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Purification of Aqueous, Protic Ionic Liquid by Distillation

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Purification of Aqueous, Protic Ionic Liquid by Distillation Phuong Nguyen Thi Thanh PURIFICATION OF AQUEOUS, PROTIC IONIC LIQUID BY DISTILLATION Master´s Programme in Chemical, Biochemical and Materials Engineering Major in Chemical Engineering Master’s thesis for the degree of Master of Science in Technology submitted for inspection, Espoo, 31st July 2020 Supervisor Professor Pekka Oinas Instructor D.Sc Petri Uusi-Kyyny Author Phuong NguyenThi Thanh Title of thesis Purification of aqueous, protic ionic liquid by distillation Degree Programme Chemical, Biochemical and Materials Engineering Major Chemical Engineering Thesis supervisor Professor Pekka Oinas Thesis advisor(s) / Thesis examiner(s) D.Sc Petri Uusi-Kyyny Date 31.07.2020 Number of pages 82 + Language English Appendices Abstract Protic ionic liquid (PIL) is an equimolar mixture of a superbase and a carboxylic acid. Acetate-based PILs have been developed to dissolve cellulose for fiber production. However, the high price of PILs currently is one of the barriers to the industrial application of PILs on a large scale. The recovery and recycling processes are essential to increasing the application of PILs. Purification is the last step of the recovery process of the fiber manufacturing process. Short path distillation is a potential purification method for thermo-sensitive materials like PILs. In this study, short path distillation experiments were conducted to study whether it is possible to distill pure PIL. The operating pressure and the evaporator jacket temperature were varied to test the separation efficiency of PIL. The recovery yield of the base was 97 wt.% at 1.3 mbar and 160°C. The maximum base yield in the distillate was 94 wt.%. The minimum base yield in the residue was 1 wt.%. By-product was lower in the distillate than in the residue. The discoloration of PIL in the distillate product indicated the removal of chromophores as impurities from the initial material. The residual water was found in the cold trap. The base was possible to trap partly in the cold trap. There is still insufficient data on the thermodynamic properties of PILs. Batch distillation experiments were implemented to study the evaporation behavior of pure acetate- based PIL. The purity of the base was 99 wt.% in the first fraction with mass fraction less than 20 wt.% of the initial material. By-product was found only in the residue. Keywords Protic ionic liquid, purification, distillation, short path distillation, vacuum, vapor pressure, hydrolysis product ACKNOWLEDGEMENTS This master’s degree thesis has been accomplished in recognition of lifelong learning and my dedication to chemical engineering research. Firstly, I express my deepest gratitude to my Prof. Pekka Oinas who has trusted my competence and given me a chance to work on an interesting research project. I am deeply grateful Prof. Herbert Sixta who has encouraged me during the research process and funded my thesis. Also, I sincerely thank Prof. Ville Alopaeus who has instructed me to work with simulation models. Secondly, I would like to express my appreciation and thanks to Dr. Petri Uusi-Kyyny who has assisted me for the last six months with thorough instructions on laboratory tests, consultation for solving problems, checking of test results as well as previewing this thesis. This thesis would also not be accomplished without supporting from group of experts. I truly appreciate technical support from Timo Ylönen, Terho Konttinen, Hans Orassaari, Tuyen Nguyen, Timo Kotilahti; those who have promptly and professionally repaired problems of the short path distillation device. In addition, I sincerely thank to Juha-Pekka Pokki for his instructions to work on batch distillation column. I truly appreciate for instructions and invaluable experience from: Inge Schlapp-Hackl; Jari Koivisto; Joanna Witos; Krishna Ojha; and Sherif Elsayed, to work on analytical instruments. I sincerely thank other colleagues from groups of Human Resources, Plant design, Biorefinery, Chemical engineering of Aalto University; those who have helped me with administration procedure or spent time after work. I am in sincere gratitude for valuable discussions with my mentor – Jyrki Kettunen, helpful proof-reading from Hendrik Hielkema, Victoria von Vagabonde, Taimi Pimentola-Heikkinen, John Powell and John Weston, as well as best encouragements from my beloved friends in Vietnam, Finland, and Portugal. Finally, I greatly appreciate my husband - Thao Pham and my son - Dang Pham, who are inseparable parts of my life, have given me strength to fulfill the research work and keep balanced between work and life. I am thankful that my mother, sister and relatives in Vietnam who are in good self-care so that I am able to concentrate on the thesis. TABLES OF CONTENTS 1. INTRODUCTION ....................................................................................................................... 9 1.1. Background ...................................................................................................................... 9 1.2. Objectives of the study ................................................................................................... 11 1.3. Structure of the thesis .................................................................................................... 12 LITERATURE REVIEW ...................................................................................................................... 13 2. PROTIC IONIC LIQUIDS OVERVIEW AND APPLICATIONS......................................................... 13 2.1. Ionic liquid classification ................................................................................................. 13 2.2. Ionic liquids in biomass processing ................................................................................. 17 2.3. Ionic liquid synthesis ...................................................................................................... 17 2.4. Ionic liquid properties..................................................................................................... 18 2.5. Ionic liquid applications .................................................................................................. 21 3. SEPARATION AND PURIFICATION PROCESS REVIEW .............................................................. 23 3.1. Common impurities from ILs........................................................................................... 23 3.2. Separation and purification methods overview ............................................................... 24 3.3. Batch distillation............................................................................................................. 25 3.4. Short-path distillation ..................................................................................................... 27 4. THERMODYNAMIC MODELS AND OPERATION UNITS REVIEW .............................................. 30 APPLIED PART................................................................................................................................. 33 5. METHODOLOGY .................................................................................................................... 33 5.1. Materials and chemicals ................................................................................................. 33 5.2. Batch distillation experiments ........................................................................................ 33 5.3. Short path distillation experiments ................................................................................. 35 5.4. Analytical methods ......................................................................................................... 39 6. RESULTS AND DISCUSSIONS FOR BATCH DISTILLATION EXPERIMENTS FOR PIL SOLVENT ...... 41 6.1. Distillation results ........................................................................................................... 41 6.2. Distillation results in comparison with Aspen model ....................................................... 52 6.3. Discussions and conclusions ........................................................................................... 55 7. RESULTS AND DISCUSSIONS FOR SHORT PATH DISTILLATION EXPERIMENTS FOR S2 ............. 58 7.1. Distillation results ........................................................................................................... 58 7.2. Distillation results in comparison to the simulation results .............................................. 68 7.3. Discussions and conclusions ........................................................................................... 71 8. RESULTS AND DISCUSSIONS FOR SHORT PATH DISTILLATION EXPERIMENTS FOR S1 ............. 73 8.1. Distillation results ................................................................................................................ 73 8.2. Discussions and conclusions ........................................................................................... 79 9. CONCLUSIONS ....................................................................................................................... 80 BIBLIOGRAPHY ............................................................................................................................... 83 APPENDICES ................................................................................................................................... 89 Appendix 1. The list of ionic liquid applications ................................................................................ 89 Appendix
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