Cellulose nanocrystal and preparation method thereof based on oxidation reduction system
A cellulose and nanocrystal technology, applied in the field of nanomaterials and their preparation, can solve the problems of complex and harsh preparation process of Tempo reagent oxidation method, unsuitable for industrialized large-scale production, expensive Tempo reagent, etc., so as to save preparation cost and reduce The effect of preparing energy consumption and shortening the total time
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[0047] Example 1
[0048] Soak 5g of pulp cellulose with 250mL of 4% sodium hydroxide solution and swell for 24h, then use a mixer to pulverize it into cotton wool, wash it with deionized water until the pH of the pulp cellulose is the same as that of deionized water, and then dry; in this step The sequence of swelling and crushing has no significant effect on the result. It can be swelled first and then crushed, or crushed and then swelled;
[0049] Disperse the pretreated cellulose raw material in 300mL deionized water, add 5g hydrogen peroxide and 1g ferrous sulfate, stir at 60°C for 1 hour, and use a cell pulverizer to perform mechanical defibrillation treatment at 49% power for 20 minutes, and then Continue to react at 60°C for 4 hours to stop the reaction, and the total reaction time is 5 hours. After the reaction, the cellulose hydrolysate was centrifuged at a speed of 8000 rpm / min for 10 minutes in a high-speed centrifuge, and then the precipitate was washed repeatedly wi...
Example Embodiment
[0052] Example 2
[0053] The oxidizing agent used is ammonium persulfate, the reducing agent used is sodium sulfite, and all other conditions (such as the type of raw material, the amount and the process flow, etc.) are the same as in Example 1, to obtain a stable suspension of cellulose nanocrystals. The average crystal length is about 283nm, the average diameter is 19nm, the yield is 50%, and the PDI is 0.3.
[0054] In addition, the oxidant ammonium persulfate in this embodiment can not only be matched with sodium sulfite, but also can be matched with reducing agents such as formic acid, succinic acid, ethanol, methanol, sodium hydride, sodium borohydride, etc., to obtain cellulose nanocrystals. The combination of sodium sulfite works best.
Example Embodiment
[0055] Example 3
[0056] The oxidizing agent used is sodium permanganate, the reducing agent used is formic acid, and all other conditions (such as the type of raw material, the amount and the process flow, etc.) are the same as in Example 1. A stable cellulose nanocrystal suspension is obtained. The cellulose obtained by measurement The average length of the nanocrystals is about 253nm, the average diameter is 18nm, the yield is 49%, and the PDI is 0.3.
[0057] In addition, the oxidant sodium permanganate in this embodiment can be matched not only with formic acid, but also with reducing agents such as oxalic acid, succinic acid, ferrous sulfate, methanol, sodium hydride, and sodium borohydride to obtain cellulose nanocrystals. , Among them, it has the best effect with formic acid.
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