Green and environment-friendly method for preparing silk fibroin powder

A technology of protein powder and silk protein solution, which is applied in the field of natural polymers, can solve the problems of complex operation process, high cost, and reduction of silk protein molecular weight, etc., and achieve the effects of high biological safety, short production cycle and simple process

Active Publication Date: 2014-04-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, using high concentrations of strong acid, strong alkali, and protease can dissolve silk fibers, but the strong corrosiveness of the solvent will significantly reduce the molecular weight of silk protein, and the mechanical properties of silk fibroin materials prepared by this method will be significantly reduced, and these are toxic and harmful. The solvent is against biological safety, corrodes production equipment, has potential danger to scientific research personnel, is harmful to the environment, etc.
In addition, high concentrations of LiBr, LiSCN and CaCl 2 Neutral saline solution can also dissolve silkworm silk, but it has the characteristics of complicated operation process, long dissolution cycle (dialysis time is more than 3 days), high cost, and environmental pollution.

Method used

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  • Green and environment-friendly method for preparing silk fibroin powder
  • Green and environment-friendly method for preparing silk fibroin powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) degumming; 7g silkworm cocoon shell is 0.5wt%Na in 700mL concentration 2 CO 3 The aqueous solution is boiled for degumming twice, and the degummed silk is washed with water and dried to obtain silk fibers; (2) pre-alkali washing; all the obtained silk fibers are added to 80mL of NaOH solution (0.02mol / L), Stand still at room temperature for 30 minutes; (3) high temperature and high pressure treatment; transfer the system substances in the above steps to an autoclave, and keep at 121° C. for 20 minutes to obtain a silk protein solution. (4) Purification; the silk protein solution obtained in the above steps is neutralized with 0.1mol / L hydrochloric acid, the pH is 7.0, then put into a dialysis bag, and dialyzed with deionized water for 24 hours; (5) Pre-concentration and drying; Part of the water was evaporated from the obtained silk solution by air drying to obtain a silk solution with a concentration of 8 wt%. The silk fibroin powder is obtained after freeze-dryi...

Embodiment 2

[0028] (1) degumming; 5 g The concentration of tussah cocoon shell in 500mL is 0.5wt%Na 2 CO 3 The aqueous solution was boiled for degumming treatment, each time for 30 minutes, and repeated three times. Wash the degummed tussah silk with water afterwards to obtain tussah silk fibers; (2) pre-alkali washing; add the obtained tussah silk fibers to 80mL of NaOH solution (0.1mol / L), and let stand at room temperature for 2 hours; (3 ) high temperature and high pressure treatment; transfer the system substances in the above steps to an autoclave, keep at 121° C. for 30 minutes, and obtain tussah silk protein solution. (4) Purification; neutralize the tussah silk protein solution obtained in the above steps with 1mol / L hydrochloric acid, put it into a dialysis bag, and perform dialysis with deionized water for 24 hours; (5) pre-concentrate and dry; the obtained silk protein Part of the water is evaporated from the solution by air-drying to obtain a tussah silk fibroin protein sol...

Embodiment 3

[0030] (1) degumming; 7g silkworm cocoon shell is 0.5wt%Na in 700mL concentration 2 CO 3 The aqueous solution is boiled and degummed twice, and the degummed silk is washed with water and dried to obtain silk fibers; (2) high temperature and high pressure treatment; all the obtained silk fibers are added to 0.01mol / L KOH solution, and then transferred to In an autoclave, keep at 121° C. for 30 minutes to obtain a silk protein solution. (3) Purification; neutralize the silk protein solution obtained in the above steps with 0.5mol / L hydrochloric acid, put it into a dialysis bag, and perform dialysis with deionized water for 12 hours; (4) Pre-concentrate and dry; the obtained silk protein The solution was concentrated by a vacuum rotary evaporation method to obtain a silk fibroin solution with a silk fibroin solution concentration of 5 wt%. After freeze-drying, silk fibroin powder is obtained; (5) 1 g of silk fibroin powder is dissolved in 10 mL of formic acid solution to prepar...

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Abstract

The invention relates to a method for preparing and dissolving silk fibroin powder, which comprises the steps of degumming, pre-alkali washing, high-temperature high-pressure treatment, purification, pre-concentration, drying, and ultrafine grinding. The method of the invention adopts a high-temperature high-pressure method combined with ultralow-concentration alkali liquor to dissolve fibroin fibers, can completely dissolve fibroin fibers, and breaks the precedent that a high-temperature high-pressure method cannot dissolve silk fibroin; when compared with other technology in the prior art, the method adopts alkali liquor with an ultralow concentration, does not destroy the internal structure of natural silk fibroin, is simple and high-efficient in process, has significantly decreased cost, is short in production period, high in biological safety, simple and convenient, does not generate other wastes, and causes no environment pollution.

Description

technical field [0001] The invention relates to a method for preparing and dissolving silk protein powder, belonging to the field of natural polymers. technical background [0002] The silk cocoon shell is composed of silk fibroin and sericin. Silk fibroin accounts for 70% to 80% of the total silk protein and is a very important textile raw material. Wild silk protein (tussah silk and celestial silk, etc.) and spider silk are also natural fiber proteins. They all have excellent mechanical properties, good biocompatibility and stability, and are essentially proteins. They are widely used in cosmetics, biomaterials, natural polymers, food, health care products and other fields. For example, in the field of cosmetics, silk fibroin has been used as one of the main raw materials for preparing beauty products. Silk fibroin can be processed to obtain regenerated silk fibroin nanofibers, silk fibroin powder, silk fibroin film, silk porous material, etc. [0003] Natural silk pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K14/435C07K1/14
CPCC07K14/43586
Inventor 杨明英帅亚俊周官山王捷朱良均
Owner ZHEJIANG UNIV
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