Preparation method of cellulose acetate
A technology of cellulose acetate and acetate, applied in the field of polymer chemistry, can solve the problems of low degree of esterification, low viscosity, uneven activation, etc. Effect
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Embodiment l
[0033] 1, the cellulose of 1 weight part is activated 1h at 40 ℃ with glacial acetic acid, and the weight ratio of cellulose and glacial acetic acid is 1: 10, and cellulose refers to wood pulp.
[0034] 2, during the esterification process, directly utilize the acetic acid in the activation process as a solvent, add 98% sulfuric acid earlier, and the consumption is 0.5% of the cellulose weight. Then add acetic anhydride as the reaction solution to fully acetylate the cellulose, and the dosage is 4.5 times that of the cellulose. The esterification temperature is 40°C, and the esterification time is 3.5h.
[0035] 3. For hydrolysis, the temperature of the esterification liquid is required to be 25° C., and the hydrolyzed liquid is 80% (mass percentage concentration) acetic acid, which is slowly added while stirring. The weight ratio of cellulose to hydrolyzate is 1:1. The hydrolysis time is 1.5 hours, so that the acetic acid content of the cellulose acetate is between 60.5-62....
Embodiment 2
[0039] 1. 1 part by weight of cellulose is activated with glacial acetic acid for 1.5 h at 35° C., the weight ratio of cellulose to glacial acetic acid is 1:15, and cellulose refers to cotton pulp.
[0040] 2, during the esterification process, directly utilize the acetic acid in the activation process as solvent, add catalyzer earlier, consumption is 0.65% of cellulose weight, and catalyzer refers to 98% sulfuric acid. Then add acetic anhydride as a reaction solution to fully acetylate the cellulose, and the dosage is 4 times that of the cellulose. The esterification temperature is 35°C, and the esterification time is 4h.
[0041] 3. For hydrolysis, the temperature of the esterification liquid is required to be 20° C., and the hydrolyzed liquid is 75% (mass percentage concentration) acetic acid, which is slowly added while stirring. The weight ratio of cellulose to hydrolyzate is 1:1.2. The hydrolysis time is 1.2 hours, so that the acetic acid content of cellulose acetate i...
Embodiment 3
[0044] 1. 1 part by weight of cellulose is activated with glacial acetic acid at 55° C. for 1.5 h, the weight ratio of cellulose to glacial acetic acid is 1:8, and cellulose refers to cotton pulp.
[0045] 2, during the esterification process, directly utilize the acetic acid in the activation process as solvent, add catalyzer earlier, consumption is 0.65% of cellulose weight, and catalyzer refers to 98% sulfuric acid. Then add acetic anhydride as a reaction solution to fully acetylate the cellulose, and the dosage is 6 times that of the cellulose. The esterification temperature is 55°C, and the esterification time is 3h.
[0046] 3. For hydrolysis, the temperature of the esterification liquid is required to be 15° C., and the hydrolyzed liquid is 65% (mass percentage concentration) acetic acid, which is slowly added while stirring. The weight ratio of cellulose to hydrolyzate is 1:1.1. The hydrolysis time is 1.2 hours, so that the acetic acid content of cellulose acetate is...
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