Production method of carboxymethyl cellulose acetate butyrate
A technology of carboxymethyl cellulose and sodium carboxymethyl cellulose, which is applied in the production field of carboxymethyl cellulose acetate butyrate, can solve the problem that the intermolecular force increases hydrogen bond force, cannot prepare CMCAB, and is disadvantageous. Esterification reaction and other problems, to achieve the effect of low production process temperature, short production cycle and simple operation process
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Embodiment 1
[0033](1) Preparation of CMC-Na: The performance index of the prepared CMC-Na is: DS=0.12, moisture content 5.3%, purity 99.0%. Disperse 80g of refined cotton powder in isopropanol / water solution, the mass ratio of isopropanol to water is 20.0:1, and the mass ratio of solution to refined cotton powder is 16.5:1. Exclude the air in the reactor, fill it with inert gas, and then add 84.0g of 25%wt NaOH aqueous solution at 10°C to 20°C for alkalization for 1.5h; after alkalization, reduce the temperature of the reaction system to about 10°C, Slowly add 42.9g of 56.0%wt monochloroacetic acid / isopropanol solution for 15-20min, then raise the temperature to 50°C for etherification for 1.5h, then continue to raise the temperature to 75°C for 30min, add 18.0g of 50%wt acetic acid / water solution Neutralize, wash 2-3 times with 85% v / v alcohol / water solution, dry, pulverize and set aside.
[0034] (2) Preparation of CMC-H: Submerge 44.8g of CMC-H in the acidifying solution for acidifica...
Embodiment 2
[0039] (1) Preparation of CMC-Na: The performance index of the prepared CMC-Na is: DS=0.23, moisture content 5.3%, purity 99.0%. Disperse 80g of refined cotton powder in isopropanol / water solution, the mass ratio of isopropanol to water is 14.0:1, and the mass ratio of solution to refined cotton powder is 16.8:1. Exclude the air in the reactor, fill it with inert gas, then add 120.0g of 25%wt NaOH aqueous solution at 10°C to 20°C, and alkalize for 1.5h; after alkalization, reduce the temperature of the reaction system to about 10°C, Slowly add 58.9g of 56.0%wt monochloroacetic acid / isopropanol solution for 15-20min, then raise the temperature to 50°C for etherification for 1.5h, then continue to raise the temperature to 75°C for 30min, add 22.0g of 50%wt acetic acid / water solution Neutralize, wash 2-3 times with 75% v / v alcohol / water solution, dry, pulverize and set aside.
[0040] (2) Preparation of CMC-H: Submerge 50.0g of CMC-H in the acidifying solution for acidification,...
Embodiment 3
[0045] (1) Preparation of CMC-Na: The performance index of the prepared CMC-Na is: DS=0.35, moisture content 5.3%, purity 99.0%. Disperse 80g of refined cotton powder in isopropanol / water solution, the mass ratio of isopropanol to water is 11.6:1, and the mass ratio of solution to refined cotton powder is 17.1:1. Exclude the air in the reactor, fill it with inert gas, then add 144.0g of 25%wt NaOH aqueous solution at 10°C to 20°C, and alkalize for 1.5h; Slowly add 75.0g of 56.0%wt monochloroacetic acid / isopropanol solution for 15-20min, then raise the temperature to 50°C for etherification for 1.5h, then continue to raise the temperature to 75°C for 30min, add 26.0g of 50%wt acetic acid / water solution Neutralize, wash 2-3 times with 75% v / v alcohol / water solution, dry, pulverize and set aside.
[0046] (2) Preparation of CMC-H: Submerge 49.4g of CMC-H in the acidifying solution for acidification, the temperature is 20°C, acidify for 30min, the mass ratio of acidifying solutio...
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