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Nano-cellulose reinforced silk fibroin composite material and preparation method thereof

A technology of nano-cellulose and composite materials, applied in the field of nano-cellulose-reinforced silk fibroin composite materials and its preparation, which can solve the problems of complex process, easy aggregation of cellulose nano-whiskers, and difficulty in dispersing fibers, etc. simple effect

Active Publication Date: 2017-03-08
WUHAN TEXTILE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method first needs to extract the cellulose nano-whiskers, the process is complicated, and the cellulose nano-whiskers are easy to agglomerate, and it is difficult to evenly disperse in the silk solution to form uniform fibers.

Method used

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  • Nano-cellulose reinforced silk fibroin composite material and preparation method thereof
  • Nano-cellulose reinforced silk fibroin composite material and preparation method thereof
  • Nano-cellulose reinforced silk fibroin composite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Immerse 100 g silkworm silk in 5 L of 0.05% NaCO 3 solution, boiled at 98-100°C for 30 min, and repeated three times to degumming the silk, fully washed and dried to obtain pure silk fibroin fibers; solution, stirring and dissolving at 60°C for 55 min to obtain a silk fibroin mixed solution;

[0035] Add 1 g of microcrystalline cellulose powder into 80 mL of 9.3 mol / L LiBr solution, stir and dissolve at 110°C for 55 min to obtain a cellulose solution;

[0036] Mix the silk fibroin solution and cellulose solution according to the mass ratio of silk fibroin and fiber 50:50, stir at 110°C for 5 minutes and mix evenly to obtain a silk fibroin / cellulose mixed solution, cool at room temperature to form a blended gel glue;

[0037] The above gel was soaked in 75% ethanol for 2 h, and then soaked in flowing deionized water for 48 h to remove LiBr;

[0038] The purified silk fibroin / cellulose gel was dried in a vacuum oven at 37 °C for 48 h to obtain a nanocellulose-reinforce...

Embodiment 2

[0041] Add 20 g of degummed silk fibroin fibers to 100 mL of 10 mol / L LiBr solution, stir and dissolve at 60°C for 58 min to obtain a silk fibroin mixed solution;

[0042] Add 2 g of microcrystalline cellulose powder into 160 mL of 10 mol / L LiBr solution, stir and dissolve at 110°C for 58 min to obtain a cellulose solution;

[0043] Mix the silk fibroin solution and the cellulose solution according to the mass ratio of silk fibroin and fiber 20:80, stir at 110° C. for 3 minutes and mix evenly to obtain a silk fibroin / cellulose mixed solution. Cooling at room temperature to form a blended gel;

[0044] The above gel was soaked in 50% ethanol for 2 h, and then soaked in running water for 48 h to remove LiBr;

[0045] The purified silk fibroin / cellulose gel was dehydrated successively with 50%, 75% tert-butanol and anhydrous tert-butanol for 30 min, and then frozen at -20°C for 24 h to obtain frozen solids.

[0046] The above-mentioned frozen solid was freeze-dried for 48 h accor...

Embodiment 3

[0049] Add 10 g of degummed silk fibroin fibers to 40 mL of 8 mol / L LiBr solution, stir and dissolve at 60°C for 120 min to obtain a silk fibroin mixed solution;

[0050] Add 1 g of cellulose filter paper into 100 mL of 8 mol / L LiBr solution, stir and dissolve at 90 °C for 4 h to obtain a cellulose solution;

[0051] Mix the silk fibroin solution and cellulose solution according to the mass ratio of silk fibroin and fiber 80:20, stir at 90°C for 5 min and mix well to obtain a silk fibroin / cellulose mixed solution; cool at room temperature to form a blended gel;

[0052] Soak the above gel in 90% methanol for 1 h, then soak in running water for 72 h to remove LiBr;

[0053] The purified silk fibroin / cellulose gel was dried in a vacuum oven at 37 °C for 48 h to obtain a nanocellulose-reinforced silk film.

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Abstract

The invention relates to the technical field of high polymer materials, and in particular relates to a nano-cellulose reinforced silk fibroin composite material and a preparation method thereof, fibroin fibers and cellulose are dissolved in LiBr as a common solvent, the nano structure of the cellulose is retained by controlling the dissolution degree of the cellulose raw materials, wherein the dissolution temperature of the cellulose is controlled at 80-150 DEG C, the obtained fibroin fiber / cellulose blending solution can quickly form a gel, and the phenomenon of aggregation and uneven distribution of nanocellulose in the solution is avoided; the gel further can be prepared into a membrane and a porous material after being dried, so as to obtain the nano-cellulose reinforced silk fibroin composite material. The preparation process disclosed by the invention is simple and controllable; and the obtained composite material comprises uniformly-distributed nano-cellulose, the strength and the elongation at break of the nano-cellulose reinforced silk fibroin composite material are significantly enhanced compared to regenerated silk fibroin materials.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a nanocellulose-reinforced silk fibroin composite material and a preparation method thereof. Background technique [0002] Silk fibroin is a high-purity protein secreted by silk glands of silkworms. It does not contain organelles and other biological impurities, and has high biological safety. Silk fibroin is composed of 20 amino acids such as tyrosine, alanine, and serine, which can be biodegraded and the final degradation products are polypeptides and free amino acids, which are easily metabolized by the body. Silk fibroin has good biocompatibility. Silk fibers have been used in medical surgical sutures for decades, and the clinical effect has been proven. In vitro and in vivo results confirmed that the regenerated silk fibroin material can support the growth of a variety of cells, showing immunological inertness and lower inflammatory response. Therefore, silk fibr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L89/00C08L1/04C08J3/075C08J3/02C08J9/28C08J5/18
CPCC08J3/02C08J3/075C08J5/18C08J9/28C08J2201/0484C08J2301/04C08J2389/00C08J2401/04C08J2489/00C08L1/04C08L89/00C08L2203/14C08L2203/16
Inventor 尤仁传冯艳飞徐卫林张捷王露萍张强李秀芳
Owner WUHAN TEXTILE UNIV
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