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  • Jogi, Ramakrishna, et al. (författare)
  • Understanding the formation of phenolic monomers during fractionation of birch wood under supercritical ethanol over iron based catalysts
  • 2020
  • Ingår i: Journal of the Energy Institute. - : Elsevier. - 1743-9671. ; 93:5, s. 2055-2062
  • Tidskriftsartikel (refereegranskat)abstract
    • The liquefaction of biomass in ethanol, at the critical point, has high potential due to low temperature and pressure (243 °C, 63 bar) when compared with water (374 °C, 220 bar). The current study deals with the fractionation of birch wood powder which was liquefied under supercritical ethanol over acidic or non-acidic catalysts, 5 wt % Fe-Beta-H-150 and 5 wt % Fe–SiO2, respectively. Based on the results, the reaction mechanism for the formation of lignin degradation products was proposed. The main phenolic product was isoeugenol over 5 wt % Fe-Beta-H-150 while intermediate products, i.e. such as coniferyl, and sinapyl alcohol, 4-propenyl syringol, syringaresinol, as well as syringyldehyde reacted rapidly further. The thermodynamic analysis was performed by Joback approach and using Gibbs-Helmholtz equation supporting the obtained results.
  • Yahia, Mohamed, et al. (författare)
  • Effect of incorporating different ZIF-8 crystal sizes in the polymer of intrinsic microporosity, PIM-1, for CO2/CH4 separation
  • 2021
  • Ingår i: Microporous and Mesoporous Materials. - : Elsevier. - 1387-1811 .- 1873-3093. ; 312
  • Tidskriftsartikel (refereegranskat)abstract
    • Effective and economical carbon dioxide-methane separation (CO2/CH4) is highly desirable in several industries such as sweetening natural gases and renewable natural gas (RNG) from biogas and landfills. Among the different separation technologies, membrane separation has been shown to have lower cost of production and lower CH4 losses. In this study, Zeolitic Imidazole Frameworks (ZIF-8) crystals with sizes varying from 45 nm to 450 nm were synthesized and incorporated in the polymer of intrinsic microporosity, PIM-1, to form mixed matrix membranes (MMMs). The structure, morphology, and physicochemical properties of the MMMs were characterized by 1H NMR, FTIR, XRD, TGA, and SEM. ZIF-8 crystal size was controlled using the concentration of sodium formate. The influence of the ZIF-8 crystal size on MMMs was studied by sorption, gas permeability, and aging of the membranes. The MMMs with ZIF-8 crystals of 120 nm particle diameter yielded the greatest improvement in gas transport properties; the CO2/CH4 selectivity-CO2 permeability was 11.4 and 9700 Barrer compared to PIM-1 with 6.4 and 9300 Barrer respectively. The former is near the Robeson 2008 upper bound, while PIM-1 is on the 1991 upper bound. After 40 days of aging, selectivity increased and permeability decreased; the changes were parallel to the Robeson upper bounds indicating increased polymer packing and diffusivity selectivity.
  • B. Erdal, Nejla, et al. (författare)
  • Green Strategy to Reduced Nanographene Oxide through Microwave Assisted Transformation of Cellulose
  • 2018
  • Ingår i: ACS Sustainable Chemistry and Engineering. - : American Chemical Society (ACS). - 2168-0485. ; 6:1, s. 1245-1255
  • Tidskriftsartikel (refereegranskat)abstract
    • A green strategy for fabrication of biobased reduced nanographene oxide (r-nGO) was developed. Cellulose derived nanographene oxide (nGO) type carbon nanodots were reduced by microwave assisted hydrothermal treatment with superheated water alone or in the presence of caffeic acid (CA), a green reducing agent. The carbon nanodots, r-nGO and r-nGO-CA, obtained through the two different reaction routes without or with the added reducing agent, were characterized by multiple analytical techniques including FTIR, XPS, Raman, XRD, TGA, TEM, AFM, UV-vis, and DLS to confirm and evaluate the efficiency of the reduction reactions. A significant decrease in oxygen content accompanied by increased number of sp2 hybridized functional groups was confirmed in both cases. The synergistic effect of superheated water and reducing agent resulted in the highest C/O ratio and thermal stability, which also supported a more efficient reduction. Interesting optical properties were detected by fluorescence spectroscopy where nGO, r-nGO, and r-nGO-CA all displayed excitation dependent fluorescence behavior. r-nGO-CA and its precursor nGO were evaluated toward osteoblastic cells MG-63 and exhibited nontoxic behavior up to 200 μg mL-1, which gives promise for utilization in biomedical applications.
  • Bui, Thai Q., et al. (författare)
  • Mesoporous Melamine-Formaldehyde Resins as Efficient Heterogeneous Catalyst for Continuous Synthesis of Cyclic Carbonates from Epoxides and gaseous CO2
  • 2020
  • Ingår i: ACS Sustainable Chemistry & Engineering. - : American Chemical Society (ACS). - 2168-0485. ; 8:34, s. 12852-12869
  • Tidskriftsartikel (refereegranskat)abstract
    • Herein we report the application of inexpensive mesoporous melamine-formaldehyde resins (MMFR and MMFR250) obtained by a novel template-free and organosolvent-free hydrothermal method as efficient heterogeneous catalysts for direct synthesis of cyclic carbonates from CO2 and epoxides (epichlorohydrin, butylene oxide and styrene oxide). The catalytic activity of the melamine resins was attributed to the abundant Lewis basic N-sites capable of activating CO2 molecules. Based on CO2-Temperature programmed desorption, the concentration of surface basic sites for MMFR and MMFR250 were estimated to be 172 and 56 µmol/g, while the activation energy of CO2 desorption (strength of basic sites) were calculated to be 92.1 and 64.5 kJ/mol. We also observed considerable differences in the catalytic activity and stability of polymeric catalysts in batch and in continuous-flow mode; due to the existence of a synergism between adsorption of CO2 and cyclic carbonates (poison). Our experiments also revealed important role of catalyst surface chemistry and CO2 partial pressure upon catalyst poisoning. Nevertheless, owing to their unique properties (large specific surface area, large mesoporous and CO2 basicity) melamine resins presented excellent activity (turnover frequency 207-2147 h-1), selectivity (>99%) for carbonation of epoxides with CO2 (20 bar initial CO2 or CO2:epoxide mole ratio ~1.5) under solvent-free and co-catalyst-free conditions at 100-120 oC. Most importantly, these low-cost polymeric catalysts were reusable and demonstrated exceptional stability in a flow reactor (tested upto 13 days time on stream, weight hourly space velocity 0.26-1.91 h-1) for continuous cyclic carbonate production from gaseous CO2 with different epoxides (conversion 76-100% and selectivity >99%) under industrially relevant conditions (120 oC, 13 bar, solvent-free/co-catalyst-free) confirming their superiority over the previously reported catalytic materials.
  • Deshpande, Raghu, 1979- (författare)
  • The initial phase of the sodium bisulfite pulping of softwood dissolving pulp
  • 2015
  • Licentiatavhandling (övrigt vetenskapligt)abstract
    • The sulfite pulping process is today practised in only a small number of pulp mills around the globe and the number of sulfite mills that use sodium as the base (cation) is less than five. However, due to the increasing interest in the wood based biorefinery concept, the benefits of sulfite pulping and especially the sodium based variety, has recently gained a lot of interest. It was therefore considered to be of high importance to further study the sodium based sulfite process to investigate if its benefits could be better utilized in the future in the production of dissolving pulps. Of specific interest was to investigate how the pulping conditions in the initial part of the cook (≥ 60 % pulp yield) should be performed in the best way.Thus, this thesis is focused on the initial phase of single stage sodium bisulfite cooking of either 100 % spruce or 100 % pine wood chips. The cooking experiments were carried out with either a lab prepared or a mill prepared cooking acid and the temperature and cooking time were varied. Activation energies for different wood components were investigated as well as side reactions concerning the formation of thiosulfate and sulfate.
  • Farzaneh, Amirfarrokh, et al. (författare)
  • Adsorption of Butanol and Water Vapors in Silicalite‑1 Films with a Low Defect Density
  • 2016
  • Ingår i: Langmuir. - 0743-7463 .- 1520-5827. ; 32, s. 11789-11798
  • Tidskriftsartikel (refereegranskat)abstract
    • Pure silica zeolites are potentially hydrophobic and have therefore been considered to be interesting candidates for separating alcohols, e.g., 1-butanol, from water. Zeolites are traditionally synthesized at high pH, leading to the formation of intracrystalline defects in the form of silanol defects in the framework. These silanol groups introduce polar adsorption sites into the framework, potentially reducing the adsorption selectivity toward alcohols in alcohol/water mixtures. In contrast, zeolites prepared at neutral pH using the fluoride route contain significantly fewer defects. Such crystals should show a much higher butanol/water selectivity than crystals prepared in traditional hydroxide (OH−) media. Moreover, silanol groups are present at the external surface of the zeolite crystals; therefore, minimizing the external surface of the studied adsorbent is important. In this work, we determine adsorption isotherms of 1-butanol and water in silicalite-1 films prepared in a fluoride (F−) medium using in situ attenuated total reflectance−Fourier transform infrared (ATR−FTIR) spectroscopy. This film was composed of well intergrown, plate-shaped b-oriented crystals, resulting in a low external area. Single-component adsorption isotherms of 1-butanol and water were determined in the temperature range of 35− 80 °C. The 1-butanol isotherms were typical for an adsorbate showing a high affinity for a microporous material and a large increase in the amount adsorbed at low partial pressures of 1-butanol. The Langmuir−Freundlich model was successfully fitted to the 1-butanol isotherms, and the heat of adsorption was determined. Water showed a very low affinity for the adsorbent, and the amounts adsorbed were very similar to previous reports for large silicalite-1 crystals prepared in a fluoride medium. The sample also adsorbed much less water than did a reference silicalite-1(OH−) film containing a high density of internal defects.The results show that silicalite-1 films prepared in a F− medium with a low density of defects and external area are very promising for the selective recovery of 1-butanol from aqueous solutions.
  • Gunnarsson, Rickard, 1989- (författare)
  • Titanium oxide nanoparticle production using high power pulsed plasmas
  • 2016
  • Licentiatavhandling (övrigt vetenskapligt)abstract
    • This thesis covers fundamental aspects of process control when growing titanium oxide nanoparticles in a reactive sputtering process. It covers the influence of oxygen containing gas on the oxidation state of the cathode from which the growth material is ejected, as well as its influence on the particles oxidation state and their nucleation. It was found that a low degree of reactive gases was necessary for nanoparticles of titanium to nucleate. When the oxygen gas was slightly increased, the nanoparticle yield and particle oxygen content increased. A further increase caused a decrease in particle yield which was attributed to a slight oxidation of the cathode. By varying the oxygen flow to the process, it was possible to control the oxygen content of the nanoparticles without fully oxidizing the cathode. Because oxygen containing gases such as residual water vapour has a profound influence on nanoparticle yield and composition, the deposition source was re-engineered to allow for cleaner and thus more stable synthesis conditions.The size of the nanoparticles has been controlled by two means. The first is to change electrical potentials around the growth zone, which allows for nanoparticle size control in the order of 25-75 nm. This size control does not influence the oxygen content of the nanoparticles. The second means of size control investigated was by increasing the pressure. By doing this, the particle size can be increased from 50 – 250 nm, however the oxygen content also increases with pressure. Different particle morphologies were found by changing the pressure. At low pressures, mostly spherical particles with weak facets were produced. As the pressure increased, the particles got a cubic shape. At higher pressures the cubic particles started to get a fractured surface. At the highest pressure investigated, the fractured surface became poly-crystalline, giving a cauliflower shaped morphology.
  • Konwar, Lakhya Jyoti, 1987-, et al. (författare)
  • Efficient hydrothermal deoxygenation of tall oil fatty acids into n-paraffinic hydrocarbons and alcohols in the presence of aqueous formic acid
  • 2020
  • Ingår i: Biomass Conversion and Biorefinery. - : Springer. - 2190-6815 .- 2190-6823.
  • Tidskriftsartikel (refereegranskat)abstract
    • Hydrothermal deoxygenation of tall oil fatty acids (TOFA) was investigated in the presence of aqueous formic acid (0.5–7.5 wt%) as a H2 donor in the presence of subcritical H2O pressure (569–599 K). Pd and Ru nanoparticles supported on carbon (5% Pd/CSigma, 5% Ru/CSigma, 10% Pd/CO850_DP, and 5% Ru/COPcomm_DP) were found to be efficient catalysts for deoxygenation of TOFA. The reaction pathway was mainly influenced by the concentration of formic acid and the catalyst. In case of Pd catalysts, in the presence of 0–2.5 wt% formic acid, decarboxylation was the dominant pathway producing n-paraffinic hydrocarbons with one less carbon atom (heptadecane yield up to 94 wt%), while with 5–7.5% formic acid, a hydrodeoxygenation/hydrogenation mechanism was favored producing C18 deoxygenation products octadecanol and octadecane as the main products (yields up to 70 wt%). In contrast, Ru catalysts produced a mixture of C5-C20 (n-and iso-paraffinic) hydrocarbons via decarboxylation, cracking and isomerization (up to 58 wt% C17 yield and total hydrocarbon yield up to 95 wt%) irrespective of formic acid concentration. Kinetic studies showed that the rates of deoxygenation displayed Arrhenius type behavior with apparent activation energies of 134.44 ± 31.36 kJ/mol and 148.92 ± 3.66 kJ/mol, for the 5% Pd/CSigma and 5% Ru/CSigma catalyst, respectively. Furthermore, the experiments with glycerol tristearate, rapeseed oil, sunflower oil, rapeseed biodiesel, and hydrolyzed rapeseed oil produced identical products confirming the versatility of the aforementioned catalytic systems for deoxygenation of C18 feedstocks.
  • Kumar Raul, Prasanta, et al. (författare)
  • Microwave assisted and in-situ generated palladium nanoparticles catalysed desulfitative synthesis of cross-biphenyls from arylsulfonyl chlorides and phenylboronic acids
  • 2021
  • Ingår i: Results in Chemistry. - : Elsevier. - 2211-7156. ; 3
  • Tidskriftsartikel (refereegranskat)abstract
    • A microwave assisted reaction protocol for Suzuki–Miyaura cross-coupling has been developed. Substituted arylboronic acids and arylsulfonyl chlorides coupled under microwave irradiation (MWI) to produce cross-biphenyls in high yields under aerobic condition. The principal advantage of this protocol is that formation of cross-biphenyls was achieved within shorter time along with desulfurization of arylsulfonyl chloride. In-situ generated Pd nanoparticles (NPs) act as catalyst in the reaction. Substituents like methyl, halogens, cyano, amino and t-butyl groups in arylboronic acids tolerate the reaction condition. Pd NPs could be reused several times under chosen reaction conditions without losing its activity significantly. The product formation and the role of the catalyst for the cross-coupling reaction has been rationalised with the help of a proposed mechanism. This reaction is one of the examples of In-situ generated Nanoparticles-catalyzed Organic Synthesis Enhancement (i-NOSE) approach. The approach derives its importance in terms of catalyst’s (i) simple preparation method, (ii) stability under the chosen reaction condition, (iii) substrate specificity, (iv) simple filtration to recover the catalyst and (v) easy regeneracy which clearly indicate that the approach could be applicable for various types of catalytic transformations.
  • Saeid, Soudabeh, et al. (författare)
  • Synthesis and Characterization of Metal Modified Catalysts for Decomposition of Ibuprofen from Aqueous Solutions
  • 2020
  • Ingår i: Catalysts. - : MDPI. - 2073-4344. ; 10:7
  • Tidskriftsartikel (övrigt vetenskapligt)abstract
    • The presence of pharmaceuticals in surface water, drinking water, and wastewater has attracted significant concern because of the non-biodegradability, resistance, and toxicity of pharmaceutical compounds. The catalytic ozonation of an anti-inflammatory pharmaceutical, ibuprofen was investigated in this work. The reaction mixture was analyzed and measured by high-performance liquid chromatography (HPLC). Liquid chromatography-mass spectrometry (LC-MS) was used for the quantification of by-products during the catalytic ozonation process. Ibuprofen was degraded by ozonation under optimized conditions within 1 h. However, some intermediate oxidation products were detected during the ibuprofen ozonation process that were more resistant than the parent compound. To optimize the process, nine heterogeneous catalysts were synthesized using different preparation methods and used with ozone to degrade the ibuprofen dissolved in aqueous solution. The aim of using several catalysts was to reveal the effect of various catalyst preparation methods on the degradation of ibuprofen as well as the formation and elimination of by-products. Furthermore, the goal was to reveal the influence of various support structures and different metals such as Pd-, Fe-, Ni-, metal particle size, and metal dispersion in ozone degradation. Most of the catalysts improved the elimination kinetics of the by-products. Among these catalysts, Cu-H-Beta-150-DP synthesized by the deposition–precipitation process showed the highest decomposition rate. The regenerated Cu-H-Beta-150-DP catalyst preserved the catalytic activity to that of the fresh catalyst. The catalyst characterization methods applied in this work included nitrogen adsorption–desorption, scanning electron microscopy, transmission electron microscopy, and Fourier-transform infrared spectroscopy. The large pore volume and small metal particle size contributed to the improved catalytic activity.
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