CERTIFICATION

THIS is to certify that the project report titled THE DEVELOPMENT OF

ZEOLITE Y CATALYST FROM OKPELLA KAOLIN CLAY is a detailed
research work done by Arowolo Ayodeji Mustapha (Reg No. 20101720883) in
partial fulfillment of the award of Bachelor of Engineering (B.Eng) in Chemical
Engineering in the School of Engineering and Engineering Technology, Federal
University of Technology Owerri.

Mr. I J Okolie

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Supervisor

Date and Signature

Engr Dr O E Onyelucheya

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Head of Department

Date and Signature

Engr Prof G I Nwandikom

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Dean SEET

Date and Signature

Prof F O Chukwuma

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External Examiner

Date and Signature

DEDICATION
This project is dedicated to God Almighty for His grace, strength and provision
throughout the course of this project and to my parents Mr. and Mrs. F. M.
Arowolo for their love, support and assistance.

ACKNOWLEDGEMENT
I will like to acknowledge God Almighty for His guidance and protection in
accomplishing this study. I would also like to acknowledge my supervisor, Mr I J
Okolie for his efforts in letting this project go through, his timely input and
corrections will never be forgotten.
Exclusive thanks to Engr. Clement, the owner of New concept lab where we did
our experiments. They provided assistance in getting us the reagents we required
for our experiment. I will like to acknowledge my group members, Joe, Godswill,
Gloria, Adindu and Joaquin for being excellent in their contributions towards the
project and for actively participating when needed. Much thanks to my roommate,
Dave, who supported me when I came back late from Obinze because of
experiments.
Finally, I will like to acknowledge chemical engineering department, FUTO for
giving me the opportunity to do such a nice project.

ABSTRACT
The aim of this research project is the development of zeolite from locally sourced
kaolin clay. Okpella kaolin clay used was sourced from Okpella village in Edo
state, Nigeria. The procured kaolin was refined because of its impurities by
beneficiation, and then it was activated for reaction by dehydroxylation. Addition
of external silicate material, sodium silicate, was used to increase the silicate to
aluminate ratio. During the experiment, the effects of heating time and temperature
were evaluated upon dehydroxylation at elevated temperatures (calcining).
Optimum conditions for the metakaolin at 650C and heating time of 60minutes
were used for the synthesis of the zeolite. Ageing and Crystallization were carried
out at various conditions to determine the optimum. Effect of aging time,
crystallization time and temperature were also evaluated in the formation of
crystals. Zeolite crystals were successfully produced at the end of the experiments.

LIST OF TABLES
Table 2.1Chemical composition of kaolin.7
Table 2.2: Location of Kaolin deposits adapted from Non-metallic mineral
endowments in Nigeria..9
Table 2.3: Application of kaolin in the industries...14
Table 2.4: Nomenclature of Zeolites and Molecular Sieves...16
Table 2.5: values of molar ratios according to type of zeolite required..27
Table 2.6 The chemical content based on XRF analysis laboratory synthesized
zeolite samples at 30C....43
Table 3.1(a-d). Experimental Conditions of Zeolite Y Synthesized from Okpella
Kaolin Based on the addition of External Silica Source.57
Table 4.1. XRF Analysis of Okpella Kaolin Clay...59
Table 4.2 Dehydroxylation/Metakaolinization at Temperature of 550oC.61
Table 4.3 Dehydroxylation/Metakaolinization at Temperature of 600oC.62
Table 4.4 Dehydroxylation/Metakaolinization at Temperature of 650oC.....63
Table 4.5 Dehydroxylation/Metakaolinization at Temperature of 700oC.64
Table 4.6 Dehydroxylation/Metakaolinization at Temperature of 750oC.65
Table 4.7 Percentage (%) mass loss of Okpella kaolin clay for different
calcination temperature and times66
Table 4.8 Degree of dehydroxylation of Okpella kaolin clay for different
calcination temperature and times.90

TABLE OF FIGURES
Figure 2.1: Kaolinite structure..6
Figure 2.2: XRD pattern of kaolin7
Figure 2.3: SEM of kaolin8
Figure 2.4: Flowsheet diagram for beneficiation of kaolin12
Figure 2.5: Structures of four selected zeolites...17
Figure 2.6: Crystals of the zeolite mineral, natrolite...18
Figure 2.7: Bronsted acid in zeolites...21
Figure 2.8: Illustration of solid-phase mechanism .32
Figure 2.9: Illustration of Solution-mediated Transport Mechanism .34
Figure 2.10: IR Analysis Spectrum ............................41
Figure 2.11: SEM of Kaolin42
Figure 2.12: XRD Analysis of a Typical Synthesized Zeolite Sample...44
Figure 3.1: Raw white and off-white Okpella kaolin......49
Figure 3.2: Project group and supervisor at kaolin mining site at Okpella 49
Figure 3.3: Project students, supervisor and plant operator at kaolin processing
plant, Okpella ..50
Figure 3.4 Process Flow Chart of the Refining of Okpella Kaolin.52
Figure 3.5: Settling tanks for refining kaolin......54
Figure 4.1 Graph of degree of dehydroxylation against heating time with different
temperatures 67

TABLE OF CONTENTS
Title Pagei
Certification...ii
Dedication....iii
Acknowledgment iv
Abstract .v
List of tables.vi
List of figures .vii
Table of Contents .viii
Chapter 1 Introduction...1
1.1Background Information..1
1.2 Problem Statement...3
1.3 Objective of the Research....3
1.4 Scope of Study.....................3
1.5 Justification of the Research4
Chapter 2 Literature Review..5
2.1 Kaolin..5
2.1.1 Properties of Kaolin..7
2.1.2 Locations of Kaolin..8
2.1.3 Processing of kaolin12
2.1.4 Applications of kaolin13
2.2 Zeolites..15
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2.2.1 Structure.17
2.2.2 Applications of Zeolite...18
2.3 Properties of Zeolite..........20
2.3.1 Ion Exchange .20
2.3.2 Catalysis.21
2.3.3 Adsorption..22
2.4 Synthesis of Zeolites..23
2.4.1 Settling time for refining kaolin.23
2.4.2 Metakaolinization of Kaolin...25
2.4.3 Synthesis and Dealumination of metakaolin to form zeolites26
2.5 Crystallization of Zeolites28
2.5.1 Crystallization Process and Formation Mechanism of Zeolites30
2.5.1.1 Solid Hydrogel Transformation Mechanism ..30
2.5.1.2 Solution-mediated Transport Mechanism ..32
2.5.1.3 Dual-phase Transition Mechanism 34
2.5.2 Influence of Various Factors on Zeolite Crystal Growth ..35
2.5.2.1 Aging of the Reaction mixture ...35
2.5.2.2 Crystallization Temperature ...36
2.5.2.3 Crystallization time .37
2.5.2.4 Alkalinity of Crystallizing System .38
2.5.2.5 Dilution of Crystallizing System 39
2.6 Product characterization40
2.6.1 IR Analysis.40
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2.6.2 Scanning Electron Microscope...41

2.6.3 X-ray Fluorescence.42
2.6.4 XRD Analysis43
2.7 Review of previous work done on synthesis of zeolite.44
2.7.1 Synthesis of Faujasite Zeolites from Kankara Kaolin Clay by (Atta et al.)...44
2.7.2 Making zeolite A membrane from kaolin by electrophoresis by (Mohammadi
and Pak)...45
2.7.3 In-situ Synthesis of NaY Zeolite with Coal-Based Kaolin by (Liu et al.)..46
2.7.4 Preparation of Zeolite Y Catalyst for Petroleum Cracking by (Mu and Mya)
47
Chapter 3Materials and Methodology.....48
3.1 Materials48
3.1.1 Kaolin.48
3.2 Reagents and apparatus.50
3.3 Experimental techniques...................................51
3.3.1 Preliminary Characterization of Raw Okpella Kaolin...51
3.3.2 Refining of Raw Okpella Kaolin .51
3.3.3 Dehydroxylation/ Metakaolinization of Refined Dried Okpella Kaolin ...54
3.3.4 Production/Synthesis of Zeolite Y .56
Chapter 4 Results and Discussions59
4.1 Chemical Analysis of raw kaolin .59
4.2 Discussion on Refining the raw kaolin 60

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4.3 Result of Dehydroxylation/Metakaolinization of Okpella Kaolin Clay61

Chapter 5 Conclusion and Recommendation..68
5.1 Conclusion .68
5.2 Recommendation .68
References...69
Appendix .74

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