Gradient pore structure silk fibroin film and preparation method thereof

A technology of silk fibroin and regenerated silk fibroin, which is applied to the field of silk fibroin film with gradient pore structure and its preparation, can solve the problems of repeatability, weak interaction, complicated operation process, etc., and achieves excellent mechanical properties, Excellent mechanical properties and simple technical solutions

Active Publication Date: 2022-04-15
ZHEJIANG LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, direct freeze-drying method, alcohol denaturation method and electrospinning method can only prepare uniform porous structure, and it is difficult to prepare gradient pore structure; template method / salting-out method and gradient drying method can be used to prepare gradient structure, but the operation process is complicated , although there have been examples of gradient pore materials prepared by these methods, there are problems in their repeatability, and it is still difficult to prepare gradient pore film materials; film materials prepared by electrospinning are weak due to the weak interaction between fibers. Its mechanical properties are not ideal
It should be pointed out that no matter what method is used, the preparation of high-performance pure silk fibroin films with gradient pore structure is still a blank.

Method used

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  • Gradient pore structure silk fibroin film and preparation method thereof
  • Gradient pore structure silk fibroin film and preparation method thereof
  • Gradient pore structure silk fibroin film and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The concentration of 0.5 wt% of the lithium chloride-formic acid solution was configured, and 0.4 g of delayed silk was dissolved in 7.8 mL of the above solution, and the oscillation of the ultrasonic cleaning machine was oscillated to obtain a regenerative silk fibroin solution.

[0040]With a clean PET substrate, it is used for 1 min using ultraviolet ozone, and the scraper wiper blade has a thickness of 10 μm, scraping a layer of regenerated silk fibroin moist film and dried; the dry film is placed in water soaked in water, then Contains with the basal and silk fibroid membrane to refrigerate the refrigerator; add the frozen silk fibroin film into a freeze dryer for freeze drying; use mechanical stripping mode, the dry gradient aperture protein film is peeled off with substrate That is, a self-supporting gradient aperture protein film is obtained, and the film formation thickness is about 10 μm, and the varying variation in the thickness direction ranges from 500 nm to 5...

Embodiment 2

[0042] The concentration of 8.7 wt% lithium bromide-formic acid solution was configured, and 2.5 g of delayed silk was dissolved in 5.7 ml of the above solution, placed in an ultrasonic cleaning machine to oscillate 2 h, resulting in a regenerative silk fibroin solution.

[0043] Using a clean polyimide PI substrate, an oxygen plasma washed 5 min, and a blade scraper wiper had a thickness of 500 μm, scraping a layer of silk fibroidin moist film and dried; 1H, then inserted into the -20 ° C refrigerator in conjunction with the basal and silk fibroin gel, the frozen silk fibroin film was placed in a freeze dryer for freeze drying; a mechanical stripping method, a dry gradient aperture protein film The gradient aperture protein film is obtained from the substrate to obtain a self-supporting gradient, and the film film has a film thickness of about 1000 μm, and the varying variation in the thickness direction is 200 nm-10 μm in the thickness direction.

Embodiment 3

[0045] The concentration of 4.8 wt% of the calcium chloride-formic acid solution was configured, and 1.3 g of delayed silk was dissolved in 6.8 ml of the above solution, placed in an ultrasonic cleaning machine to oscillate 1 h, resulting in a regenerative silk fibroin solution.

[0046] With a clean PET substrate, a four-sided preparator having a thickness of 300 μm is used, and the silkwater wet film is applied and dried; the dry film is placed in water for 10 min, and then together with the base and silk fibroin gel film directly into the frozen Dryer; through -50 ° C cold trap and low vacuum effects, the surface of the silk fibroin film is spontaneously nucleated, and the in situ freeze is carried out; the dry gradient, the dried gradient, the film is peeled off. The self-supporting gradient aperture protein film is obtained, and the film film has a film thickness of about 80 μm, and the aperture in the thickness direction ranges from 200 nm to 5um.

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Abstract

The invention discloses a preparation method of a gradient pore silk fibroin film. Blade-coating the regenerated silk fibroin wet film on a substrate, and drying to obtain a regenerated silk fibroin film; placing the regenerated silk fibroin membrane in water; and performing vacuum freeze drying on the regenerated silk fibroin film and the substrate, and stripping from the substrate after drying to obtain the gradient pore silk fibroin film. The method is simpler, more effective and more reliable, the flexible film has excellent mechanical and mechanical properties, the pore size presents gradient change in the thickness direction, and the flexible film has a compact layer and a porous layer, is excellent in biocompatibility, free of additives, free of templates, low in production cost, short in period, good in repeatability and suitable for batch preparation.

Description

Technical field [0001] The present invention belongs to a filament protein film in the field of polymer materials and a method of preparation thereof, and a technique of a gradient aperture structure and a preparation method thereof. Background technique [0002] Preparation of porous membranes and membrane separation techniques have important application prospects in food, medical hygiene, biotechnology, chemical, and environments, for example, as a catalyst carrier, a pharmaceutical carrier or a filtration film. In most cases, the aperture in the porous material is uniformly distributed; in some cases, the aperture or porosity of the porous material can vary in a particular direction, and such a material is referred to as a gradient porous material. A typical example of gradient porous material, such as bones, which contain sponge-like loose kernels and dense cortical shells, which can provide excellent permeability and mechanical stability. It is worth mentioning that gradient...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L89/00C08K3/16C08J5/18A61L27/22A61L27/54A61L27/56
CPCC08J5/18A61L27/56A61L27/227A61L27/54C08J2389/00C08K3/16C08K2003/162
Inventor 刘海涛张磊肖建亮王珊
Owner ZHEJIANG LAB
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