Synthesis of zeolites from geological materials and industrial wastes for potential application in environmental problems




НазваниеSynthesis of zeolites from geological materials and industrial wastes for potential application in environmental problems
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DOCTORAL THESIS


Synthesis of zeolites from geological materials and industrial wastes for potential application in environmental problems


Carlos Alberto Ríos Reyes





Synthesis of zeolites from geological materials and industrial wastes for potential application in environmental problems


A thesis submitted to the Graduate School of the University of Wolverhampton


By


Carlos Alberto Ríos Reyes


In partial fulfilment of the requirements for the degree of Doctor in Philosophy in the School of Applied Sciences


2008

Table of Contents

Page

Declaration

vi

Abstract

vii

Acknowledgments

ix

List of Tables

xi

List of Figures

xiii

List of Abbreviations

xix

Publications: Journals and Conferences

xxiv







Chapter 1. Introduction

1

1.1. Background

2

1.2. Environmental impact

4

1.3. Water treatment technology

4

1.4. Zeolites and the environment

5

1.5. Scope and objectives of this research

6

1.6. Structure of the thesis

7







Chapter 2. Literature survey

9

2.1. Historical remarks

10

2.2. Zeolite framework structure and properties

11

2.3. Environmental applications

15

2.4. Zeolite synthesis

16

2.4.1. Background

16

2.4.2. Zeolite synthesis from kaolinite, natural clinker and fly ash

18

2.4.2.1. Kaolinite-based zeolitic materials

18

2.4.2.2. Natural clinker-based zeolitic materials

20

2.4.2.3. Fly ash-based zeolitic materials

21







Chapter 3. Materials and Experimental Methods

24

3.1. Raw materials

25

3.2. Zeolite synthesis

25

3.2.1. Classic hydrothermal synthesis

26

3.2.2. Alkaline-fusion followed by hydrothermal reaction

29

3.3. Preparation of synthetic solutions and sampling of acid mine drainage (AMD)

31

3.4. Batch experiments

32

3.5. Techniques of characterization

33

3.5.1. X-Ray Diffraction (XRD) Analysis

33

3.5.2. Fourier Transform Infrared (FT-IR) Spectroscopy

34

3.5.3. Scanning Electron Microscopy (SEM)

35

3.5.4. Thermogravimetric Analysis (TGA)

35

3.5.5. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance (MAS NMR)

36

3.5.6. Standard Methods for the Examination of Water and Wastewater

36







Chapter 4. Characterization of the raw materials

38

4.1. Raw kaolinite

40

4.1.1. Introduction

40

4.1.2. Chemical and mineralogical analyses

40

4.1.3. Dehydroxylation of kaolinite

41

4.1.4. Characterization of the unreacted and thermally treated kaolinite

43

4.2. Raw natural clinker

48

4.2.1. Geological setting

48

4.2.2. Chemical and mineralogical analyses

50

4.3. Raw fly ash

54

4.3.1. Industrial context

54

4.3.2. Chemical and mineralogical analyses

54

4.4. Conclusions to chapter 4

59







Chapter 5. Synthesis of kaolinite-based zeolitic materials

60

5.1. Kaolinite as a starting material

61

5.2. Conversion of kaolinite in the system Na2O-SiO2-Al2O3-H2O

63

5.2.1. Chemical and mineralogical analyses

63

5.2.2. Fourier Transform Infrared Spectroscopy

69

5.2.3. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance

70

5.2.4. Thermogravimetric analysis

73

5.2.5. Phase transformation

76

5.2.6. Summary

77

5.3. Hydrothermal transformation of kaolinite in the system K2O-SiO2-Al2O3-H2O

78

5.3.1. Chemical and mineralogical analyses

78

5.3.2. Fourier Transform Infrared Spectroscopy

83

5.3.3. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance

83

5.3.4. Thermogravimetric analysis

87

5.3.5. Summary

87

5.4. Metakaolinite as a starting material

88

5.5. Hydrothermal transformation of metakaolinite in the system Na2O-SiO2-Al2O3-H2O

90

5.5.1. Chemical and mineralogical analyses

90

5.5.2. Fourier Transform Infrared Spectroscopy

93

5.5.3. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance

94

5.5.4. Thermogravimetric analysis

96

5.5.5. Summary

96

5.6. Hydrothermal transformation of kaolinite and metakaolinite in the system CaO-SiO2-Al2O3-H2O

97

5.6.1. Chemical and mineralogical analyses

98

5.6.2. Fourier Transform Infrared Spectroscopy

101

5.6.3. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance

103

5.6.4. Thermogravimetric analysis

106

5.6.5. Summary

108

5.7. Conclusions to chapter 5

109







Chapter 6. Synthesis of natural clinker-based zeolites

111

6.1. Chemical and mineralogical analyses

113

6.1.1. Synthesis experiments in NaOH media

113

6.1.2. Synthesis experiments in KOH media

114

6.1.3. Synthesis experiments using a fusion process followed by hydrothermal reaction

114

6.2. Fourier Transform Infrared Spectroscopy

118

6.3. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance

121

6.4. Thermogravimetric analysis

124

6.5. Conclusions to chapter 6

125







Chapter 7. Synthesis of fly ash-based zeolites

127

7.1. Conversion of fly ash by alkaline hydrothermal treatment

128

7.1.1. Synthesis experiments in NaOH media

128

7.1.2. Synthesis experiments in KOH media

135

7.2. Conversion of fly ash using a fusion process followed by hydrothermal reaction

139

7.3. 29Si and 27Al Magic Angle Spinning Nuclear Magnetic Resonance

144

7.3.1. 29Si MAS NMR spectra

144

7.3.2. 22Al MAS NMR spectra

146

7.4. Reaction mechanism during zeolite synthesis

146

7.5. Conclusions to chapter 7

149







Chapter 8. Application of different adsorbent materials for the removal of metal ions and ammonium from polluted effluents

151

8.1. Introduction

152

8.2. Removal of heavy metals and ammonium from synthetic solutions

154

8.2.1. Preliminary experiment of treatment using fly ash and fly ash- based GIS-type zeolite

154

8.2.2.1. pH and EC

154

8.2.2.2. Heavy metal removal

156

8.2.2. Treatment using kaolinite, natural clinker and fly ash

158

8.2.2.1. pH and EC

158

8.2.2.2. Heavy metal removal

160

8.2.2.3. Ammonium removal

163

8.2.3. Treatment using different zeolite-like materials

164

8.2.3.1. pH and EC

164

8.2.3.2. Heavy metal removal

166

8.2.3.3. Ammonium removal

168

8.3. Removal of heavy metals and ammonium from acid mine drainage

171

8.3.1. Introduction

171

8.3.2. Chemistry of acid mine drainage

171

8.3.3. Characterization of acid mine drainage samples

173

8.3.4. Acid mine drainage treatment using fly ash, natural clinker and synthetic zeolites

175

8.3.4.1. Kinetics of the neutralization reaction

175

8.3.4.2. Heavy metal removal

176

8.3.4.3. Ammonium removal

180

8.3.4.4. Effect of sorbent dosage

182

8.3.4.5. pH vs. dissolved metal content

185

8.3.4.6. Regeneration and long-term stability of the sorbents

186

8.4. Conclusions to chapter 8

187







Chapter 9. Conclusions

190

9.1. Critical overview

191

9.2. Overall significance

193

9.3. Future work

194







Bibliography

197

Appendices



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