DEVELOPMENT OF MESOSCALE OSCILLATORY BAFFLED REACTOR (MOBR) FOR BIOETHANOL PRODUCTION SYAMSUTAJRI BINTI SYAMSOL BAHRI

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1 DEVELOPMENT OF MESOSCALE OSCILLATORY BAFFLED REACTOR (MOBR) FOR BIOETHANOL PRODUCTION SYAMSUTAJRI BINTI SYAMSOL BAHRI MASTER OF ENGINEERING (CHEMICAL) UNIVERSITI MALAYSIA PAHANG

2 UNIVERSITI MALAYSIA PAHANG DECLARATION OF THESIS AND COPYRIGHT Author s Full Name : SYAMSUTAJRI BINTI SYAMSOL BAHRI Date of Birth : 19 MARCH 1988 Title : DEVELOPMENT OF MESOSCALE OSCILLATORY BAFFLED REACTOR (MOBR) FOR BIOETHANOL PRODUCTION Academic Session : 2015/2016 I declare that this thesis is classified as: CONFIDENTIAL RESTRICTED OPEN ACCESS (Contains confidential information under the Official Secret Act 1997) (Contains restricted information as specified by the organization where research was done) I agree that my thesis to be published as online open access (Full text) I acknowledge that Universiti Malaysia Pahang reserve the right as follows: 1. The Thesis is the Property of Universiti Malaysia Pahang. 2. The Library of Universiti Malaysia Pahang has the right to make copies for the purpose of research only. 3. The Library has the right to make copies of the thesis for academic exchange. Certified By: (Student s Signature) (Supervisor s Signature) W.M. Hafizuddin bin W.Yussof New IC/Passport Number Name of Supervisor Date : Date :

3 SUPERVISOR S DECLARATION I hereby declare that I have checked this thesis and in my opinion, this thesis is adequate in terms of scope and quality for the award of the degree of Master of Engineering in Chemical Engineering. (Supervisor s Signature) Full Name Position : DR WAN MOHD HAFIZUDDIN BIN WAN YUSSOF : SENIOR LECTURER Date :

STUDENT S DECLARATION I hereby declare that the work in this thesis is based on my original work except for quotations and citation which have been duly acknowledged.

4 STUDENT S DECLARATION I hereby declare that the work in this thesis is based on my original work except for quotations and citation which have been duly acknowledged. I also declare that it has not been previously or concurrently submitted for any other degree at Universiti Malaysia Pahang or any other institutions. (Author s Signature) Full Name ID Number : SYAMSUTAJRI BINTI SYAMSOL BAHRI : MKC12010 Date : SEPTEMBER 2015

5 DEVELOPMENT OF MESOSCALE OSCILLATORY BAFFLED REACTOR (MOBR) FOR BIOETHANOL PRODUCTION SYAMSUTAJRI BINTI SYAMSOL BAHRI Thesis submitted in fulfilment of the requirements for the award of the degree of Master of Engineering Faculty of Chemical & Natural Resources Engineering UNIVERSITI MALAYSIA PAHANG MAY 2016

6 TABLE OF CONTENTS DECLARATION TITLE PAGE DEDICATION ACKNOWLEDGEMENTS ABSTRACT ABSTRAK TABLE OF CONTENTS LIST OF FIGURES LIST OF TABLES LIST OF ABBREVIATIONS LIST OF SYMBOLS i ii iii iv v vi x xiii xv xvii INTRODUCTION 1.1 Background Significance of Study Research Objectives Research Scope Thesis Outline 6 LITERATURE REVIEW 2.1 Introduction Reactor Engineering 8 Batch Reactor (BR) 8 Fed Batch Reactor (FBR) 9 Continuous-Flow Stirred Tank Reactor (CSTR) 9 Plug Flow Reactor (PFR) 10 Flow Pattern Oscillating Reactor 13 vi

7 Oscillatory Baffled Reactor (OBR) 15 Power Density 17 Advantages of OBR 18 Mesoscale Oscillatory Baffled Reactor (MOBR) Oscillatory Flow Mixing 22 Parameters Governing Oscillatory Flow 25 Effect of Dynamic Parameters 28 Effect of Geometrical Parameters 30 Effect of Frequency (f) and Amplitude (xo) 32 Effectiveness Mixing in Mobr Residence Time Distribution (RTD) in MOBR 34 Introduction 34 Measurement of RTD 36 Reactor Modelling Using RTD 40 Tanks-In-Series Model Application of OBR 46 OBR in Chemical and Biochemical Processes 48 OBR in Bioethanol Production 50 METHODOLOGY 3.1 Introduction Development of MOBR 54 Fabrication of MOBR Characterization of MOBR 58 Evaluation of Mixing Conditions 58 Residence Time Distribution Analysis 59 Effect of Frequency 62 Effect of Amplitude 63 Effect of Net Flow and Oscillatory Flow 63 Dependence of The Fluid Mixing on The Velocity Ratio Bioethanol Production 63 Introduction 63 Media Preparation 65 vii

8 Chemical Nutrient Broth Yeast 66 Inoculum Preparation 66 Cell Washing 67 Bioethanol Production Using STR 67 Bioethanol Production Using MOBR Analytical Method 69 Glucose Concentration 69 Biomass Concentration 70 Bioethanol Concentration 71 RESULT AND DISCUSSION 4.1 Introduction Development of Mesoscale Oscillatory Baffled Reactor (MOBR) Residence Time Distribution (RTD) Effect of Oscillation Frequency Effect of Oscillation Amplitudem Effect of Net Flow and Oscillatory Flow Dependence of The Fluid Mixing on The Velocity Ratio Bioethanol Production 88 CONCLUSION AND RECOMMENDATION 5.1 Conclusion Recommendations 94 REFERENCES 96 APPENDICES A Reactor Power Density Calculation 107 B Dynamic Parameters Calculation 108 viii

9 C Standard Curve of Glucose Concentration 110 D Calibration Curve of Cell Concentration 111 E Standard Curve of Bioethanol Concentration 112 F HPLC Chromatograph 113 G Pump Command 114 H Other Calculations 116 I Batch Fermentation 118 J Data Analysis for RTD 123 K Bioethanol Theoretical Yield Calculation 125 ix

10 LIST OF FIGURES Figure Title Page 2.1 Typical proportion of a STR Continuous stirred tank reactor a) with agitator and internal heat transfer surface b) with pump around mixing and external heat transfer surface Three basic ideal flows for ideal reactor types (batch, plug flow and mixed flow) Types of nonideal flows in reactors Velocity profiles for laminar, turbulent and plug flows The oscillatory baffled reactor design Geometry of a single smooth periodic constrictions (SPCs) tube Schematic diagram of integral baffles (Thickness of baffle = 3 mm, L = 7.5 mm, D = 5 mm) Mechanism of oscillatory flow mixing (OFM) in an OFR: (A) Start of up stroke. (B) Maximum velocity in up stroke, i.e. flow reversal. (C) Start of down stroke. (D) Maximum velocity in down stroke Parameters of net flow in a plain tube Oscillatory motion superimposed onto a net flow Parameters of net flow in a plain tube in the presence of baffles Representation of mixing zones in a baffled tube The CSTR and its RTD The PFR, its RTD and the velocity profile within the tube Typical concentration-time curves at the inlet and outlet of reactor Tank-in-series: (a) real system (b) model system Tank-in-series response to a pulse tracer input for different numbers of tanks in a (a) two-dimensional plot and (b) threedimensional plot 45 x

11 3.1 Flowchart of the research methodology A three way valve that connect column with tube for three inlets: 1) tracer; 2) superficial flow; and 3) oscillation The central baffle design with stainless steel rods of 2 mm diameter and 340 mm length as supported rods Central baffles tube dimension for MOBR Conductivity probe (4 mm in diameter and 103 mm in length) connected to a conductivity meter Syringe pump system for a) P1 inject tracer; b) P2 provide superficial flow and c) P3 fluid oscillation Sapphire Engineering Software with command pump to control parameters (net flow, oscillation frequency and amplitude) Experimental set-up for RTD analysis ml conical flask containing inoculate fermentation broth A 2-L STR setup A MOBR setup for fermentation Samples analyzed using DNS method The experimental setup for MOBR RTD profiles at oscillation condition: Ren = 12.6; 2 mm; 5 Hz (dotted line: without oscillatory motion and solid line: with oscillatory motion) RTD curves at Ren = 4.2, 8.4 and 12.6 without oscillatory flow Effect on frequency on RTD profiles Effect on amplitude on RTD profiles at frequency 5 Hz Graphs of variance versus oscillatory Reynolds number at Ren = 12.6; amplitude, xo at 1 mm 4 mm Graph of variances versus Reo at different oscillatory flow (Ren = 4.2, 8.4 and 12.6) Graph of skewness versus oscillatory Reynolds number at Ren = 12.6 (Str = 0.1, 0.13, 0.2 and 0.4) 84 xi

12 4.9 Effect of net Reynolds number (Ren = 4.2, 8.4 and 12.6) on the mixing at an amplitude of 2 mm (Str = 0.2) Graph of dependence of number of tanks versus Reo at different net Reynolds number at amplitude xo = 2mm (Str = 0.2) RTD profiles obtained from the experiment (dash line) and model for number of tanks-in-series (solid line) at Ren = 4.2, f = 6 Hz, xo = 2 mm, N = 4 tanks RTD Graph of glucose consumption in bioethanol fermentation Graph of biomass concentration in bioethanol fermentation 89 xii

13 LIST OF TABLES Table Title Page 2.1 Applications of oscillating devices since 2000 s Publications on the OBR Overview design parameters of mesoscale oscillatory baffled reactor Overview design parameters of mesoscale oscillatory baffled reactor Overview design parameters of mesoscale oscillatory baffled reactor Overview design parameters of mesoscale oscillatory baffled reactor Models for predicting conversion from RTD data Summary of the main features of reactor classes Advantages provided by OBRs over conventional CSTRs and tubular reactor Parameters that use yeast in the bioethanol production Design specification of MOBR and its dimensions Experimental value of amplitude, xo and frequency, f for dynamic parameters calculation Calculated value of frequency and agitation speed for MOBR and STR respectively at same power density of 57.38, and Wm The analytical conditions of HPLC system Variance of the RTD curves obtained at Ren = 12.6 and 5 Hz with a series of oscillation conditions Effect of frequency on characteristics of RTD: variance (flow rate, Q = 1.0 ml/min and amplitude xo = 2 mm) Effect of amplitude on characteristics of RTD: variance (flow rate, Q = 3.0 ml/min and frequency f = 5 Hz) Variance at different oscillatory Reynolds number and net flow Reynold number. 84 xiii

14 4.5 Skewness at oscillatory Reynolds number, Reo = 497, amplitude, xo = 2 and frequency, f = The effect of Strouhal number (Str) at net flow Reynolds number, Ren Summary result of bioethanol production 90 xiv

15 LIST OF ABBREVIATIONS ALR BCR BR CDW COBR CSTR DNS FAME FBR FR HPLC KCl MOBR NaOH NB OBB OBBC OBF OBR OD OFM OFR PBR air-lift loop reactor bubble column reactor batch reactor cell dry weight continuous oscillatory baffled reactor continuous stirred tank reactor dinitrosalicyclic acid fatty acid methyl ester fed bed reactor fluidized reactor high performance liquid chromatography potassium chlorite mesoscale oscillatory baffled reactor sodium hydroxide nutrient broth oscillatory baffled bioreactor oscillatory baffled batch crystallizer oscillatory baffled fermenter oscillatory baffled reactor optical density oscillatory flow mixing oscillatory flow reactor packed bed reactor xv

16 PFR POF rpm rps RTD SPC STR TBR plug flow reactor pure oscillatory flow revolutions per minute revolutions per second residense time distribution smooth periodic constrictions stirred tank reactor tubular baffled reactor xvi

17 LIST OF SYMBOLS Ci Co d do E(t) E(θ) Tracer concentration Orifice coefficient Tube diameter, m Orifice diameter, m The age exit RTD function Distribution normalized RTD function f Oscillation frequency, s -1 Kla l L N No Po Oxygen mass transfer coefficient Mixing length, m Baffle spacing, m Number of tanks Tracer Power number Q Volumetric flow rate, ml.min -1 Rep Reₒ Ren γ S Str T Δt Pulsating Reynolds number Oscillatory Reynolds number Net flow Reynolds number Skewness Open cross-sectional fractional open area of baffle Strouhal number Time Increment of time u Superficial velocity of the liquid, m.s -1 xvii

18 up V Pulsating velocity Reactor volume X Cell mass concentration, g.l -1 xₒ Oscillation amplitude (centre-to-peak), m Z Column length, m Greeks Letters ɛv Power density, W.m -3 μ Viscocity, m 2.s Pa.s ρ Liquid density, kg.m -3 Θ ψ τ σ θ Dimensionless form Velocity ratio, Reₒ/Ren Mean residense time Variance Dimensionless time ν kinematic viscocity of water, m 2.s -1 ω Angular frequency (2πf), rad.s -1 xviii

DESIGN, ANALYSIS, AND FABRICATE OF LOW SPEED WATER TUNNEL AHMAD ZULFADHLI BIN MOHD KHALID UNIVERSITI MALAYSIA PAHANG

DESIGN, ANALYSIS, AND FABRICATE OF LOW SPEED WATER TUNNEL AHMAD ZULFADHLI BIN MOHD KHALID UNIVERSITI MALAYSIA PAHANG DESIGN, ANALYSIS, AND FABRICATE OF LOW SPEED WATER TUNNEL AHMAD ZULFADHLI BIN MOHD KHALID