Preparation method of high-molecular-weight cellulose acetate butyrate
A technology of acetic acid butyric acid and high molecular weight, which is applied in the field of preparation of high molecular weight cellulose acetate butyrate, can solve the problems of high cost, high metal content, high viscosity of reaction liquid, etc., reduce operating time, reduce waste water discharge, and reduce production cost effect
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Embodiment 1
[0039] Prepare cellulose acetate butyrate as follows:
[0040] (1) Use a pulverizer to pulverize the refined cotton, take 100g of the pulverized 100-200 mesh sieve, put it in a beaker, add 1000g of acetic acid, mix well, soak for 10h, and then centrifuge to remove part of the solution to obtain acetic acid content of 40.5 The activated cellulose powder 168g of wt%.
[0041](2) Weigh 55g of acetic anhydride, 600g of butyric anhydride, 200g of n-butyric acid, and 5g of concentrated sulfuric acid into a 3L jacketed glass kettle, then add the above-mentioned 168g of activated cellulose powder, stir and control the temperature at 20°C, and keep it warm for 10 hours, the esterification reaction solution was obtained.
[0042] (3) Add 4.3 g of sodium acetate into the esterification reaction solution, control the temperature at 20° C. under stirring, and stop the reaction after 20 minutes to obtain a neutralization reaction solution.
[0043] (4) Add 5 g of sodium triacetoxyborohydr...
Embodiment 2
[0046] Prepare cellulose acetate butyrate as follows:
[0047] (1) Use a pulverizer to pulverize the refined cotton, take 100g of the pulverized 100-200 mesh sieve, put it in a beaker, add 2500g of acetic acid, mix well, soak for 5h, and then centrifuge to remove part of the solution to obtain 60wt of acetic acid % activated cellulose powder 250g.
[0048] (2) Weigh 185g of acetic anhydride, 450g of butyric anhydride, 600g of n-butyric acid, and 25g of concentrated sulfuric acid into a 3L jacketed glass kettle, then add the above-mentioned 250g of activated cellulose powder, stir and control the temperature at 30°C, and keep it warm for 5 hours, the esterification reaction solution was obtained.
[0049] (3) Add 30.8 g of sodium acetate to the above-mentioned esterification reaction liquid, control the temperature at 30° C. under stirring, stop the reaction after 30 min, and obtain a neutralization reaction liquid.
[0050] (4) Add 12 g of sodium triacetoxyborohydride to the...
Embodiment 3
[0053] Prepare cellulose acetate butyrate as follows:
[0054] (1) Use a pulverizer to pulverize the refined cotton, take 100g of the pulverized 100-200 mesh sieve, put it in a beaker, add 4500g of acetic acid, mix well, soak for 1h, and then centrifuge to remove part of the solution to obtain acetic acid content of 51.5 206g of activated cellulose powder by wt%.
[0055] (2) Weigh 300g of acetic anhydride, 120g of butyric anhydride, 1000g of n-butyric acid, and 50g of concentrated sulfuric acid into a 3L jacketed glass kettle, then add the above-mentioned 206g of activated cellulose powder, control the temperature at 40°C under stirring, and keep it warm for 3h , to obtain an esterification reaction solution.
[0056] (3) Add 82 g of sodium acetate to the above-mentioned esterification reaction solution, control the temperature at 40° C. under stirring, and stop the reaction after 60 minutes to obtain a neutralization reaction solution.
[0057] (4) Add 30 g of sodium triac...
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