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Tesis Doctoral: Aprovechamiento De Residuos Lignocelulósicos Para La ESCUELA TÉCNICA SUPERIOR DE INGENIERÍAS AGRÁRIAS DEPARTAMENTO DE INGENIERÍA AGRÍCOLA Y FORESTAL TESIS DOCTORAL: APROVECHAMIENTO DE RESIDUOS LIGNOCELULÓSICOS PARA LA PRODUCCIÓN DE BIOCOMBUSTIBLES Y BIOPRODUCTOS Presentada por Viviane da Silva Lacerda para optar al grado de Doctora por la Universidad de Valladolid Dirigida por: Jesús Martín-Gil Adriana Correa Guimarães Santo Evangelio según san Mateo (25, 31-46) i AGRADECIMIENTOS Le agradezco a Dios por haberme acompañado y guiado a los largo de todo este proceso, por ser mi fortaleza en los momentos de debilidad y por mostrarme día a día que con humildad, paciencia y sabiduría todo es posible. Quiero expresar mi mas sincero agradecimiento a mis directores de tesis, Dr. Jesus Martín Gil y la Dra. Adriana Correa Guimarães, por su apoyo en todas las etapas de la elaboración de esta Tesis. Tambien quiero agradecer el apoyo financiero recibido por parte de proyecto VA036A12-2, de la Junta de Castilla y León, y al programa de Formación del Personal Investigador (FPI-Uva) ii INDICE DE CONTENIDOS INDICE DE CONTENIDOS......................................................................................... II ÍNDICE DE TABLAS ................................................................................................ VII ÌNDICE DE FIGURAS ................................................................................................ IX ÍNDICE DE SIGLAS Y ABREVIATURAS ............................................................. XII RESUMEN ................................................................................................................. XVI ABSTRACT ................................................................................................................ XIX 1. INTRODUCCIÓN TEORICA…………… ....... ……………………………………1 1.1. La biomasa lignocelulósica como materia prima para biorrefinería ............................................. 2 1.1.1. Introducción .................................................................................................................................. 2 1.1.2. Composición de los materiales lignocelulósicos ........................................................................... 2 1.1.3. Procesos de aprovechamiento de la biomasa residual: Biorrefinerías ........................................... 8 1.2. Material precursor ............................................................................................................................ 11 1.2.1. Carnauba (Copernicia prunifera (Miller) H.E.Moore) ................................................................ 11 1.2.2. Macaúba (Acrocomia aculeata (Jacq.) Lodd. ex Mart.) .............................................................. 14 1.2.3. Piñón (Pinus pinea L.) ................................................................................................................. 17 1.3. Procesos de producción de biocombustibles ................................................................................... 19 1.3.1. Introducción ................................................................................................................................ 19 1.3.2. Pretratamiento de la biomasa lignocelulósica.............................................................................. 20 1.3.3. Líquidos iónicos .......................................................................................................................... 29 1.3.4. Técnicas de Hidrólisis ................................................................................................................. 31 1.4. Biomaterial: carbón activado........................................................................................................... 33 1.4.1. Antecedentes Históricos .............................................................................................................. 33 1.4.2. Tipos de carbón activado ............................................................................................................. 34 1.4.3. Características Físicas: Importancia de los poros ........................................................................ 37 1.4.4. Características Químicas: Estructura química del carbón activado ............................................. 38 1.4.5. Procesos de Activación ............................................................................................................... 40 1.4.6. Adsorción. .................................................................................................................................. 46 1.4.7. Usos y aplicaciones del Carbón Activado ................................................................................... 48 1.5. Referencias ....................................................................................................................................... 50 2. MARCO Y OBJETIVOS DE LA TESIS…………………………....................... 64 2.1. Marco de referencia del proyecto de tesis ....................................................................................... 65 2.1.1. Elección del material lignocelulósico .......................................................................................... 67 2.1.2. Elección de los métodos síntesis para la producción de furanos y azúcares reductores totales ... 69 2.1.3.Producción de carbón activado a partir de residuos lignocelulósicos. .......................................... 75 2.1.4. Estudio integrado de adsorción de colorantes y hidrólisis enzimática ........................................ 79 2.2. Objetivos ....................................................................................................................................... 82 2.3.Referencias ....................................................................................................................................... 86 iii 3. A KINETIC STUDY ON MICROWAVE-ASSISTED CONVERSION OF CELLULOSE AND LIGNOCELLULOSIC WASTE INTO HMF/FURFURAL .. 91 3.1. Abstract ....................................................................................................................................... 92 3.2. Introduction ...................................................................................................................................... 93 3.3.Materials and methods ...................................................................................................................... 94 3.3.1. Materials .................................................................................................................................. 94 3.3.2. Optimization of the hydrolysis process for HMF and furfural production .................................. 95 3.3.3. Analytical methods ...................................................................................................................... 96 3.4. Results and discussion ...................................................................................................................... 97 3.4.1. Effect of the ionic liquid, catalyst and organic diluent on the conversion of native cellulose into HMF and furfural .................................................................................................................................. 97 3.4.2. Effect of water dosage on HMF and furfural production, from native cellulose and lignocellulosic waste ............................................................................................................................. 99 3.4.3. Effect of time and temperature on furan compounds production from native cellulose and lignocellulosic materials ...................................................................................................................... 101 3.4.4. Kinetic study of the effect of time and temperature on the separate production of furfural and HMF from native cellulose and lignocellulosic materials ................................................................... 103 3.4.5. Changes in the functional parameters of the process: ultrasonic treatment and stirring. ........... 108 3.5.Conclusion ..................................................................................................................................... 109 3.6.Acknowledgements .......................................................................................................................... 110 3.7.References ..................................................................................................................................... 110 4. EFFICIENT MICROWAVE-ASSISTED ACID HYDROLYSIS OF LIGNOCELLULOSIC MATERIALS INTO TOTAL REDUCING SUGARS IN IONIC LIQUIDS…………………………………………………… .... …………….114 4.1.Abstract ..................................................................................................................................... 115 4.2.Introduction ..................................................................................................................................... 116 4.3.Material and methods ...................................................................................................................... 117 4.3.1. Raw materials and reagents ....................................................................................................... 117 4.3.2. Characterization of the raw lignocellulosic waste ..................................................................... 118 4.3.3. Microwave-assisted acid-catalyzed hydrolysis procedure ......................................................... 118 4.3.4. Analysis ...............................................................................................................................
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