cleaned with deionized water to desalinize the ...

Embodiment 3

[0035]1) Cut silkworm cocoons into about 1×1cm 2 For small pieces, use 1000ml of 0.5% (w / w) Na 2 CO 3 The solution was boiled for 30 minutes to degumming, washed with deionized water repeatedly, repeated 3 times, and dried overnight at 60°C to obtain silk fibroin;

[0036] 2) Take a dialysis bag with an appropriate length and a molecular weight cut-off of 7000kDa, boil it with deionized water for 10 minutes, wash it with deionized water for 3 times, and set aside;

[0037] 3) Configure 45wt% H 2 SO 4 After solution, put it in a constant temperature water bath and preheat it to 45°C, transfer it to a 200w ultrasonic reactor, pull apart the more obvious entangled part of the silk fibroin obtained in step 1), and put it in a preheated well H 2 SO 4 React in solution for 180min, silk fibroin and H 2 SO 4 The mass ratio of the solution is 1:20, the reaction is terminated by using room temperature deionized water with 5 times the volume of the acid solution, and the acid sol...

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Abstract

The invention discloses a preparation method of silk fibroin nanofiber whiskers. The preparation method is characterized in that after silkworm cocoons are degummed, silk fibroin is obtained, catalytic hydrolysis is carried out on silk fibers by using sulfuric acid, ultrasonic assistance is adopted for mass transfer, and the silk fibroin nanofiber whiskers are collected through freeze-drying. Themethod is rapid and efficient, and is especially suitable for preparing of the silk fibroin nanofiber whiskers. In the method for preparing the silk fibroin nanofiber whiskers, the method for preparing the silk fibroin nanofiber whiskers by utilizing sulfuric acid is introduced, so that the range of the preparation method of the silk fibroin nanofiber whiskers is expanded, and the method is beneficial to accelerating breakthrough of the limitation of the preparation method of the silk fibroin nanofiber whiskers; and meanwhile, the manner of utilizing ultrasonic assistance for mass transfer isprovided, the whiskers which are uniformly dispersed and are uniform in length-diameter ratio can be obtained easily, the experimental repeatability is good, the consumed time is short, and the methodis of great significance to preparation of the silk fibroin nanofiber whiskers.

Description

technical field [0001] The invention relates to a method for preparing silk fibroin nanofiber whiskers, in particular to a method for preparing silk fibroin nanofiber whiskers by using ultrasonic-assisted sulfuric acid, and belongs to the technical field of biomaterials. Background technique [0002] Silk fibroin, or silk fiber, is a natural protein fiber mainly derived from silkworms. Its basic structure consists of crystalline and non-crystalline regions, of which the crystalline region is mainly composed of residues of glycine, alanine and serine. Accounting for about 2 / 3, these residues form a sheet structure. The main function of the crystalline region is to maintain mechanical strength. The non-crystalline region is mainly composed of phenylalanine, tyrosine, and tryptophan, accounting for about 1 / 3. The main function of the crystal region is moisture absorption and UV resistance. There are two main molecular conformations of silk fibroin, SilkⅠtype and SilkⅡtype: Sil...

Claims

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Application Information

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IPC IPC(8): D01F4/02
CPCD01F4/02
Inventor 蔡玉荣林敏婕谢文姣王振宇
Owner ZHEJIANG SCI-TECH UNIV
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