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.
A thermosensitive copolymer composed of amphiphilic triblock copolymer, poloxamer 407, grafted on hydrophilic pullulan with pendant carboxymethyl groups (CMP) was prepared and characterized. The structure of the new copolymer was assessed by Fourier transform infrared (FT-IR) and 1H nuclear magnetic resonance (1H NMR) spectroscopy. The content of the poloxamer in the grafted copolymer was 83.8% (w/w). The effect of the copolymer concentration on the gelation behavior was analyzed by the vertical method and rheological tests; the gel phase of the copolymer occurred at a lower concentration (11%, w/v) as compared with poloxamer (18%, w/v). The starting gelation time under the simulated physiological conditions (phosphate buffer with a pH of 7.4, at 37 °C) was sensitive on the rest temperature before the test, this being 990 s and 280 s after 24 h rest at 4 °C and 20 °C, respectively. The rheological tests evidenced a high elasticity and excellent ability of the copolymer to recover the initial structure after the removal of the applied force or external stimuli. Moreover, the hydrogel has proved a sustained release of amoxicillin (taken as a model drug) over 168 h. Taken together, the results clearly indicate that this copolymer can be used as an injectable hydrogel.
Three imine macrocycles having rhomboidal shape were synthesized in good yields by [2+2] cyclocondensation reaction between equimolar quantities of (R,R)-1,2-diaminocyclohexane and 4,4'-bisformyl triphenylamine derivatives. The macrocycles structure was assigned by electrospray ionization mass spectrometry (ESI-MS), (1)H-NMR, and elemental analysis. UV, FTIR spectroscopy, and TG measurements were also used to characterize and prove the structure of these compounds. A conformational modification arising out of the rotation of triphenylamine group around the flexible cyclohexane-N bonds was observed in solution by (1)H-NMR and UV spectroscopy for all three macrocycles.
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.
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