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Dy & Development of an Integrated & Additive-Free Waste Orange Peel Biorefinery

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Dy & Development of an Integrated & Additive-Free Waste Orange Peel Biorefinery The study & development of an integrated & additive-free waste orange peel biorefinery. Lucie Anne Pfaltzgraff Doctor of Philosophy University of York Chemistry September 2014 2 Abstract The overall aim of this thesis is to demonstrate how food supply chain waste (FSCW) could be used as a renewable feedstock for a product-focused biorefinery. The volumes of FSCW produced as a result of common food processing operations have been estimated using a new methodology. The latter is based on sold manufactured goods published every year by the European Union (PRODCOM) and highlights the geographical waste hot spots for common food processing operations. The use of this methodology led to the selection of waste orange peel (WOP) as a raw material for the design of an integrated biorefinery. A SWOT analysis was carried out to analyse the opportunity for the design of a WOP valorisation process aimed at the extraction of a maximum of the chemical components, while avoiding the use of acid, additives or pretreatment. The successful development of a microwave biorefinery process centred on the valorisation of WOP was designed based on the integration of microwave assisted D-limonene extraction and a low temperature hydrothermal extraction of pectin. The work carried-out using microwave hydrothermal treatment proved that pectin can be extracted between 100 and 150 °C under acid-less conditions on a 100 mL scale. A competitive molecular weight distribution was obtained for pectin produced at a temperature of 110 and 120 °C using WOP from which D-limonene, flavonoids and sugar had been previously extracted. A CPMAS 13C-NMR technique was developed to determine the degree of esterification of pectin. D-limonene was extracted under microwave-assisted solvent-less conditions. The optimised conditions studied led to a yield of 1.09 ± 0.18% food grade D-limonene with a high reproducibility on a 1 L scale (500 mbars). Finally, the process used also allowed for the isolation and characterisation of flavonoids and monosaccharides. Following ethanol extraction, a mixture of polymethoxy flavonoids (tetra-O-methyl scutellarein, tangeritin, nobiletin and heptamethoxyflavone), hesperidin and sugar monosaccharides were obtained with yields of 5.87%, 0.24% and 18.35% respectively on a wet basis. The later fraction was composed of 74.21% glucose and 25.35% fructose, as determined by quantitative 13C NMR, showing the potential for this fraction as a fermentation feedstock. 3 4 List of contents Abstract........................................................................................................................................................... 3 List of contents ............................................................................................................................................ 5 List of tables................................................................................................................................................11 List of figures ..............................................................................................................................................15 Acknowledgements .................................................................................................................................21 Author’s declaration................................................................................................................................23 1 Introduction ......................................................................................................................................28 1.1 Green chemistry and the biorefinery ...........................................................................28 1.1.1 The 12 green chemistry principles......................................................................28 1.1.2 Green chemistry and Industry...............................................................................30 1.1.3 Drivers for change ......................................................................................................32 1.1.4 The bio-based economy ...........................................................................................34 1.1.5 Product-focused biorefinery ..................................................................................34 1.1.6 Technologies used ......................................................................................................36 1.1.7 Waste as a renewable feedstock...........................................................................38 1.2 Fundamentals of microwave technology ...................................................................40 1.2.1 Heat production mechanisms under microwave conditions...................41 1.2.1.1 Single and multimode microwaves ................................................................43 1.2.1.2 Temperature control and super-heating .....................................................43 1.2.1.3 Application of microwave technology at larger scale ............................44 1.2.2 Associated benefits of the use of microwaves on food supply chain waste 45 2 The use of FSCW as a feedstock for the production of chemicals. Availability and location in Europe. ...................................................................................................................................48 2.1 Use of food supply chain waste (FSCW) as a resource .........................................48 2.1.1 Definition of the term food supply chain waste.............................................48 2.1.2 Drivers for the use of FSCW as an alternative carbon feedstock for chemical production......................................................................................................................49 5 2.2 FSCW selection criteria- Food for thoughts.............................................................. 52 2.3 Method for the evaluation of FSCW volumes produced by the food sector in Europe...................................................................................................................................................... 55 2.3.1 Methodology used ...................................................................................................... 56 2.3.2 Main results obtained ............................................................................................... 59 2.4 Conclusion and future work ............................................................................................ 62 3 The Orange Peel Extraction Company. Opportunity for the valorisation of waste orange peel.................................................................................................................................................. 66 3.1 Availability of citrus peel waste around the world ............................................... 66 3.1.1 Amount of citrus waste produced by the top five producers of orange juice 66 3.1.2 Process flow sheet for the production of orange juice ............................... 68 3.2 Orange peel waste composition and value................................................................ 70 3.2.1 D-limonene and orange oil ..................................................................................... 71 3.2.2 Pectin................................................................................................................................ 73 3.2.3 Flavonoids...................................................................................................................... 75 3.2.3.1 Hesperidin................................................................................................................. 76 3.2.3.2 Polymethoxylated flavonoids ........................................................................... 77 3.3 Scope of this thesis............................................................................................................... 78 4 Microwave hydrothermal extraction of pectin from waste orange peel under acid free conditions ................................................................................................................................. 84 4.1 Introduction to pectin ........................................................................................................ 84 4.2 Occurrence of pectin and traditional extraction of pectin ................................. 86 4.3 Precedents in acid-based microwave assisted extraction of pectin .............. 88 4.4 Characterisation of pectin ................................................................................................ 90 4.4.1 ATR-IR characterisation of pectin ....................................................................... 92 4.4.2 Determination of the degree of esterification of pectin by double titration 94 4.4.3 Pectin characterisation and determination of the degree of esterification by solution nuclear magnetic resonance (NMR).................................. 96 4.4.3.1 Characterisation by solution nuclear magnetic resonance ................. 96 6 4.4.3.2 Solid state carbon nuclear magnetic resonance analysis .................. 103 4.5 Hydrothermal microwave extraction of pectin .................................................... 109 4.5.1 Small scale screening experiments .................................................................. 110 4.5.1.1 Gel permeation chromatography analysis of pectin............................ 115 4.5.1.2 Gel formation properties of pectin extracted under acid less conditions..................................................................................................................................
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