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Natural silk micro-nano-fiber preparation method

A technology of micro-nano fiber and natural silk, which is applied in the direction of spinning solution preparation, rayon manufacturing, fiber chemical characteristics, etc., can solve the problems of limited application prospects, difficulty in mechanical crushing, and limited diameter adjustment of silk fibroin nanofibers. Reduce mechanical force and time, reduce excessive decomposition and waste, and can adjust a wide range of effects

Active Publication Date: 2019-04-19
WUHAN TEXTILE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, a solution composed of inorganic salts (one of calcium sulfate, calcium chloride, ammonium chloride, ammonium acetate, and ammonium nitrate) or small molecular compounds of weak acids or weak bases, deionized water, and alcohols can loosen the hierarchical structure of silk. The solution effect is very limited, so that mechanical crushing is very difficult, it is difficult to achieve macro-production, and the aspect ratio of the fiber is not ideal
The diameter adjustment of silk fibroin nanofibers prepared by this method is also very limited, and can only be controlled within the range of 50-150 nm, which greatly limits its application prospects.

Method used

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Embodiment 1

[0029] A kind of preparation method of natural silk micro-nano fiber of the present embodiment, described method comprises the steps:

[0030] (1) Immerse silkworm raw silk into 0.6% NaCO 3 In the solution, boil at 98-100°C for 30 minutes, repeat 3 times, pretreat the silk, remove sericin and weaken the force between silk fibrils, and then fully wash and dry the degummed silk Obtain pure silk fiber;

[0031] (2) Shred the pure silk fiber obtained in step (1) to a length of 0.1-10 cm, and then add it to a ternary mixed solution composed of calcium nitrate / ethanol / deionized water to obtain a dispersed silk fiber-containing liquid, wherein: the mass volume concentration of calcium nitrate in the ternary mixed solution is 2g / ml, and the volume ratio of the deionized water to ethanol is 2:1;

[0032] (3) subjecting the dispersion liquid containing silk fibers obtained in step (2) to mechanical stirring at 45° C. for 2 hours to obtain silk micro-nano fiber slurry;

[0033] (4) Th...

Embodiment 2

[0036] A kind of preparation method of natural silk micro-nano fiber of the present embodiment, described method comprises the steps:

[0037] (1) Immerse silkworm raw silk into 1.0% NaCO 3 In the solution, boil at 98-100°C for 30 minutes, repeat 3 times, pretreat the silk, remove sericin and weaken the force between silk fibrils, and then fully wash and dry the degummed silk Obtain pure silk fiber;

[0038] (2) Shred the pure silk fiber obtained in step (1) to a length of 0.1 to 10 cm, and then add it to a ternary mixed solution composed of calcium nitrate / butanol / deionized water to obtain silk fiber-containing Dispersion liquid, wherein: the mass volume concentration of calcium nitrate in the ternary mixed liquid is 5 g / ml, and the volume ratio of deionized water to butanol is 3:1;

[0039] (3) Dispersing the silk fiber-containing dispersion liquid obtained in step (2) under the condition of 50° C., mechanically agitating and loosening for 4 hours to obtain silk micro-nano f...

Embodiment 3

[0043] A kind of preparation method of natural silk micro-nano fiber of the present embodiment, described method comprises the steps:

[0044] (1) Immerse silkworm raw silk into NaCO with a mass fraction of 2.0% 3 In the solution, boil at 98-100°C for 30 minutes, repeat 3 times, pretreat the silk, remove sericin and weaken the force between silk fibrils, and then fully wash and dry the degummed silk Obtain pure silk fiber;

[0045] (2) Shred the pure silk fiber obtained in step (1) to a length of 0.1 to 10 cm, and then add it to a ternary mixed solution composed of calcium nitrate / propanol / deionized water to obtain silk fiber-containing Dispersion liquid, wherein: the mass volume concentration of calcium nitrate in the ternary mixed liquid is 4g / ml, and the volume ratio of deionized water to propanol is 4:1;

[0046] (3) Dissolving the silk fiber-containing dispersion liquid obtained in step (2) under the condition of 60° C. for 3 hours with mechanical stirring to obtain sil...

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Abstract

The invention discloses a natural silk micro-nano-fiber preparation method, and belongs to the technical field of micro-nano material preparation. According to the preparation method, the diameter ofa fiber can be adjusted and controlled within the range of 20nm-2000nm at random. According to the method, the acting force between micro-fibers of natural silks is weakened or removed, a hierarchicalstructure of meso-scale of the natural silks is deconstructed, and micro-nano-fibroin fibers with controllable sizes are acquired. The method includes the steps: pretreating natural silks in 0.6-5.0%of sodium carbonate solution; mechanically loosening the acquired fibroin fibers in a calcium nitrate / saturated mono-fatty alcohol / deionized water ternary system with the temperature of 45-70 DEG C to obtain micro-nano-natural silk fiber solution; centrifuging, extracting, filtering and washing the solution to obtain the purified natural silk micro-nano-fiber. A preparation process is green, simple, convenient and controllable, the natural silk micro-nano-fiber is high in yield, size adjusting range is wide, and industrialization is easily achieved.

Description

technical field [0001] The invention relates to a method for preparing natural silk micro-nano fibers, which belongs to the technical field of micro-nano material preparation. Background technique [0002] Silk is a natural protein fiber with good mechanical properties and biocompatibility, and can be degraded. As a traditional high-grade textile raw material, it also has broad application prospects in the fields of composite materials, biomedicine and fine chemicals. Natural silk is formed by silkworm spinners through mechanical drafting and various environmental factors. It has a remarkable fibril-assembled micro-nano hierarchical structure. The longitudinal connections of the chains are assembled into giant fibrils with a scale of hundreds of nanometers, and then further assembled to form silk fibers. Micro-nano-scale fiber materials have excellent surface effects, small size effects, and quantum size effects, and have been widely used in medicine, computer and electron...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F4/00D01F1/10D01D1/02
CPCD01D1/02D01F1/10D01F4/00
Inventor 张强尤仁传韩国聪闫书芹李秀芳罗祖维徐安长
Owner WUHAN TEXTILE UNIV
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