Michigan Technological University Digital Commons @ Michigan Tech Dissertations, Master's Theses and Master's Dissertations, Master's Theses and Master's Reports - Open Reports 2012 THE POTENTIAL OF INDUSTRIAL WASTE AND AGRICULTURAL FEEDSTOCK TOWARDS SUSTAINABLE BIOFUELS PRODUCTION: TECHNO-ECONOMIC AND ENVIRONMENTAL IMPACT PERSPECTIVES Felix K. Adom Michigan Technological University Follow this and additional works at: https://digitalcommons.mtu.edu/etds Part of the Chemical Engineering Commons, and the Sustainability Commons Copyright 2012 Felix K. Adom Recommended Citation Adom, Felix K., "THE POTENTIAL OF INDUSTRIAL WASTE AND AGRICULTURAL FEEDSTOCK TOWARDS SUSTAINABLE BIOFUELS PRODUCTION: TECHNO-ECONOMIC AND ENVIRONMENTAL IMPACT PERSPECTIVES", Dissertation, Michigan Technological University, 2012. https://doi.org/10.37099/mtu.dc.etds/619 Follow this and additional works at: https://digitalcommons.mtu.edu/etds Part of the Chemical Engineering Commons, and the Sustainability Commons THE POTENTIAL OF INDUSTRIAL WASTE AND AGRICULTURAL FEEDSTOCK TOWARDS SUSTAINABLE BIOFUELS PRODUCTION: TECHNO-ECONOMIC AND ENVIRONMENTAL IMPACT PERSPECTIVES By Felix K. Adom A DISSERTATION Submitted in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY In Chemical Engineering MICHIGAN TECHNOLOGICAL UNIVERSITY 2012 ©2012 Felix K. Adom This dissertation has been approved in partial fulfillment of the requirements for the Degree of DOCTOR OF PHILOSOPHY in Chemical Engineering Department of Chemical Engineering Dissertation Advisor: Robbins Professor. David R Shonnard Committee Member: Professor. Susan T Bagley Committee Member: Dr. Tony N Rogers Committee Member: Dr. Wenzhen Li Department Chair: Professor Komar Kawatra. Table of contents List of figures………………………………………………………………………….x List of tables…………………………………………………………………………...xv Preface………………………………………………………………………………..xxi Acknowledgements…………………………………………………………………xxiii List of abbreviations………………………………………………………………..xxiv Abstract……………………………………………………………………………..xxv Chapter 1……………………………………………………………………………….1 1 Introduction .......................................................................................................... 1 1.1Motivation ........................................................................................................... 1 1.2PhD research objectives ...................................................................................... 4 1.3Dissertation outline ............................................................................................. 5 1.4References ........................................................................................................... 6 Chapter 2……………………………………………………………………………….8 2 Compositional Analysis of Defatted Syrup from a Corn Ethanol Dry Mill as a Feedstock for Bio-Based Products ............................................................................... 8 2.1Introduction ......................................................................................................... 8 2.2Materials and methods ...................................................................................... 10 2.2.1 Total solids analysis ............................................................................. 11 2.2.2 Ash content analysis............................................................................. 11 2.2.3 Inorganic element profile ..................................................................... 11 2.2.4 Protein content analysis ....................................................................... 11 2.2.5 Amino acid analysis of syrup ............................................................... 12 2.2.6 Total carbohydrate analysis ................................................................. 12 iii 2.2.7 Lignin analyses .................................................................................... 14 2.2.8 Glycerol analysis .................................................................................. 15 2.2.9 Total organic acid analysis ................................................................... 15 2.2.10 Functional group analysis using FTIR-ATR .................................... 16 2.3Results and discussion ....................................................................................... 16 2.3.1 Total solids and ash content ................................................................. 16 2.3.2 Inorganic element profile ..................................................................... 18 2.3.3 Protein content analysis ....................................................................... 19 2.3.4 Glycerol analysis .................................................................................. 19 2.3.5 Total carbohydrate content analysis of DCS........................................ 20 2.3.6 Acid soluble and acid insoluble lignin analysis ................................... 21 2.3.7 Amino acid analysis ............................................................................. 22 2.3.8 FTIR-ATR analysis .............................................................................. 24 2.3.9 Mass balance closure of DCS .............................................................. 26 2.4Potential yields from biorefining using syrup as a feedstock ............................ 27 2.5Conclusions ....................................................................................................... 29 2.6References ......................................................................................................... 30 Chapter 3………………………………………………………………………………35 3 Optimization of the Dilute Acid and Enzymatic Pretreatment of Defatted Syrup from a Corn Ethanol Dry Mill .................................................................................... 35 3.1Introduction ....................................................................................................... 35 3.2Materials and methods ...................................................................................... 37 3.2.1 Hydrolysis scheme and experimental matrix ....................................... 37 3.2.2 Materials............................................................................................... 38 3.2.3 Equipment ............................................................................................ 38 iv 3.2.4 Characterization of soluble sugars and inhibitors ................................ 39 3.2.5 Dilute acid pretreatment (DAP) procedure (First pretreatment stage) . 39 3.2.6 Oligomer analysis (Second pretreatment stage) ................................... 40 3.2.7 Enzymatic hydrolysis (EH) .................................................................. 40 3.3Results ............................................................................................................... 41 3.3.1 Results for soluble carbohydrates and inhibitors in DCS .................... 41 3.3.2 Results for experiment set 1 ................................................................. 41 3.3.3 Results for experiment set 2 ................................................................. 44 3.3.4 Results for experiment set 3 ................................................................. 46 3.3.5 Results for experiment set 4 ................................................................. 49 3.3.6 Results for experiment set 5 ................................................................. 51 3.3.7 Results for experiment set 7 ................................................................. 53 3.4Discussion ......................................................................................................... 56 3.5Conclusions ....................................................................................................... 58 3.6References ......................................................................................................... 59 Chapter 4………………………………………………………………………………61 4 Optimization of the Protein Hydrolysis Scheme of Defatted Syrup from a Corn Ethanol Dry Mill Facility ........................................................................................... 61 4.1Introduction ....................................................................................................... 61 4.2Materials and methods ...................................................................................... 64 4.2.1 Protein hydrolysis scheme and experimental matrix ........................... 64 4.2.2 Amino acid analysis of crude DCS ...................................................... 65 4.2.3 Hydrolysis pathway 1: Experiment description of amino acid hydrolysis using DAP ........................................................................................ 66 v 4.2.4 Hydrolysis pathway 2: Experiment description of DAP followed by protein hydrolysis using proteases ..................................................................... 66 4.2.5 Hydrolysis pathway 3: Experiment description of amino acid hydrolysis on unpretreated DCS using proteases, cellulases, α-amylase and amyloglucosidase ............................................................................................... 68 4.2.6 Hydrolysis pathway 4: Experiment description of amino acid hydrolysis using protease & cellulases (Simultaneous Hydrolysis) .................. 70 4.2.7 HPLC analysis of amino acids ............................................................. 71 4.3Results and discussion ......................................................................................