\r鲍 颖^{1, 2}，刘小涵¹，赵 佩¹，张 峰\r¹\r
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AuthorsHTML:\r鲍 颖^{1, 2}，刘小涵¹，赵 佩¹，张 峰\r¹\r
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AuthorsListE:\rBao Ying^{1, 2}，Liu Xiaohan¹，Zhao Pei¹，Zhang Feng\r¹\r
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AuthorsHTMLE:\rBao Ying^{1, 2}，Liu Xiaohan¹，Zhao Pei¹，Zhang Feng\r¹\r
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Unit:\r1. 天津大学化工学院，天津 300072；
2. 天津市现代药物传递及功能高效化重点实验室，天津 300072\r
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Unit_EngLish:\r1. School of Chemical Engineering and Technology，Tianjin University，Tianjin 300072，China；
2. Key Laboratory for Modern Drug Delivery and High Efficiency of Tianjin，Tianjin 300072，China\r
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Abstract_Chinese:\r针对苯基双(2，4，6-三甲基苯甲酰基)氧化膦(XBPO)晶体产品粒度小、流动性差、易团聚等问题，以增大粒度、改善粒度分布和晶习为目标，开展XBPO 结晶工艺研究．采用静态法测定了XBPO 在甲苯中的溶解度．采取单因素法研究了温度、真空度、搅拌速率、晶种加入量和养晶时间对XBPO 晶体产品粒度、粒度分布和收率的影响，以及降温速率对XBPO 晶体产品粒度分布、晶习和流动性的影响．使用Mastersizer 3000 型激光粒度分析仪测定晶体粒度分布，BK 系列生物显微镜和Stemi 508 体视显微镜观察晶习，BT-1000 型粉体综合特性测试仪测量晶体产品的流动性．结果表明，XBPO 的溶解度随温度的升高快速增大，可以采用蒸发和冷却的方式结晶．优化了结晶工艺条件，在60℃、0.04 MPa、150 r/min，加入溶质质量1%～1.8%的晶种并养晶120 min 的蒸发条件下，所得蒸发结晶晶体产品与原工艺晶体产品相比，中值粒度显著增大，由134 μm 增加到330 μm，粒度分布更加集中，变异系数由56.7 降至39.1，收率可达96%．在5℃/h 的降温速率下，晶习由不规则块状聚集体变为椭球状，显著提高了晶体产品流动性，休止角由35.1° 降至23.2°．所开发的蒸发-冷却结晶工艺增大了XBPO 晶体粒度、改善了粒度分布和晶习，新工艺的研究结果为XBPO晶体生产工艺的改进提供了新思路．\r
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Abstract_English:\rThe crystallization process of phenyl bis (2，4，6-trimethylbenzoyl) phosphine oxide (XBPO) was investigated to increase its crystal size and improve the crystal size distribution (CSD) and crystal habit because XBPO productshave many defects，including small particle size，poor flowability，and serious agglomeration. The solubility of XBPO in toluene was determined using a static analysis method and then the evaporative crystallization process was optimized via the single factor method. Next，the effects of the operational conditions including temperature，vacuum，stirring rate，number of seed crystals，and breeding time on the crystal size，CSD，and crystallization yield of XBPO products were investigated. The effects of the cooling rate on the CSD，crystal habit，and flowabilityof XBPO crystals were studied. To measure the CSD and flowability of XBPO，we used a Mastersizer 3000 laser particle-size analyzer and a BT-1000 powder comprehensive characteristic tester，respectively. The crystal habit was observed using a BK series biomicroscope and a Stemi 508 stereoscopic microscope. The results show that the solubility of XBPO increases with the increase of temperature，indicating that the crystallization of XBPO can be achieved by evaporation and cooling. Then，an optimal XBPO crystallization process was developed. Under evaporation conditions of 60 ℃，0.04 MPa，150 r/min，the addition of crystal seeds with a solute quality of 1.00%—1.80%，and breeding the crystal seeds for 120 min，we produced a relatively optimal product. Compared to the original product，the median size of the optimized crystals increases significantly from 134 μm to 330 μm，the coefficient of variation decreases from 56.7 to 39.1，the CSD narrows，and the yield is 96%. At a cooling rate of 5 ℃/h，the crystal habit is transformed from irregular block agglomerates to ellipsoids，with the angle of repose decreasing from 35.1° to 23.2° and the flowability significantly increasing. The evaporation-cooling crystallization process increases the XBPO crystal size and improves the CSD and crystal habit. The results of this work provide a new approach to improving the industrial crystallization of XBPO.\r
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Keyword_Chinese:苯基双(2，4，6-三甲基苯甲酰基)氧化膦；蒸发结晶；冷却结晶；粒度分布；晶习\r

Keywords_English:phenyl bis(2，4，6-thrimethylbenzoyl)phosphine oxide；evaporation crystallization；cooling crystallization；crystal size distribution；crystal habit\r


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