SLOW PYROLYSIS OF IMPERATA CYLINDRICA IN A FIXED BED REACTOR AZDUWIN BINTI KHASRI A thesis submitted in fulfilment of the requirements for the award of the Master of Engineering (Chemical) Faculty of Chemical Engineering Universiti Teknologi Malaysia JULY 2012
25
Embed
SLOW PYROLYSIS OF IMPERATA CYLINDRICA IN A FIXED …eprints.utm.my/id/eprint/32517/1/AzduwinKhasriMFKK2012.pdf · Oksigen (CHNS/O), Bom Kalorimeter, dan beberapa kaedah analisis.
This document is posted to help you gain knowledge. Please leave a comment to let me know what you think about it! Share it to your friends and learn new things together.
Transcript
SLOW PYROLYSIS OF IMPERATA CYLINDRICA IN A FIXED BED REACTOR
AZDUWIN BINTI KHASRI
A thesis submitted in fulfilment of the requirements for the award of the Master of Engineering (Chemical)
Faculty of Chemical Engineering Universiti Teknologi Malaysia
JULY 2012
iii
To my beloved husband, mother and father
iv
ACKNOWLEDGEMENT
A million thanks goes to my supervisor Dr. Tuan Amran Tuan Abdullah for
his guidance, and encouragement to complete my dissertation. He gave full
cooperation and helps to ensure the progress of this dissertation run smoothly and
successfully. I wish to express my appreciation to all the technician and lab assistant
as well for helping me in doing the experiments.
I am also indebted to University Malaysia Perlis together with Ministry of
Higher Education for funding my Master study. Without their fund, it is impossible
for me to further study and complete my dissertation project. Other than that, special
thanks to my beloved husband Mohd Ridzuan Mohd Jamir, my laboratory partner
Redza Shah Azmeer Hasanudin, all my family members, colleagues, and friends for
their advice, and support. Hopefully, this thesis will benefit all of us.
v
ABSTRACT
Slow pyrolysis of Imperata Cylindrica has been conducted in a fixed bed
reactor to determine the effect of temperature and particle sizes towards the product
yield. The characterization of the Imperata Cylindrica has been analysed using
several instruments such as Thermogravimetric Analysis (TGA), Carbon Hidrogen
Nitrogen Sulfur and Oxygen (CHNS/O) analyzer, Bomb Calorimeter, and several
analytical methods. Pyrolysis experiments were performed at temperature between
450- 600 °C, and particle sizes of 0.25-1.00 mm with constant nitrogen flow rate of
100 cm3min-1 and heating rate of 22 ºC . min-1 (slow mode). The highest liquid oil
yield obtained was 20.88 % at temperature 500 °C, with particle size of 0.5-1.0 mm,
and heating rate of 22 ºC . min-1. The obtained yield of liquid, solid and gas from
pyrolysis were found in the range of 3.25-20.88 %, 22.63-30.50 % and 49.13-74.13
% respectively at different pyrolysis conditions. Liquid bio-oil produced from the
pyrolysis of Imperata Cylindrica shows high water content in the range of 58.09-
72.74 % which was checked using Karl Fisher Titration. From Gas Chromatography-
Mass Spectrometry (GC-MS), the chemical components present in the liquid oil from
pyrolysis of Imperata cylindrica include acids, phenols, ketones, aldehydes, ethers,
and some species of aromatics.
.
vi
ABSTRAK
Pirolisis perlahan Imperata cylindrica telah dijalankan di dalam reaktor katil
tetap untuk menentukan kesan suhu dan saiz zarah terhadap hasil produk. Pencirian
cylindrica Imperata telah dianalisis dengan menggunakan beberapa instrumen seperti
Termogravimetri Analisis (TGA),Penganalisa Sulfur Nitrogen Karbon Hidrogen dan
Oksigen (CHNS/O), Bom Kalorimeter, dan beberapa kaedah analisis. Eksperimen
pirolisis telah dijalankan pada suhu antara 450-600 ° C, dan saiz zarah 0.25-1.00 mm
dengan kadar aliran nitrogen malar 100 cm3. min-1 dan kadar pemanasan 22 º C .
min-1 (mod perlahan). Hasil minyak cecair tertinggi yang diperolehi adalah 20.88 %
pada suhu 500 °C, dengan saiz zarah 0.5-1.0 mm, dan kadar pemanasan 22 º C . min-
1. Hasil yang diperolehi cecair, pepejal dan gas daripada pirolisis ditemui dalam julat
3.25-20.88 %, 22.63-30.50 % dan 49.13-74.13 % masing-masing pada keadaan
pirolisis yang berbeza. Cecair bio-minyak yang dihasilkan daripada pirolisis
Imperata cylindrica menunjukkan kandungan air yang tinggi dalam julat 58.09-72.74
% yang telah diperiksa menggunakan Pentitratan Karl Fisher. Daripada Gas
Kromatografi-Jisim Spektrometri (GC-MS), komponen kimia yang hadir dalam
minyak cecair daripada pirolisis Imperata cylindrica termasuk asid, fenol, keton,
aldehid, eter, dan beberapa spesies aromatik.
vii
TABLE OF CONTENTS
CHAPTER TITLE PAGE
DECLARATION ii
DEDICATION iii
ACKNOWLEDGEMENTS iv
ABSTRACT v
ABSTRAK vi
TABLE OF CONTENTS vii
LIST OF TABLES x
LIST OF FIGURES xi
LIST OF ABBREVIATIONS xiii
LIST OF SYMBOLS xiv
LIST OF APPENDICES xv
1
INTRODUCTION
1.1 General Background 1
1.2 Problem statement 2
1.3 Objectives 3
1.4 Scopes of research 4
1.5 Hypothesis 4
1.6 Significant of Research 5
viii
1.7 Thesis Organisation 6
2 LITERATURE REVIEW
2.1 Imperata Cylindrica 7
2.1.1 Introduction
7
2.1.2 Cultivation 8
2.1.3 Usage 8
2.2 Characterization of biomass
8
2.3 Pyrolysis 11
2.3.1 Type of Pyrolysis 12
2.3.1.1Conventional(slow) Pyrolysis 13
2.3.1.2 Fast Pyrolysis 16
2.3.1.3 Flash Pyrolysis 17
2.3.2 Pyrolysis feed stock 18
2.3.3 Process features and requirements 19
2.3.3.1 Reactor configuration 19
2.3.3.2 Heat transfer 20
2.3.3.3 Char removal 20
2.3.3.4 Liquids collection 21
2.3.3.5 By-products 22
2.4 Pyrolysis liquid (bio-oil) 23
2.4.1 Physicochemical properties 23
2.4.1.1 Water content 24
2.4.1.2 Oxygen 25
2.4.1.3 Viscosity 26
2.4.1.4 Acidity 26
2.4.1.5 Heating Value 26
2.4.1.6 Ash 27
3 RESEARCH METHODOLOGY
3.1 Feedstock sample and preparation 28
3.2 Apparatus 29
3.3 Chemicals 29
ix
3.4 Characterization of Biomass 29
3.4.1Proximate analysis 30
3.4.2 Ultimate Analysis 30
3.4.3 Component Analysis 31
3.4.3.1 Analysis of extractives 31
3.4.3.2 Analysis of hemicellulose 31
3.4.3.3 Analysis of lignin 33
3.4.3.4 Analysis of cellulose 33
3.4.4 Heating value Analysis 34
3.5 Pyrolysis Procedure 35
3.6 Bio-oil analysis 39
3.6.1 GC-MS 40
3.6.2 Water content 40
4 RESULTS AND DISCUSSION
4.1 Characterization of Imperata Cylindrica 41
4.1.1 Proximate Analysis 41
4.1.2 Ultimate Analysis 44
4.1.3 Component Analysis 45
4.1.4 Heating value Analysis 47
4.2 Pyrolysis Experimental 49
4.3 Bio-oil Analysis 55
4.3.1 Water content
55
4.3.2 GC-MS
57
5 CONCLUSIONS AND RECOMMENDATIONS
62
5.1 Conclusions
62
5.2 Recommendations 63
REFERENCES 65
Appendices A-C 70-77
x
LIST OF TABLES
TABLE NO. TITLE PAGE
2.1 The main operating parameters for different type of
pyrolysis
12
2.2 Characterization analysis of Rice husk 14
2.3 Various type of reactor used for pyrolysis and the heating
method
19
2.4 Comparison of common properties of bio-oil (wood
biomass) and Heavy fuel oil
24
4.1 Proximate analysis of Imperata cylindrica 43
4.2 Ultimate analysis of Imperata Cylindrica 46
4.3 Result data for component analysis calculation 47
4.4 Component analysis of Imperata Cylindrica 48
4.5 Heating value of Imperata Cylindrica 49
4.6 Characterization of Imperata Cylindrica 49
4.7 Product yield and conversion of Imperata Cylindrica 52
4.8 Functional group presents in Imperata Cylindrica liquid
oil
59
4.9 Summary of component present in all samples analyzed
by GC-MS
60
xi
LIST OF FIGURES
FIGURE NO. TITLE PAGE
2.1 Selective parameters of biomass characterization 9
2.2 Pyrolyser set-up of rice husk experiment 14
2.3 Effect of temperature on slow pyrolysis of Rice husk 15
2.4 Effect of Particle size on slow pyrolysis of Rice husk 16
3.1 Sample of Imperata Cylindrica 29
3.2 Flow chart of Characterization analysis 31
3.3 Residue of G1 34
3.4 Residue of G2 34
3.5 A bomb Calorimeter 36
3.6 Pyrolysis experimental set-up 37
3.7 Flow chart of pyrolysis experimental for first run 39
3.8 Flow chart of pyrolysis experimental for second run 40
3.9 Karl Fisher Titration 41
4.1 The proximate analysis 44
4.2 TGA and DTG curves for Imperata Cylindrica 44
4.3 Pyrolysis set-up 51
4.4 Liquid oil 51
4.5 Solid char 51
4.6 Effect of temperature on slow pyrolysis of Imperata Cylindrica
54
4.7 Effect of particle size on slow pyrolysis of Imperata
Cylindrica
55
4.8 Water content of liquid oil for different pyrolysis 57
xii
temperature
4.9 Water content of liquid oil for different particle size 57