Sulfuric acid esterification modified cellulose nanofibers and method for producing cellulose nanofibers
A technology for modifying cellulose and nanofibers, which is applied in the field of sulfated modified cellulose nanofibers and cellulose nanofibers. small damage effect
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Embodiment 1
[0224] Put 9g of DMSO, 1.5g of acetic anhydride (concentration in the defibrillation solution: 14% by weight) and 0.2g of sulfuric acid (concentration in the defibrillation solution: 1.87% by weight) into a 20ml sample bottle, and place it at a room temperature of 23°C. Use a magnetic stirrer to stir for about 30 seconds to prepare a fibrillation solution.
[0225] Next, 0.3 g of cellulose pulp was added, and the mixture was stirred at the same room temperature for another 60 minutes. After stirring, a defibrillation solution containing cellulose was added to 160 ml of a 0.2% by weight aqueous sodium hydrogen carbonate solution and mixed to neutralize the sulfuric acid. Then, the supernatant was removed by centrifugation. Then add 80 ml of distilled water and 80 ml of ethanol, stir until evenly dispersed, and then centrifuge under the same centrifugal conditions to remove the supernatant. Repeat the same steps to clean 3 times. Among them, the centrifugal separation speed is 1...
Embodiment 2
[0231] Except that the addition amount of acetic anhydride is set to 1g (concentration in the defibrillation solution: 9.9% by weight), the addition amount of sulfuric acid is set to 0.13g (the concentration in the defibrillation solution: 1.28% by weight), and the treatment time is set to Except for 110 minutes, the same operation as in Example 1 was carried out to obtain cellulose nanofibers.
[0232] The obtained cellulose nanofibers were evaluated in the same manner as in Example 1. The appearance of the obtained dispersion liquid was a transparent gel almost equivalent to that of Example 1, and the cellulose nanofiber concentration was 0.546% by weight. Show the SEM photo on Image 6 . As a result of SEM observation, the average fiber diameter of the obtained fiber was basically 10 nm or less, and it did not substantially contain nanofibers or fine fibers with a fiber diameter of 20 nm or more. In addition, the 0.3% by weight aqueous dispersion of cellulose nanofibers had ...
Embodiment 3
[0233] Except that the addition amount of acetic anhydride was changed to 1.2 g (concentration in the defibrillation solution: 11.7% by weight), and the addition amount of sulfuric acid was changed to 0.09 g (concentration in the defibrillation solution: 0.87% by weight), the same as the examples 2 The same operation is performed to obtain cellulose nanofibers. Among them, in order to neutralize sulfuric acid, 150 ml of a 0.1% by weight sodium bicarbonate aqueous solution was used.
[0234] The obtained cellulose nanofibers were evaluated in the same manner as in Example 2. The appearance of the obtained dispersion liquid was a transparent gel almost equivalent to that of Example 1, and an aqueous dispersion liquid having a cellulose nanofiber concentration of 0.540% by weight was obtained. Show the SEM photo on Figure 7 . The average fiber diameter of the obtained fiber was 10 nm or less, and it contained substantially no nanofiber or micro fiber with a fiber diameter of 20 n...
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Abstract
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