Process for producing cellulose ether acetate succinate
A technology of ether succinate and cellulose acetate, applied in the field of preparing cellulose acetate ether succinate, can solve the problems of difficult handling, insufficient film strength and the like
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[0053] All parts and percentages are by weight unless otherwise mentioned. In the examples, the following test procedure was used.
[0054] Viscosity of hydroxypropylmethylcellulose (HPMC) samples
[0055] The viscosity of cellulose ethers was determined as a 2% by weight aqueous solution at 20°C as described in the United States Pharmacopoeia (USP 35, "Hypromellose", pp. 423-424 and 3467-3469). Viscosities of less than 600 mPa·s were determined by Ubbelohde viscometry and viscosities of 600 mPa·s or greater were determined using a Brookfield viscometer as described in the US Pharmacopoeia. A description of the preparation of 2 wt% HPMC solutions and the conditions for Ubbelohde and Brookfield viscosity measurements is published in the United States Pharmacopoeia (USP 35, "Hypromellose", pages 423-424 and 3467-3469 and ASTM D-445 cited therein and ISO 3105).
[0056] Viscosity of hydroxypropylmethylcellulose acetate succinate (HPMCAS)
[0057] A 2.0% by weight solution ...
example 9 and 10
[0093] Generate HPMCAS of Examples 9 and 10
[0094] Glacial acetic acid, acetic anhydride, succinic anhydride, HPMC E100LV, sodium acetate (anhydrous) and potassium chlorate were introduced into a 1 L volume reaction vessel in the amounts listed in Table 3 below. The weight ratios of reactants in Examples 9 and 10 corresponded to those in Examples 1-5 (Table 1) of US Patent No. 4,226,981, except that potassium chlorate was not used in the procedure of US Patent No. 4,226,981.
[0095] Glacial acetic acid is readily absorbed by HPMC powder. The reaction mixture had a solid appearance and could not be stirred sufficiently to obtain a homogeneous reaction mixture. The mixture was heated at 80°C for 5 hours to effect esterification. As the esterification and partial depolymerization proceed, the viscosity of the reaction mixture decreases and the reaction mixture can be sufficiently stirred to obtain a homogeneous mixture. After 5 hours, HPMCAS was precipitated from the reac...
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