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Formation of Biodegradable Polymeric Fine Particles by Supercritical Antisolvent Precipitation Process

机译:超临界反溶剂沉淀法制备可生物降解的聚合物细颗粒

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The supercritical antisolvent (SAS) precipitation process as a 'green' alternative to specialty particles recrystalli-zation was successfully used to generate poly(L-lactide) acid (L-PLA) from dichloromethane (DCM) solution using CO2 as antisolvent. The influence of main operating parameters on the synthesis of L-PLA particles in the SAS process was methodically examined. In particular, anti-solvent addition rate (30, 40, 50, and 60 g/min), temperature (35, 40 C, 45°C, and 50C), solute concentration (50, 75,100, and 150 mg/10 ml), and solution addition rate (1, 2.5,5, and 7.5 ml/min). These parameters could be tuned to give a mean particle diameter of 0.62 μm. It was found using scanning electron microscopy and laser diffraction that increasing the antisolvent addition rate and the solution addition rate, while decreasing the temperature and solute concentration, led to a decrease in the L-PLA mean particle diameter. Furthermore, a unimodal particle size distribution was obtained at the higher solution and antisolvent addition rates. Spherical-like primary particles have been obtained in all the experimental runs; thus, no change of particle morphology with the process parameters has been noticed. These results manifested that SAS recrystallization process is a valuable technique to generate reproducibly polymer particles with controlled size and size distribution.
机译:作为特殊颗粒重结晶的“绿色”替代品,超临界抗溶剂(SAS)沉淀工艺已成功用于以二氧化碳(DCM)为反溶剂的二氯甲烷(DCM)溶液中生成聚(L-丙交酯)酸(L-PLA)。系统地研究了主要操作参数对SAS工艺中L-PLA颗粒合成的影响。特别是抗溶剂添加速度(30、40、50和60 g / min),温度(35、40 C,45°C和50C),溶质浓度(50、75,100和150 mg / 10 ml) )和溶液添加速率(1、2.5、5和7.5 ml / min)。可以调整这些参数以提供0.62μm的平均粒径。使用扫描电子显微镜和激光衍射发现,增加抗溶剂添加速率和溶液添加速率,同时降低温度和溶质浓度,导致L-PLA平均粒径减小。此外,在较高的溶液和反溶剂添加速率下获得了单峰粒度分布。在所有实验运行中均获得了球状的初级粒子。因此,没有注意到颗粒形貌随工艺参数的变化。这些结果表明,SAS重结晶过程是一种有价值的技术,可以生成具有可控尺寸和尺寸分布的可再现聚合物颗粒。

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