Preparation method of cellulose diacetate
A technology of cellulose diacetate and cellulose is applied in the field of resource utilization of cellulose, which can solve the problems of uneven product properties, non-toxicity, and difficulty in finding products.
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Embodiment 1
[0019] Add 1g of cellulose (about 6.2mmol), 0.25g of acetic acid, 2.5g of acetic anhydride, 30ml of 1-butyl-3-methylimidazole chloride and 0.5mmol of Amberlyst15 into a three-necked flask, react at 80°C for 8h, and cool to room temperature , filtered, and the solid is the recovery catalyst; 120ml of deionized water was added to the ionic liquid phase, and a precipitate was precipitated, which was centrifuged. The supernatant liquid was recovered into a flask, deionized water was removed by rotary evaporation, and vacuum-dried at 100° C., the recovered ionic liquid was obtained. Transfer the precipitate at the bottom of the centrifuge tube into a flask, add dichloromethane, dissolve, filter, and evaporate the solvent in the clear liquid. A film-like product can be obtained in the flask. The product is removed with acetone, rotary evaporated, and dried to obtain the product. The degree of substitution is 2.03.
Embodiment 2
[0021] Add 1g of cellulose (about 6.2mmol), 0.25g of acetic acid, 2.5g of acetic anhydride, 30ml of 1-butyl-3-methylimidazole chloride and 0.5mmol of Amberlyst15 into a three-necked flask, react at 80°C for 10h, and cool to room temperature , filtered, and the solid is the recovered catalyst; 120ml of deionized water was added to the liquid phase, and a precipitate was precipitated, which was then centrifuged. The supernatant liquid was recovered into a flask, deionized water was removed by rotary evaporation, and vacuum-dried at 100° C., the recovered ionic liquid was obtained. Transfer the precipitate at the bottom of the centrifuge tube into a flask, add dichloromethane, dissolve, filter, and evaporate the solvent in the clear liquid. A film-like product can be obtained in the flask. The product is removed with acetone, rotary evaporated, and dried to obtain the product. The degree of substitution is 2.16.
Embodiment 3
[0023] Add 1g of cellulose (about 6.2mmol), 0.25g of acetic acid, 2.5g of acetic anhydride, 30ml of 1-butyl-3-methylimidazole chloride and 0.5mmol of Amberlyst15 into a three-necked flask, react at 100°C for 8h, and cool to room temperature , centrifugal separation, the solid is the recovery catalyst, 120ml of deionized water is added to the liquid phase, there is precipitation, and the centrifugal separation is carried out. The supernatant liquid was recovered into a flask, deionized water was removed by rotary evaporation, and vacuum-dried at 100° C., the recovered ionic liquid was obtained. Transfer the precipitate at the bottom of the centrifuge tube into a flask, add dichloromethane, dissolve, filter, and evaporate the solvent in the clear liquid. A film-like product can be obtained in the flask. The product is removed with acetone, rotary evaporated, and dried to obtain the product. The degree of substitution is 2.38.
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