The main objective of this study was to investigate two of the possible exploitation routes of anaerobic digestion (acid-phase and methane-phase) for the treatment of sugar-beet processing wastes, while producing valuable biobased products. For this purpose, four sets of laboratory experiments were carried out in a stepwise fashion: First, in the biochemical methane potential (BMP) assay (Set-up 1) wastewater and beet-pulp were efficiently digested (63.7&ndash / 87.3% COD removal and 69.6&ndash / 89.3% VS reduction) in batch anaerobic reactors. Secondly, wastewater and beet-pulp could simultaneously be converted to VFAs in acidogenic anaerobic reactors with considerable acidification degrees (43.8&ndash / 52.9%), optimizing the operational conditions (Set-up 2). Then, the produced VFAs were recovered by liquid-liquid extraction (Set-up 3), in which highest VFA recoveries (60.7&ndash / 97.6%) were observed at 20% trioctylphosphine oxide (TOPO) in kerosene with KD values ranging between 1.54 and 40.79 at pH 2.5. Finally, methane-phase anaerobic digestion was evaluated in two different reactor configurations, namely fed-batch continuously mixed reactor (FCMR) and anaerobic sequencing batch reactor (ASBR) (Set-up 4). Methane production yield of 255 &plusmn / 11 mL/g COD-added was increased to 337 &plusmn / 15 mL/g COD-added (32.2% increase in methane yield) when configuration was changed from FCMR to ASBR. In addition, tCOD removal was increased from 68.7 &plusmn / 2.2 to 79.7 &plusmn / 1.1%. Based on the result obtained in this study, it is postulated that, biorefining of sugar-beet processing wastes by anaerobic digestion can not only be a solution for environmental related problems, but also contribute to resource conservation and sustainable production via valuable bio-based product formation.

abstract: The aims of this project are to demonstrate the design and implementation of separations modalities for 1) in situ product recovery and 2) upstream pretreatment of toxic feedstocks. Many value-added bioproducts such as alcohols (ethanol and butanol) developed for the transportation sector are known to be integral to a sustainable future. Likewise, bioproduced aromatic building blocks for sustainable manufacturing such as phenol will be equally important. The production of these compounds is often limited by product toxicity at 2- 20 g/L, whereas it may desirable to produce 20-200 g/L for economically feasible scale up. While low-cost feedstocks are desirable for economical production, they contain highly cytotoxic value-added byproducts such as furfural. It is therefore desirable to design facile detoxification methods for lignocellulose-derived feedstocks to isolate and recover furfural preceding ethanol fermentation by Escherichia coli. Correspondingly it is desirable to design efficient facile in situ recovery modalities for bioalcohols and phenolic bioproducts. Accordingly, in-situ removal modalities were designed for simultaneous acetone, butanol, and ethanol recovery. Additionally, a furfural removal modality from lignocellulosic hydrolysates was designed for upstream pretreatment. Solid-liquid adsorption was found to serve well each of the recovery modalities characterized here. More hydrophobic compounds such as butanol and furfural are readily recovered from aqueous solutions via adsorption. The primary operational drawback to adsorption is adsorbent recovery and subsequent desorption of the product. Novel magnetically separable mesoporous carbon powders (MMCPs) were characterized and found to be rapidly separable from solutions at 91% recovery by mass. Thermal desorption of value added products was found efficient for recovery of butanol and furfural. Fufural was desorbed from the MMCPs up to 57% by mass with repeated adsorption/thermal desorption cycles. Butanol was recovered from MMCPs up to an average 93% by mass via thermal desorption. As another valuable renewable fermentation product, phenol was also collected via in-situ adsorption onto Dowex Optipore L-493 resin. Phenol recovery from the resins was efficiently accomplished with tert-butyl methyl ether up to 77% after 3 washes. / Dissertation/Thesis / Doctoral Dissertation Chemical Engineering 2017

The electromagnetic shielding effectiveness of kenaf bast fiber based composites with different iron oxide impregnation levels was investigated. The kenaf fibers were retted to remove the lignin and extractives from the pores in fibers, and then magnetized. Using the unsaturated polyester and the magnetized fibers, kenaf fiber based composites were manufactured by compression molding process. The transmission energies of the composites were characterized when the composite samples were exposed under the irradiation of electromagnetic (EM) wave with a changing frequency from 9 GHz to 11 GHz. Using the scanning electron microscope (SEM), the iron oxide nanoparticles were observed on the surfaces and inside the micropore structures of single fibers. The SEM images revealed that the composite’s EM shielding effectiveness was increased due to the adhesion of the iron oxide crystals to the kenaf fiber surfaces. As the Fe content increased from 0% to 6.8%, 15.9% and 18.0%, the total surface free energy of kenaf fibers with magnetizing treat increased from 44.77 mJ/m2 to 46.07 mJ/m2, 48.78 mJ/m2 and 53.02 mJ/m2, respectively, while the modulus of elasticity (MOE) reduced from 2,875 MPa to 2,729 MPa, 2,487 MPa and 2,007 MPa, respectively. Meanwhile, the shielding effectiveness was increased from 30-50% to 60-70%, 65-75% and 70-80%, respectively.

The thesis acquaints readers with the basic ideas of a new trend in marketing -- green marketing. It points out its particularities, historical evolution and potential application, including warning about common mistakes. The thesis aspires to bring an overview of the topic.

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[ES] En esta tesis doctoral se discuten una serie de cuestiones científicas relacionadas con a la producción y el procesamiento de algunas especies de cítricos de especial relevancia en Sicilia y en el área mediterránea. Los objetivos se centran en estudiar la trazabilidad y sostenibilidad de la producción de algunas especies de cítricos, así como encontrar nuevas aplicaciones a los subproductos y productos de desecho de la industria, con el fin de mejorar su rentabilidad. Por lo tanto, los temas que se desarrollarán serán los siguientes: caracterización de los compuestos bioactivos presentes en aceites esenciales y en el hidrolato de diferentes especies de cítricos; seguimiento del efecto del estrés hídrico controlado sobre la producción de aceites esenciales en hojas y flores del cv. Sanguinelli de Citrus sinensis y del cv. Clemenules de Citrus reticulata; estudio de los efectos fitotóxicos de los aceites esenciales en cuatro especies arvenses importantes en el área mediterránea, dos monocotiledóneas (Echinochloa crus-galli (L.) P.Beauv. y Avena fatua L.) y dos dicotiledóneas (Amaranthus retroflexus L. y Portulaca oleracea L.) mediante experimentos in vitro e in vivo; estudio del efecto bioestimulantes de las aguas residuales de la industria procesadora de cítricos sobre la comunidad microbiana del suelo; cuantificación de elementos de tierras raras en frutos de limón cultivados en diferentes áreas geográficas, para su posible uso como trazador geoquímico. Los principales resultados obtenidos son la caracterización de diferentes aceites esenciales, de los cuales los producidos por los residuos de la poda podrían ser utilizados como método de extracción de nuevos aceites esenciales con alto rendimiento. También se han encontrado sustancias nutracéuticas y farmacológicas en los hidrolatos industriales de naranja. Por otra parte, el aceite esencial industrial de limón mostró un buen potencial como agente herbicida, siendo, por tanto, de gran interés en la fabricación de herbicidas de origen natural, biodegradables y ecológicos. La aplicación del estrés hídrico controlado después del reposo invernal y, por tanto, en el momento de la brotación incrementó el diámetro final del fruto. La respuesta en el árbol no fue inmediata. La aplicación de hidrolatos de limón, naranja y mandarina al suelo junto al agua de riego, potenció los depósitos de C contribuyendo a aumentar la biomasa y mejoró la actividad microbiana. Estos resultados ponen de manifiesto el papel que los hidrolatos pueden desempeñar en la agricultura sostenible mejorando la fertilidad del suelo. Finalmente, el modelo de elementos de tierras raras podría utilizarse como una herramienta de conexión entre la producción de limón y el suelo del que proviene, contribuyendo, de esta manera, a su caracterización geográfica. En resumen, los resultados obtenidos en esta tesis contribuyen a impulsar el sector cítrico siciliano ya que: proporcionan medios para una agricultura sostenible; aumentan el valor de los subproductos y residuos de la industria; proponen aplicaciones para que el ciclo de producción y transformación sea más rentable y revalorizan los limones sicilianos vinculándolos a su zona de producción. / [CA] En esta tesi doctoral es discutixen una sèrie de qüestions científiques relacionades amb la producció i el processament d'algunes espècies de cítrics d'especial rellevància a Sicília i a l'àrea mediterrània. Els objectius, acordats prèviament amb la indústria de cítrics "EuroFood" i finançats pel projecte d'investigació "PON Industrial Ph.D. - a.a. 2016/2017", es centren en estudiar la traçabilitat i sostenibilitat de la producció d'algunes espècies de cítrics, així com de trobar noves aplicacions als subproductes i productes de rebuig de la indústria, amb el fi de millorar la seua rentabilitat. Per tant, els temes que es desenvoluparan seran els següents: caracterització dels compostos bioactius presents en els olis essencials i en el l'hidrolato de diferents espècies de cítrics; seguiment de l'efecte de l'estrés hídric controlat en la producció d'olis essencials en fulles i flors del cv. Sanguinelli de Citrus sinensis i del cv. Clemenules de Citrus reticulata; estudi dels efectes fitotòxicos dels olis essencials de cítrics en quatre espècies arvenses importants en l'àrea mediterrània, dos monocotiledònies (Echinochloa crus-galli (L.) P.Beauv. i Avena fàtua L.) i dos dicotiledònies (Amaranthus retroflexus L. i Portulaca oleracea L.) per mitjà de diferents experiments in vitro i in vivo; estudi de l'efecte bioestimulant de les aigües residuals de la indústria processadora de cítrics sobre la comunitat microbiana del sòl; quantificació d'elements de terres rares en fruits de llima cultivats en diferents àrees geogràfiques, per al seu possible ús com a traçador geoquímic. Els principals resultats obtinguts són la caracterització de diferents olis essencials, dels quals els produïts pels residus de la poda podrien ser utilitzats com a mètode d'extracció de nous olis essencials amb alt rendiment. També s'han trobat substàncies nutracéutiques i farmacològiques en els hidrolats industrials de taronja. D'altra banda, l'oli essencial industrial de llima va mostrar un bon potencial com a agent herbicida, sent, per tant, de gran interés en la fabricació d'herbicides d'origen natural, biodegradables i ecològics. L'aplicació de l'estrés hídric controlat després del repòs hivernal i, per tant, en el moment de la brotació va incrementar el diàmetre final del fruit. La resposta en l'arbre no va ser immediata. L'aplicació de hidrolats de llima, taronja i mandarina al sòl amb l'aigua de reg, va augmentar els depòsits de carbó (C) contribuint a augmentar la biomassa i va millorar l'activitat microbiana. Aquests resultats posen de manifest el paper dels hidrolats en l'agricultura sostenible millorant, d'aquesta manera, la fertilitat del sòl. Finalment, el model d'elements de terres rares podria utilitzar-se com una ferramenta d'enllaç entre la producció de llima i el sòl del què prové, contribuint, d'esta manera, a la seua caracterització geogràfica. En resum, els resultats obtinguts en esta tesi doctoral contribueixen a impulsar el sector cítric sicilià ja que: - proporcionen mitjans per a una agricultura sostenible; - augmenten el valor dels subproductes i residus de la indústria; - proposen aplicacions perquè el cicle de producció i transformació siga de més rendabilitat; - revaloritzen les llimes d'origen sicilià vinculant-les a la seua zona de producció. / [EN] In this doctoral thesis are discussed a series of scientific issues regarding citrus fruits production and processing, species of particular relevance in Sicily and in the Mediterranean area. Objectives and research activities addressed in this thesis were agreed with the citrus industry "EuroFood" and financed by the research project "PON industrial Ph.D. - a.a. 2016/2017". The research project was targeted to study the traceability and sustainability of citrus production, and to find new applications to the by-products and waste products of citrus industry with the objective of appreciate and enhance the Sicilian citrus industry. The following topics are addressed and developed in this thesis: - Characterization of the bioactive compounds present in essential oils (EOs) and in the hydrolate of different citrus species. - Monitoring of the effect of controlled water stress on the production of EOs in leaves and flowers of Citrus sinensis (L.) Osbeck cv. 'Sanguinelli' and Citrus reticulata Blanco cv. 'Clemenules'; -Test the phytotoxic effects of citrus EOs on four important weed species in the Mediterranean area, two monocotyledon (Echinochloa crus-galli (L.) P.Beauv. and Avena fatua L.) and two dicotyledon (Amaranthus retroflexus L., and Portulaca oleraceaL.) by different experiments in vitro and in greenhouse conditions; -Evaluation of the effect as natural biostimulants of wastewaters from citrus processing industry by its application on soil microbial community; -Quantification of rare earth elements in lemon fruits from different geographical areas for its possible use as geochemical tracers applied to lemon production. Different Citrus EOs have been characterized in this study and it has been verified that the oils produced by the pruning waste could be used for the extraction of EOs with high yields. In addition, nutraceutical and pharmacological substances have been found in the orange industrial hydrolates. Industrial lemon EO showed good potential when testing its herbicidal activity. Lemon EO represents a good basis for the development of herbicides of natural origin, biodegradable and eco-friendly. Thanks to the application of water stress after the winter vegetative restart, a conclusion found was that water stress increased the diameter of the fruit and it was observed that the effects of stress were not immediate on citrus trees, but were evident after some time. The study of the application of lemon, orange and mandarin hydrolates in the soil, as irrigation water provided the effects on stable and labile soil C pools, on biomass and microbial activity and on main microbial groups. Overall, hydrolates can play a role in sustainable agriculture because when added to a soil, they improve soil quality and fertility. The Rare Earth Element model could be used as a tool to connect lemon production to the soil where they were produced, for a possible geographical characterization and a direct link between the production and the territory or soil. The results obtained were very interesting because: - they provided the means for sustainable agriculture; - they increased the value of the by-products and waste products of the citrus industry; - they proposed applications for the citrus production and transformation cycle being more sustainable; - they could valorize the Sicilian lemons by linking them to their production area. These results could have practical repercussions in the production cycle of citrus fruits and give a boost to the Sicilian citrus fruit sector. / Objectives and research activities addressed in this thesis were agreed with the citrus industry "EuroFood" and financed by the research project PON industrial Ph.D. - a.a. 2016/2017 / Ioppolo, A. (2020). Valorization of Citrus spp. Cultivars cultivated in Sicily for the industrial use of citrus derivatives and in particular for potential alternative uses of essential oils for the enhancement of the island's citrus production [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/159385 / TESIS

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The objectives of this study were: verify the adequation to the presuppositions of the mathematical model and, identify data transformation for productive and morphological variables of tomato in experiments in plastic tunnel and in field, considering each harvest date and grouped harvests during spring-summer and autumn-winter seasons; and, to evaluate the effect of the application of Acrescent Solus® in complementation and/or substitution to the mineral fertilization in coverage over productive and morphological variables, quality of fruit and color of leaves of tomato cultivated in plastic tunnel and in field during springsummer and autumn-winter seasons. Two experiments were conducted in plastic tunnel (spring-summer and autumn-winter) and one in field (spring-summer), both in a randomized block design with three replications in a bifactorial (2x4), with four additional controls. The tests of: non-additivity of Tukey, Lilliefors, Bartlett and Run Test, were used, respectively, for verify the adequation to the presuppositions of: additivity of the model, normality, homogeneity and randomness of errors. In cases of violation, the data were transformed and, submitted again to the analysis of the presuppositions of the mathematical model. The productive and morphological variables of tomato present adequation to the presupposition of additivity of the model. Violations of the productive and morphological variables occur to the presupposition of: normality, homogeneity and randomness of errors. The grouping of all harvests for analysis provides adequation of productive and morphological variables to the presuppositions of normality and homogeneity of errors. The data transformation that provides more proportion of adequation of productive and morphological variables to the presuppositions of normality, homogeneity and randomness of errors is the square root. In the spring-summer, the Acrescent Solus® does not alter the productive and morphological variables and, the quality of fruits of tomato, while, in the autumn-winter, it reduces the length, the width and the mass of fruits and, also, it does not alters the quality of fruits. The increase of the dose of Acrescent Solus®, combined with the mineral fertilization in coverage results in intensification of the green color of leaves, from the second and fourth harvest fruit in the spring-summer and autumn-winter, respectively, nevertheless, without showing favorable correlation with the expression of productive and morphological variables of tomato. / Os objetivos deste estudo foram: verificar o atendimento às pressuposições do modelo matemático e, identificar transformações de dados para variáveis produtivas e morfológicas de tomateiro em experimentos em túnel plástico e em campo, considerando cada data de colheita e colheitas agrupadas na primavera-verão e outono-inverno; e, avaliar o efeito da aplicação de Acrescent Solus® em complementação e/ou substituição à adubação mineral em cobertura sobre variáveis produtivas, morfológicas, de qualidade de frutos e de coloração de folhas de tomateiro cultivado em túnel plástico e em campo na primavera-verão e outonoinverno. Dois experimentos foram conduzidos em túnel plástico (primavera-verão e outonoinverno) e um em campo (primavera-verão), ambos no delineamento de blocos ao acaso com três repetições em um bifatorial (2x4), com quatro testemunhas adicionais. Para verificar o atendimento às pressuposições de: aditividade do modelo, normalidade, homogeneidade e aleatoriedade dos erros foram utilizados, respectivamente, os testes de: não aditividade de Tukey, Lilliefors, Bartlett e de Sequência. Nos casos de violação, os dados foram transformados e, novamente submetidos à análise das pressuposições do modelo matemático. As variáveis produtivas e morfológicas de tomateiro apresentam atendimento ao pressuposto de aditividade do modelo. Ocorrem violações das variáveis produtivas e morfológicas às pressuposições de: normalidade, homogeneidade e aleatoriedade dos erros. O agrupamento de todas as colheitas para análise proporciona atendimento das variáveis produtivas e morfológicas aos pressupostos de normalidade e homogeneidade dos erros. A transformação que possibilita maior proporção de atendimento das variáveis produtivas e morfológicas aos pressupostos de normalidade, homogeneidade e aleatoriedade dos erros é a raiz quadrada. Na primavera-verão o Acrescent Solus® não influencia as variáveis produtivas, morfológicas e de qualidade dos frutos de tomateiro, enquanto no outono-inverno reduz o comprimento, a largura e a massa de frutos e, também não influencia a qualidade de frutos. O aumento da dose de Acrescent Solus®, combinada com a adubação mineral em cobertura resulta em intensificação da coloração verde das folhas, a partir da segunda e quarta colheita de frutos na primavera-verão e outono-inverno, respectivamente, porém, sem apresentar correlação favorável com a expressão das variáveis produtivas e morfológicas de tomateiro.