【作者】 刘宏伟；

【导师】 汪文川； 屈一新；

【作者基本信息】 北京化工大学 ， 化学工程， 2001， 硕士

【摘要】 本文对多元体系相平衡及反应做了如下三方面的工作：1)超临界抗溶剂重结晶在药物微粉化中的应用；2)用反应蒸馏法水合环氧乙烷生产乙二醇的工艺研究；3)C5醚化体系相平衡的研究。得出如下结论： 第一部分研究了超临界抗溶剂重结晶法在药物微粉化中的应用。据我们了解，在国内还没有其他人做过这方面的工作。我们研究了胰岛素试剂、牛血清蛋白+二甲基甲酰胺(DMF)、牛血清蛋白+乙醇、木瓜蛋白酶+DMF、头孢拉啶(头VI)+甲醇等溶液体系的间歇法超临界重结晶过程，得到了不同粒径和形状的晶体颗粒。本部分还对头VI+甲醇溶液的间歇法超临界重结晶过程的工艺条件进行了详细研究，得到如下结论： (1) 随着系统温度的升高，晶体的平均粒径增大，晶体形状不随温度变化，且在低浓度(＜10g／L)时呈球形。 (2) 随着系统压力的升高，晶体的平均粒径减小，晶体形状不随压力变化，且在低浓度(＜10g／L)时呈球形。 (3) 随着溶液初始浓度的增加，晶体的平均粒径增大，晶体形状亦有所变化。如当浓度为10gm时，出现了松针状晶体。 另外，随着系统升压速率的增加，晶体的粒径也是减小的。 第二部分在用反应蒸馏法水合环氧乙烷生产乙二醇的工艺研究中，考察了摩尔回流比、塔压、水与环氧乙烷之比、理论板数以及进料位置等对反应转化率和选择性的影响，同时考察了温度和能量随回北京化工大学硕士学位论文流比的变化关系。结果如下: (1)随着回流比的增加，转化率和选择性均有所增加。在较小回流比(R=2)时，转化率就己接近100%，而直至全回流时，选择性才接近100%。所以该工艺最好是在全回流下操作。 (2)水与环氧乙烷之摩尔比已降至了3:1。 (3)当塔压P<0.2Mpa时模拟无法进行，当P口OZN于a时，随着塔压的增加，转化率不断增加直至100%，而选择性却在P=0.SMPa时有一个最大值。如综合环氧乙烷在水中的溶解度和节能两方面，最佳操作压力应是0.SMPa。 (4)最佳的理论板数是8块理论板。 (5)最佳进料板为第4块板。第三部分得到如下几个结论: (1)收集并整理了CS馏份的各组成成份、甲醇及TA州田的纯物质的物性。(2)收集并整理了体系中两两组份间的相平衡数据。(3)利用AsPen Plus模拟软件关联出体系中各组份两两之间的N眠JL，UN IQUAC，Wilson的模型参数。关键词:超临界抗溶剂结晶药物微粉化环氧乙烷反应蒸馏 水合乙二醇CS醚化相平衡更多还原

【Abstract】 Supercritical antisolvent precipitation of micronizing pharmacy particles and hydration process with reactdistillation to produce glycol and the phase equilibrium of etherifying C5 system are all examined and discussed in this work.According to our investigation, supercritical antisolvent(SAS) precipitation of micronizing pharmacy particles is not studied by other authors in China until now. Solvent and solute in SAS can show different results. How do experiment conditions such as temperature, pressure, preliminary concentration, influence particle size and morphology when micronizing pharmacy by supercritical antisolvent processes.(1) Particle size reduced and sphere morphology is invariable with decreasing temperature(2) Particle size reduced and sphere morphology is invariable with increasing pressure(3) Particle size increased and morphology is variable with increasing preliminary concentration. Pine leaf-like particles can be observed at 10g/L.In addition, particle size reduced with the rate of increasing pressure.To produce glycol a hydration process of water(H2O) and ethylene oxide(EO) by reactdistillation has been studied. Molar reflux, the pressure, the ratio of H2O to EO, the number of perfect plates and the location offeeds have been simulated. The results show as follows.(1) The conversion rate and selectivity increase with increasing molar reflux. The conversion rate has been close to 100% at low molar reflux(R=2), but the selectivity approaches 100% until total reflux.(2) The molar ratio of H2O to EO has gone down to 3:1.(3) When pressure is less than 0.2MPa, the simulation shows errors. When pressure is more than 0.2MPa, the conversion rate goes up with the increasing pressure and the selectivity has reached maximum at 0.5MPa. But 0.8MPa is the optimal value when solubility and energy saving are taken into account.(4) The optimal number of perfect plates is 8.(5) The optimal location of feed plate is the 4th.Properties and phase equilibrium data of etherifying C5 system have been collected. Simulation parameters of NRTL, UNIQUAC and Wilson equation have also been calculated through Aspen Plus.更多还原