RESEARCH REPORT PRODUCTION OF BIODIESEL FROM CHICKEN FAT WITH COMBINATION SUBCRITICAL METHANOL AND WATER PROCESS

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RESEARCH REPORT PRODUCTION OF BIODIESEL FROM CHICKEN FAT WITH COMBINATION SUBCRITICAL METHANOL AND WATER PROCESS Submitted by: Felix Harijaya Santosa NRP. 5203014015 Ryan Sumule NRP. 5203014037 DEPARTMENT OF CHEMICAL ENGINEERING FACULTY OF ENGINEERING WIDYA MANDALA CATHOLIC UNIVERSITY SURABAYA 2017

PREFACE The authors would like to thank God for His blessing so our research project has been accomplished. This report is one of the prerequisites in achieving Bachelor of Engineering degree in Chemical Engineering. The authors realize that the completion of this report is achieved by the support of many people. Therefore, the authors would like to thank to: 1 Ir. Suryadi Ismadji, Ph.D., as Principal Supervisor and Felycia Edi S., Ph.D. as Co Supervisor 2 Wenny Irawaty, Ph.D. as Head of the Committees, Dra. A. Anteng Anggorowati, M. Si., and Ir. Yohanes Sudaryanto, MT., as members of committees 3 Ir. Suryadi Ismadji, Ph.D and Dra. Adriana Anteng Anggorowati, M.Si. as the Head of Process and Chemical Analysis Laboratory, respectively. 4 Mr. Novi and Mr. Pudjo as the technicians in Process and Unit Operation Laboratories, respectively. 5 Our parents and family who have given a lot of help and support, both materially and morally. 6 Our lecturers, friends and also those who are too many to be listed by name that had contributed their kind assistance The authors realize that this report is far from perfect, therefore any critics and comments which will better improve the research is gladly accepted. Lastly, the authors hope that the report will be useful to all readers who need information regarding the research of the report. Surabaya, 2 nd June, 2017 Authors viii

ABSTRACT The world demand for energy to fuel (fossil fuel) increases as consumption levels increase. However, the availability of fossil fuels in nature cannot meet demand for fuel in the future. In addition, fossil fuels produce emissions that are harmful to the environment such as greenhouse gases that cause global warming. Currently, the production of biodiesel using vegetable oils that will lead to competition utilization of vegetable oils for food and industrial sectors. Biodiesel can be produced through a transesterification reaction by reacting fats and alcohol, where the transesterification reaction can be performed in critical conditions (subcritical and critical condition) and atmospheric. Subcritical method considered more environmentally friendly because during the process does not use catalysts and more efficient time (compared to the conventional method) and energy (compared supercritical method). The aim of this study is to investigate the effect of molar ratio of chicken fat and methanol and process temperature on biodiesel and to obtain the optimum temperature and molar ratio to produce the highest yield of biodiesel. In this study, the production of biodiesel using subcritical and chicken fat as raw materials that become waste in the food industry (nuggets, sausages, etc.) has been investigated. The production process has been varied in processing temperature (100, 125, and 150 o C) and the molar ratio of fats with methanol (1:14 1:70). Temperature and molar ratio is the main factor in biodiesel production through subcritical process, where the result of factorial method shows both variables give value of P-Value below 0.05 also the interaction between both variables. The optimum condition that obtained from Response Surface to produce biodiesel from chicken fat is 160.4 o C with molar ratio 1:81.6 Based on gas chromatography analysis, the purity of biodiesel obtained 80.17% and composed of Tridecanoic Acid Methyl Ester (C13:0), Myristoleic Acid Methyl Ester (C14:1), cis-10-pentadecenoic Acid Methyl Ester (C15:1), Linoleic Acid Methyl Ester (C18:2n6c), Linolelaidic Acid Methyl Ester (C18:2n6t), cis-11-eicosenoic Acid Methyl Ester (C20:1n9), Erucic Acid Methyl Ester (C22:1n9), Lignoceric Acid Methyl Ester (C24:0), cis-4,7,10,13,16,19-docosahexaenoic Acid Methyl Ester (C22:6n3), and Nervonic Acid Methyl Ester (C24:1n9). ix

CONTENTS LETTER OF APPROVAL... ii COPY RIGHT AGREEMENT... iv LETTER OF DECLARATION... vi PREFACE... viii ABSTRACT... ix CONTENTS... x LIST OF FIGURES... xii LIST OF TABLES... xiii INTRODUCTION... 1 I.1 Background... 1 I.2 Objectives... 3 I.3 Problem limitation... 4 LITERATURE REVIEW... 5 II.1 Biodiesel... 5 II.2 Esterification... 7 II.3 Transesterification... 8 II.4 Subcritical Process... 15 II.5 Free Fatty Acid... 16 II.6 Chicken Fat... 17 II.7 Response Surface Methodology (RSM)... 17 EXPERIMENTAL METHOD... 19 III.1 Research Design... 19 III.2 Material... 21 III.3 Equipment... 21 III.4 Research Variables... 22 III.4.1 Fixed Variables... 22 III.4.2 Manipulated Variables... 22 x

III.5 Chicken Fat Analysis (Proximate analysis)... 22 III.6 Production of Biodiesel from Chicken Tallows with SCW-Methanol Process... 22 III.7 Subcritical Reactor Scheme... 24 RESULT AND DISCCUSION... 25 IV.1 Characteristic of Chicken Fat... 25 IV.2 Effect of temperature on Crude Biodiesel Yield... 26 IV.3 Effect of Molar Ratio on Crude Biodiesel Yield... 27 IV.4 Optimization of Biodiesel Production with Combination... 28 Subcritical Methanol and Water Process... 28 IV.5 Gas Chromatography Analysis... 32 CONCLUSION AND RECOMMENDATION... 35 V.1 Conclusions... 35 V.2 Recommendations... 36 REFERENCE... 37 APPENDIX A... 42 APPENDIX B... 44 APPENDIX C:... 48 APPENDIX D... 52 APPENDIX E... 53 xi

LIST OF FIGURES Figure II. 1 Transesterification reaction... 8 Figure II. 2 Overall trans-esterification reaction of biodiesel production... 8 Figure II. 3 Transesterification reaction mechanism... 9 Figure II. 4 Phase diagram of water.... 15 Figure II. 5 Response surface contour plot... 18 Figure III. 1 Biodiesel Production Scheme... 20 Figure III. 2 Subcritical Reactor System... 24 Figure IV. 1 Biodiesel Yield as Function of Ratio... 26 Figure IV. 2 ANOVA of First Order Factorial Method... 28 Figure IV. 3 ANOVA of Second Order Factorial Method... 28 Figure IV. 4 Contour Plot of Response Surface... 31 Figure IV. 5 Response Surface Plot for Interaction Crude Biodiesel Yield vs Molar Ratio and Temperature... 32 Figure IV. 6 Optimization Plot of Biodiesel Production... 32 Figure IV. 7 Chromatogram of Biodiesel from Chicken Fat... 33 Figure E. 1 Chromatogram of Biodiesel Standard 47885U... 53 Figure E. 2 Chromatogram of Biodiesel from Chicken Fat... 55 xii

LIST OF TABLES Table II. 1 Standard of ASTM for diesel fuel... 6 Table II. 2 Biodiesel standard SNI 7182:2015 and ASTM D6751... 7 Table II. 3 Summary of biodiesel production via transesterification... 13 Table II. 4 Critical Point of Solvent... 16 Table IV. 1 DOE Second Order for Response Surface Methodology... 29 Table IV. 2 Estimation Coefficient Value of Second Order Regression... 30 Table IV. 3 Peak Analysis for Chromatogram of Biodiesel from Chicken Fat... 34 Table B. 1 Standardize of Sodium Hydroxide with Oxalic Acid... 45 Table B. 2 Characteristic of Chicken Fat... 46 Table B. 3 Molecular Weight Calculation of Triglycerides using eq. (B.3)... 47 Table E. 1 FAME Component in Biodiesel from Chicken Fat at Optimum Condition... 56 xiii