香兰醇结晶过程开发与优化
发布时间：2021-02-01 20:55
在本研究中,测定了香兰醇在不同溶剂中的溶解度、介稳区,并对其结晶工艺进行了优化。在293.15K到343.15 K温度范围内,采用静态法测定了香兰醇在8种溶剂中的溶解度。发现香兰醇的溶解度随着温度的升高而增大,在乙醇中溶解度最大,而在乙酸丁酯中最小。除此之外,采用改进的Apelblat方程、λh方程和Wilson方程对香兰醇的溶解度进行拟合。基于Wilson方程和实验获得的溶解度数据对香兰醇在不同溶剂中的热力学性质进行了研究。采用激光法测定了香兰醇在乙醇、异丙醇和丙酮中的介稳区宽度。发现介稳区宽度受诸多因醇的影响,如冷却速率、饱和温度、搅拌速率等等。在这三种溶剂中的所有实验,介稳区的宽度都随着饱和温度的升高而变窄,随降温速率增大而变宽。并采用用三种经典理论:Nyvlt理论,Nyvlt自缔合理论和经典3D成核理论研究香草醇的成核动力学。然而,由于成核常数k值的物理意义在Nyvlt方法中不确定,所以Nyvlt自缔合理论和3D经典成核理论更适合。结果表明,香兰醇在乙醇中成核是瞬时的,遵循多核（PN）机制,在异丙醇和丙酮中以high nucleation规则发生。最后,本文对香兰醇的结晶工艺进...
【文章来源】：天津大学天津市 211工程院校 985工程院校 教育部直属院校
【文章页数】：73 页
【学位级别】：硕士
【文章目录】：
摘要
ABSTRACT
Chapter 1 Introduction
1.1.Background
1.2.Statement of Problem
1.3.Objectives
Chapter 2 Solubility and Thermodynamic Properties of Vanillyl Alcohol in Different Solvents
2.1.Introduction
2.2.Experimental Section
2.2.1.Materials
2.2.2.Apparatus and Procedure
2.2.3.Characterization
2.3.Thermodynamic Models
2.3.1.Modified Apelblat Equation
2.3.2.λh Equation
2.3.3.Local Composition Models
2.3.4.Wilson Model
2.4.Results and Discussion
2.4.1.Identification and Characterization of Pure Chemicals
2.4.2.Solubility of Vanillyl Alcohol
2.4.3.Dissolution Thermodynamic Properties
2.5.Conclusions
Chapter 3 Metastable Zone width Determination and Modelling
3.1.Introduction
3.2.Theory
3.2.1.Nyvlt's Approach
3.2.2.Self-Consistent Nyvlt-Like Approach
3.2.3 Classical3D Nucleation Theory
3.3.Experimental Section
3.3.1.Materials
3.3.2.Metastable Zone Width Measurements
3.4.Results and Discussion
3.4.1.Effect of Cooling Rate and Saturation Temperature on MSZW
3.5.Conclusions
Chapter 4 Process Characterization and Optimization of Vanillyl Alcohol Crystallization
4.1.Introduction
4.2.Experimental Section
4.2.1.Materials and Equipment's
4.2.2.Experimental Procedure
4.3.Results and Discussion
4.3.1 Effect of Solvent
4.3.2.Effect of Cooling Rate
4.3.3.Effect of Agitation Speed
4.3.4 Seeding Effect
4.4.Conclusions
Chapter 5 Conclusions and Future Scopes
1.Conclusions
2.Future Scopes
References
Published Papers and Participated Scientific Research
ACKNOWLEDGEMENT
本文编号：3013421
【文章来源】：天津大学天津市 211工程院校 985工程院校 教育部直属院校
【文章页数】：73 页
【学位级别】：硕士
【文章目录】：
摘要
ABSTRACT
Chapter 1 Introduction
1.1.Background
1.2.Statement of Problem
1.3.Objectives
Chapter 2 Solubility and Thermodynamic Properties of Vanillyl Alcohol in Different Solvents
2.1.Introduction
2.2.Experimental Section
2.2.1.Materials
2.2.2.Apparatus and Procedure
2.2.3.Characterization
2.3.Thermodynamic Models
2.3.1.Modified Apelblat Equation
2.3.2.λh Equation
2.3.3.Local Composition Models
2.3.4.Wilson Model
2.4.Results and Discussion
2.4.1.Identification and Characterization of Pure Chemicals
2.4.2.Solubility of Vanillyl Alcohol
2.4.3.Dissolution Thermodynamic Properties
2.5.Conclusions
Chapter 3 Metastable Zone width Determination and Modelling
3.1.Introduction
3.2.Theory
3.2.1.Nyvlt's Approach
3.2.2.Self-Consistent Nyvlt-Like Approach
3.2.3 Classical3D Nucleation Theory
3.3.Experimental Section
3.3.1.Materials
3.3.2.Metastable Zone Width Measurements
3.4.Results and Discussion
3.4.1.Effect of Cooling Rate and Saturation Temperature on MSZW
3.5.Conclusions
Chapter 4 Process Characterization and Optimization of Vanillyl Alcohol Crystallization
4.1.Introduction
4.2.Experimental Section
4.2.1.Materials and Equipment's
4.2.2.Experimental Procedure
4.3.Results and Discussion
4.3.1 Effect of Solvent
4.3.2.Effect of Cooling Rate
4.3.3.Effect of Agitation Speed
4.3.4 Seeding Effect
4.4.Conclusions
Chapter 5 Conclusions and Future Scopes
1.Conclusions
2.Future Scopes
References
Published Papers and Participated Scientific Research
ACKNOWLEDGEMENT
本文编号：3013421
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