A method for preparing nano-cellulose crystals by ultra-low acid hydrolysis of fibers
A technology of nanocellulose and hydrolyzed fibers, applied in the field of nanocellulose crystal preparation, can solve the problems of strong corrosion, hindering the industrialization process of nanocellulose, and environmental pollution.
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Embodiment 1
[0021] 1) Take 2g of bamboo pulp fiber (1.8 mm≤length≤2.5mm, 15μm≤width≤20μm), and perform ultrasonic pretreatment, ultrasonic time 30min, power 500W;
[0022] 2) Add 38ml of hydrochloric acid with a mass fraction of 0.08% and 0.8ml of distilled water to the bamboo pulp fiber after ultrasonic pretreatment in the previous step; the reaction temperature is 160°C, the reaction time is 50min, and the reaction pressure is 5MPa;
[0023] 3) After the reaction is over, centrifuge the reaction product at a speed of 5000rpm, take the precipitate and wash it repeatedly with deionized water and centrifuge until the upper layer liquid is in a light blue or milky white suspension state, take the upper layer liquid for dialysis for 4 days; then ultrasonically disperse , the supernatant is the nanocellulose crystals.
[0024] The yield of nanocellulose crystals obtained by the above preparation method is 32%, the length is 100 nm, and the width is 16 nm.
Embodiment 2
[0026] 1) Take 3g of bamboo pulp fiber (1.8 mm≤length≤2.5mm, 15μm≤width≤20μm), and perform ultrasonic pretreatment, ultrasonic time 40min, power 750W;
[0027] 2) Add 39ml of hydrochloric acid with a mass fraction of 0.1% and 0.5ml of distilled water to the bamboo pulp fiber after ultrasonic pretreatment in the previous step; the reaction temperature is 170°C, the reaction time is 45min, and the reaction pressure is 10MPa;
[0028] 3) After the reaction is over, centrifuge the reaction product at a speed of 5000rpm, take the precipitate and wash it repeatedly with deionized water and centrifuge until the upper layer liquid is in a light blue or milky white suspension state, take the upper layer liquid for dialysis for 4 days, and then ultrasonically disperse , the supernatant is the nanocellulose crystals.
[0029] The yield of nanocellulose crystals obtained by the above preparation method is 34%, the length is 80nm, and the width is 10nm.
Embodiment 3
[0031] 1) Take 3g of wheat straw pulp fiber (1 mm≤length≤1.5mm, 10μm≤width≤16μm), and perform ultrasonic pretreatment, ultrasonic time 40min, power 600W;
[0032] 2) Add 38ml of hydrochloric acid with a mass fraction of 0.07% and 0.5ml of distilled water to the wheat straw fiber pretreated by ultrasonic in the previous step; the reaction temperature is 170°C, the reaction time is 40min, and the reaction pressure is 10MPa;
[0033] 3) After the reaction is over, centrifuge the reaction product at a speed of 6000rpm, take the precipitate and wash it repeatedly with deionized water and centrifuge until the upper layer liquid is in a light blue or milky white suspension state, take the upper layer liquid for dialysis for 4 days, and then ultrasonically disperse , the supernatant is the nanocellulose crystals.
[0034] The yield of nanocellulose crystals obtained by the above preparation method is 36%, the length is 60nm, and the width is 20nm.
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