Chaudemanche, Cyril (2007) Polysaccharides, an alternative for the development of a new plant hard capsule. PhD thesis Sciences et Génie des Matériaux, CEMEF Centre de Mise en Forme des Matériaux, ENSMP p.269.

Abstract

The manufacturing of a new plant hard capsule was performed in this work using two well known biopolymers: starches and carrageenans. In relation with the current industrial process parameters, structure and properties of these polysaccharides in the liquid and in the gel states were determined using mainly rheological tools. By applying shear stresses on pastes, solutions and gels and by plotting phase diagrams, the influences of the botanical origin of starches and of different chemical treatment such as the hydroxypropylation were discussed. Flow and viscoelastic properties of components alone and mixtures were measured to reproduce as close as possible the rheological behaviour (gelation temperatures, gel strength…) of the gelatin, the classical material used to manufacture hard-capsules. Finally, a numerical approach of the hot dip coating process was performed. On the bases of a 3D thermomechanical model, the average growth rate of solidified layer during the dipcoating process was simulated and the influences of the polymer viscosity and the velocity of the mould motion on the solidified layer thickness were calculated.

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Table of content

Table of contents

RESUME FRANCOPHONE

INTRODUCTION

NOMENCLATURE

CHAPTER 1

RESUME DU CHAPITRE 1

MEDICINAL HARD CAPSULES, STATE OF THE ART

INTRODUCTION

2. THE HISTORY OF THE GELATIN CAPSULE

2.1 Invention of the gelatin capsule

2.2 Invention of the gelatin hard capsule

2.3 Development of gelatin hard capsules

3. MANUFACTURE OF TWO-PIECE HARD CAPSULES

3.1 Preparation of the gelatin solution

3.2 Capsule formation

3.3 Drying

3.4 Capsule assembly

3.5 Hard capsules properties

4. GELATIN MANUFACTURE AND PROPERTIES

4.1 Gelatin application

4.2 Gelatin structure

4.3 Physical characteristics

5. GELATIN ALTERNATIVES

5.1 The fear of transmissible encephalopathies

5.2 Alternatives

5.3 Current alternative

6. CONCLUSIONS OF CHAPTER I

REFERENCES

CHAPTER 2

THE CARRAGEENANS

1. REVIEW OF CARRAGEENAN STRUCTURES AND PROPERTIES

1.1 Chemical structure

1.2 Conformation in the sol state

1.3 Aggregation and gelation in carrageenans

1.4 Basic concepts on rheology for gelation analysis

2. EXPERIMENTAL RESULTS: FLOW AND GELATION OF k-CARRAGEENAN SOLUTIONS

2.1 Materials and method

2.2 Results and discussion

3. CONCLUSIONS OF CHAPTER II

REFERENCES

CHAPTER 3

RESUME DU CHAPITRE 3

THE STARCHES.

1. STRUCTURES AND PROPERTIES OF STARCHES: A REVIEW

1.1 Introduction

1.2 Chemical structure

1.3 The gelatinisation process

1.4 Gelation

1.5 Behaviour of starch suspensions under flow.

2. EXPERIMENTAL RESULTS: PROPERTIES OF STARCHES

2.1 Materials and methods

2.2 Results and discussion

3. CONCLUSIONS OF CHAPTER III

REFERENCES

CHAPTER 4

RESUME DU CHAPITRE 4

MIXTURES OF PREGELATINISED MAIZE STARCH AND k-CARRAGEENAN COMPATIBILITY, RHEOLOGY AND GELATION

1. ABSTRACT

2. INTRODUCTION

3. MATERIALS AND METHODS

3.1 Materials and preparation of solutions and mixtures

3.2 Methods

4. RESULTS

4.1 Visual observations

4.2 Dilute mixtures

4.3 Semi-dilute mixtures

5. DISCUSSION

6. CONCLUSIONS OF CHAPTER IV

7. ACKNOWLEDGEMENTS

REFERENCES.

CHAPTER 5

RESUME DU CHAPITRE 5

THERMODYNAMIC STUDY OF THE (IN)COMPATIBILITY BETWEEN A HYDROXYPROPYLATED AND A WAXY MAIZE STARCH WITH k-CARRAGEENAN

1. REVIEW OF THERMODYNAMICS OF MIXED POLYMER SOLUTIONS

1.1 Introduction

1.2 Thermodynamics of polymers in solution

1.3 Consequences of mixing polymers in ternary systems

1.4 Flory-Huggins model for ternary polymer solutions

2. EXPERIMENTAL RESULTS.

2.1 Materials and Methods

2.2 Results and Discussion

3. CONCLUSIONS OF CHAPTER V

REFERENCES

CHAPTER 6

RESUME DU CHAPITRE 6

EXPERIMENTAL, ANALYTICAL AND NUMERICAL STUDIES OF THE DIP-COATING PROCESS.

INTRODUCTION

2. BUILDING UP OF A DIP COATING PROTOTYPE

2.1 Dip-coating prototype

2.2 Measurement of capsule thickness.

2.3 Determination of contact angle and surface energy

3. ANALYTICAL DESCRIPTION OF THE DIP-COATING PROCESS

3.1 The Stephan approach

3.2 The Stephan method applied to the dip-coating process.

3.3 Analytical resolution

3.4 Comparison between analytical and experimental results

4. 3D NUMERICAL MODELLING OF A DIP-COATING PROCESS BY A MULTIDOMAIN MACROSCOPIC APPROACH

4.1 Abstract

4.2 Introduction

4.3 Basic thermal and mechanical equations

4.4 General solution obtained with finite element method

4.5. Applications

4.6 Conclusions

4.7 Comparison between experimental and numerical results

5. CONCLUSIONS OF CHAPTER VI

REFERENCES

CONCLUSIONS

APPENDIX A: SURFACE TENSION

APPENDIX B: METHODS FOR DETERMINING THE SURFACE ENERGY

APPENDIX C: METHODS OF EVALUATING THE DROP SHAPE

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