The effect of the time process of enzymatic hydrolysis on nanocellulose properties

2021 ◽  
Vol 115 ◽  
pp. 101-107
Author(s):  
Marta Babicka ◽  
Magdalena Wożniak ◽  
Kinga Szentner ◽  
Sławomir Borysiak ◽  
Krzysztof Dwiecki ◽  
...  
Keyword(s):  
Enzymatic Hydrolysis ◽  
Reaction Times ◽  
Raw Material ◽  
Degree Of Crystallinity ◽  
Cellulolytic Enzyme ◽  
Time Process ◽  
X Ray Diffraction ◽  
Hydrolysis Time ◽  
Xrd Patterns ◽  
Cellulose Materials

The effect of the time process of enzymatic hydrolysis on nanocellulose properties - the aim of the study was to evaluate the effect of enzymatic hydrolysis time on the properties of obtained nanocellulose. Two cellulose materials were tested as a raw material for nanocellulose production in the experiment: Avicel and Whatman. The cellulolytic enzyme obtained from the fungus Trichoderma reesei was used to carry out the enzymatic hydrolysis reaction. Enzymatic hydrolysis was performed on cellulose using the reaction times of 0.5, 1, 2 and 4 hours. In order to characterize the obtained materials, the following analyses were used: infrared spectroscopy, X-ray diffraction and dynamic light scattering. The recorded results showed that cellulose after enzymatic hydrolysis showed similar parameters (particle size, XRD patterns and degree of crystallinity) after all the applied reaction times.

Preparation of nanocellulose by hydrolysis with ionic liquids and two-step hydrolysis with ionic liquids and enzymes

2021 ◽  
Vol 116 ◽  
pp. 5-14
Author(s):  
Marta Babicka ◽  
Magdalena Woźniak ◽  
Kinga Szentner ◽  
Sławomir Borysiak ◽  
Krzysztof Dwiecki ◽  
...  
Keyword(s):  
Ionic Liquids ◽  
Degree Of Crystallinity ◽  
Cellulolytic Enzyme ◽  
X Ray Diffraction ◽  
Production Methods ◽  
Step Process ◽  
X Ray ◽  
One Step ◽  
Xrd Patterns ◽  
The One

The aim of this study was to compare parameters of nanocellulose obtained by two different procedures: hydrolysis with ionic liquids (1-allyl-3-methylimidazolium chloride and 1-ethyl-3-methylimidazolium acetate) and hydrolysis with ionic liquids in combination with hydrolysis using a cellulolytic enzyme from Trichoderma reesei. Avicel cellulose was treated with two ionic liquids: 1-allyl-3-methylimidazolium chloride (AmimCl) and 1-ethyl 3-methylimidazolium acetate (EmimOAc). In the two-step hydrolysis cellulose after treatment with ionic liquids was additionally hydrolyzed with a solution of enzymes. In order to characterize the obtained material, the following analyses were used: infrared spectroscopy, X-ray diffraction and dynamic light scattering. The results indicated that cellulose obtained by two-step nanocellulose production methods (first hydrolysis with ionic liquids and then with enzymes) showed similar parameters (particle size, XRD patterns and degree of crystallinity) as the material after the one-step process, i.e. hydrolysis with ionic liquids.

scholarly journals Characterization of Serpentines from Different Regions by Transmission Electron Microscopy, X-ray Diffraction, BET Specific Surface Area and Vibrational and Electronic Spectroscopy

Fibers ◽  
2019 ◽  
Vol 7 (5) ◽  
pp. 47 ◽  
Author(s):  
Miguel A. Rivero Crespo ◽  
Dolores Pereira Gómez ◽  
María V. Villa García ◽  
José M. Gallardo Amores ◽  
Vicente Sánchez Escribano
Keyword(s):  
Electron Microscopy ◽  
Relative Intensity ◽  
Electronic Spectroscopy ◽  
Visible Region ◽  
Band Gap Energy ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Oh Groups ◽  
X Ray ◽  
Xrd Patterns

Serpentinite powdered samples from four different regions were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), SBET and porosity measurements, UV-Vis and Infrared Spectroscopy of the skeletal region and surface OH groups. SEM micrographs of the samples showed a prismatic morphology when the lizardite was the predominant phase, while if antigorite phase prevailed, the particles had a globular morphology. The few fibrous-shaped particles, only observed by SEM and weakly detected by XRD on MO-9C and MO13 samples, were characteristic of the chrysotile phase. All diffraction XRD patterns showed characteristic peaks of antigorite and lizardite serpentine phases, with crystallite sizes in the range 310–250 Å and with different degrees and types of carbonation processes, one derived from the transformation of the serpentine, generating dolomite, and another by direct precipitation of calcite. The SBET reached values between 38–24 m2∙g−1 for the samples less crystalline, in agreement with the XRD patterns, while those with a higher degree of crystallinity gave values close to 8–9 m2∙g−1. In the UV region all electronic spectra were dominated by the absorption edge due to O2− → Si4+ charge transfer transition, with Si4+ in tetrahedral coordination, corresponding to a band gap energy of ca 4.7 eV. In the visible region, 800–350 nm, the spectra of all samples, except Donai, presented at least two weak and broad absorptions centred in the range 650–800 and 550–360 nm, associated with the presence of Fe3+ ions from the oxidation of structural Fe2+ ions in the serpentinites ((MgxFe2+1−x)3Si2O5(OH)4). The relative intensity of the IR bands corresponding to the stretching modes of the OH’s groups indicated the prevalence of one of the two phases, antigorite or lizardite, in the serpentinites. We proposed that the different relative intensity of these bands could be considered as diagnostic to differentiate the predominance of these phases in serpentinites.

Phase formation and composition of Mn–Zn ferrite powders prepared by hydrothermal method

1999 ◽  
Vol 14 (1) ◽  
pp. 204-208 ◽  
Author(s):  
Wen-Hao Lin ◽  
Shiuh-Ke Jang Jean ◽  
Chii-Shyang Hwang
Keyword(s):  
Inductively Coupled Plasma ◽  
Hydrothermal Process ◽  
Ammonium Hydroxide ◽  
Significant Loss ◽  
Degree Of Crystallinity ◽  
Hydrothermal Time ◽  
X Ray Diffraction ◽  
Inductively Coupled ◽  
Zn Ferrite ◽  
Xrd Patterns

Mn–Zn ferrite powders were prepared by hydrothermally aging the coprecipitates of compositional metal ions using ammonium hydroxide as a precipitant. R value (alkalinity) = (moles of added OH−)/[(moles of added Zn2+) × 2 + (moles of added Mn2+) × 2 + (moles of added Fe3+) × 3] was introduced to adjust the amount of added ammonia. The results show that the R value of starting suspension and hydrothermal time have similar and dominant effects on the composition, spinel ratio, and crystallite size of synthesized powders. From the analyses of x-ray diffraction (XRD) and inductively-coupled plasma (ICP), it notes that no α–Fe2O3 peak in the XRD patterns of powders synthesized at R = 2–3, 150 °C × 2 h, may be due to lower degree of crystallinity and less amount of α–Fe2O3 existing in these powders. Both the increase of hydrothermal time and of R value can promote the crystallinity of powders and also cause a significant loss of zinc, hinting that in the hydrothermal process, the loss of zinc may play a crucial role in the crystallinity of hydrothermally synthesized powders.

Geopolymer Obtention Using Calcined Rice Husk Ash

2016 ◽  
Vol 881 ◽  
pp. 373-378
Author(s):  
Carlos Eduardo Pereira ◽  
André Miranda da Silva ◽  
Josiele Souza Batista Santos ◽  
Bianca Viana de Sousa
Keyword(s):  
Rice Husk ◽  
Bending Strength ◽  
Raw Material ◽  
Molar Ratio ◽  
Rice Hull ◽  
X Ray Diffraction ◽  
Rice Hull Ash ◽  
Hydrated Calcium Silicate ◽  
Irregular Shapes ◽  
Xrd Patterns

This study aimed to synthesize geopolymer materials using the ash of burned rice husk. The material was prepared from bauxite slurry, rice hull ash was calcined at 600 °C, metakaolin and sodium hydroxide 12 M solution. The material was cured at 60 °C for 6 h and then at ambient temperature for up to 28 days. We used the same mixture of experimental design to synthesize geopolymer. Through techniques spectroscopy energy dispersive X rivers and X-ray diffraction, it appears that the silica and alumina contents of the identified raw material meets the conditions laid down as minimum for precursors with geopolymer activation potential, as evidenced by the molar ratio Si/Al sample. Geopolymer obtained from the XRD patterns showed characteristic peaks of hydrated calcium silicate. It was found that the particles had irregular shapes and sizes, and the presence of voids affecting the strength of the material. The geopolymeric material obtained showed improvements in the bending strength in a curing time of 28 days.

scholarly journals Effect of the acetylation process on native starches of yam (Dioscorea spp.)

2016 ◽  
Vol 69 (2) ◽  
pp. 7997-8006 ◽  
Author(s):  
Jairo Salcedo Mendoza ◽  
Jorge Hernández RuyDiaz ◽  
Alfredo Fernández Quintero
Keyword(s):  
Structural Changes ◽  
Raw Materials ◽  
Amylose Content ◽  
Reaction Times ◽  
Absorption Capacity ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Modified Starches ◽  
Granule Morphology ◽  
Low Degrees

In Colombia, it is necessary to produce native and modified starches for the use of amylaceous raw materials of major socioeconomic importance. In this study, the effects of the acetylation process on structural, morphological and functional properties of native starches yam, Dioscorea spp. (D. alata and D. rotundata) were evaluated. Chemical modification by esterification with acetic anhydride was performed at different reaction times, and morphological and structural changes were assessed using the following techniques: infrared spectroscopy (FTIR), X-ray diffraction and scanning electron microscopy (SEM). Acetylation produced slight changes in the granule morphology, and a decreased degree of crystallinity (DC) associated with a slight increase in the amylose content was observed. The introduction of acetyl groups into the starch structure caused a decrease in the gelatinization temperature and an increased retro gradation tendency. The acetylated starches had low degrees of substitution (DS<0.2), meaning they can be used in the food industry, considering that they showed greater stability, greater water absorption capacity and better solubility than native starches.

scholarly journals Extraction and characterization of Nanocellulose obtained from sugarcane bagasse as agro-waste

2016 ◽  
Vol 12 (3) ◽  
pp. 4256-4264 ◽  
Author(s):  
Mohammed B Ghazy ◽  
Farag A Esmail ◽  
Waleed K El-Zawawy ◽  
Mariam. A Al-Maadeed ◽  
Medhat E Owda
Keyword(s):  
Electron Microscopy ◽  
Sugarcane Bagasse ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Hydrolysis Time ◽  
Amorphous Cellulose ◽  
Cellulose Whiskers ◽  
Cellulose Nanowhisker ◽  
Transmission Electron ◽  
Ft Ir

This study aimed to characterize nanocellulose extracted from sugarcane bagasse (SCB) by acid hydrolysis 60% (w/w) H2SO4 at 45 ◦C. The effect of hydrolysis time (20, 30 and 40 min) on the structure and properties of the nanofibers was investigated. Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD) results indicated that the hemicellulose and lignin were removed extensively in the cellulose whiskers. The morphology and dimensions of the fibers and acid-released cellulose nanowhisker (CNW) were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results showed that SCB could be used as source to obtain cellulose whiskers and they had needle-like structures. Longer hydrolysis time produced a lower yield of nanofibers; whereas the degree of crystallinity increased from 38.22% to 65.37% with increasing hydrolysis time due to removal of amorphous cellulose.

Characterization of Amylose-lipid Complexes Derived from Different Wheat Varieties and their Susceptibility to Enzymatic Hydrolysis

2008 ◽  
Vol 14 (1) ◽  
pp. 29-37 ◽  
Author(s):  
I. Kwaśniewska-Karolak ◽  
E. Nebesny ◽  
J. Rosicka-Kaczmarek
Keyword(s):  
Enzymatic Hydrolysis ◽  
Polymorphic Form ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Lipid Complex ◽  
Wheat Varieties ◽  
Reversible Dissociation ◽  
Starch Gel ◽  
Considerable Degradation

Starches from eight wheat varieties were analyzed for contents of dry matter, protein, pentosans, apparent and total amylose, total lipids, starch lipids, phosphorus, lysophospholipids and amylose-lipid complex (AML). Processes of starch gelatinization, reversible dissociation of AMLs and its susceptibility to degradation by α-amylase were monitored by differential scanning calorimetry (DSC). Degree of crystallinity of starches were evaluated based on X-ray diffraction pattern. Starches from different wheat varieties show some slight differences in terms of chemical composition, thermal properties and susceptibility to enzymatic hydrolysis. Endotherms and exotherms of most starch samples obtained by DSC contained single peaks, which indicated that AML complexes existed in one polymorphic form. Only AMLs formed by amylose from Symfonia cultivar was reflected by the double-peak exotherm on cooling of starch gel. Our studies showed that there was no correlation between AML content and enthalpy of its degradation in native starch. During enzymatic hydrolysis of starch AML complex in all examined starches underwent considerable degradation. Enthalpies of dissociation of AMLs, which remained after amylolysis were significantly lowered (80—90%) as compared to that of undigested starch. The susceptibility of AMLs to degradation by α-amylase did not depend on its amount (based on calculation from LPLs), but probably on its structure.

scholarly journals Investigation of Thermal Behavior of Layered Double Hydroxides Intercalated with Carboxymethylcellulose Aiming Bio-Carbon Based Nanocomposites

2019 ◽  
Vol 3 (2) ◽  
pp. 55
Author(s):  
Vagner R. Magri ◽  
Alfredo Duarte ◽  
Gustavo F. Perotti ◽  
Vera R.L. Constantino
Keyword(s):  
Layered Double Hydroxides ◽  
Mixed Oxides ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Experimental Conditions ◽  
X Ray ◽  
Vibrational Spectroscopies ◽  
Xrd Patterns ◽  
Double Hydroxides ◽  
The Degree Of Crystallinity

Carboxymethylcellulose (CMC), a polymer derived from biomass, was intercalated into layered double hydroxides (LDH) composed by M2+/Al3+ (M2Al-CMC, M = Mg or Zn) and evaluated as precursors for the preparation of biocarbon-based nanocomposites by pyrolysis. M2Al-CMC hybrids were obtained by coprecipitation and characterized by X ray diffraction (XRD), vibrational spectroscopies, chemical analysis, and thermal analysis coupled to mass spectrometry. Following, pyrolyzed materials obtained between 500–1000 °C were characterized by XRD, Raman spectroscopy, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Above 600 °C, Raman spectra of all samples showed the presence of graphitic carbon, which plays a role in the degree of crystallinity of produced inorganic phases (for comparison purposes, M2Al-CO3 materials were investigated after calcination in the same experimental conditions). XRD patterns of Mg2Al-CMC pyrolyzed between 600–1000 °C showed poorly crystallized MgO and absence of spinel reflections, whereas for Zn2Al-CMC, it was observed well crystallized nanometric ZnO at 800 °C, and ZnAl2O4 and γ-Al2O3 phases at 1000 °C. Above 800 °C, the carbothermic reaction was noticed, transforming ZnO to zinc vapour. This study opens perspectives for nanocomposites preparation based on carbon and inorganic (mixed) oxides through precursors having organic-inorganic interactions at the nanoscale domain.

scholarly journals Performance Evaluation and Microstructure Characterization of Metakaolin-Based Geopolymer Containing Oil Palm Ash

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Abideng Hawa ◽  
Danupon Tonnayopas ◽  
Woraphot Prachasaree
Keyword(s):  
Compressive Strength ◽  
Oil Palm ◽  
Raw Materials ◽  
Drying Shrinkage ◽  
Raw Material ◽  
X Ray Diffraction ◽  
Molar Ratios ◽  
Heat Curing ◽  
Oil Palm Ash ◽  
Xrd Patterns

This study reports on the microstructure, compressive strength, and drying shrinkage of metakaolin (MK) based geopolymers produced by partially replacing MK by oil palm ash (OPA). The OPA was used as raw material producing different molar ratios of SiO2/Al2O3and CaO/SiO2. The geopolymer samples were cured at 80°C for 1, 2, or 4 hours and kept at ambient temperature until testing. The compressive strength was measured after 2, 6, and 24 hours and 7 and 28 days. The testing results revealed that the geopolymer with 5% OPA (SiO2 : Al2O3 = 2.88 : 1) gave the highest compressive strength. Scanning electron microscopy (SEM) indicated that the 5% OPA sample had a dense-compact matrix and less unreacted raw materials which contributed to the higher compressive strength. In the X-ray diffraction (XRD) patterns, the change of the crystalline phase after heat curing for 4 hours was easily detectable compared to the samples subjected to a shorter period of heat curing.

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