Preparation method of nano-cellulose
A nano-cellulose and cellulose technology, applied in the field of nano-materials, can solve the problems of difficult hydrolysis acid solution, complicated post-treatment process, and difficult treatment of reaction acid solution, so as to speed up the oxidation reaction speed, improve the oxidation reaction efficiency, and react The effect of increased accessibility
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Embodiment 1
[0023] Example 1: Preparation of nanocellulose:
[0024] (1) Pretreatment: After soaking 5 grams of microcrystalline cellulose with 50 grams of sodium hydroxide aqueous solution with a mass concentration of 7% for 10 hours at room temperature, filter out the cellulose and wash with deionized water until the pH of the filtrate The value is 8.
[0025] (2) Oxidation reaction: Disperse the filtered cellulose in 100mL deionized water, add 0.5g sodium bromide and 0.05g 2,2,6,6-tetramethylpiperidine-1-oxide, and stir to After dissolving, add 20g of sodium hypochlorite solution with a mass concentration of 5%, turn on the ultrasonic oscillation, the ultrasonic power is 300w, the frequency is 20kHz, and the pH of the reaction solution is adjusted with 0.5mol / L sodium hydroxide aqueous solution to maintain the pH value of the reaction solution at 10. -11 or so.
[0026] (3) Post-treatment: When the pH value does not change significantly (the reaction lasts for 150 minutes), the reaction sol...
Embodiment 2
[0027] Example 2: Preparation of nano cellulose:
[0028] Disperse 5 grams of microcrystalline cellulose in 30 grams of 9% sodium hydroxide aqueous solution, soak at room temperature for 15 hours, filter out the cellulose and wash with deionized water until the pH of the filtrate is 7. Disperse the filtered cellulose in 200mL deionized water, add 0.75g sodium bromide and 0.1g 2,2,6,6-tetramethylpiperidine-1-oxide respectively, stir to dissolve, add 25g mass The sodium hypochlorite solution with a concentration of 5% is turned on ultrasonic oscillation, the ultrasonic power is 500w, the frequency is 30kHz, and the pH value of the reaction solution is adjusted with 0.5mol / L sodium hydroxide aqueous solution to maintain the pH value of the reaction solution at about 10-11. When there is no significant change in the pH value (reaction lasts 85 minutes), the reaction solution is centrifuged 4 times at 10000 rpm to remove large-size cellulose, and the suspension is freeze-dried to obta...
Embodiment 3
[0029] Example 3: Preparation of nanocellulose:
[0030] Disperse 5 grams of microcrystalline cellulose in 80 grams of 4% potassium hydroxide aqueous solution, soak at room temperature for 20 hours, filter out the cellulose and wash with deionized water until the pH of the filtrate is 6. Disperse the filtered cellulose in 300mL of deionized water, add 0.7g of sodium bromide and 0.03g of 2,2,6,6-tetramethylpiperidine-1-oxide respectively, stir to dissolve, add 15g of mass The sodium hypochlorite solution with a concentration of 5%, turn on the ultrasonic oscillation, the ultrasonic power is 400w, the frequency is 40kHz, and the pH of the reaction solution is adjusted with 0.5mol / L sodium hydroxide aqueous solution to maintain the pH value of the reaction solution at about 10-11. When the reaction reaches the same pH value (reaction lasts 115 minutes), the reaction solution is centrifuged twice at a speed of 15000 rpm to remove large-size cellulose, and the suspension is freeze-dri...
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