A kind of preparation method of natural silk micro-nano fiber

A technology of micro-nano fiber and natural silk, which is applied in the direction of spinning solution preparation, artificial silk manufacturing, fiber chemical characteristics, etc., can solve the problems of limiting application prospects, difficult to achieve macro-production, and difficult mechanical crushing, so as to reduce the mechanical effect effort and time, achieve high yield and macro-preparation, and reduce excessive decomposition and waste

Active Publication Date: 2021-02-23
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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  • A kind of preparation method of natural silk micro-nano fiber

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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 method for preparing natural silk micro-nano fibers, which belongs to the technical field of micro-nano material preparation. The preparation method of the present invention can realize arbitrary regulation and control of the fiber diameter within the range of 20nm to 2000nm. The invention obtains micro-nano silk fibroin fibers with controllable size by weakening or eliminating the force between silk micro-fibrils and deconstructing the mesoscopic hierarchical structure of silk. First, the silk is pretreated in a sodium carbonate solution with a mass fraction of 0.6-5.0%, and the resulting silk fiber is mechanically loosened in a ternary system of calcium nitrate / saturated monohydric fatty alcohol / deionized water at a temperature of 45-70°C. The silk micronanofiber slurry is obtained through hydrolysis treatment, and the purified natural silk micronanofibers can be obtained through further centrifugation, suction filtration and water washing. The preparation process of the invention is green, simple and controllable, the output of silk micro-nano fibers is high, the size control range is wide, and industrialization is easy.

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 Patents(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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