Verfügbarkeit: Precision crystallization

Precision crystallization: theory and practice of controlling crystal size

"Despite the fact that crystals make up an estimated 80% of chemical and pharmaceutical products, few resources exist that provide practical guidance on achieving precision control of their size and size distribution. Based on a model developed by the author and his colleagues, Precision Crysta...

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Bibliographische Detailangaben
1. Verfasser:	Leubner, Ingo (VerfasserIn)
Format:	Buch
Sprache:	English
Veröffentlicht:	Boca Raton [u.a.] CRC Press 2010
Schlagworte:	Crystal growth Nucleation Crystallization Keimbildung Kristallwachstum Kristallisation
Online-Zugang:	Inhaltsverzeichnis Klappentext
Zusammenfassung:	"Despite the fact that crystals make up an estimated 80% of chemical and pharmaceutical products, few resources exist that provide practical guidance on achieving precision control of their size and size distribution. Based on a model developed by the author and his colleagues, Precision Crystallization: Theory and Practice of Controlling Crystal Size presents scientists and product engineers with the tools to control crystal nucleation, enabling them to ultimately control crystal size and size distribution for batch and continuous crystallizations. At the cutting edge of crystallization science and technology, this volume presents information never before available. Introducing the Balanced Nucleation and Growth (BNG) model, the book demonstrates how the results of the nucleation process are quantitatively related to practical experimental control values such as: reaction addition rate, crystal solubility, temperature, residence time (continuous crystallizations), the effect of ripening agents (crystal supersizing) during nucleation, the effect of crystal growth restrainers (crystal nanosizing) during nucleation, and control of renucleation. The author shows how the BNG theory predicts previously unknown phenomena and also how it corrects erroneous perceptions of the importance of reaction volume on the outcome of crystal nucleation. Going above and beyond classical nucleation theories which rely to a large extent on guesswork, the BNG model gives precise guidance to scientists working in a range of critical areas, leading to promising implications for research, quality control, product development, production processes, pilot plant operations, and manufacturing."--Publisher's description.
Beschreibung:	Includes bibliographical references and index
Beschreibung:	XVIII, 206 S. Ill., graph. Darst.
ISBN:	9781439806746

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520	3		\|a "Despite the fact that crystals make up an estimated 80% of chemical and pharmaceutical products, few resources exist that provide practical guidance on achieving precision control of their size and size distribution. Based on a model developed by the author and his colleagues, Precision Crystallization: Theory and Practice of Controlling Crystal Size presents scientists and product engineers with the tools to control crystal nucleation, enabling them to ultimately control crystal size and size distribution for batch and continuous crystallizations. At the cutting edge of crystallization science and technology, this volume presents information never before available. Introducing the Balanced Nucleation and Growth (BNG) model, the book demonstrates how the results of the nucleation process are quantitatively related to practical experimental control values such as: reaction addition rate, crystal solubility, temperature, residence time (continuous crystallizations), the effect of ripening agents (crystal supersizing) during nucleation, the effect of crystal growth restrainers (crystal nanosizing) during nucleation, and control of renucleation. The author shows how the BNG theory predicts previously unknown phenomena and also how it corrects erroneous perceptions of the importance of reaction volume on the outcome of crystal nucleation. Going above and beyond classical nucleation theories which rely to a large extent on guesswork, the BNG model gives precise guidance to scientists working in a range of critical areas, leading to promising implications for research, quality control, product development, production processes, pilot plant operations, and manufacturing."--Publisher's description.
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Datensatz im Suchindex

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adam_text	Contents Preface ....................................................................................................................xiii Acknowledgments ....................................................................................................xv The Author .............................................................................................................xvii Chapter 1 Prior Models for Nucleation and Growth .............................................1 The Primitive Model ............................................................................1 The Total Crystal Number ....................................................................2 The Classical Nucleation Model (Becker-Doering) .............................2 Derivation of the Classical Nucleation Model .....................................3 The Klein-Moisar Model ......................................................................5 Kharitanova Derivation ........................................................................6 Comments .............................................................................................6 Growth Rate and Maximum Growth Rate ...........................................7 Growth Rate below the Maximum Growth Rate ............................7 Maximum Growth Rate ...................................................................7 References ............................................................................................8 Chapter 2 The Balanced Nucleation and Growth Model ....................................11 The BNG Model and the Nucleation Phase .......................................11 Assumptions for Modeling .................................................................11 Assumptions for Calculations ............................................................11 Preliminary Considerations: Nucleation Rate ....................................12 The Balanced Nucleation and Growth Model ....................................13 Modeling Variables .......................................................................13 Initial Time Interval ......................................................................13 Second and Following Time Intervals ...........................................14 Subsequent Time Intervals ............................................................16 End of Nucleation, Final Time Interval for Nucleation, te ............16 Crystal Size and Size Distribution ................................................17 BNG Modeling of the Nucleation Phase and Size Distribution .........17 Reaction Parameters for the Calculations ..........................................18 Results and Discussion .......................................................................18 Time Dependence of Nucleation Rate, Growth Rate, and Supersaturation ..............................................................................18 Size Distribution .......................................................................19 Modeling the Reaction Parameters ...............................................20 Addition Rate, Ra ......................................................................20 Maximum Growth Rate, Gm .....................................................21 Contents Critical Nucleus Size, Ln ...........................................................22 Nucleation Efficiency, Fn ..........................................................23 Practical Considerations ................................................................24 Conclusion ..........................................................................................26 References ..........................................................................................27 Chapters The Analytical BNG Model ...............................................................29 Crystal Formation (Nucleation) under Kinetically and Diffusion-Controlled Growth Conditions ..........................................29 Derivation of the General BNG Nucleation Equation ...................29 Nucleation under Diffusion-Controlled Growth Conditions .........30 Nucleation under Kinetically Controlled Growth Conditions .......31 References ..........................................................................................32 Chapter 4 Kinetically Controlled Nucleation .....................................................33 Experiment: Kinetically Controlled Crystal Nucleation ....................33 Theory ...........................................................................................33 Determination of the Kinetic Integration Constant, K¡ .........34 Mechanism ....................................................................................35 Conclusion ..........................................................................................35 Appendix I: Experimental Conditions for Agi Precipitation .............36 References ..........................................................................................36 Chapterő Diffusion-Controlled Nucleation ........................................................37 Reaction Variables, Constants, Predictions ........................................37 Theory ...........................................................................................37 Critical Crystal Size, r, and Supersaturation ...............................37 Reaction Variables T, R, Cs ...........................................................38 Reactant Addition Rate, R ........................................................38 Solubility ...................................................................................38 Physicochemical Constants ...........................................................39 Reaction Volume ...........................................................................40 Constancy of Crystal Number ..................................................41 Modeling: Separation of Variables R, Cs, and T ................................43 Theory ...........................................................................................43 Diffusion Coefficient, D ...........................................................43 Surface Energy, y ......................................................................44 Addition Rate, R ............................................................................44 Solubility, Cs ..................................................................................45 Temperature, T ..............................................................................45 Addition Rate .....................................................................................46 Silver Chloride ...............................................................................48 Experimental: AgCl ..................................................................48 Contents vii Stirring/Mixing ........................................................................48 Peptizer .....................................................................................48 Calculation of r/r .....................................................................49 Results .......................................................................................49 Silver Bromide ...............................................................................51 Experimental: AgBr ..................................................................51 Results .......................................................................................51 Practical Applications ...............................................................52 Solubility ............................................................................................53 Silver Chloride ...............................................................................53 Experimental ............................................................................53 Results: AgCl ............................................................................54 Silver Bromide ...............................................................................57 Experimental ............................................................................57 Results: AgBr ............................................................................58 AgBr Morphology as a Function of Solubility ..............................61 Temperature ........................................................................................62 Silver Chloride ...............................................................................63 Silver Bromide ...............................................................................65 References ..........................................................................................67 Chapter 6 Supersizing with Ripeners ..................................................................69 Crystal Formation (Nucleation) in the Presence of Ostwald Ripening Agents: Theory ...................................................................69 Summary .......................................................................................69 Introduction ...................................................................................69 Theory ...........................................................................................70 Crystal Formation (Nucleation) of Silver Bromide in the Presence of a Di-Thia Crown Ether as an Ostwald Ripening Agent .................................................................................................73 Introduction ...................................................................................73 Experimental .................................................................................75 Results and Discussion ..................................................................75 Crystal Number .........................................................................75 Crystal Size ....................................................................................76 Conclusions ....................................................................................76 Crystal Formation (Nucleation) of AgClBr (15:85) in the Presence of Ammonia as an Ostwald Ripening Agent ......................77 Introduction ...................................................................................77 Experimental .................................................................................78 Results ...........................................................................................78 Crystal Number and Size ..........................................................78 Ammonia Effects in the Reactor on pH...................................81 Ammonia Effects in the Reactor on pAg .................................82 Conclusion .....................................................................................82 Contents Crystal Formation (Nucleation) of AgBrI (97.4:2.6) in the Presence of US-dihydroxy^ó-dithiaoctane as an Ostwald Ripening Agent ..................................................................................83 Introduction ...................................................................................83 Experimental .................................................................................83 Results ...........................................................................................85 60°C Results: Crystal Size/Number with Ripener Correlation ................................................................................85 All Data: Size/Number with Ripener Correlation ....................85 Retained Ripener ......................................................................87 Summary .......................................................................................89 References ..........................................................................................89 Chapter 7 Nanosizing with Restrainers..............................................................91 Crystal Formation (Nucleation) in the Presence of Growth Restrainers..........................................................................................91 Introduction ...................................................................................91 Model .............................................................................................93 Surface Integration Model of Nucleation and Effect of Crystal Growth Restrainers..................................................93 Surface Adsorption Model ........................................................95 Experimental .................................................................................96 Results ...........................................................................................97 Conclusions ....................................................................................99 References ........................................................................................100 Chapter 8 Crystal Growth and Renucleation ....................................................101 Crystal Growth, Renucleation, and Maximum Growth Rate: Theory and Experiments ..................................................................101 Introduction .................................................................................101 General Experimental Procedures ..............................................103 Control of Reactant Addition Rate: Fixed Seed Concentration ..........................................................................103 Control of Crystal Seed Concentration: Fixed Addition Rate .........................................................................................103 The Renucleation Model ..............................................................103 Crystal Nucleation ..................................................................104 Crystal Growth ............................................................................104 Growth Rate and Crystal Number ..........................................104 Growth Rate and Surface Area ...............................................105 Growth Rate and Crystal Size ................................................105 Substitutions ............................................................................106 Growth and Renucleation ............................................................106 Aspects of the Renucleation Model .............................................107 Contents ix Determination of a, b, and c ...................................................107 Variable Seed Concentration ..................................................107 Variable Addition Rate ...........................................................108 No Seed Crystals ....................................................................108 Maximum Growth Rate Conditions .......................................109 Renucleation Conditions .........................................................109 Experimental ...............................................................................110 Seed Emulsion ........................................................................110 Precipitation Procedure for Growth/Renucleation Experiments ............................................................................110 Determination of the Number of Renucleation Crystals, Zn ....... 110 Results and Discussion ................................................................ Ill Summary and Conclusions .......................................................... 114 References ........................................................................................114 Chapter 9 Continuous Crystallization ...............................................................117 Continuous Crystallization in the Mixed-Suspension, Mixed-Product-Removal (MSMPR), or Continuous Stirred Tank Reactor (CSTR) Crystallizer ................................................... 117 Introduction ................................................................................. 117 Experimental ...............................................................................117 Prior Models: The Randolph-Larson Model ...............................118 Growth .........................................................................................119 Example of Size Distribution in CSTR Precipitation ..................120 Transient Behavior of Silver Bromide Precipitation in a Continuous Suspension Crystallizer ................................................122 Summary .....................................................................................122 Introduction .................................................................................122 Model for the Initial Transient Phase ..........................................123 Experimental ...............................................................................127 Results and Discussion ................................................................128 The Transition Stage ...............................................................128 Initial Nucleation versus Batch Nucleation .............................129 Maximum Growth Rate and Critical Supersaturation ............131 After the Renucleation Point ...................................................132 Summary ................................................................................133 A New Crystal Nucleation Theory for Size Control in Continuous Precipitations ................................................................133 Summary .....................................................................................133 Introduction .................................................................................134 Theory .........................................................................................134 Preconditions ..........................................................................134 Model Derivation .........................................................................135 Crystal Nucleation .......................................................................136 Crystal Growth ............................................................................138 x Contents Crystal Growth and Nucleation in the Continuous Crystallizer ..................................................................................138 Practical Analyses .......................................................................139 Special Limiting Conditions for Continuous Crystallization ......140 Large Average Crystal Size, L ................................................140 Short Residence Time, Plug-Flow Reactor. r-> zero .............140 Calculation of Reaction Processes .............................................. 141 Nucleation versus Growth, Rn/R¡ ............................................ 141 Nascent Nuclei Size ................................................................ 141 Conclusions ..................................................................................142 Size Dependence on Residence Time in Continuous Precipitations ....................................................................................143 Summary .....................................................................................143 Introduction .................................................................................143 Experimental ...............................................................................144 Results and Discussion ................................................................147 Crystal Size. Addition Rate, and Suspension Density .................147 Crystal Size and Residence Time ................................................149 Maximum Growth Rate, Gm ........................................................149 Minimum Crystal Size (r->0) ......................................................150 Determination of Ψ and L/L^., Supersaturation Ratio. S. and Supersaturation, Css ..............................................................150 Nucleation versus Growth, R^R, ................................................152 Nascent Nuclei Size .....................................................................152 Conclusions ..................................................................................153 Size Dependence on Solubility in Continuous Precipitations ..........153 Summary .....................................................................................153 Introduction .................................................................................154 The BNG Model for the CSTR System .......................................154 Size Control by Crystal Solubility ...............................................155 The Solubility Model ..............................................................155 Solubility .....................................................................................157 Experimental ...............................................................................157 Results .........................................................................................159 Suspension Density .................................................................159 Size-Solubility Correlation .....................................................159 Experimental, Critical, and Nascent Crystal Sizes, L, Lc, andLn ............................................................................................161 Supersaturation Ratio, S .......................................................162 Reactant Split Ratios, RJR¡, Rn/R(„ and R/R,, .......................162 Conclusions ............................................................................162 References ........................................................................................164 Chapter 10 Crystal Growth in the Continuous Crystallizer ...............................167 Seeded Precipitations in the Continuous Stirred Tank Reactor Crystallizer .......................................................................................167 Contents x¡ Summary .....................................................................................167 Introduction .................................................................................167 Seeded Crystallization in the CSTR System ...............................170 Modeling the Seeded CSTR Crystallizer ....................................171 Mathematical Processing Steps ...................................................174 Results and Discussion ................................................................174 Addition Rate, R, as a Function of Residence Time, r, for Constant Growth Rate, G .......................................................175 Steady-State Addition Rate as a Function of Growth Rate, G ....................................................................................176 Steady-State Addition Rate, R, as Function of Residence Time, г ....................................................................................177 Steady-State Addition Rate, R, as Function of Seed Size, L(l ....................................................................................178 Steady-State Addition Rate. R, as a Function of Seed Number Addition Rate, dN,/dt ...............................................179 Conclusion ...................................................................................180 References ........................................................................................180 Epilogue ................................................................................................................183 Final Thoughts .................................................................................183 Glossary of Terms ................................................................................................185 Bibliography .........................................................................................................187 Index ......................................................................................................................189 CHEMISTRY Precision Crystallization Theory and Practice of Controlling Crystal Size Despite the fact that crystals make up an estimated 80% of chemical and pharmaceutical products, few resources exist that provide guidance on achieving precision control of their size and size distribution. Based on a model developed by the author and his colleagues, Precision Crystallization: Theory and Practice of Controlling Crystal Size presents scientists and product engineers with the tools to control crystal nucleation, enabling them to ultimately control crystal size and size distribution. At the cutting edge of crystallization science and technology, this volume presents information never before available. Introducing the Balanced Nucleation and Growth (BNG) model, the book demonstrates how the results of the nucleation process are quantitatively related to practical experimental control values such as • Reaction addition rate • Crystal solubility • Temperature • Residence time (continuous crystallizations) ·» The effect of ripening agents (crystal supersizing) during nucleation • The effect of crystal growth restrainers (crystal nanosizing) during nucleation The author shows how the BNG theory predicts previously unknown phenomena and also how it corrects erroneous perceptions of the importance of reaction volume on the outcome of crystal nucleation. Going above and beyond classical nucleation theories that rely to a large extent on guesswork, the BNG model gives precise guidance to scientists working in a range of critical areas, leading to promising implications for research, quality control, product development, production processes, pilot plant operations, and manufacturing.
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publisher	CRC Press
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spelling	Leubner, Ingo Verfasser aut Precision crystallization theory and practice of controlling crystal size Ingo H. Leubner Boca Raton [u.a.] CRC Press 2010 XVIII, 206 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Includes bibliographical references and index "Despite the fact that crystals make up an estimated 80% of chemical and pharmaceutical products, few resources exist that provide practical guidance on achieving precision control of their size and size distribution. Based on a model developed by the author and his colleagues, Precision Crystallization: Theory and Practice of Controlling Crystal Size presents scientists and product engineers with the tools to control crystal nucleation, enabling them to ultimately control crystal size and size distribution for batch and continuous crystallizations. At the cutting edge of crystallization science and technology, this volume presents information never before available. Introducing the Balanced Nucleation and Growth (BNG) model, the book demonstrates how the results of the nucleation process are quantitatively related to practical experimental control values such as: reaction addition rate, crystal solubility, temperature, residence time (continuous crystallizations), the effect of ripening agents (crystal supersizing) during nucleation, the effect of crystal growth restrainers (crystal nanosizing) during nucleation, and control of renucleation. The author shows how the BNG theory predicts previously unknown phenomena and also how it corrects erroneous perceptions of the importance of reaction volume on the outcome of crystal nucleation. Going above and beyond classical nucleation theories which rely to a large extent on guesswork, the BNG model gives precise guidance to scientists working in a range of critical areas, leading to promising implications for research, quality control, product development, production processes, pilot plant operations, and manufacturing."--Publisher's description. Crystal growth Nucleation Crystallization Keimbildung (DE-588)4201506-6 gnd rswk-swf Kristallwachstum (DE-588)4123579-4 gnd rswk-swf Kristallisation (DE-588)4033215-9 gnd rswk-swf Kristallwachstum (DE-588)4123579-4 s Keimbildung (DE-588)4201506-6 s Kristallisation (DE-588)4033215-9 s DE-604 Digitalisierung UB Bayreuth application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=017728827&sequence=000003&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis Digitalisierung UB Bayreuth application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=017728827&sequence=000004&line_number=0002&func_code=DB_RECORDS&service_type=MEDIA Klappentext
spellingShingle	Leubner, Ingo Precision crystallization theory and practice of controlling crystal size Crystal growth Nucleation Crystallization Keimbildung (DE-588)4201506-6 gnd Kristallwachstum (DE-588)4123579-4 gnd Kristallisation (DE-588)4033215-9 gnd
subject_GND	(DE-588)4201506-6 (DE-588)4123579-4 (DE-588)4033215-9
title	Precision crystallization theory and practice of controlling crystal size
title_auth	Precision crystallization theory and practice of controlling crystal size
title_exact_search	Precision crystallization theory and practice of controlling crystal size
title_full	Precision crystallization theory and practice of controlling crystal size Ingo H. Leubner
title_fullStr	Precision crystallization theory and practice of controlling crystal size Ingo H. Leubner
title_full_unstemmed	Precision crystallization theory and practice of controlling crystal size Ingo H. Leubner
title_short	Precision crystallization
title_sort	precision crystallization theory and practice of controlling crystal size
title_sub	theory and practice of controlling crystal size
topic	Crystal growth Nucleation Crystallization Keimbildung (DE-588)4201506-6 gnd Kristallwachstum (DE-588)4123579-4 gnd Kristallisation (DE-588)4033215-9 gnd
topic_facet	Crystal growth Nucleation Crystallization Keimbildung Kristallwachstum Kristallisation
url	http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=017728827&sequence=000003&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=017728827&sequence=000004&line_number=0002&func_code=DB_RECORDS&service_type=MEDIA
work_keys_str_mv	AT leubneringo precisioncrystallizationtheoryandpracticeofcontrollingcrystalsize

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