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Interfacial induction and regulation for microscale crystallization process: a critical review

《化学科学与工程前沿（英文）》 2022年 第16卷 第6期   页码 838-853 doi: 10.1007/s11705-021-2129-8

摘要： Microscale crystallization is at the frontier of chemical engineering, material science, and biochemical research and is affected by many factors. The precise regulation and control of microscale crystal processes is still a major challenge. In the heterogeneous induced nucleation process, the chemical and micro/nanostructural characteristics of the interface play a dominant role. Ideal crystal products can be obtained by modifying the interface characteristics, which has been proven to be a promising strategy. This review illustrates the application of interface properties, including chemical characteristics (hydrophobicity and functional groups) and the morphology of micro/nanostructures (rough structure and cavities, pore shape and pore size, surface porosity, channels), in various microscale crystallization controls and process intensification. Finally, possible future research and development directions are outlined to emphasize the importance of interfacial crystallization control and regulation for crystal engineering.

关键词： interfacial crystallization     heterogeneous nucleation     supersaturation     micro/nanostructure     process control and intensification    

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Progress in membrane distillation crystallization: Process models, crystallization control and innovative

Xiaobin Jiang, Linghan Tuo, Dapeng Lu, Baohong Hou, Wei Chen, Gaohong He

《化学科学与工程前沿（英文）》 2017年 第11卷 第4期   页码 647-662 doi: 10.1007/s11705-017-1649-8

摘要： Membrane distillation crystallization (MDC) is a promising hybrid separation process that has been applied to seawater desalination, brine treatment and wastewater recovery. In recent years, great progress has been made in MDC technologies including the promotion of nucleation and better control of crystallization and crystal size distribution. These advances are useful for the accurate control of the degree of supersaturation and for the control of the nucleation kinetic processes. This review focuses on the development of MDC process models and on crystallization control strategies. In addition, the most important innovative applications of MDC in the last five years in crystal engineering and pharmaceutical manufacturing are summarized.

关键词： membrane distillation crystallization     mathematics model     nucleation     separation     hybrid process    

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Applications of the crystallization process in the pharmaceutical industry

Sohrab ROHANI

《化学科学与工程前沿（英文）》 2010年 第4卷 第1期   页码 2-9 doi: 10.1007/s11705-009-0297-z

摘要： The applications of the crystallization technique in the pharmaceutical industry as a purification and separation process for the isolation and synthesis of pure active pharmaceutical ingredients (API), co-crystals, controlled release pulmonary drug delivery, and separation of chiral isomers are briefly discussed using a few case studies. The effect of process variables and solvent on the polymorphism and morphology of stavudine is discussed. The implementation of external control in the form of feedback and real-time optimal control using cooling and antisolvent crystallization of paracetamol in water-isopropyl alcohol is introduced. Two methods to prepare micron-sized drug particles, namely, micro-crystallization and polymer-coated API-loaded magnetic nanoparticles for pulmonary drug delivery, are discussed. The significance of co-crystals in drug administration is highlighted using the theophylline-nicotinamide co-crystal system. Resolution of chloromandelic acid derivatives, a racemic compound, is achieved using direct crystallization and diastereomeric salts crystallization. The crystal structures of diastereomeric salts of chloromandelic acid and phenylethylamine are determined. The structure comparison between the less soluble and more soluble salts shows that weak interactions such as CH/π interactions and van der Waals forces contribute to chiral recognition when the hydrogen bonding patterns are similar.

关键词： feedback     morphology     pulmonary     paracetamol     recognition    

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Utilizing melt crystallization fundamentals in the development of a new tabletting technology

Ahmed ABOUZEID,Sandra PETERSEN,Joachim ULRICH

《化学科学与工程前沿（英文）》 2014年 第8卷 第3期   页码 346-352 doi: 10.1007/s11705-014-1443-9

摘要： Increasing production effeciency and lowering costs are some of the many advantages melt crystallization technology offers over the conventional methodology of tabletting. A normal tablet consists of a pure shell or a coat and a separate core constituting the pharmaceutical active ingredient. Great emphasis is put on the purity of the shell since its purpose is to solely protect and deliver the active ingredient to its target. Melt crystallization is a purification (separation) process. It is discussed here for its ability to produce coated tablets, by separating the “coating” material from the “to be coated” material coming from one molten mixture. Molten drops of lutrol-ibuprofen mixture are produced using the drop forming technique. The subsequent analysis involves proving and quantifying the phase separation (coat purity). The mechanism of a crystallizing drop is shown as direct evidence of the ongoing process. Moreover, solidified tablet batches are analyzed for the purity of their coating by measuring the ibuprofen concentration. This optimization process is carried out through multiple stages of development and condition enhancements in order to produce the most pure tablet coating. As a result, a trial showing an almost purely coated tablet is presented here.

关键词： phase separation     melt crystallization     tablets     process optimization    

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Permeability analysis and seepage process study on crystal layer in melt crystallization with fractal

Xiaobin JIANG, Baohong HOU, Yongli WANG, Jingkang WANG

《化学科学与工程前沿（英文）》 2011年 第5卷 第4期   页码 435-441 doi: 10.1007/s11705-011-1139-3

摘要： In this paper a porous media seepage model was applied to analyze the permeability and study the seepage process of crystal pillar formed in the preparation of electronic grade phosphoric acid (EGPA). By inspecting the seeping process, the structure parameter of crystal pillar could be obtained. Two basic ideal models (perfectly separated model and perfectly connected model) were presented and a characterized factor was introduced to modify the model. A good simulation result was obtained which met the experiment result well. The relationship between and permeability were also discussed. The characterized factor showed potential application on optimizing process.

关键词： melt crystallization     porous media     fractal     permeability     hyperpure material     simulation    

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制药工业中结晶过程的最新进展 Review

高振国, Rohani Sohrab, 龚俊波, 王静康

《工程（英文）》 2017年 第3卷 第3期   页码 343-353 doi: 10.1016/J.ENG.2017.03.022

摘要：

结晶是古老的分离与提纯单元操作之一，如今已发展成为生产具有特定性质的高附加值产品以及建立高效制造过程的技术。本文中，我们综述了制药工业中晶体工程以及结晶过程设计和控制的最新研究进展，系统地总结了理解和开发新型晶体如共晶、多晶型、溶剂化物的方法，包括一些重要的进展，如第一个共晶药物Entresto (诺华) 的诞生以及Orkambi (福泰) 连续制造过程获批。与不同的过程控制策略和新型的结晶器相结合，传统的釜式和日渐成熟的连续结晶过程正不断地满足制药工业的需求。结晶过程的设计和控制已使几种创新型结晶器的设计实现连续操作且性能良好。本文还综述了过程分析技术最新的重要研究进展。

关键词： 结晶     晶体工程     多晶型     结晶过程设计和控制     晶体粒度分布    

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膜结晶过程强化与控制研究进展 Review

姜晓滨, 邵钰珊, 盛磊, 李培钰, 贺高红

《工程（英文）》 2021年 第7卷 第1期   页码 50-62 doi: 10.1016/j.eng.2020.06.024

摘要：

结晶是用于固体颗粒制备的基本分离技术，其中成核和生长过程的精确调控至关重要。目前，发展同时增强整个结晶过程的新型控制技术仍然面临巨大挑战。膜结晶（MCr）是一种新兴耦合技术，近年来取得了长足的进步，有望实现上述目标。本文综述了MCr的基本概念及其在结晶控制和过程强化中的应用前景，对MCr用的关键膜材料、过程控制机制以及基于多种混合膜和结晶工艺的优化策略进行简述。最后，概述了将MCr技术推广到工业应用的尝试，以及需要解决的问题和研究方向。

关键词： 膜结晶     成核     过程控制     过程强化    

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Effects of a structurally related substance on the crystallization of paracetamol

Ali SALEEMI, I.I. ONYEMELUKWE, Zoltan NAGY

《化学科学与工程前沿（英文）》 2013年 第7卷 第1期   页码 79-87 doi: 10.1007/s11705-013-1308-7

摘要： Paracetamol (PCM) was crystallized from an isopropanol (IPA) solution containing various small amounts of metacetamol as an additive. The effect on the nucleation kinetics was studied by measuring the induction time to nucleation and the metastable zone width using focused beam reflectance measurements (FBRM) and attenuated total reflectance (ATR-UV/Vis) spectroscopy. Both the induction time and the metastable zone width were expressed as functions of the additive concentration. Small amounts of metacetamol (1–4 mol-%) were found to cause significant inhibition to the nucleation by extending both the induction time and the metastable zone width. A progressive change in the morphology of the paracetamol crystals from tabular to columnar habit was observed with increasing metacetamol concentration. The solvent also had a significant effect on the size of the paracetamol crystals as smaller crystals were obtained in IPA than in aqueous solution. The dissolution rate of paracetamol was improved by the incorporation of metacetamol with 4 mol-% having the most effect. A supersaturation control (SSC) approach was implemented for the PCM-IPA system with and without metacetamol in an attempt to control and obtain larger metacetamol-doped paracetamol crystals.

关键词： acetaminophen     metacetamol     crystallization     metastable zone width     induction time     supersaturation control    

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The feasibility of coating by cooling crystallization on ibuprofen naked tablets

Fatima Mameri, Ouahiba Koutchoukali, Mohamed Bouhelassa, Anne Hartwig, Leila Nemdili, Joachim Ulrich

《化学科学与工程前沿（英文）》 2017年 第11卷 第2期   页码 211-219 doi: 10.1007/s11705-017-1619-1

摘要： Sugar spray coating is a frequently used process in the pharmaceutical industry. However, this process presents the disadvantage to form an amorphous coating around the active ingredient. A crystalline coating formed on the surface of a tablet is highly desirable. Recently, a new process of coating by cooling crystallization has been developed and applied on bisacodyl pastilles obtained by melt crystallization. In this work, we investigated the feasibility of coating by cooling crystallization on ibuprofen “naked tablets” manufactured by compression. In the first part of this work, the solubility and the metastable zone width have been determined experimentally for the coating solution because they are essential factors for any crystallization process. In the second part, the coating process is investigated on the operating conditions that affect the surface morphology and the crystal growth rate. These experimental conditions include concentration of the coating solution, degree of sub-cooling, agitation speed, retention time, and surface properties of the naked ibuprofen tablets. The results show that naked tablet coating by cooling crystallization is feasible and can be applied in the pharmaceutical industry.

关键词： coating     solution crystallization     ibuprofen tablets     sucrose    

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Nucleic acid crystallization and X-ray crystallography facilitated by single selenium atom

Wen Zhang,Jack W. Szostak,Zhen Huang

《化学科学与工程前沿（英文）》 2016年 第10卷 第2期   页码 196-202 doi: 10.1007/s11705-016-1565-3

摘要： X-ray crystallography is a powerful strategy for 3-D structure determination of macromolecules, such as nucleic acids and protein-nucleic acid complexes. However, the crystallization and phase determination are the major bottle-neck problems in crystallography. Recently we have successfully developed synthesis and strategy of selenium-derivatized nucleic acids (SeNA) for nucleic acid crystallography. SeNA might not only provide the rational strategies to solve the phase determination problem, but also offer a potential strategy to explore crystallization solutions.

关键词： selenium     DNA     RNA     nucleic acid     crystallization    

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Preparation and crystallization kinetics of micron-sized Mg(OH)

Xingfu SONG, Kefeng TONG, Shuying SUN, Ze SUN, Jianguo YU

《化学科学与工程前沿（英文）》 2013年 第7卷 第2期   页码 130-138 doi: 10.1007/s11705-013-1332-7

摘要： Magnesium hydroxide is an important chemical, and is usually obtained from seawater or brine via precipitation process. The particle size distribution of magnesium hydroxide has great effects on the subsequent filtration and drying processes. In this paper, micron-sized magnesium hydroxide with high purity, large particle size and low water content in filter cake was synthesized via simple wet precipitation in a mixed suspension mixed product removal (MSMPR) crystallizer. The effects of reactant concentration, residence time and impurities on the properties of magnesium hydroxide were investigated by X-Ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Malvern laser particle size analyzer. The results show that NaOH concentration and residence time have great effects on the water content and particle size of Mg(OH) . The spherical Mg(OH) with uniform diameter of about 30 μm was obtained with purity higher than 99% and water content less than 31%. Furthermore, the crystallization kinetics based on the population balance theory was studied to provide the theoretical data for industrial enlargement, and the simulation coefficients ( ) based on ASL model and C-R model are 0.9962 and 0.9972, respectively, indicating that the crystal growth rate of magnesium hydroxide can be well simulated by the size-dependent growth models.

关键词： magnesium hydroxide     precipitation     micron-sized     crystallization kinetics    

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Importance of emulsions in crystallization—applications for fat crystallization

Sandra PETERSEN, K. CHALEEPA, Joachim ULRICH

《化学科学与工程前沿（英文）》 2013年 第7卷 第1期   页码 43-48 doi: 10.1007/s11705-013-1309-6

摘要： Emulsions and crystallization are two independent research topics which normally do not overlap although a combination of the two could be applicable to many areas. Here, the importance of emulsions in the field of fat crystallization is described. Three applications with industrial relevance were chosen for investigation: fat fractionation, the solidification of phase change materials and solid lipid nanoparticles. For fat fractionation and phase change materials, emulsification can be applied as a tool to improve the fat crystallization process, and thus the product quality of the crystallized fat. Furthermore, the use of emulsification creates new application fields such as solid lipid nanoparticles in the area of fat crystallization.

关键词： emulsion     fat crystallization     phase change material     emulsion fractionation     emulsion solidification    

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Effect of polyethylene glycol on the crystallization, rheology and foamability of poly(lactic acid) containing

《化学科学与工程前沿（英文）》 2023年 第17卷 第12期   页码 2074-2087 doi: 10.1007/s11705-023-2342-8

摘要： In this study, the rheological properties, crystallization and foaming behavior of poly(lactic acid) with polyamide 6 nanofibrils were examined with polyethylene glycol as a compatibilizer. Polyamide 6 particles were deformed into nanofibrils during drawing. For the 10% polyamide 6 case, polyethylene glycol addition reduced the polyamide 6 fibril diameter from 365.53 to 254.63 nm, owing to the smaller polyamide 6 particle size and enhanced interface adhesion. Rheological experiments revealed that the viscosity and storage modulus of the composites were increased, which was associated with the three-dimensional entangled network of polyamide 6 nanofibrils. The presence of higher aspect ratio polyamide 6 nanofibrils substantially enhanced the melt strength of the composites. The isothermal crystallization kinetics results suggested that the polyamide 6 nanofibrils and polyethylene glycol had a synergistic effect on accelerating poly(lactic acid) crystallization. With the polyethylene glycol, the crystallization half-time reduced from 103.6 to 62.2 s. Batch foaming results indicated that owing to higher cell nucleation efficiency, the existence of polyamide 6 nanofibrils led to a higher cell density and lower expansion ratio. Furthermore, the poly(lactic acid)/polyamide 6 foams exhibited a higher cell density and expansion ratio than that of the foams without polyethylene glycol.

关键词： poly(lactic acid)     foaming     microfibrillation     rheological property     crystallization    

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Control of the agglomeration of crystals in the reactive crystallization of 5-(difluoromethoxy)-2-mercapto

Yongli WANG, Shuyuan MA, Xiaodong Lü, Chuang XIE

《化学科学与工程前沿（英文）》 2012年 第6卷 第4期   页码 423-431 doi: 10.1007/s11705-012-1211-7

摘要： 5-(Difluoromethoxy)-2-mercapto-1 -benzimidazole (DMB) was precipitated by adding acetic acid to the DMB sodium salt solution. The spherical agglomeration of DMB during the reactive crystallization in a batch crystallizer was monitored by real-time Particle Video Microscope (PVM). We found that the low feeding rate of acetic acid, high crystallization temperature, low agitation rate or adding seed crystal can facilitate the formation of spherical agglomerates. By using a simple model, the mean crystal agglomerate size of DMB thus predicted is generally in agreement with the experimental data. In addition, the crystallization process of DMB was optimized by a new control strategy of supersaturation to avoid disadvantages brought by agglomeration.

关键词： 5-(difluoromethoxy)-2-mercapto-1H-benzimidazole (DMB)     reactive crystallization     agglomeration     feeding rate     crystallization temperature     agitation rate    

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标题 作者 时间 类型 操作

Interfacial induction and regulation for microscale crystallization process: a critical review

期刊论文

Progress in membrane distillation crystallization: Process models, crystallization control and innovative

Xiaobin Jiang, Linghan Tuo, Dapeng Lu, Baohong Hou, Wei Chen, Gaohong He

期刊论文

Applications of the crystallization process in the pharmaceutical industry

Sohrab ROHANI

期刊论文

Utilizing melt crystallization fundamentals in the development of a new tabletting technology

Ahmed ABOUZEID,Sandra PETERSEN,Joachim ULRICH

期刊论文

Permeability analysis and seepage process study on crystal layer in melt crystallization with fractal

Xiaobin JIANG, Baohong HOU, Yongli WANG, Jingkang WANG

期刊论文

制药工业中结晶过程的最新进展

高振国, Rohani Sohrab, 龚俊波, 王静康

期刊论文

膜结晶过程强化与控制研究进展

姜晓滨, 邵钰珊, 盛磊, 李培钰, 贺高红

期刊论文

Effects of a structurally related substance on the crystallization of paracetamol

Ali SALEEMI, I.I. ONYEMELUKWE, Zoltan NAGY

期刊论文

姜晓滨：膜结晶过程调控与强化（2022年4月16日）

2022年06月09日

会议视频

The feasibility of coating by cooling crystallization on ibuprofen naked tablets

Fatima Mameri, Ouahiba Koutchoukali, Mohamed Bouhelassa, Anne Hartwig, Leila Nemdili, Joachim Ulrich

期刊论文

Nucleic acid crystallization and X-ray crystallography facilitated by single selenium atom

Wen Zhang,Jack W. Szostak,Zhen Huang

期刊论文

Preparation and crystallization kinetics of micron-sized Mg(OH)

Xingfu SONG, Kefeng TONG, Shuying SUN, Ze SUN, Jianguo YU

期刊论文

Importance of emulsions in crystallization—applications for fat crystallization

Sandra PETERSEN, K. CHALEEPA, Joachim ULRICH

期刊论文

Effect of polyethylene glycol on the crystallization, rheology and foamability of poly(lactic acid) containing

期刊论文

Control of the agglomeration of crystals in the reactive crystallization of 5-(difluoromethoxy)-2-mercapto

Yongli WANG, Shuyuan MA, Xiaodong Lü, Chuang XIE

期刊论文