Structure Of Microcrystalline Cellulose Research Articles

Ultrafast improvement of cellulose accessibility via non-dissolving pretreatment with LiBr·3H2O under room temperature

The development of sustainable and effective pretreatment methods to improve the accessibility of cellulose is of vital importance for its utilization. Herein, a novel high-efficiency pretreatment method based on lithium bromide trihydrate (LBTH) was established, which realized the fast improvement of cellulose accessibility under ambient conditions without dissolution of cellulose. The cellulose I structure of microcrystalline cellulose (MCC) was transformed into amorphous structure just within 5 min of LBTH pretreatment, and the crystallinity was reduced from 79.1 to 19.9%. After pretreatment for 30 min, the BET surface area of MCC increased from 2.1 to 125.9 m2/g. Particularly, the pretreated cellulose could be near-completely saccharified to glucose (98.3%) with ultra-low enzyme dosage (2.5 mg protein/g-glucan) just within 24 h, while the conversion of untreated MCC under the same conditions was only 16.7%. Additionally, this non-dissolving pretreatment is beneficial to the separation and recycling of LBTH, guaranteeing a clean and sustainable process.

Impact of Nonthermal Atmospheric Plasma on the Structure of Cellulose: Access to Soluble Branched Glucans

We have investigated the effect of non-thermal atmospheric plasma (NTAP) on the structure of microcrystalline cellulose. In particular, by means of different characterization methods, we demonstrate that NTAP promotes the partial cleavage of the β-1,4 glycosidic bond of cellulose leading to the release of short-chain cellodextrins that are reassembled in situ, preferentially at the C6 position, to form branched glucans with either a glucosyl or anhydroglucosyl terminal residue. The ramification of cellulosic chain induced by NTAP yields branched glucans that are soluble in DMSO or in water, thus opening a straightforward access to processable glucans from cellulose. Importantly, the absence of solvent and catalyst considerably facilitates downstream processing as compared to (bio)catalytic processes which typically occur in diluted conditions.

Изучение сульфатов микрокристаллической целлюлозы, полученных с использованием хлорсульфоновой и сульфаминовой кислот

Composition and structure of microcrystalline cellulose (MCC) sulfates obtained by traditional and new advanced methods of MCC sulfation were compared. Data on the composition and structure of MCC sulfates synthesized in the medium of chlorosulfonic acid –1,4-dioxane and by sulfation of MCC with sulfamic acid in the presence of urea in N,N-dimethylformamide and diglyme were obtained with the use of elemental analysis, FTIR, Raman, 13C NMR, XRD, XPS, SEM and AFM methods. It was shown that MCC sulfates synthesized by new methods have more homogeneous composition and morphology as compared to sulfates obtained by known methods.

Effect of Ball Milling on Structure of Microcrystalline Cellulose

The main objective of this work was investigate the effect of ball milling on microcrystalline cellulose (MCC) structure. FTIR results shows there are no obvious different in the function groups of between neat and ball milling MCC. Both FTIR and WAXD analysis indicate that the crystalline of MCC samples are change with the ball milling time. The WAXD results also show MCC change from typical cellulose IV to amorphous state when ball milled for 6h, and after 30h the characteristic shape ball milling transformed into cellulose II.

Castor Oil and Microcrystalline Cellulose Based Polymer Composites with High Tensile Strength

Castor oil and microcrystalline cellulose were employed as biomass feedstock to produce bio-based polymer composites with increased tensile strength. The polymer composites were prepared by curing castor oil with 4,4'-methylenebis (phenyl isocyanate) (MDI) in the presence of microcrystalline cellulose (MC) or modified MC (MMC). The MMC was prepared by reacting MDI with MC to introduce isocyanate groups to the surface of MC. X-ray diffraction spectra suggested the good retention of the crystalline structure of MC or MMC in the composites. SEM analysis showed the well dispersion of MC or MMC in the composites. All of these factors are critical to reinforcing the composites. Mechanical tests of the composites revealed that the reinforcing effect of MMC was more significant than MC at high cellulose content such that the highest tensile strengths of 4.87 MPa was obtained for the composite containing 43% (wt) of MMC. That is almost 5 times higher than that of neat castor oil-based polyurethane.

Change of the Microstructure of Microcrystalline Cellulose with Grinding and Compression

The microstructure of microcrystalline cellulose was investigated by use of a radial distribution function (RDF) based on the intensity of X-ray scattering data. Changes in the microstructure of the cellulose as a result of grinding and compression were detected by use of the RDF. The RDF of intact microcrystalline cellulose had peak maxima corresponding to distances of approximately 1.5, 2.6, 5.0, 8.2, 13.3 and 17.0 A. The first two corresponded to the intramolecular atomic distances; other peaks were attributable to the intermolecular (inter-fibre) atomic distance. Changes in the RDF as a result of grinding indicated that the regular intermolecular atomic arrangement was gradually lost. Compression resulted in formation of long-range (> 20 A) ordering of the intermolecular (inter-fibre) atomic arrangement. These results show that RDF analysis is suitable for monitoring changes in the structure of microcrystalline cellulose which occur as a result of grinding and compression.

Changes in Submicrometer Structure of Enzymatically Hydrolyzed Microcrystalline Cellulose

To understand the limitations occurring during enzymatic hydrolysis of cellulosic materials in renewable energy production, we used wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), X-ray microtomography, and transmission electron microscopy (TEM) to characterize submicrometer changes in the structure of microcrystalline cellulose (Avicel) digested with the Trichoderma reesei enzyme system. The microtomography measurements showed a clear decrease in particle size in scale of tens of micrometers. In all the TEM pictures, similar elongated and partly ramified structures were observed, independent of the hydrolysis time. The SAXS results of rewetted samples suggested a slight change in the structure in scale of 10-20 nm, whereas the WAXS results confirmed that the degree of crystallinity and the crystal sizes remained unchanged. This indicates that the enzymes act on the surface of cellulose bundles and are unable to penetrate into the nanopores of wet cellulose.

Understanding the Primary Liquid Products of Cellulose Hydrolysis in Hot-Compressed Water at Various Reaction Temperatures

Knowledge on the primary liquid products is essential to understanding the primary hydrolysis reactions that take place on the surface of microcrystalline cellulose particles during hydrolysis in hot-compressed water (HCW). This study reports the experimental results on the primary liquid products from the hydrolysis of cellulose using a semicontinuous reactor system under optimized reaction conditions. The primary liquid products contain glucose oligomers and their derivatives with a wide range of degrees of polymerization (DPs), from 1 to a maximal DP, which increases with temperature from 23 at 230 °C, to 25 at 250 °C, then to 28 at 270 °C. Temperature also has a significant influence on the distribution of glucose oligomers in the primary liquid products. The results suggest that the hydrolysis reactions proceed on the surface of reacting cellulose particles via the cleavage of the accessible glycosidic bonds within the structure of microcrystalline cellulose in a manner with randomness. Thermal degra...

Structure of cellulose and microcrystalline cellulose from various wood species, cotton and flax studied by X-ray scattering

The structure of microcrystalline cellulose (MCC) made by mild acid hydrolysis from cotton linter, flax fibres and sulphite or kraft cooked wood pulp was studied and compared with the structure of the starting materials. Crystallinities and the length and the width of the cellulose crystallites were determined by wide-angle X-ray scattering and the packing and the cross-sectional shape of the microfibrils were determined by small-angle X-ray scattering. The morphological differences were studied by scanning electron microscopy. A model for the changes in microfibrillar structure between native materials, pulp and MCC samples was proposed. The results indicated that from softwood or hardwood pulp, flax cellulose and cotton linter MCC with very similar nanostructures were obtained with small changes in reaction conditions. The crystallinity of MCC samples was 54–65%. The width and the length of the cellulose crystallites increased when MCC was made. For example, between cotton and cotton MCC the width increased from 7.1 nm to 8.8 nm and the length increased from 17.7 nm to 30.4 nm. However, the longest crystallites were found in native spruce wood (35–36 nm).

Thermophysical properties of some pharmaceutical excipients compressed in tablets.

Thermophysical properties of three tableting excipients; microcrystalline cellulose, lactose and dicalcium phosphate dihydrate were observed to evaluate their ability to resist temperature induced changes in tablet form. Two thermophysical parameters, thermal diffusivity and specific heat, were measured by a pulse heating method. The materials were also evaluated by differential scanning calorimetry (DSC). Microcrystalline cellulose in tablet form was found to be rather insensitive to heating and cooling treatments, even though the tablets seemed to remain in a stressed state four weeks after tableting. This stress, indicated by low temperature anomalies, was observed by the pulse method, but not by DSC. When magnesium stearate was incorporated as a lubricant within the microcrystalline cellulose powder, the thermophysical parameters indicated that the internal structure of the tablets changed with heating and cooling. Magnesium stearate eliminated the low temperature anomalies as well. The heat treatment changed the thermophysical properties of tablets made of the crystalline excipients lactose and dicalcium phosphate dihydrate, permanently causing irreversible structural changes. The melting of the lubricant together with enhanced stress relaxation in the structure of microcrystalline cellulose most probably caused the improved thermal diffusivity. The observed thermophysical changes with the crystalline excipients were due to changes in tablet's structure and material. The combination of methods used was found to be an accurate and reliable way to obtain useful information on the structural changes and material relaxations of intact tablets during temperature treatment and age-related changes in material properties.