Preparation method of cellulose acetate butyrate
A technology of acetate butyric acid and cellulose, which is applied in the field of cellulose derivatives, can solve the problems of severe cellulose degradation, uneven heating, long hydrolysis time, etc., and achieve the effects of improved reaction efficiency, stable performance, and avoiding serious degradation
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Embodiment 1
[0053] (1) join coconut shell gac to soak 3h in glacial acetic acid, obtain the gac of adsorbing glacial acetic acid;
[0054] (2) Add 10 g of refined cotton linters and 80 g of activated carbon for absorbing glacial acetic acid into 200 g of 95% butyric acid aqueous solution, stir and activate for 1.2 h at 25° C., filter to obtain a mixture of activated refined cotton linters and activated carbon;
[0055] (3) Add the mixture of the activated refined cotton linters and activated carbon into DMSO / TBAF 180g and stir for 15min, filter to obtain a solution containing activated cellulose;
[0056] (4) Add 98% concentrated sulfuric acid 0.8g, acetic anhydride 15g and butyric anhydride 35g in the solution containing the activated cellulose, stir while microwave heating carries out esterification reaction, the esterification reaction temperature is 45 ℃, the esterification reaction time For 1h, the esterification feed liquid was obtained;
[0057] (5) Add 50 g of water to the esteri...
Embodiment 2
[0063] (1) Join coconut shell activated carbon and soak 2h in glacial acetic acid, obtain the activated carbon of adsorption glacial acetic acid;
[0064] (2) Add 10 g of refined cotton linters and 50 g of activated carbon for absorbing glacial acetic acid into 130 g of 93% butyric acid aqueous solution, stir and activate for 1.5 h at 20° C., filter to obtain a mixture of activated refined cotton linters and activated carbon;
[0065] (3) Add the mixture of the activated refined cotton linters and activated carbon into DMSO / TBAF 120g and stir for 30min, filter to obtain a solution containing activated cellulose;
[0066] (4) Add 0.5g of 98% concentrated sulfuric acid, 10g of acetic anhydride and 30g of butyric anhydride to the solution containing activated cellulose, stir while heating with microwave to carry out esterification reaction, the esterification reaction temperature is 40 ℃, the esterification reaction time For 2h, obtain the esterification feed liquid;
[0067] (5...
Embodiment 3
[0073] (1) join coconut shell gac to soak 6h in glacial acetic acid, obtain the gac of adsorbing glacial acetic acid;
[0074] (2) Add 10 g of refined cotton linters and 90 g of activated carbon for absorbing glacial acetic acid into 220 g of 94% butyric acid aqueous solution at 30° C. for stirring and activation for 1 h, filter to obtain a mixture of activated refined cotton linters and activated carbon;
[0075] (3) Add the mixture of activated refined cotton linters and activated carbon into DMSO / TBAF 200g and stir for 20min, filter to obtain a solution containing activated cellulose;
[0076] (4) Add 98% concentrated sulfuric acid 1g, acetic anhydride 20g and butyric anhydride 50g in the solution containing the cellulose after activation, stir while microwave heating carries out esterification reaction, and the esterification reaction temperature is 60 ℃, and the esterification reaction time is 0.5h, obtain esterification feed liquid;
[0077] (5) Add 60 g of water to the...
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Abstract
Description
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Application Information
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