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1.
为了研究卡马西平的结晶工艺,以甲醇为溶剂,正己烷为反溶剂,采用溶析结晶制备卡马西平晶体。利用X射线粉末衍射、红外光谱、拉曼光谱、光学显微镜等对卡马西平的晶型进行筛选和表征,考察卡马西平质量浓度、结晶温度、溶剂与反溶剂的体积比等参数对结晶得率和晶型的影响。研究结果表明,甲醇与正己烷溶析结晶得到两种晶型的卡马西平,分别为针状的晶型Ⅱ和棱镜状的晶型Ⅲ;结晶温度是影响晶体得率的主要因素,在0℃时,结晶得率可达98.5%,在40℃时,结晶得率仅为15.2%;溶剂与反溶剂的体积比是影响晶型的主要因素,体积比越大越利于晶型Ⅲ的生成。研究结果可为卡马西平晶型Ⅲ的生产提供参考。  相似文献   

2.
为考察溶析结晶纯化去乙酰真菌环氧乙酯的效果,研究了不同的溶剂、反溶剂含量和导入方式对去乙酰真菌环氧乙酯结晶的影响.在静态结晶实验的基础上,通过设计正交实验L9(34)研究动态结晶过程中各因素对去乙酰真菌环氧乙酯收率和纯度的影响.结果表明:有效地控制反溶剂含量及其导入方式可以提高晶体的纯度和收率并影响晶体的形态.去乙酰真菌环氧乙酯动态结晶最佳条件:结晶温度为15℃,溶剂-反溶剂体积比(丙酮-水)为2∶3,反溶剂流加时间为3 h.  相似文献   

3.
THE MECHANISM AND ENHANCING METHODS OF SOLVENTING OUT CRYSTALLIZATION   总被引:1,自引:0,他引:1  
溶析结晶广泛用于有机工业结晶过程,但目前溶析结晶过程普遍存在着以下问题:晶体主粒度小,变异系数高;产品过滤分离难度大,杂质含量高.针对这些问题,本文研究了溶析结晶体系的介稳区性质,并采用了如下几种强化方法:用压力溶解和静置冷却来提高过饱和度;在沉淀剂中添加表面活性剂以及采用弹性叶片摩擦和超声波刺激来提高成核速率;动静态交替育晶减少生长分散;加入促进构型转变的物质获得所需晶型的晶体;按照最佳操作程序流加沉淀剂维持恒定的结晶过饱和度等.实验证明,采用这些方法可以显著地提高溶析结晶产品的质量.  相似文献   

4.
以铁尾矿为主要原料制备微晶玻璃,通过DTA,XRD,SEM分析方法,全面考察了晶化温度和晶化时间对微晶玻璃结构的影响.实验发现:随着析晶温度的升高,主晶相钙铁辉石没有改变,但晶体形态和析晶率发生了较大的变化;随着析晶温度的升高,晶体的规则程度增加,晶体尺寸增大,析晶率呈先增加后减小的趋势;当析晶温度高于1250℃时,晶体分布均匀程度降低;最佳晶化温度为1200~1250℃,晶化时间为180 min.  相似文献   

5.
溶析结晶广泛用于有机工业结晶过程,但目前溶析结晶过程普遍存在着以下问题;晶体主粒度小,变异系数高,产品过滤分离难度大,杂质含量高,针对这些问题。本文研究了溶析结晶体系的介稳区性质,并采用了如下几种强化方法;用压力溶解和静置冷却来提高过饱和度;在沉淀中添加表面活性剂以及采用弹性叶片摩擦和超声波刺激来提高成核速度;动静态交替育晶减少生长分散;加入促进构型转变的物质获得所需晶型的晶体;按照最佳操作程序流  相似文献   

6.
采用亚临界水法制备了克拉霉素纳米颗粒,通过调节亚临界水温度、反溶剂(普通去离子水)温度、亚临界水/反溶剂体积比、表面活性剂浓度等因素,得到形貌均匀的克拉霉素纳米颗粒。优化后的工艺条件为:亚临界水、反溶剂的温度分别为140℃,0℃,亚临界水/反溶剂体积比为1∶3,搅拌时间25min,表面活性剂α-乳糖质量分数为0.4%。在上述条件下制备得到的颗粒的平均粒径为65nm左右,原料药和样品的红外光谱图和X射线衍射对比结果显示其化学结构没有发生变化。溶出结果表明,亚临界水法制备的克拉霉素纳米颗粒溶出度有了明显的提高。  相似文献   

7.
药物结晶工艺是药物工业生产流程中至关重要的环节。通过单因素实验,以伊曲茶碱晶体收率、粒度分布作为评价标准,考察结晶液初始浓度、溶析剂用量、结晶温度、陈化时间、溶析剂滴加速率等因素的影响。通过分析各种影响因素,得到伊曲茶碱较佳结晶条件:结晶液初始浓度12 mg/ml,水和DMF体积分数比3:1,滴加速率2 ml/min,结晶温度20 ℃、陈化时间60 min。通过该方案获得伊曲茶碱晶体呈短针状,收率、平均粒径(MS)、变异系数(CV)分别为93.7 %、12.6 μm、4.25,为工业上制备高质量的伊曲茶碱产品提供基础依据和参考。  相似文献   

8.
为了研究加氢生物柴油-乙醇-柴油三元燃料的低温性能,基于热力学相平衡模型,计算了该三元燃料的析晶点和析晶量,同时对比了加氢生物柴油-柴油二元燃料的析晶点和析晶量,探究了乙醇对该二元燃料低温性能的影响。试验结果表明,相比加氢生物柴油-柴油二元燃料,加氢生物柴油-乙醇-柴油三元燃料的析晶点均有不同程度的降低,三元燃料PHC5E5、PHC10E10、PHC15E15、PHS5E5、PHS10E10和PHS15E15的析晶点分别降低了4.5、5.7、6.1、4.3、5.3、6.1 K,所对应三元燃料在不同温度下析晶量也有不同程度的降低。在初始析晶温度下,三元燃料中的乙醇与生物柴油同时开始析晶,这说明乙醇以共晶方式与高熔点组分同时析出,改变了高熔点组分在晶核形成、生长过程中的结晶趋向和结晶形态,延滞了三元燃料在低温过程中的析晶趋势;未结晶的乙醇大量分布在燃料液相以及网状和片状晶体间隙之中,一定程度上提高了已结晶组分在基液中的溶解度。这两者共同改善了加氢生物柴油-乙醇-柴油三元燃料的低温性能。该研究为优化加氢生物柴油的低温性能提供了一种有效可靠的方法。  相似文献   

9.
反溶剂重结晶法制备多晶型比卡鲁胺   总被引:1,自引:0,他引:1  
采用反溶剂重结晶法制备多晶型比卡鲁胺,通过改变重结晶过程中所使用的溶剂,对比单一溶剂和共溶剂对所制得晶体的晶型和颗粒形貌差别,探索最优化的共溶剂类型和体积比参数,以达到将比卡鲁胺原料药进行晶型纯化的目的。在反溶剂重结晶过程中采用共溶剂制备比卡鲁胺晶体发现:共溶剂(二甲基亚砜+乙醇)以及(丙酮+乙醇)可制备比卡鲁胺晶型I,并通过调节共溶剂中乙醇的用量可得到粒度均一,分散性好的I型比卡鲁胺。  相似文献   

10.
对三水合艾司奥美拉唑镁制备过程中晶型控制进行研究,同时对产物的粒度分布等性质进行了工艺优化实验。通过X射线粉末衍射表征产物晶型,借助于二维在线成像系统监测三水合艾司奥美拉唑镁反应结晶过程中的晶体形貌变化,运用马尔文激光粒度仪辅助监测晶体的粒度分布变化。考察了结晶温度、反应物的浓度等因素对三水合艾司奥美拉唑镁晶型与晶习的影响。结果表明,三水合艾司奥美拉唑镁结晶方式为球形结晶,结晶温度是影响晶型的关键因素,优化后的结晶温度为25 ℃。优化后的工艺可以制备晶型固定、粒度分布均匀、平均粒度大的三水合艾司奥美拉唑镁药物颗粒。  相似文献   

11.
Language markedness is a common phenomenon in languages, and is reflected from hearing, vision and sense, i.e. the variation in the three aspects such as phonology, morphology and semantics. This paper focuses on the interpretation of markedness in language use following the three perspectives, i.e. pragmatic interpretation, psychological interpretation and cognitive interpretation, with an aim to define the function of markedness.  相似文献   

12.
何延凌 《科技信息》2008,(4):258-258
Language is a means of verbal communication. People use language to communicate with each other. In the society, no two speakers are exactly alike in the way of speaking. Some differences are due to age, gender, statue and personality. Above all, gender is one of the obvious reasons. The writer of this paper tries to describe the features of women's language from these perspectives: pronunciation, intonation, diction, subjects, grammar and discourse. From the discussion of the features of women's language, more attention should be paid to language use in social context. What's more, the linguistic phenomena in a speaking community can be understood more thoroughly.  相似文献   

13.
理论推导与室内实验相结合,建立了低渗透非均质砂岩油藏启动压力梯度确定方法。首先借助油藏流场与电场相似的原理,推导了非均质砂岩油藏启动压力梯度计算公式。其次基于稳定流实验方法,建立了非均质砂岩油藏启动压力梯度测试方法。结果表明:低渗透非均质砂岩油藏的启动压力梯度确定遵循两个等效原则。平面非均质油藏的启动压力梯度等于各级渗透率段的启动压力梯度关于长度的加权平均;纵向非均质油藏的启动压力梯度等于各渗透率层的启动压力梯度关于渗透率与渗流面积乘积的加权平均。研究成果可用于有效指导低渗透非均质砂岩油藏的合理井距确定,促进该类油藏的高效开发。  相似文献   

14.
As an American modern novelist who were famous in the literary world, Hemingway was not a person who always followed the trend but a sharp observer. At the same time, he was a tragedy maestro, he paid great attention on existence, fate and end-result. The dramatis personae's tragedy of his works was an extreme limit by all means tragedy on the meaning of fearless challenge that failed. The beauty of tragedy was not produced on the destruction of life, but now this kind of value was in the impact activity. They performed for the reader about the tragedy on challenging for the limit and the death.  相似文献   

15.
正The periodicity of the elements and the non-reactivity of the inner-shell electrons are two related principles of chemistry,rooted in the atomic shell structure.Within compounds,Group I elements,for example,invariably assume the+1 oxidation state,and their chemical properties differ completely from those of the p-block elements.These general rules govern our understanding of chemical structures and reactions.Using first principles calcula-  相似文献   

16.
We have developed an adiabatic connection to formulate the ground-state exchange-correlation energy in terms of pairing matrix linear fluctuations.This formulation of the exchange-correlation energy opens a new channel for density functional approximations based on the many-body perturbation theory.We illustrate the potential of such approaches with an approximation based on the particle-particle Random Phase Approximation(pp-RPA).This re-  相似文献   

17.
正The electronic and nuclear(structural/vibrational)response of 1D-3D nanoscale systems to electric fields gives rise to a host of optical,mechanical,spectral,etc.properties that are of high theoretical and applied interest.Due to the computational difficulty of treating such large systems it is convenient to model them as infinite and periodic(at least,in first approximation).The fundamental theoretical/computational problem in doing so is that  相似文献   

18.
For molecular systems,the quantum-mechanical treatment of their responses to static electromagnetic fields usually employs a scalar-potential treatment of the electric field and a vector-potential treatment of the magnetic field.Although the potential for each field separately is associated with the choice of an(unphysical)origin,the precise choice of the origin for the electrostatic field has little consequences for the results.This is different for the  相似文献   

19.
<正>"The Journal of Shanghai Normal University:Mathematics"is published by Shanghai Normal University as regular issues of The Journal of Shanghai Normal University each year from 2014 in English.The editors-in-chief of the issues are professors Yuhao Cong and Maoan Han.The Journal of Shanghai Normal University was started in 1958 with  相似文献   

20.
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