Preparation method of low-propionyl-content cellulose acetate propionate mixed ester
A technology of cellulose acetate propionate and low propionyl group is applied in the field of cellulose lipid derivatives, and can solve the problems of rare cellulose acetate propionate mixed ester, inaccurate control of hydrolysis reaction, long esterification reaction time, etc. Reduce corrosion and environmental pollution, increase application, and stabilize product performance
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Embodiment 1
[0033] The preparation method of the low propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:
[0034] (1) Weigh 650g of wood pulp, 296g of propionic acid, 2250g of acetic acid, 118g of acetic anhydride, 2070g of propionic anhydride, and 19.5g of catalyst. Polyacid Catalyst H 3 PW 12 o 40 11.7g;
[0035] (2) Spray 650g of wood pulp with 325g of acetic acid, and then activate it at 25°C for 0.5h;
[0036] (3) Mix the remaining acetic acid with propionic acid, propionic anhydride, acetic anhydride and catalyst, and cool the mixture to -10°C for use;
[0037] (4) Put the solid wood pulp activated in step (2) into the cooling liquid in step (3) within 5 minutes, fully stir without external cooling, and the reaction will naturally heat up so that the temperature in the final esterification reaction system does not exceed 50 ℃, the reaction time is set to 90min;
[0038] (5) Add 45g of magnesium acetat...
Embodiment 2
[0042] The preparation method of the low propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:
[0043] (1) Weigh 650g of wood pulp, 296g of propionic acid, 2250g of acetic acid, 118g of acetic anhydride, 2070g of propionic anhydride, and 52g of catalyst. Acid Catalyst H 3 PW 12 o 40 20.8g;
[0044] (2) Spray 650g of wood pulp with 1300g of acetic acid, and then activate it at 35°C for 3 hours;
[0045] (3) Mix the remaining acetic acid with propionic acid, propionic anhydride, acetic anhydride and catalyst, and cool the mixture to 5°C for use;
[0046] (4) Put the solid wood pulp activated in step (2) into the cooling liquid in step (3) within 8 minutes, fully stir without external cooling, and the reaction will naturally heat up so that the temperature in the final esterification reaction system does not exceed 50 ℃, the reaction time is set to 120min;
[0047] (5) Add 50g of magnesium acetate s...
Embodiment 3
[0051] The preparation method of the low propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:
[0052] (1) Weigh 650g of wood pulp, 296g of propionic acid, 2250g of acetic acid, 118g of acetic anhydride, 2070g of propionic anhydride, and 36g of catalyst. The catalyst is a mixture of liquid acid catalyst and heteropolyacid catalyst. Catalyst H 3 PW 12 o 40 18g;
[0053] (2) Spray 650g of wood pulp with 650g of acetic acid, and then activate it at 30°C for 2 hours;
[0054] (3) Mix the remaining acetic acid with propionic acid, propionic anhydride, acetic anhydride and catalyst, and cool the mixture to 5°C for use;
[0055] (4) Put the solid wood pulp activated in step (2) into the cooling liquid in step (3) within 6 minutes, fully stir without external cooling, and the reaction will naturally heat up so that the temperature in the final esterification reaction system does not exceed 50 ℃, the react...
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