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Preparation method of silk fibroin/graphene oxide high-concentration blended aqueous solution

A technology of silk fibroin and regenerated silk fibroin, which is applied in the field of preparation of silk fibroin/graphene oxide high-concentration blended aqueous solution, can solve problems such as graphene oxide agglomeration, and achieve good quality and broad application prospects

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

But adding Ca 2+ Severe agglomeration of graphene oxide occurs after ionic silk fibroin solution is blended with aqueous solution of graphene oxide
The reason for this phenomenon may be that silk fibroin molecules interact with Ca 2+ The chelating structure formed by ions will affect the interaction between the hydrophilic groups on the surface of graphene oxide and silk fibroin molecules, and lead to the agglomeration of graphene oxide. The reason needs to be further studied

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 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. A concentration of 0.5 mg / mL graphene oxide aqueous solution is ultrasonically dispersed; then the graphene oxide aqueous solution is added to the regenerated silk fibroin aqueous solution at a ratio of 1:200 according to the mass ratio of graphene oxide and silk fibroin, and Shake well. Add an aqueous calcium chloride solution with a molar concentration of 1.5 mol / L to adjust the molar con...

Embodiment 2

[0032] With a mass percentage of 0.5% Na 2 CO 3 The aqueous solution degummed the cocoon, and then dissolved it with 8.5 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 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 20% by mass by using the wind speed method. The graphene oxide aqueous solution with a concentration of 0.5mg / ml is ultrasonically dispersed, and then the graphene oxide aqueous solution is added to the regenerated silk fibroin aqueous solution at a ratio of 1:500 according to the mass ratio of graphene oxide and silk fibroin, and Shake well. Add an aqueous calcium chloride solution with a molar concentration of 1.5 mol / L to adjust the mola...

Embodiment 3

[0034] 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 7°C, the dialysis time was 72 hours, and the water change cycle was 4 hours. Then, at a temperature of 7°C, the regenerated silk fibroin aqueous solution was concentrated to 30% 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 shaken uniform. Add a calcium chloride aqueous solution with a molar concentration of 2.25 mol / L to adju...

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Abstract

The invention relates to a preparation method of a silk fibroin / graphene oxide high-concentration blended aqueous solution. The preparation method comprises the following steps of 1, degumming silkworm cocoons, dissolving the degummed silkworm cocoons, carrying out solution dialysis to obtain a silk fibroin aqueous solution, concentrating the silk fibroin aqueous solution until a silk fibroin concentration is in a range of 10-30wt%, and taking out the concentrated silk fibroin aqueous solution, 2, blending a graphene oxide aqueous solution subjected to ultrasonic treatment and the concentrated silk fibroin aqueous solution according to a certain ratio, 3, adding a CaCl2 aqueous solution into the mixture obtained by the step 2 to adjust a calcium ion molar concentration to 0.15-0.3mol / L, and 4, sequentially carrying out concentration to obtain the silk fibroin / graphene oxide high-concentration blended aqueous solution having silk fibroin content of 50-58wt%. The preparation method has simple processes, can be operated easily and can prepare the silk fibroin / graphene oxide high-concentration blended aqueous solution. The silk fibroin / graphene oxide high-concentration blended aqueous solution can be used for dry spinning or film coating.

Description

technical field [0001] The invention belongs to the field of composite materials, and relates to a preparation method of a silk fibroin / graphene oxide high-concentration blended aqueous solution. Background technique [0002] Known as the "Fiber Queen", silk is one of the earliest natural proteins used by humans. It has been widely used as a material for high-end clothing for thousands of years. Nowadays, with the continuous development of spinning technology, it is related to The field of research is gradually expanding. Researchers have extracted regenerated silk fibroin from cheap and easy-to-obtain silk. This regenerated silk fibroin has excellent mechanical properties, good biocompatibility and degradability, and can be widely used in biology, medicine, Textile and other fields. [0003] Graphene, as the thinnest but hardest nanomaterial in the world, has become a research hotspot as soon as it appeared, and graphene oxide is an important derivative of graphene. The ...

Claims

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Application Information

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IPC IPC(8): C08J3/07C08L89/00C08K9/00C08K3/04C08K3/16D01F4/00D01F1/10
Inventor 张耀鹏张超潘辉邵惠丽胡学超
Owner DONGHUA UNIV
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