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Correa, CR, Bernardo M, Ribeiro RPPL, Esteves IAAC, Kruse A.  2017.  Evaluation of hydrothermal carbonization as a preliminary step for the production of functional materials from biogas digestate. Journal of Analytical and Applied Pyrolysis. 124:461-474. AbstractWebsite

Digestate from a biogas plant that uses solely biomass for biogas production was used as precursor material for the production of activated carbon as an alternative to increase its added value. The digestate was converted into hydrochar by hydrothermal carbonization varying the temperature (190–250°C), residence time (3 and 6h), and pH (5 and 7). Temperature followed by residence time had the strongest influence on the chemical composition and thermal stability of the hydrochars. A significant effect of the pH was not observed. The hydrochars were chemically activated to enhance the surface area and use them as activated carbon. As a consequence, the surface areas increased from 8 to 14m2/g (hydrochars) to 930–1351m2/g (activated carbons). Furthermore, large micropore volumes were measured (0.35–0.50cm3/g). The activated carbons were studied as adsorbents in gas phase applications, showing that the product of digestate is a very effective adsorbent for carbon dioxide (CO2). Especially the activated carbon obtained from the hydrochar produced at 250°C for 6h, which adsorbed 8.80mol CO2/kg at 30°C and 14.8bar. Additionally, the activated carbons showed a stronger affinity towards CO2 compared to methane (CH4), which makes this material suitable for the upgrading of raw biogas to biomethane.

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Fernandes, MJ, Moreira MM, Paíga P, Dias D, Bernardo M, Carvalho M, Lapa N, Fonseca I, Morais S, Figueiredo S, Delerue-Matos C.  2019.  Evaluation of the adsorption potential of biochars prepared from forest and agri-food wastes for the removal of fluoxetine. Bioresource Technology. 292:121973. AbstractWebsite

Twelve biochars from forest and agri-food wastes (pruning of Quercus ilex, Eucalyptus grandis, Pinus pinaster, Quercus suber, Malus pumila, Prunus spinosa, Cydonia oblonga, Eriobotrya japonica, Juglans regia, Actinidia deliciosa, Citrus sinensis and Vitis vinifera) were investigated as potential low-cost and renewable adsorbents for removal of a commonly used pharmaceutical, fluoxetine. Preliminary adsorption experiments allowed to select the most promising adsorbents, Quercus ilex, Cydonia oblonga, Eucalyptus, Juglans regia and Vitis vinifera pruning material. They were characterized by proximate, elemental and mineral analysis, thermogravimetric analysis, Fourier transform infrared spectroscopy, determination of specific surface area and pH at the point of zero charge. Batch and equilibrium studies were performed, and the influence of pH was evaluated. The equilibrium was reached in less than 15 min in all systems. The maximum adsorption capacity obtained was 6.41 mg/g for the Eucalyptus biochar, which also demonstrated a good behavior in continuous mode (packed column).

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Godino-Ojer, M, Milla-Diez L, Matos I, Durán-Valle CJ, Bernardo M, Fonseca IM, Pérez Mayoral E.  2018.  Enhanced Catalytic Properties of Carbon supported Zirconia and Sulfated Zirconia for the Green Synthesis of Benzodiazepines. ChemCatChem. 10:5215-5223., Number 22 AbstractWebsite

Abstract This work reports for the first time a new series of promising porous catalytic carbon materials, functionalized with Lewis and Brønsted acid sites useful in the green synthesis of 2,3-dihydro-1H-1,5-benzodiazepine – nitrogen heterocyclic compounds. Benzodiazepines and derivatives are fine chemicals exhibiting interesting therapeutic properties. Carbon materials have been barely investigated in the synthesis of this type of compounds. Two commercial carbon materials were selected exhibiting different textural properties: i) Norit RX3 (N) as microporous sample and ii) mesoporous xerogel (X), both used as supports of ZrO2 (Zr) and ZrO2/SO42− (SZr). The supported SZr led to higher conversion values and selectivities to the target benzodiazepine. Both chemical and textural properties influenced significantly the catalytic performance. Particularly relevant are the results concerning the non-sulfated samples, NZr and XZr, that were able to catalyze the reaction leading to the target benzodiazepine with high selectivity (up to 80 %; 2 h). These results indicated an important role of the carbon own surface functional groups, avoiding the use of H2SO4. Even very low amounts of SZr supported on carbon reveal high activity and selectivity. Therefore, the carbon materials herein reported can be considered an efficient and sustainable alternative bifunctional catalysts for the benzodiazepine synthesis.

M
Mestre, AS, Nabiço A, Figueiredo PL, Pinto ML, Santos SMCS, Fonseca IM.  2016.  Enhanced clofibric acid removal by activated carbons: Water hardness as a key parameter. Chemical Engineering Journal. 286:538-548. AbstractWebsite

Clofibric acid is the metabolite and active principle of blood lipid regulators, it represents the class of acidic pharmaceuticals, and is one of the most persistent drug residues detected in the aquatic environment worldwide. This interdisciplinary work evaluates the effect of solution pH and water hardness in clofibric acid adsorption onto commercial activated carbons. Kinetic and equilibrium assays revealed that the highest clofibric acid removal efficiencies (>70%) were attained at pH 3, and that at pH 8 water hardness degree plays a fundamental role in the adsorption process. In hard water at pH 8 the removal efficiency values increased by 22 or 46% points depending on the carbon sample. Adsorbents’ textural properties also affect the adsorption process since for the microporous sample (CP) the increase of water hardness has a great influence in kinetic and equilibrium data, while for the micro+mesoporous carbon (VP) the variation of the water hardness promoted less significant changes. At pH 3 the increase of water hardness leads to changes in the adsorption mechanism of clofibric acid onto CP carbon signaled by a transition from an S-type to an L-type curve. At pH 8 the change from deionized water to hard water doubles the maximum adsorption capacity of sample CP (101.7mgg−1 vs 211.9mgg−1, respectively). The adsorption enhancement, with water hardness under alkaline conditions, was reasoned in terms of calcium complexation with clofibrate anion exposed by molecular modeling and conductivity studies. Ca2+ complexation by other acidic organic compounds may also occur, and should be considered, since it can play a fundamental role in improved design of water treatment processes employing activated carbons.

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Silva, CAC, Figueiredo FCA, Rodrigues R, Sairre MI, Gonçalves M, Matos I, Fonseca IM, Mandelli D, Carvalho WA.  2016.  Enhancing the biodiesel manufacturing process by use of glycerin to produce hyacinth fragrance, Jun. Clean Technologies and Environmental Policy. 18:1551–1563., Number 5 AbstractWebsite

Oxidized and sulfonated-activated carbons (AC) were tested in the catalytic conversion of glycerol by acetalization reactions. The solids were treated with concentrated nitric acid and/or fuming sulfuric acid (AC, AC-N, AC-S, and AC-NS). The presence of sulfur and an increase in the acidity of the solids demonstrate the suitability of the oxidation as well as the sulfonation process, especially in the sample treated with concentrated nitric acid and fuming sulfuric acid (AC-NS). The best catalyst for the reaction of glycerol acetalization with phenylacetaldehyde was AC-NS, with a phenylacetaldehyde conversion of 95 {%} after 90 min at 383 K and selectivity of 88 and 12 {%}, respectively, to dioxolane and dioxane. These products can be used as hyacinth fragrance flavoring compounds. Furthermore, a contribution of homogeneous catalysis in these systems was not identified. Thus, we identified a possibility of glycerol conversion, a biodiesel by-product, into value-added products by suitable catalysts produced from activated carbons.

Surra, E, Bernardo M, Lapa N, Esteves IAAC, Fonseca I, Mota JP.  2018.  Enhanced Biogas Production through Anaerobic co-Digestion of OFMSW with Maize Cob Waste Pre-Treated with Hydrogen Peroxide. Chemical Engineering Transactions. 65:121-126.