Natural and Synthetic Polymers/Pulp and Paper Technology Group, Faculty of Chemical Engineering and Environmental Protection, “Gheorghe Asachi” Technical University of Iasi, 700050 Iasi, Romania
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Dr. Adrian Puitel
Natural and Synthetic Polymers/Pulp and Paper Technology Group, Faculty of Chemical Engineering and Environmental Protection, “Gheorghe Asachi” Technical University of Iasi, 700050 Iasi, Romania
In this paper, we describe an experimental study on the hot alkali extraction of hemicelluloses from wheat straw and corn stalks, two of the most common lignocellulosic biomass constituents in Romania. The chemical compositions of the raw materials were determined analytically, and the relevant chemical components were cellulose, hemicelluloses, lignin, and ash. Using the response surface methodology, the optimum values of the hot alkaline extraction parameters, i.e., time, temperature, and NaOH concentration, were identified and experimentally validated. The physicochemical characterization of the isolated hemicelluloses was performed using HPLC, FTIR, TG, DTG, and 1H-NMR spectroscopy. The main hemicellulose components identified experimentally were xylan, arabinan, and glucan. The study emphasizes that both corn stalks and wheat straw are suitable as raw materials for hemicellulose extraction, highlighting the advantages of alkaline pretreatments and showing that optimization methods can further improve the process efficiency.
This paper aims to provide an overview of the fundamentals, development, and evolution of residence time distribution (RTD) methodology and its applications to the flow and mixing of fluids (and solid particles) modeling in different systems. A concise literature analysis is followed by a succinct presentation of RTD methodology’s experimental and theoretical foundations and RTD-based mathematical modeling, highlighting its importance. An experimental demonstration of RTD diagnostics on a photochemical reactor is performed to identify the most practical locations for the inlet/outlet pipes (axial or radial) and the photochemical reactor’s ideal working posture (horizontal, vertical, or inclined) and to understand the level of mixing and to determine the fluid flow defects. Using the relevant RTD functions and the corresponding central moments, it was possible to show that short circuits and dead zones occurred in each of the six considered reactor configurations. Following these investigations, design solutions were proposed to achieve a convenient exposure time, proper mixing, and uniform irradiation inside the reactor.
The alkaline extraction of hemicelluloses from a mixture of three varieties of wheat straw (containing 40.1% cellulose, 20.23% xylan, and 26.2% hemicellulose) was analyzed considering the following complementary pre-treatments: freeze–thaw cycles, microwaves, and ultrasounds. The two cycles freeze–thaw approach was selected based on simplicity and energy savings for further analysis and optimization. Experiments planned with Design Expert were performed. The regression model determined through the response surface methodology based on the severity factor (defined as a function of time and temperature) and alkali concentration as variables was then used to optimize the process in a multi-objective case considering the possibility of further use for pulping. To show the properties and chemical structure of the separated hemicelluloses, several analytical methods were used: high-performance chromatography (HPLC), Fourier-transformed infrared spectroscopy (FTIR), proton nuclear magnetic resonance spectroscopy (1H-NMR), thermogravimetry and derivative thermogravimetry analysis (TG, DTG), and scanning electron microscopy (SEM). The verified experimental optimization result indicated the possibility of obtaining hemicelluloses material containing 3.40% glucan, 85.51% xylan, and 7.89% arabinan. The association of hot alkaline extraction with two freeze–thaw cycles allows the partial preservation of the hemicellulose polymeric structure.
Natural polymers have proven to be extremely interesting matrices for the immobilization of microbial biomasses, via various mechanisms, in order to bring them into a form easier to handle—the form of composites. This article aimed to study composites based on a residual microbial biomass immobilized in sodium alginate via an encapsulation technique as materials with adsorbent properties. Thus, this study focused on the residual biomass resulting from beer production (Saccharomyces pastorianus yeast, separated after the biosynthesis process by centrifugation and dried at 80 °C)—an important source of valuable compounds, used either as a raw material or for transformation into final products with added value. Thus, the biosorptive potential of this type of composite was tested—presenting in the form of spherical microcapsules 900 and 1500 μm in diameter—in a biosorption process applied to aqueous solutions containing the reactive dye Brilliant Red HE-3B (16.88–174.08 mg/L), studied in a batch system. The preparation and characterization of the obtained polymeric composites (pHPZC, SEM, EDS and FTIR spectra) and an analysis of different equilibrium isotherms (Langmuir, Freundlich and Dubinin-Radushkevich—D–R) were investigated in order to estimate the quantitative characteristic parameters of the biosorption process, its thermal effects, and its possible mechanisms of action. The modelling of the experimental data led to the conclusion that the studied biosorption process took place after reaching the Langmuir isotherm (LI), and that the main mechanism was possibly physical, being spontaneous and probably exothermic according to the values obtained for the free energy of biosorption (E = 8.45–13.608 kJ/mol, from the DR equation), as well as the negative values for the Gibbs free energy and the enthalpy of biosorption (ΔH0 = −87.795 kJ/mol). The results obtained lead to the conclusion that encapsulation of this residual microbial biomass in sodium alginate leads to an easier-to-handle form of biomass, thus being an efficient biosorbent for static or dynamic operating systems for effluents containing moderate concentrations of reactive organic dyes.
The current study deals with an examination of strategies for the sequential treatment of corn stalks (CSs) in an integrated manner aiming to obtain papermaking fibers and to recover both lignin and hemicelluloses (HCs). Several pathways of valorization were experimentally trialed, focusing on getting information from mass balance analysis in an attempt to reveal the potential outcomes in terms of pulp yield, chemical composition, and papermaking properties such as tensile and burst strength. The raw lignin amounts and purity as well as separated hemicelluloses were also characterized. In this work, pulp yields in the range of 44–50% were obtained from CSs, while lignin and hemicelluloses yielded maximum values of 10 g/100 g of CS and 6.2 g/100 g of CS, respectively. Other findings of mass balance analysis evidenced that besides the papermaking pulp, the lignin and HCs also have interesting output values. The recovered lignin yield values were shown to be less than 50% in general, meaning that even if 67 to 90% of it is removed from CSs, only about half is recovered. The removal rates of hemicelluloses were found to be in the range of approx. 30 to 60%. About 15 to 25% of the original HCs could be recovered, and polysaccharides-based products with 67 to 75% xylan content could be obtained. Some key opinions were developed regarding how the mass balance could turn as a result of the chosen CS valorization set-up. The determined antioxidant activity showed that both lignin and hemicelluloses had interesting values for IC50.
The present study deals with the valorization of corn stalks in an integrated processing strategy targeting two products: extracted hemicelluloses (HC) and papermaking fibers. Preliminary trials were conducted to assess the individual or the combined effects of biomass treatment on the quality of the obtained hemicelluloses and papermaking fibers. Depending on the hot alkaline extraction (HAE) conditions, the extracted HC had a xylan content between 44–63%. The xylan removal yield ranged between 19–35%. The recovery of HC from the extraction liquor and final black liquor was significantly affected by process conditions. The experimental approach continued with the study of HAE conditions on the obtained paper’s mechanical properties. The optimization approach considered conserving paper strength properties while achieving an equilibrium with the highest possible HC extraction yield. The optimal values are sodium hydroxide concentration (1%), process time (33 min), and temperature (100 °C). The xylan content in the separated HC sample was ~55%. An extended extraction of HC from the resulting pulp under hot alkaline conditions with 5% NaOH was performed to prove the HC influence on paper strength. The xylan content in HC samples was 65%. The consequence of xylan content reduction in pulp leads to 30–50% mechanical strength loss.