A method for preparing nanocrystalline cellulose from ultra-low acid hydrolyzed fibers
A nano-microcrystalline and hydrolyzed fiber technology, applied in the field of nano-microcrystalline cellulose preparation, can solve the problem that nano-microcrystalline cellulose is difficult to control the degree of cellulose degradation, equipment is highly corrosive, and hinders the industrialization process of nano-microcrystalline cellulose. and other problems, to achieve the effect of broad industrial application prospects, less equipment corrosion and less pollution
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Embodiment 1
[0020] 1) Take 4g of bamboo pulp fiber (1.8mm≤length≤2.5mm, 15μm≤width≤20μm), add 38ml of hydrochloric acid with a mass fraction of 0.08% and 0.8ml of distilled water; the reaction temperature is 150°C, the reaction time is 50min, and the reaction pressure is 5MPa ;
[0021] 2) 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 nano-microcrystalline cellulose.
[0022] The nanocrystalline cellulose obtained by the above preparation method has a yield of 41%, a length of 800nm, and a width of 60nm.
Embodiment 2
[0024] 1) Take 4g of bamboo pulp fiber (1.8mm≤length≤2.5mm, 15μm≤width≤20μm), add 38ml of hydrochloric acid with a mass fraction of 0.1% and 0.9ml of distilled water; the reaction temperature is 160°C, the reaction time is 70min, and the reaction pressure is 10Mpa ;
[0025] 2) After the reaction is over, centrifuge the reaction product at a speed of 6000rpm, take the precipitate, wash and centrifuge it repeatedly with deionized water until the upper layer is in the state of a light blue or milky white suspension, and dialyze the upper layer for 4 days; then Ultrasonic dispersion, the supernatant is nano-microcrystalline cellulose.
[0026] Its yield of nano-microcrystalline cellulose obtained by the above-mentioned preparation method is 45%, such as figure 1 , figure 2 As shown in Table 1, the prepared nanocrystalline cellulose has a length of 450nm and a width of 30nm.
[0027] Table 1 is the size distribution of nano-microcrystalline cellulose
[0028] ...
Embodiment 3
[0031] 1) Take 5g of wheat straw pulp fiber (1 mm≤length≤1.5mm, 10μm≤width≤16μm), add 39ml of sulfuric acid with a mass fraction of 0.08% and 0.6ml of distilled water; the reaction temperature is 180°C, the reaction time is 60min, and the reaction pressure is 15Mpa ;
[0032] 2) After the reaction is over, centrifuge the reaction product at a speed of 7000rpm, 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 nano-microcrystalline cellulose;
[0033] The nanocrystalline cellulose obtained by the above preparation method has a yield of 44%, a length of 600nm, and a width of 40nm.
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