Method for separating straw acetylized component and preparing straw cellulose acetate
A technology of cellulose acetate and acetylation, applied in the field of utilization of straw waste resources, to achieve the effects of increasing reactivity, saving resources, and improving utilization
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Embodiment 1
[0030] Embodiment 1: 3 g of steam-exploded corn stalks after drying, then add equal volumes of glacial acetic acid and acetic anhydride, liquid-solid ratio 12: 1 (weight ratio), add sulfuric acid 0.03 g, add in the flask after fully mixing, in Stir at 50°C for 30min, then raise the temperature to 120°C, keep it warm for 2h, and cool to room temperature after the reaction;
[0031] Pour it into a centrifuge tube, centrifuge at 10000r / min for 10min, then separate the supernatant from the precipitate, the supernatant is the acetylated product;
[0032] Discard the precipitate; wash the supernatant with water, precipitate occurs after washing, then suction filter, wash with water until neutral, pulverize, boil, dry, and weigh the obtained acetylated product;
[0033] Then the washed supernatant precipitate is refluxed with acetone for 2 hours, the insoluble in acetone is cellulose triacetate, and the soluble in acetone is cellulose diacetate, acetylated lignin and acetylated hemic...
Embodiment 2
[0041] Embodiment 2: 3 g of steam-exploded corn stalks after drying, then add equal volumes of glacial acetic acid, acetic anhydride, liquid-solid ratio 12: 1 (weight ratio), sulfuric acid 0.11 g, add in the flask after fully mixing, at 50 ℃ Stir for 30 minutes, then heat up to 120°C, keep warm for 2 hours, and cool to room temperature after the reaction is complete;
[0042] Pour it into a centrifuge tube, centrifuge at 8000r / min for 20min, then separate the supernatant from the precipitate, the supernatant is the acetylated product;
[0043]Discard the precipitate; wash the supernatant with water, precipitate occurs after washing, then suction filter, wash with water until neutral, pulverize, boil, dry, and weigh the obtained acetylated product;
[0044] Then the washed supernatant precipitate was refluxed with acetone for 0.5h, the insoluble in acetone was cellulose triacetate, and the soluble in acetone was acetylated lignin and acetylated hemicellulose. Most of the aceto...
Embodiment 3
[0052] Example 3: 3 g of steam-exploded corn stalks after drying, then add equal volumes of glacial acetic acid, acetic anhydride, liquid-solid ratio 12: 1 (weight ratio), sulfuric acid 0.22 g, add in the flask after fully mixing, at 50 ℃ Stir for 30 minutes, then heat up to 120°C, keep warm for 2 hours, cool to room temperature after the reaction, pour it into a centrifuge tube, and centrifuge at 9000r / min for 15 minutes, then separate the supernatant from the precipitate, the supernatant is the acetylated product, discard the precipitate; wash the supernatant with water, precipitate occurs after washing, then suction filter, wash with water until neutral, pulverize, boil, dry, and weigh. Then the washed supernatant was refluxed with acetone for 1 hour, the insoluble in acetone was cellulose triacetate, and the soluble in acetone was acetylated lignin and acetylated hemicellulose. Most of the acetone was distilled off, and substances soluble in acetone after adding water prec...
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