A kind of preparation method of cellulose-based carbon nanofiber
A carbon nanofiber, cellulose-based technology, applied in plant fibers, fiber treatment, fiber chemical characteristics, etc., can solve the problems of limited electrochemical energy storage characteristics, lack of internal connection and support, etc., to achieve good electrochemical performance and cycle. Effects of stability, improved electrical conductivity and ion transport efficiency
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[0035] The present invention proposes a preparation method for cellulose-based carbon nanofibers, combining figure 1 The schematic flow chart of an embodiment of the preparation method of the cellulose-based carbon nanofiber shown, the preparation method of the cellulose-based carbon nanofiber comprises the following steps:
[0036] S10. Add a mixed solution of acetic acid and acetic anhydride to the cellulose, then add concentrated sulfuric acid for reaction, add aqueous acetic acid for hydrolysis after the reaction, add water after the hydrolysis to precipitate acetylated modified cellulose.
[0037] Wherein, the cellulose is bamboo pulp cellulose, and the mass fraction of α-cellulose in the bamboo pulp cellulose is not less than 96%. In the mixed solution, the volume ratio of acetic acid to acetic anhydride is (4.5-5.5):9, preferably 5:9 in this embodiment; the amount of cellulose and acetic acid added is 4.5-5.5 per 1 g of cellulose ml acetic acid, preferably add 5ml acet...
Embodiment 1
[0053] (1) take by weighing 2.5g bamboo cellulose and soak in acetic acid and acetic anhydride, control acetic acid / acetic anhydride volume ratio to be 5:9, the mass volume ratio of bamboo cellulose and acetic acid is 1 / 5 (g / ml), constantly Stir and add concentrated sulfuric acid to react at a constant temperature of 50°C for 2.5 hours, then add acetic acid aqueous solution for hydrolysis for 3 hours, add water to precipitate a precipitate after the reaction, wash the precipitate with deionized water 3 times, and then wash 3 times with absolute ethanol, and then the product Drying in an oven at 80°C to obtain solid powdered acetylated modified cellulose;
[0054] (2) Dissolve acetylated modified cellulose in acetone-N,N-dimethylacetamide (2 / 1, v / v) mixed solvent to form a solution with a mass fraction of 37%, and spin at a spinning voltage of 22kV, Under the conditions of a spinning distance of 15 cm and a flow rate of spinning solution of 1 ml / h, acetylated modified nanofiber...
Embodiment 2
[0058] (1) take by weighing 2.5g bamboo cellulose and soak in acetic acid and acetic anhydride, the control acetic acid / acetic anhydride volume ratio is 4.5:9, and the mass volume ratio of bamboo cellulose and acetic acid is 1 / 4.5 (g / ml), constantly Stir and add concentrated sulfuric acid to react at a constant temperature of 40°C for 3 hours, then add acetic acid aqueous solution for hydrolysis for 1 hour, add water to precipitate a precipitate after the reaction is completed, wash the precipitate with deionized water for 3 times, and then wash with absolute ethanol for 3 times, and then release the product drying in an oven at 60°C to obtain solid powdered acetylated modified cellulose;
[0059] (2) Dissolve acetylated modified cellulose in acetone-N,N-dimethylacetamide (2 / 1, v / v) mixed solvent to form a solution with a mass fraction of 24%, and spin at a spinning voltage of 15kV, Under the conditions of spinning distance 10cm and spinning solution flow rate 0.5ml / h, electro...
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