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Strengthened toughened regenerated silk fibers and preparation method thereof

A regenerated silk, strengthening and toughening technology, applied in fiber processing, animal fiber, artificial silk manufacturing, etc., can solve the problems of graphene oxide agglomeration and inability to effectively prepare silk fibroin, and achieve simple preparation process and easy Promotion and application, the effect of high modulus

Active Publication Date: 2014-02-12
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to maintain the stable structure of silk fibroin in solution in this system, it is necessary to add Ca 2+ ions, but adding Ca 2+ After the ionic silk fibroin solution is blended with the graphene oxide aqueous solution, the graphene oxide will be seriously agglomerated, so this is the main reason why the silk fibroin / graphene oxide composite system cannot be effectively prepared at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] With a mass percentage of 0.5% Na 2 CO 3 The aqueous solution degummed the silk cocoon, and then dissolved it with a 9.0 mol / L LiBr aqueous solution. After dilution, centrifuge with a high-speed centrifuge. After suction filtration, the silk fibroin solution was placed in a cellulose dialysis bag, sealed, immersed in deionized water for dialysis, the temperature was 6°C, the dialysis time was 72 hours, and the water change cycle was 4 hours. Then, at a temperature of 6°C, the regenerated silk fibroin aqueous solution was concentrated to 10% by mass by using the wind speed method. The graphene oxide aqueous solution with a concentration of 3 mg / ml is ultrasonically dispersed, and then the graphene oxide aqueous solution is added to the regenerated silk fibroin aqueous solution according to the mass ratio of graphene oxide and silk fibroin at a ratio of 1:500, and shaken well . Then add TiO 2 Nano-TiO with a mass fraction of 30% and a particle size of 20nm 2 water s...

Embodiment 2

[0039] With a mass percentage of 1.0% Na 2 CO 3 The aqueous solution degummed the silk cocoon, and then dissolved it with a 9.0 mol / L LiBr aqueous solution. After dilution, centrifuge with a high-speed centrifuge. After suction filtration, the silk fibroin solution was placed in a cellulose dialysis bag, sealed, immersed in deionized water for dialysis, the temperature was 8°C, the dialysis time was 72 hours, and the water change cycle was 4 hours. Then, at a temperature of 8°C, the regenerated silk fibroin aqueous solution was concentrated to 20% by mass by using the wind speed method. The graphene oxide aqueous solution with a concentration of 3 mg / ml is ultrasonically dispersed, and then the graphene oxide aqueous solution is added to the regenerated silk fibroin aqueous solution according to the mass ratio of graphene oxide and silk fibroin at a ratio of 1:1000, and shaken well . Then add TiO 2 Nano-TiO with a mass fraction of 10% and a particle size of 100nm 2 water...

Embodiment 3

[0043] With a mass percentage of 1.0% Na 2 CO 3 The aqueous solution degummed the cocoon, and then dissolved it with a 9.5 mol / L LiBr aqueous solution. After dilution, centrifuge with a high-speed centrifuge. After suction filtration, the silk fibroin solution was placed in a cellulose dialysis bag, sealed, immersed in deionized water for dialysis, the temperature was 12°C, the dialysis time was 72 hours, and the water change cycle was 4 hours. Then, at a temperature of 12°C, the regenerated silk fibroin aqueous solution was concentrated to 20% by mass by using the wind speed method. The graphene oxide aqueous solution with a concentration of 3mg / ml is ultrasonically dispersed, and then the graphene oxide aqueous solution is added to the regenerated silk fibroin aqueous solution according to the mass ratio of graphene oxide and silk fibroin at a ratio of 1:10000, and shake well . Then add TiO 2 Nano-TiO with a mass fraction of 50% and a particle size of 10nm 2 water sol ...

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Abstract

The invention relates to strengthened toughened regenerated silk fibers and a preparation method thereof. The preparation method comprises the following steps of 1, degumming silkworm cocoons, and dissolving the degummed silkworm cocoons to obtain a regenerated silk fibroin aqueous solution, 2, blending a graphene oxide aqueous solution subjected to ultrasonic treatment and the regenerated silk fibroin aqueous solution according to a certain ratio, 3, adding metal-oxide hydrosol into the mixture according to a certain ratio, 4, adding a CaCl2 solution into the mixture obtained by the step 3 to adjust a calcium ion molar concentration to 0.15-0.3mol / L, and sequentially carrying out concentration, 5, carrying out dry spinning on the concentrated solution as a spinning liquid at a room temperature, and 6, after-treating the composite fibers by an ethanol-water solution. The preparation method has simple processes and utilizes the raw materials having wide sources. The treated composite fibers have good strength and good toughness and have breaking strength of 70-380MPa, breaking elongation of 20-150% and breaking energy of 30-100J / g.

Description

technical field [0001] The invention belongs to the field of silk fibers, and relates to a reinforced and toughened regenerated silk fiber and a preparation method thereof, in particular to a preparation of a reinforced and toughened regenerated silk fiber based on a graphene oxide / silk fibroin composite system by adding a third component The method, wherein the third component is mainly metal oxide nanoparticles. Background technique [0002] Spider silk and silk have attracted the attention of the world because of their many excellent properties, especially the traction silk in spider silk is one of the strongest fibers in nature so far. However, due to the spider's cannibalistic nature, spider silk has not been widely used commercially. The application of silk in textiles, clothing, medicine, cosmetics, biotechnology and other fields has been very far-reaching. [0003] As we all know, spider silk is a high-strength, high-tenacity fiber with a breaking strength of up to...

Claims

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Application Information

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IPC IPC(8): D01F4/00D01F1/10D06M13/144D06M101/10
Inventor 张耀鹏张超潘辉邵惠丽胡学超
Owner DONGHUA UNIV
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