scholarly journals Spanish Poplar Biomass as a Precursor for Nanocellulose Extraction

2021 ◽  
Vol 11 (15) ◽  
pp. 6863
Author(s):  
Sherif Mehanny ◽  
Ehab E. Abu-El Magd ◽  
Simona Sorbara ◽  
Jorge Navarro ◽  
Rodrigo Gil-San-Millan
Keyword(s):  
Aspect Ratio ◽  
Microcrystalline Cellulose ◽  
Crystallinity Index ◽  
Drastic Change ◽  
Raw Material ◽  
Acidic Hydrolysis ◽  
Characterization Techniques ◽  
Crystal Whisker ◽  
Fiber Treatment ◽  
Future Work

The effect of acidic hydrolysis duration on nanocellulose size, morphology, and proper ties was investigated, which opens up a whole new horizon of versatility in poplar applications. This study aimed to examine Spanish poplar wastes as raw material to extract crystalline nanocellulose (CNC), which substantiates the importance of poplar wastes. Wastes were pulped using 1 L of 10% NaOH (wt./wt.) solution, and bleached several times by NaClO2; afterwards, white wastes were subjected to acidic hydrolysis by 60% H2SO4 for either 5, 10, or 15 min. Microcrystalline cellulose (MCC) underwent a similar hydrolysis protocol as poplar as control. TEM, IR, and XRD characterization techniques were performed. Poplar based nanocellulose sized 219 nm length and 69 nm width after 15 min acidic hydrolysis. MCC yielded 122 nm length and 12 nm width crystals after 10 min acidic hydrolysis. Hydrolysis resulted in a drastic change and intense peaks at 3500 and 2900 cm−1 for nanocellulose. Although pre-hydrolysis fiber treatment was not influencial on the crystallinity of poplar, acidic hydrolysis remarkably raised the crystallinity index (CI) by 7–8%. The more hydrolysis duration was prolonged, the size of the resulting crystal (whisker) decreased, and the aspect ratio increased. Hydrolysis was more impactful on MCC than poplar. However, for future work, it seems that longer duration of pulping and bleaching could have significantly removed unwanted components (hemicellulose and lignin), showcased in IR and XRD, and hence smoothened the following hydrolysis.

scholarly journals Investigating microcrystalline cellulose crystallinity using Raman spectroscopy

Cellulose ◽  
2021 ◽  
Author(s):  
Ana Luiza P. Queiroz ◽  
Brian M. Kerins ◽  
Jayprakash Yadav ◽  
Fatma Farag ◽  
Waleed Faisal ◽  
...  
Keyword(s):  
Raman Spectra ◽  
Microcrystalline Cellulose ◽  
Web Application ◽  
Principal Component ◽  
Raw Material ◽  
Least Squares Regression ◽  
Analysis Model ◽  
General Reference ◽  
Material Source ◽  
Univariate Model

AbstractMicrocrystalline cellulose (MCC) is a semi-crystalline material with inherent variable crystallinity due to raw material source and variable manufacturing conditions. MCC crystallinity variability can result in downstream process variability. The aim of this study was to develop models to determine MCC crystallinity index (%CI) from Raman spectra of 30 commercial batches using Raman probes with spot sizes of 100 µm (MR probe) and 6 mm (PhAT probe). A principal component analysis model separated Raman spectra of the same samples captured using the different probes. The %CI was determined using a previously reported univariate model based on the ratio of the peaks at 380 and 1096 cm−1. The univariate model was adjusted for each probe. The %CI was also predicted from spectral data from each probe using partial least squares regression models (where Raman spectra and univariate %CI were the dependent and independent variables, respectively). Both models showed adequate predictive power. For these models a general reference amorphous spectrum was proposed for each instrument. The development of the PLS model substantially reduced the analysis time as it eliminates the need for spectral deconvolution. A web application containing all the models was developed. Graphic abstract

The Effect of Different Methods to Pretreat Reed Pulp on the Crystallinity of Microcrystalline Cellulose

2014 ◽  
Vol 1056 ◽  
pp. 12-15 ◽  
Author(s):  
Wen Long Zhang ◽  
Wen Long Zhao ◽  
Ya Jie Dai
Keyword(s):  
Crystallite Size ◽  
Microcrystalline Cellulose ◽  
Average Crystallite Size ◽  
Comprehensive Analysis ◽  
Raw Material ◽  
Type I ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimethyl Acetamide ◽  
Crystal Type

Reed Pulp was Raw Material that Pretreated by Four Methods {ultrasonic, Microwave, N, N-Dimethyl Acetamide (DMAc) and Tetrahydrofuran (THF)}. Reed Microcrystalline Cellulose (MCC) was Prepared by the Dilute Hydrochloric Acid Hydrolysis from Pretreated Reed Pulp. the Influences of Pretreatment Methods on Crystalline Type, Crystallinity and Crystallite Size of MCC were Investigated by X-Ray Diffraction (XRD). the Results Showed that the Crystallinity of MCC with Four Pretreatment Methods was 68.45%, 62.28%, 63.21% and 69.56%, Respectively. the Average Crystallite Size of MCC Prepared by Hydrolysis after Pretreated by Dmac was the Largest. whereas, the Crystal Type of MCC was Not Changed, it was still the Cellulose Type I. Comprehensive Analysis Indicated that the Effects of MCC Prepared by Hydrolysis after Pretreated by Ultrasonic were the Best.

Characterization of Several Microcrystalline Cellulose (MCC)-Based Agricultural Wastes via X-Ray Diffraction Method

2018 ◽  
Vol 280 ◽  
pp. 340-345 ◽  
Author(s):  
Muhammad Hanif Sainorudin ◽  
Masita Mohammad ◽  
Nurul Huda Abd Kadir ◽  
Nur Athirah Abdullah ◽  
Zahira Yaakob
Keyword(s):  
Sugarcane Bagasse ◽  
Microcrystalline Cellulose ◽  
Value Added ◽  
Crystallinity Index ◽  
Agricultural Wastes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coconut Coir ◽  
Pineapple Leaves ◽  
Banana Stem

In this study, microcrystalline cellulose (MCC) was extracted from various types of local agricultural wastes. Four types of agricultural waste such as coconut coir, banana stem, sugarcane bagasse and pineapple leaves were collected, extracted and hydrolyzed into microcrystalline cellulose, using pre-treatment (alkaline and bleaching) and acid hydrolysis, respectively. The extracted MCC were analyzed and compared with those of commercially available MCC. The study of crystallinity behaviors of the obtained MCC was performed by X-Ray Diffraction (XRD) analysis. The XRD of MCC revealed that the crystallinity of pineapple leaves has the highest crystallinity index with 75% in value and closest compared to commercial MCC, 81.25%. The value of crystallinity index for banana stem is 74.55% followed by coconut coir, 72.73% and sugarcane bagasse, 66.50%. All of the MCC samples showed the similar pattern with the typical crystalline structure of cellulose I. The crystallite size of all MCC samples was calculated and found in the range of 4.04 – 5.14 nm. These extracted MCC that obtained from several agricultural wastes was supposed to have a high potential as value-added products in industrial applications.

Microwave-Driven Sugar Beet Pulp Liquefaction in Polyhydric Alcohols

2017 ◽  
Vol 13 (7) ◽  
Author(s):  
Zhao-Qi Zheng ◽  
Yi Liu ◽  
Dong Li ◽  
Li‐jun Wang ◽  
Benu Adhikari ◽  
...  
Keyword(s):  
Particle Size ◽  
Sugar Beet ◽  
Crystallinity Index ◽  
Sugar Beet Pulp ◽  
Raw Material ◽  
Crystalline Cellulose ◽  
Limiting Factor ◽  
Heating Source ◽  
Beet Pulp ◽  
Liquefaction Process

Abstract Liquefaction of sugar beet pulp (SBP) was carried out using microwave irradiation as the heating source, ethylene glycol/glycerol at a ratio of 80/20 (w/w) as the liquefaction solvent and sulfuric acid as the catalyst at 160 °C. The effects of different liquefaction conditions, including two particle size ranges of SBP, liquefying solvent-to-SBP solids (LS/S) ratio and reaction time on the liquefaction yield, viscosity of the liquefaction products, chemical characteristics and morphology of residues were studied using viscometry, Fourier transform infrared (FTIR), X-ray diffraction (XRD), scanning electronic microscopy (SEM). The efficiency of liquefaction of SBP was found to depend on its particle size of SBP raw material and the LS/S ratio. The smaller SBP particles improved liquefaction efficiency and reduced the amount of solvent required. The crystallinity index of liquefaction residues indicated that crystalline cellulose was no longer the rate limiting factor of liquefaction process when the particle size of SBP was small (75–177 μm). A rugged and deformed surface of the liquefaction residue (observed through SEM) indicated that severe damage in the native fiber structure occurred during the liquefaction.

scholarly journals Cellulose Nanocrystals Obtained From Microcrystalline Cellulose by p-toluene Sulfonic Acid Hydrolysis, NaOH and Ethylenediamine Treatment

2021 ◽  
Author(s):  
Songlin Wang ◽  
Qian Wang ◽  
Yao Kai
Keyword(s):  
Microcrystalline Cellulose ◽  
Cellulose Nanocrystals ◽  
Sulfonic Acid ◽  
Crystallinity Index ◽  
X Ray Diffraction ◽  
Cellulose I ◽  
Good Thermal Stability ◽  
Transmission Electron ◽  
Toluene Sulfonic Acid ◽  
Comprehensive Characterization

Abstract Cellulose nanocrystals (CNC) were first isolated from microcrystalline cellulose (MCC) by p-toluene sulfonic acid (p-TsOH) hydrolysis. Cellulose II nanocrystal (CNC II) and cellulose III nanocrystal (CNC III) were then formed by swelling the obtained cellulose I nanocrystal (CNC I) in concentrated sodium hydroxide solutions and ethylenediamine (EDA) respectively. The properties of CNC I, CNC II and CNC III were subjected to comprehensive characterization by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). The results indicated that CNC I, CNC II and CNC III obtained in this research had high crystallinity index and good thermal stability. The degradation temperatures of the resulted CNC I, CNC II and CNC III were 300 ℃, 275 ℃ and 242 ℃, respectively. No ester bonds were found in the resulted CNC. CNC prepared in this research also had large aspect ratio and high negative zeta potential.

scholarly journals Catalytic Performance of Sulfonated Carbon Catalysts for Hydrolysis of Palm Oil Empty Fruit Bunch

2020 ◽  
Vol 23 (6) ◽  
pp. 209-215
Author(s):  
Anis Kristiani ◽  
Kiky Corneliasari Sembiring ◽  
Yosi Aristiawan ◽  
Fauzan Aulia ◽  
Luthfiana Nurul Hidayati ◽  
...  
Keyword(s):  
Ionic Liquid ◽  
Lignocellulosic Biomass ◽  
Palm Oil ◽  
Microcrystalline Cellulose ◽  
Ambient Pressure ◽  
Raw Material ◽  
Empty Fruit Bunch ◽  
Fermentable Sugar ◽  
Carbon Catalysts ◽  
Hydrolysis Of

Utilizing lignocellulosic biomass into valuable products, such as chemicals and fuels, has attracted global interest. One of lignocellulosic biomass, palm oil empty fruit bunch (EFB), has major content of cellulose (30-40%), which is highly potential to be a raw material for fermentable sugar production. In this research, a series of sulfonated carbon catalysts with various concentrations of sulfuric acid (H2SO4, 10-30 v/v%) solutions have been successfully prepared and applied for a single stage of heterogeneous acid-catalyzed hydrolysis over microcrystalline cellulose and EFB under moderate temperature condition and ambient pressure. The catalysts’ physical and chemical properties were characterized by using a Thermogravimetric Analyzer (TGA), X-ray diffractometer, surface area analyzer, and Fourier-transform infrared spectrophotometer. The characterization results showed that sulfonated carbon had relatively similar physical properties with the parent of active carbon. The hydrolysis activity of sulfonated carbon catalysts gave various Total Reducing Sugar (TRS). The effects of sulfate loading amount in catalyst samples and various ionic liquids were investigated. The hydrolysis of pure microcrystalline cellulose powder (Avicel) using 30%-sulfonated carbon (30-SC) catalyst in 1-butyl-3-methylimidazolium chloride ([BMIM]Cl) ionic liquid at 150°C yielded the highest TRS of 16.11%. Subsequently, the catalyst of 30-SC was also tested for hydrolysis of EFB and produced the highest TRS of 40.76% in [BMIM]Cl ionic liquid at 150°C for 4 h. The obtained results highlight the potential of sulfonated carbon catalysts for hydrolysis of EFB into fermentable sugar as an intermediate product for ethanol production.

scholarly journals Isolation and Characterization of Microcrystalline Cellulose and Preparation of Nano-Crystalline Cellulose from Tropical Water Hyacinth

2018 ◽  
Vol 31 (1) ◽  
pp. 180 ◽  
Author(s):  
Mohammed H. Abdul Latif ◽  
Yasir Fathi Mahmood
Keyword(s):  
Microcrystalline Cellulose ◽  
Water Hyacinth ◽  
Crystal Size ◽  
Crystallinity Index ◽  
Crystalline Cellulose ◽  
Gravimetric Analysis ◽  
Average Crystal Size ◽  
Isolation And Characterization ◽  
Nano Crystalline ◽  
Stretching Vibration

Because of the conservation problems causes by the existence of water hyacinth (W.H) as an watery plant in water bodies of Iraq, our study aimed to make  use of (W.H) by isolation of microcrystalline cellulose, and a new method of preparation of Nano crystalline cellulose. Microcrystalline cellulose was produced using base bleaching method by sodium hypochlorite [NaOCl] to remove unorganized region of cellulose and lignin to create particles comprising of micro crystal and preparing of Nano crystalline cellulose from microcrystalline cellulose by acid hydrolysis and ultrasonic treatment. The Nano crystalline and microcrystalline cellulose characterized by AFM, FTIR, XRD and TGA. FT-IR spectra of microcrystalline cellules and Nano crystalline cellulose show peaks at (1076.28, 1058.92) cm-1 and (1118.71, 1112.93) cm-1 refer to the stretching vibration of   C–O and stretching vibration intermolecular ester bonding.         The AFM image shows that isolated microcrystalline cellulose have a diameter of (141.37 nm) and the prepared Nano crystalline have a diameter of (87.39 nm). The Thermo gravimetric analysis of cellulose showed a high decomposition temperature at (283°C) for microcrystalline cellulose and (253)°C for Nano crystalline cellulose .The thermal stability of microcrystalline cellulose was more than Nano crystalline cellulose XRD result possessed a segal crystallinity index of 92.8 % and a average crystal size of 41.7 A ° for Nano crystalline cellulose and a Segal Crystallinity Index of 86.4 % and a average crystal size of 55.3°A    of microcrystalline cellulose.   

scholarly journals Non-Acidic Method for Isolation of Microcrystalline Cellulose From Oil Palm Empty Fruit Bunch Fiber

2019 ◽  
Vol 7 (4.14) ◽  
pp. 339
Author(s):  
N. Samat ◽  
N. N. Ghazali ◽  
Z. Ahmad ◽  
F. Ali
Keyword(s):  
Thermal Stability ◽  
Microcrystalline Cellulose ◽  
Oil Palm ◽  
Milling Time ◽  
Crystallinity Index ◽  
Ammonium Persulfate ◽  
Milling Process ◽  
Degree Of Crystallinity ◽  
Empty Fruit Bunch ◽  
Oxidation Treatment

In this study, the microcrystalline cellulose (MCC) was extracted via a non-acidic method from the oil palm empty fruit bunch (EFB) cellulose. The extraction was conducted through Ammonium Persulfate (APS) oxidation treatment, which was followed by the ball milling process. The effects of varied temperature levels from APS oxidation treatment (60, 80 and 90oC) and different milling time (1, 4 hours) were investigated. APS oxidation treatment at 90oC was found to produce the most optimum results. The size of the MCC was less than 20μm and had demonstrated the highest degree of crystallinity index and thermal stability. The high crystallinity index is associated with the removal of non-cellulosic components as seen from FTIR analysis, where a decrease was observed in the characteristic peak intensity of 1735 and 1510 cm-1. The milling time had also affected the formation of MCC. Although a relatively longer milling time had produced smaller MCC with narrow size distribution, it had, however, given rise to a slight adverse effect on the crystallinity index and thermal stability.              

scholarly journals Characterization of microcrystalline cellulose from fast-growing species Artocarpus elasticus

2021 ◽  
Vol 5 (1) ◽  
pp. 1-8
Author(s):  
Sunardi Sunardi ◽  
Wiwin Tyas Istikowati ◽  
Norhidayah Norhidayah ◽  
Dahlena Ariyani ◽  
Azlan Kamari
Keyword(s):  
Hydrochloric Acid ◽  
Microcrystalline Cellulose ◽  
Crystallinity Index ◽  
Cellulosic Material ◽  
X Ray Diffraction ◽  
Cellulose I ◽  
X Ray ◽  
Artocarpus Elasticus ◽  
Fast Growing Species

Microcrystalline cellulose is an important derivative of cellulosic material obtained from wood and non-wood sources, and is used for pharmaceutical, food, cosmetics, and other industries. The aim of this study was to determine the effect of various hydrochloric acid concentrations on the characteristics of cellulose microcrystals isolated from terap wood (Artocarpus elasticus). The microcrystalline cellulose was hydrolyzed using hydrochloric acid, at concentrations of 1.5 N, 2.5 N, and 3.5 N for 15 minutes, and within a temperature range of 100-105o C. Thesamples were then analyzed for changes in color and functional groups with Fourier Transform Infrared spectroscopy (FTIR), while crystallinity index was evaluated through X-Ray Diffraction Analysis (X-RDF). The FTIR results showed similarity with commercial products, while X-Ray Diffraction confirms the highest crystallinity index in the 2.5 N of cellulose I (69.395 %) and cellulose II (82.73 %).

scholarly journals Preparation of Nanocellulose Using Ionic Liquids: 1-Propyl-3-Methylimidazolium Chloride and 1-Ethyl-3-Methylimidazolium Chloride

Molecules ◽  
2020 ◽  
Vol 25 (7) ◽  
pp. 1544 ◽  
Author(s):  
Marta Babicka ◽  
Magdalena Woźniak ◽  
Krzysztof Dwiecki ◽  
Sławomir Borysiak ◽  
Izabela Ratajczak
Keyword(s):  
Electron Microscopy ◽  
Ionic Liquids ◽  
Microcrystalline Cellulose ◽  
Crystallinity Index ◽  
X Ray Diffraction ◽  
Cellulose I ◽  
Transmission Electron ◽  
Cation Type ◽  
Particle Size And Morphology ◽  
Size And Morphology

Cellulose nanocrystals were prepared using ionic liquids (ILs), 1-ethyl-3-methylimidazolium chloride [EMIM][Cl] and 1-propyl-3-methylimidazolium chloride [PMIM][Cl], from microcrystalline cellulose. The resultant samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), dynamic light scattering (DLS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The XRD results showed that nanocellulose obtained by treatment with both ILs preserved basic cellulose I structure, but crystallinity index of samples (except for Sigmacell treated with [EMIM][Cl]) was lower in comparison to the starting microcrystalline cellulose. The DLS results indicated noticeably smaller particle sizes of prepared cellulose for material treated with [PMIM][Cl] compared to cellulose samples hydrolyzed with [EMIM][Cl], which were prone to agglomeration. The obtained nanocellulose had a rod-like structure that was confirmed by electron microscopy analyses. Moreover, the results described in this paper indicate that cation type of ILs influences particle size and morphology of cellulose after treatment with ionic liquids.

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