Bionic regenerated silk fibroin filament fiber and preparation method thereof
A technology for regenerating silk fibroin and filament fibers, which is applied in the direction of single-component fibroin artificial filament, dry spinning method, wet spinning method, etc., can solve the problems of poor mechanical properties and lack of natural silk fibril structure, etc. Achieve the effect of low cost, efficient preparation process and controllable preparation conditions
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[0031] Example one
[0032] A method for preparing biomimetic regenerated silk fibroin filament fiber includes the following steps:
[0033] (1) Put 0.5Kg of raw silk (a by-product of silkworm cocoon reeling in the silk reeling factory) into 10 liters of 0.1% sodium carbonate aqueous solution, boil for 30 minutes, repeat 3 times, and then dry naturally to obtain pure silk Silk fibroin
[0034] (2) Use 98% formic acid to prepare 2 liters of formic acid / calcium chloride mixed solution, in which the content of calcium chloride is 5.0%. After the solution is evenly mixed, put pure silk fibroin into formic acid / calcium chloride In the mixed solution, stir at room temperature for 3 hours to obtain a silk fibroin solution with a mass fraction of 25.0%, which is purified by filtration and defoamed by ultrasound for 0.5 hours to make spinning dope;
[0035] (3) Under the action of 1.0MPa nitrogen, using a spinning hole with a hole diameter of 0.9mm, at a temperature of 25°C, at a speed of 5g ...
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[0038] Example two
[0039] (1) Put 1 kg of mulberry silkworm cocoon silk into 20 liters of sodium carbonate solution with a mass fraction of 0.05%, boil for 30 minutes, repeat 3 times, and then dry naturally to obtain pure silk fibroin;
[0040] (2) Use 98% phosphoric acid to prepare 2 liters of a phosphoric acid / hydroxyapatite mixture, in which the content of hydroxyapatite is 10.0%. After the solution is uniformly mixed, put the pure silk fibroin into the phosphoric acid / hydroxyapatite mixture, stir at room temperature for 6 hours to obtain a silk fibroin solution with a mass fraction of 10.0%, which is purified by filtration and defoamed by ultrasonic for 0.5 hours. Into spinning dope;
[0041] (3) Under the action of 0.5MPa nitrogen, use a spinning hole with a hole diameter of 0.9mm, and at a temperature of 20℃, spray the silk fibroin spinning dope at a rate of 3g per minute, and then enter the concentration of 60% In the ammonium sulfate coagulation bath, the temperature of t...
Example Embodiment
[0043] Example three
[0044] (1) Put 1 kg of cocoon silk into 20 liters of sodium carbonate solution with a mass fraction of 0.1%, boil for 30 minutes, repeat 3 times, and then dry naturally to obtain pure silk fibroin;
[0045] (2) Using 98% formic acid to prepare 1 liter of formic acid / hydroxyapatite mixed solution, the content of hydroxyapatite is 10.0%. After the solution is evenly mixed, put the pure silk fibroin into the formic acid / hydroxyapatite mixture and stir at room temperature for 4 hours to obtain a silk fibroin solution with a mass fraction of 15.0%, which is purified by filtration and defoamed by ultrasonic for 0.5 hours. Into spinning dope;
[0046] (3) Under the temperature condition of 30℃, the silk fibroin is sprayed into the hot air at a speed of 5g per minute to form the nascent fiber; the nascent fiber is drafted twice, and the first draft is 1.0 times , The second drafting ratio is 1.5 times to obtain a stable filament fiber;
[0047] (4) Winding the fiber i...
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