CHEMICAL AND STRUCTURAL CHANGES IN POPLAR WOOD UPON STEAM TREATMENT AT CONSTANT TEMPERATURE AND PRESSURE CONDITIONS FOR DIFFERENT TIME INTERVALS

Technology advancement has helped in the development of high-throughput equipment for the analysis of raw material in paper industries. In this research, we have used some advanced techniques to analyze the pore size, structural and chemical changes, and cellulose crystallinity of poplar wood pretreated with steam at constant temperature and pressure conditions for different treatment time. Samples were analyzed by the nitrogen adsorption test, Fourier-transform infrared spectroscopy – attenuated total reflectance (FTIR–ATR), X-ray diffraction (XRD), and field scanning electron microscopy (FE-SEM). Slit-shaped pores were formed, with a diameter of 2.12 nm, after 30 minutes of treatment. FTIR results revealed the degradation of the lignin skeleton through the formation of guaiacyl and syringyl units and deformation in the cellulose and hemicelluloses structure. The crystallinity index (CI) increased upon steam treatment for up to 15 min, but after that, a drop in the CI was observed. The crystallite thickness (d200) increased after 15 min of treatment, due to the rearrangement of cellulose chains. However, a further increase in steam treatment duration to 30 min resulted in a decline of d200, followed by an increase in the cellulose II crystalline region and d020. The steam treatment duration of 15-30 min was found to be a critical time interval, which led to increases in the number of mesopores, CI, d200, and the cellulose II region in the poplar wood.

Theoretical study of cellulose II nanocrystals with different exposed facets

Derived from the most abundant natural polymer, cellulose nanocrystal materials have attracted attention in recent decades due to their chemical and mechanical properties. However, still unclear is the influence of different exposed facets of the cellulose nanocrystals on the physicochemical properties. Herein, we first designed cellulose II nanocrystals with different exposed facets, the hydroxymethyl conformations distribution, hydrogen bond (HB) analysis, as well as the relative structural stability of these models (including crystal facets {A, B, O} and Type-A models vary in size) are theoretically investigated. The results reveal that the HB network of terminal anhydroglucose depends on the adjacent chain’s contact sites in nanocrystals exposed with different facets. Compared to nanocrystals exposed with inclined facet, these exposed with flat facet tend to be the most stable. Therefore, the strategy of tuning exposed crystal facets will guide the design of novel cellulose nanocrystals with various physicochemical properties.

Crystalline structure analysis of all-cellulose nanocomposite films based on corn and wheat straws

Cellulose solution and nanocellulose were prepared from corn straw and wheat straw and then used to fabricate an all-cellulose nanocomposites film (ANF). The crystal structure (CS) of ANFs was analyzed by X-ray diffraction (XRD) and Fourier transform infrared spectrometry (FTIR). Cellulose-I and cellulose-II were found to coexist within regenerated cellulose films (RCF) and ANFs. With the change of nanocellulose content, the proportions of cellulose-I and cellulose-II changed. Cellulose transformation was found to depend on the raw material and the preparation method. When cellulose solution was prepared from corn straw that had been extracted, the cellulose type tended to be transformed from cellulose-I to cellulose-II; the proportion of cellulose-I showed a tendency to increase when nanocellulose content exceeded 1.5%. When the dissolved cellulose had been treated by an acid-alkali method, the results did not follow a clear pattern. However, when cellulose solution was prepared from wheat straw, under extraction method, the cellulose type tended to transform from cellulose-I to cellulose-II; under acid-alkali method, cellulose-I did not follow a clear pattern with nanocellulose content. Though the small amount of nanocellulose can’t dominate the content of cellulose-I, it could cause an increase in disorder of the cellulose matrix.

Terahertz Time-domain Spectroscopy as a Novel Tool for Crystallographic Analysis in Cellulose: Cellulose I to Cellulose Ii, Tracing the Structural Changes Under Chemical Treatment

Terahertz time-domain spectroscopy (THz-TDS) has expanded possibilities in cellulose crystallography research, as THz radiation detects most intermolecular vibrations and responds to the phonons of crystalline lattices. In this study, we traced the transformation of the cellulose crystalline lattice from cellulose I to cellulose II by THz-TDS and X-ray powder diffraction. Cellulose II was obtained by treating cellulose I with NaOH of different concentrations (0 wt%–20 wt%, at 2 wt% intervals). The THz absorption coefficient spectra of cellulose II showed three characteristic peaks (at 1.32 THz, 1.76 THz, and 2.77 THz). The THz absorption coefficient spectra of cellulose II treated with 20-wt% NaOH and cellulose I without NaOH treatment were fitted by a seventh-order Fourier series. Thus, the THz absorption coefficient spectra of samples treated with NaOH of other concentrations could be considered a combination of these two fitted profiles of cellulose I and cellulose II, multiplied by different coefficients. Furthermore, the coefficients could reflect the relative contents of cellulose I and cellulose II in the samples.

Enzymatic Synthesis of Cellulose in Space: Gravity Is a Crucial Factor for Building Cellulose II Gel Structure

We previously reported in vitro synthesis of highly ordered crystalline cellulose II by reverse reaction of cellodextrin phosphorylase from the cellulolytic bacterium Clostridium ( Hungateiclostridium ) thermocellum ( Ct CDP), but the formation mechanism of the cellulose crystals and highly ordered structure has long been unclear. Considering the specific density of cellulose versus water, the formation of crystalline and highly ordered structure in an aqueous solution should be affected by gravity. Thus, we synthesized cellulose with Ct CDP at the International Space Station, where sedimentation and convection due to gravity are negligible. Optical microscopic observation suggested that cellulose in space has a gel-like appearance without apparent aggregation, in contrast to cellulose synthesized on the ground. Small-angle Xray scattering (SAXS) and wide-angle X-ray scattering (WAXS) indicated that cellulose synthesized in space has a more uniform particle distribution in the ~100 nm scale region than cellulose synthesized on the ground. Scanning electron microscopy (SEM) showed that both celluloses have a micrometer scale network structure, whereas a fine fiber network was constructed only under microgravity. These results indicate that gravity plays a role in cellulose II crystal sedimentation and the building of network structure, and synthesis in space could play a role in the design of unique materials.

Extraction and Characterization of Cellulose Nanowhiskers from TEMPO Oxidized Sisal Fibers

Cellulose nanowhiskers as one kind of renewable and biocompatible nanomaterials evoke much interest because of its versatility in various applications. Herein, the sisal cellulose nanowhiskers with length of 100–500 nm, ultrathin diameter of 6–61 nm, high crystallinity of 74.74 % and C6 carboxylate groups converted from C6 primary hydroxyls were prepared via a 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)/NaBr/NaClO system selective oxidization combined with mechanical homogenization. The effects of sodium hydroxide concentration in alkali pretreatment on the final sisal cellulose nanowhiskers were explored. It was found that with the increase of sodium hydroxide concentration, the sisal fiber crystalline type would change from cellulose I to cellulose II. The versatile sisal cellulose nanowhiskers would be particularly useful for applications in the nanocomposites as reinforcing phase, as well as in tissue engineering, filtration, pharmaceutical and optical industries as additives.

Microcrystalline Cellulose Generation from Laboratory Cotton Waste and Conventional Characterizations

Microcrystalline cellulose (MCC) is a green material that has widespread applications in pharmaceuticals, food, cosmetics, and other industries owing to its biocompatibility, biodegradability, hydrophilicity, and acid-insolubility. Therefore, this study presented a simple, fast, and cost-effective approach for preparing MCC from laboratory cotton via alkaline treatment and sulfuric acid hydrolysis. Further, the synthesized cotton-based MCC was characterized using FTIR, XPS, and EDX. Based on these results, the major components were identified as carbon and oxygen. This finding was evidenced by the FTIR analysis, which displayed peak wavelength at 3446.94 cm− 1, 2891.11 cm− 1, 1649.50 cm− 1, 1380.1 cm− 1, 1061.19 cm− 1, and 1050–1150 cm− 1. The surface morphology was also examined by FESEM and FETEM, which showed that the prepared MCC has a smooth surface and a consistent, rod-like shape. In addition, the MCC exhibited the typical diffraction peaks of a crystalline structure of cellulose II at 12.2°, 20°, and 22.03°, which correspond to the diffraction planes of 1–10, 110, and 020, respectively, and had a crystallinity index of 78.7%. Moreover, the prepared MCC had a diameter of 37.80 µm and exhibited good stability with a peak at -76.51 mV. Further, the cotton-based MCC exhibited high thermal stability, as revealed by the TGA.