【作者】 王秋明；

【导师】 许湧深；

【作者基本信息】 天津大学 ， 材料化学工程， 2008， 硕士

【摘要】 以邻苯二甲酸酐对羟丙基甲基纤维素(HPMC)功能化改性,分别在经典的冰醋酸体系和新型的有机溶剂体系合成了符合药典要求的羟丙基甲基纤维素邻苯二甲酸酯(HPMCP)粉末,IR测试结果表明粉末为目标产物。重点考察了有机溶剂体系下各因素对酯化反应的影响。实验证明,通过调节邻苯二甲酸酐的用量可以控制HPMCP粉末的苯甲酸甲酰基含量。反应温度太高容易引发第二羧基参与到酯化反应中,温度太低催化剂活性不能得到充分发挥,所得到的产品的苯甲酸甲酰基含量过低。有机溶剂体系比冰醋酸体系具有更大优点,主要表现在:反应收率高;溶剂对设备无腐蚀;后处理过程简易,游离酸含量易达标;溶剂可回收利用,无溶剂外排所带来的环境污染等问题。以自制的HPMCP为起始物,在不使用任何有机溶剂的情况下,采用水乳化方法,成功制备了HPMCP的乳液水分散体。TEM测试表明所得HPMCP水分散体乳胶粒为近似光滑球形。DLS测试表明,乳化剂用量较多时可得到粒径更加均一的乳胶粒。HPMCP水分散体游离膜具有良好的成膜性能,SEM表征游离膜具有良好的致密性。拉伸测试表明,粒度均匀的HPMCP水分散体具有较好的力学性能。以HPMC作为乳化剂,比Tween80为乳化剂的水分散体,可以赋予游离膜材料更为优良的力学性能。不同苯甲酸甲酰基含量的HPMCP水分散体游离膜样品在模拟人工胃液中2小时内均不溶解,这符合药典中对于肠溶包衣材料的要求。HPMCP游离膜样品在模拟人工肠液中的溶解速率随HPMCP中苯甲酸甲酰基含量的增加而增大。更多还原

【Abstract】 Hydroxypropyl methylcellulose phthalate (HPMCP) was prepared in classic Glacial Acetic Acid-Sodium Acetate system and new organic solvent system respectively, with HPMC as starting material and phthalic anhydride as functional graft monomer, which meet for the requirements of the Pharmacopoeia. IR test indicated that the product is the target product HPMCP. The experiments proved that the phthalyl content can be controlled by the dosage of phthalic anhydride. The reaction temperature should not be too high or too low, while high temperature will cause the reaction of the second carboxyl and low temperature can not provide enough power to the catalyst. By comparison, organic system has more benefits than Glacial Acetic Acid-Sodium Acetate system. It has higher yield than the Glacial Acetic Acid-Sodium Acetate system. The solvent it used does not corrode the equipment. It’s easier to wash the product and easier to control the content of free acid in organic system. The solvent can be recycled and so avoid the environment pollution caused by solvent discharge.Hydroxypropyl methylcellulose phthalate (HPMCP) prepared was used as the starting material to prepare HPMCP water dispersion by water emulsion method, during which none of the organic solvent was used. TEM test showed HPMCP water dispersion latex particle is near-spherical. DLS test indicated that with the increase of the dosage of emulsification, the latex particle has more uniform micelle particles. SEM test showed that HPMCP water dispersion dissociate film has high compact-ability. Stretching test indicated that the HPMCP water dispersion with better particle size distribution have better mechanical property. The water dispersion with HPMC as emulsifier has excellent mechanical property. HPMCP water dispersion dissociate film has better film forming property, and HPMCP water dispersion dissociate films with different phthalyl contents were all insoluble in the simulated gastric fluid within 2 hours, which meets the requirement of China pharmacopeia. The solution rate of HPMCP water dispersion dissociate film can be accelerated with increasing the phthalyl content.更多还原