Extraction, Preparation and Characterization Of Cellulose Fibres and Nanocrystals from Arachis Hypogaea Peel
Fahmida Hoque Maha
Dept. of Textile Engineering
BGMEA University of Fashion and Technology
Email: [email protected]
Abstract
Cellulose is the biomass that is most easily found in plants, bacteria, and marine organisms. However, it is not found in pure conditions in nature because always bound to other materials such as lignin, hemicellulose, silica, wax, and ash. One of the objectives for this project is to extract cellulose from Arachis Hypogaea peel by stirring. Fibres were obtained by submitting the industrial Arachis Hypogaea peel to alkali (NaOH) and bleaching treatments by Sodium Chlorite(NaCl). Nanocrystals were extracted from these fibres using Hydrochloric acid hydrolysis treatment. The material obtained after each stage of the treatments was carefully characterized and its chemical composition was determined. Morphological investigation was performed using scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy showed the progressive removal of non-cellulosic constituents. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with successive treatments and use to characterize the structure of Arachis Hypogaea peel and its direct sample. The thermal stability of the Arachis Hypogaea peelfibres and cellulose nanocrystals was also investigated using thermogravimetric analysis (TGA).
1. Introduction
Cellulose is a natural, nontoxic, and biodegradable high-molecular polymer and one of the most abundant renewable natural resources on the earth and can be obtained from numerous resources, such as wood, eucalyptus, sisal, cotton, coconut fibers, and non-plant sources, including forms produced by bacteria and found in local place. Cellulose is a carbohydrate formed by both crystalline and disordered amorphous domains. Its structure is organized into fibrils, which are gridled by a matrix of lignin, extractive inorganics and hemicellulose. Thus, these components must be extracted and cellulose chains must be explicated to extract cellulose nanocrystals from plant fibers. Cellulose nanocrystals consisting of highly crystalline rod-shaped nanoparticles can be obtained through controlled acid hydrolysis of different cellulose sources [1]. In the past decade, the production and extraction of nanoscale cellulose particles have attracted adding interest from both industry and academia because of its excellent physical properties and cost-efficient feedstock. Thus, Cellulose nanocrystals can widely be applied into biomedical engineering, paper industry, cosmetic and pharmaceutical, optical and electronic engineering, and packing materials, and many other industrial fields [2]. Cellulose is a renewable feedstock with intriguing properties similar as biocompatibility and biodegradability. It’s set up to be chemically inert, displays excellent stiffness, high strength and dimensional stability, low density and fluently functionalized face chemistry [3]. cellulose can be prepared by different methods depending on the type of cellulosic material, including Alkali treatment, bleaching process & acid hydrolysis [4] [5]. Cellulose is generally set prepared via the acid hydrolysis process, which uses a strong acid like HCl, as an acid catalyst to prevent the amorphous part of the cellulose to yield particles conforming of microcrystals [6]. Acid hydrolysis has numerous advantages, including low cost, short duration, continuous process, limited quantity of consumed acid, and nano particles of fine products [7] [8].
As a result, in the present study, cellulose was prepared from laboratory waste means Aeachis hypogaea peel using three steps: alkaline treatment, bleaching process and acid hydrolysis. The peel was treated with an alkaline solvent caustic soda to remove impurities, such as hemicellulose and lignin, before acid hydrolysis and bleaching process. Then the treated peel was bleached with sodium chlorite to produce cellulose. Then, the treated peel was hydrolyzed with acid to decrease the size of the cellulose. In addition, the prepared cellulose was characterized [9]. In this study, Alkali & bleaching combined with Acid hydrolysis pretreatment were used to prepare nano fibrillated cellulose from Arachis hypogaea peel fibers. By optimizing the treatment time and concentration, cellulose with a high yield was prepared. Scanning electron microscopy (SEM), XRD, Fourier-transform infrared spectroscopy (FTIR), TGA, Moisture regain, Moisture content, Cellulose lignin and hemi-cellulose content were used to characterize and test the properties of the prepared cellulose. cellulose with different morphological and structural characteristics were used as composite materials and applied in the composite process to explore the influence of cellulose on the strength of composite [10]. Cellulose-based smart materials with the grafed stimuli responsive side polymer chains have potential applications in variousfields such as active packaging, biosensors, cancer therapy, tissue engineering, antimicrobial surfaces, separation and detection, smart clothing, and drug release system. Cellulose-based functional materials have the new coming application parts as the sensing materials, which are in line with the science of innovation and technological development trend of artificial intelligence. It has wide applications potential in biomedical fields. Obviously cellulose-based functional materials are exceptionally important for humankind.
1.1 Problem Statement
When the Arachis Hypogaea peel are thrown to the ground, they are responsible for environmental pollution because they are completely non-degradable in nature. As a result of burning, carbon monoxide gas is released from this fuel. This carbon monoxide is a threat to the environment. As per our knowledge, the cellulose extraction on Arachis Hypogaea peel have yet to be clarified clearly. If we extract cellulose from this waste material and use the cellulose obtained from it to make textile pulp, sizing agents, levelling agents, paper, medicine, and composite materials, then the environment will be saved from this serious threat.
1.2 Motivation
Although Arachis Hypogaea is a potential choice in the world applications, however, this peel has several detriments which minimize its application area. Cellulose is a natural, nontoxic, and biodegradable high-molecular polymer and one of the most abundant renewable natural resources on the earth. As per our knowledge, if we extract cellulose from this waste material, the world will be more benefit & the environment will be protected. In the following chapters, details about the cellulose extraction process and use of cellulose have been discussed. The cellulose extraction on Arachis Hypogaea peel have yet to be clarified clearly. Research on Arachis Hypogaea is still in its infancy. This research will, therefore, assist in enhancing the current understanding of the cellulose extraction from waste material.
1.3 Arachis Hypogaea peel
TheArachis Hypogaeais an annual herbaceous plant growing 30 to 50 cm (12 to 20 in) tall. As a legume, it belongs to the botanical family Fabaceae, also known as Leguminosae, and commonly known as the legume, bean, or pea family. Like most other legumes, Arachis Hypogaea harbor symbiotic nitrogen-fixing bacteria in their root nodules. Arachis Hypogaeaare similar in taste and nutritional profile to tree nuts such as walnuts and almonds, and, as a culinary Arachis Hypogaea, are often served in similar ways in Western cuisines. The botanical definition of a Arachis Hypogaea is “a fruit whose ovary wall becomes hard at maturity.” Using this criterion, the Arachis Hypogaea is not aArachis Hypogaea[11]. However, Arachis Hypogaea are usually categorized as Arachis Hypogaea for culinary purposes and in common English more generally. Arachis Hypogaea, while grown in tropical and subtropical regions around the world, are native to the Western Hemisphere. It probably originated in South America and spread to the New World as Spanish explorers discovered theArachis Hypogaea versatility. Which produces a (or another related mixture like / NaClO2 / NaClO) in water. The solution is placed in (2,2,6,6-tetramethyl-1-oxyl) is melted, while NaBr melted in H2O by adding NaClO to the oxidation mechanism as primary oxygen. The reagent will be moved to N-oxoammo- nium salt under some cases in order to catalyst for more reactions. Then, return the cata- lyst to the form of of sodium hypochlorite and sodium Bromide. In addition, compared to the nanocellulose characteristic attained these are seen in another study in a simple pH status surface hydroxyls groups are majorly moved to carboxylate groups during this in which C6 hydroxyl groups present with a higher reactivity than C2 and C3. Actually, this reaction occurs in external amorphous areas of cellulose fibres which imply negative surface nanocellulose that leaves the crystalline structure almost intact. NaCl is subsequently by-product of this process. When the Spaniards returned to Europe, Arachis Hypogaea went with them. Traders were later responsible for the spread of Arachis Hypogaea to Asia and
growing and harvesting techniques were slow and difficult until the Civil War, Demand for Arachis Hypogaea increased rapidly after the Civil War. In the late 19th century, the development of machinery for growing, harvesting and shelling Arachis Hypogaea, as well as processing techniques, contributed to the expansion of the Arachis Hypogaea industry. New 20th-century labor-saving equipment led to a rapid increase in demand for Arachis Hypogaea oil, roasted and salted Arachis Hypogaea, Arachis Hypogaea butter, and confectionery also involved in the expansion of the Arachis Hypogaea industry was research conducted by George Washington Carver at the Tuskegee Institute in Alabama in the early 20th century. Talented botanists recognized the inherent value of Arachis Hypogaea as a cash crop. Dr. Carver proposed that Arachis Hypogaea be planted as a rotation crop in the cotton-growing regions of the Southeast where the boll weevil threatened the agricultural base of the region. Dr. Carver not only contributed to changing the face of Southern farming, but he developed more than 300 uses for Arachis Hypogaea, from recipes to industrial products (American Peanut Council).
1.4 Peel
Arachis hypogaea peel have an abundant amount of natural antioxidants and a high content of dietary fiber, says new study. Even different types of roasted Arachis hypogaea peel, such as light-roasted or dark-roasted, contain these high amounts. Adding Arachis hypogaea peel to foods, such Arachis hypogaea butter, can increase its nutritious content. It has been noted that the when Arachis hypogaea are consumed with their peel, their antioxidant capacity doubles and roasting can at times actually increase this capacity.
1.5 Cellulose
Cellulose is an organic compound belonging to the category of polysaccharides. It is a polymer made up of glucose subunits. It is found in bacterial and plant cells and is abundantly present in their cell walls. Cellulose plays an important role in the structure and strength of plants. It also finds great importance in the industry. Cellulose is a specific type of molecules which is consisting of hundreds or even thousands of carbon, hydrogen and oxygen atoms. Cellulose is the kind of main substance that can be found in the walls of plant cells. It is helping plants to remain stiff and upright. Although we cannot digest cellulose, still it is important in the diet in the form of fibre. For example, cellulose is present in the ratio of 30% in a tree which can be made into paper. Actually, it is a kind of polysaccharide having the molecular formula C6H10O5)n, which is composed of glucose monomers. It is very useful in the manufacture of numerous products such as paper, textiles, pharmaceuticals, and insulation. Some other names of Cellulose are cellulose ester, fibre, paper, cellulosic, fibre. Cellulose is a made up of thousands of D-glucose subunits. The glucose subunits in cellulose are linked via beta 1-4 glycosidic bonds. Contrary to the other polysaccharides, the orientation of glucose molecules in cellulose is reversed. They have beta orientation in which the hydroxyl group of the anomeric carbon or carbon number one is directed above the plane of the glucose ring. The hydroxyl groups of the rest of the carbon atoms are directed below the plane of the ring. In order to make beta 1-4 glycosidic bonds, every alternate glucose molecule in cellulose is inverted. The hydroxyl group of carbon 1 is directed upwards, and that of carbon 4 is directed downward. Now, to make a beta 1-4 glycosidic bond, one of these molecules should be inverted so that both the hydroxyl groups come in the same plane. This is the reason for the inversion of every alternate glucose molecule in cellulose. Cellulose is an unbranched molecule. The polymeric chains of glucose are arranged in a linear pattern. Unlike starch or glycogen, these chains do not undergo any coiling, helix formation or branching. Rather, these chains are arranged parallel to each other. The hydrogen bonds are formed between these chains due to hydrogen atoms and hydroxyl groups which firmly hold the chains together. Thisresults in the formation of cellulose microfibrils that are firm and strong. Cellulose is present in plant cells in the form of cellulose microfibrils. These microfibrils together form polysaccharide or cellulose matrix. The ‘reactivity’ of cellulose can refer to its capacity to participate in diverse chemical reactions. Each anhydro-glucose unit in a cellulose polymer has three different hydroxyl groups. The hydroxyl groups at O(2) H, O(3) H and O(6) H are the main reactive groups susceptible to chemical modification When discussing reactivity of cellulose I, the accessibility of the hydroxyl groups on the surface of fibrils or fibril aggregates to the chemical reagents is a crucial factor This accessibility is limited by the compact structure of cellulose I, which is determined by the presence of highly ordered regions formed by strong hydrogen bonds.
2. Historical Background
The history of cellulose extraction is long and dates back to when people first understood how helpful plant fibers might be. Ropes, baskets, and textiles were among the many things that early humans made from plant fibers, including cellulose. To obtain cellulose fibers, they most likely manually ground, crushed, or retted plant materials. With the start of the Industrial Revolution in the 18th century, the demand for cellulose fibers saw a tremendous surge. Labor-intensive manual extraction techniques were replaced by mechanical ones. The invention of textile gear like the spinning jenny and power loom greatly helped the extraction of cellulose fibers from plants like cotton and flax. A substantial source of cellulose, the industrial manufacturing of wood pulp, began in the middle of the 19th century Initially, wood pulp was extracted chemically using alkaline solutions. Large-scale cellulose fiber production was achieved by this procedure, which also provided the foundation for the growth of the paper industry.
Cellulose is an important structural component of green plants which is, in the paper industry, used to produce paperboard and paper. For industrial use, this material is mainly sourced from wood and cotton. Between cotton and wood, cotton is better than wood. The reason for that is cotton consists of over 90% cellulose while wood consists of 40-50% cellulose.
Cellulose can be used in many fields such as papermaking, clothing, pharmaceuticals etc. Cotton, linen, and other natural fibers might be used directly or after being processed to make rayon. Microcrystalline and powdered ones are used as drug fillers and as food thickeners, emulsifiers, and stabilizers. Scientists use this natural material, too. It can be a useful substance for liquid filtration and thin-layer chromatography. Another use for it is as a building material and electrical insulator. It is used in daily household items like coffee filters, sponges, glues, eye drops, laxatives, and films. The main commercial use for cellulose is paper manufacturing, where the kraft process is used to separate it from lignin. Tissue production includes many kinds of products such as toilet papers, kitchen towels, disposable napkins, handkerchiefs, facial tissues and also kinds of AFH tissue products. The substance that gives these products softness is hardwood pulp which is made of eucalyptus and birch pulp. In addition to softness, it also provides the product with strength. Even though cotton is richer in cellulose than wood, while making pulp, wood is the preferred raw source. The most famous variant of tissue paper products is the one that includes 100% virgin pulp. Virgin pulp is made only by using cellulose which means it does not contain any recycled content and is made directly of the pulp of trees or cotton. Papers and tissue papers that are produced with virgin pulp is categorized as high-quality products.
2.1 Empirical Literature Relevant to Research
2.1.1 Pretreatment method for CNF
The purpose of employing pre-treatment methods on wood cellulose is to reduce the consumption of energy during the nano-fibrillation process [12] as shown in Figure 3. Pre-treatment also improve the fibrillation process with an enhanced productivity rate of nano fibres. The pre-treatments of cellulosic fibers improve the accessibility of hydroxyl groups, increase the inner surface, and further alter the crystallinity of the fibers leading to breakage of hydrogen bonds of cellulose [13]. It involves various hydrolysis and those are summarized here.
2.1.2 Enzyme hydrolysis
The enzymes can hydrolyse selective components. The lignocellulosic fibres consist of various organic compounds which cannot be degraded by a single enzyme. Hence, a set of enzymes is required that make the process more complex [14] The following sets of enzymes for defibrillation are A and B type cellulases which attack the crystalline part of the cellulose; C and D type cellulases that are specifically attacking the disordered structure of cellulose [15] showed the production of nanofibrillated cellulose (NFC) from bleached softwood pulp. The method incorporated mild enzymes (Cellulases C and D), followed by refining and homogenization [16].
2.1.3 Alkaline acid
The most commonly used method is alkaline–acid pre-treatment which involves the solubilisation of lignin, hemicellulose, and pectin before employing a mechanical process for the isolation of CNF [17]The alkaline-acid method comprises of three steps as follows [18]
- Alkali treatment: It involves soaking of fibers in 12–17.5 wt% of sodium hydroxide solution for 2 h which increases the surface area of the fibers and facilitates the hydrolysis
- Acid treatment: Further, treated fibers are mixed in 1 M hydrochloric acid solution at 60–80°C. This process allows the solubilisation of hemicelluloses.
- Sodium hydroxides (NaOH): Finally, the material is again treated with 2 wt% alkali solution for 2 h at 60–80°C which disintegrate the linkages between the carbohydrate and lignin. Alkaline acid pre-treatment is an efficient method that tends to improve cellulose yield from 43 to 84% [19]
2.1.4 Mechanical Process
The defibrillation of cellulosic materials through mechanical process requires pre-treatment processing to facilitate the process in an efficient manner [20] Numerous mechanical processes are available for converting cellulose to nanocelluloses which are as follows [21]
2.1.5 High-Pressure Homogenization
HPH is an effective method for the fibrillation of cellulosic fibers to prepare CNF. HPH is a simple process and does not involve the utilization of any organic solvents.[22] In this process, the pulp of cellulose is passed through a nozzle with high pressure (50–2000 MPa) which generates the shear rate in the stream and facilitates the reduction in the size of the fibres.[23] The cellulose fibres reduction can be achieved through large pressure drops, high shear forces, turbulent flow and interparticle collision. The extent of pressure applied and the number of homogenization cycles play a critical role in cellulose fibrillation. Habibi et al. performed homogenization of cellulosic material such as cotton, sugar beet and mangosteen rind at 50 MPa at a temperature below 95°C with 15 cycles of homogenization (Habibi et al., 2010). There are some drawbacks associated with HPH such as fiber clogging and high energy consumption to overcome such problems pulp can be subjected to chemical purification or pre-treatment. Also, excessive mechanical damage occurred in the crystalline structure of CNF.[24]
2.1.6 Microfluidization
Microfluidizers work on the same principle of HPH in the production of nanocellulose fibers. In contrast to the homogenizer which operates at constant pressure, the microfluidizer function at constant shear rate. It involves an intensifier pump which enhances the pressure whereas the interaction chamber generates the shear and impact forces against the colliding particles to defibrillate the fibres as depicted in Figure 5 [25] demonstrated that the aspect ratio of cellulose fiber was increased after 10–15 passing cycles whereas additional 20 cycles may cause agglomeration of CNFs due to the higher surface area [26]
2.1.7 Grinding
Grinding is another process of breaking the cellulose to nano-form. The pulp is passed through a couple of stones, in which one stone is fixed and the other stone rotates which provides the shear force to break down the hydrogen bond of the fibres[27][28] utilized the commercial stone grinder to generate the nanocellulose fibrils from the bleached pulp of eucalyptus. Scientists studied the relation between energy consumption and fibrillation time of the fibres as a function of crystallinity. The friction between the stones generates heat which leads to the evaporation of water content and increases the solid content.
2.1.8 Cryocrushing
Another mechanical method is cryocrushing in which fibers are soaked in water and cellulose absorbs water in its cavity. The water-soaked cellulose is then immersed in liquid nitrogen that rapidly solidifies the water content of the cellulose, and is subsequently crushed by mortar and pestle [29][30] investigated the HPH and cryocrushing processes together to develop nanofibers from soybean stock and reported that the diameter of nanofibers lies in the range of 50–100 nm after examine through transmission electron microscopy (TEM).
2.1.9 Steam Explosion
Ana Lorenzo-Hernando, Judit Martín-Juárez, Silvia Bolado-Rodríguez investigated the steam explosion pretreatment and preservation methods of commercial cellulose. Steam explosion experiments were conducted in a 5 L stainless-steel reactor, connected on top to a steam generator. Reactor bottom discharged through an electro-valve to a flash vessel partially open to the atmosphere. The reactor was loaded with 50.0 g of cellulose, tightly closed and filled with saturated steam at the desired temperature and pressure. After reaching experimental conditions (this period was called “demand time”, td), a countdown for the defined “reaction time” (tSE) started. Once it finished, the bottom electrovalve automatically opened, discharging the reactor content into the flash vessel. A set of four experiments was conducted for each sample, combination of two reaction temperatures (150 or 200°C) and two reaction times (5 or 30 min). Resulting pretreated cellulose was vacuum-filtrated in a Buchner funnel to eliminate excess water, weighed and stored in plastic flasks at 4°C before analysis. Samples of pretreatment liquid fraction were also stored for chemical analysis to determine possible solubilization and degradation due to pretreatment. The aim of this work was to study steam explosion as a pretreatment for commercial cellulose samples presented in two different handlings, to explore the possibilities of this treatment as a substitute for other mechanical pretreatments and its effects on the modification of several physicochemical properties of cellulose fibers regarding a future use. To that end, several analyses were performed such as chemical composition, particle size distribution, crystallinity rate, limiting viscosity number and degree of polymerization. In addition, two different preservation methods of pretreated samples (acetone washing and freezing) were tested to study the effects of preservation methods could have on the stability and quality of pretreated samples. [31]
2.1.10 Ball Milling Process and Chemical Hydrolysis
PatchiyaPhanthong, GuoqingGuan, Yufei Ma1, Xiaogang Hao, AbulitiAbudula investigation that effects of ball milling on the production of nanocellulose using mild acid hydrolysis method. Cellulose materials were ball-milled with an ITO LP-1 Planetary pot mill. 80 mL of jar with the three different diameters of zirconia ball (10, 5, and 2 mm) was used, in which the ball to material weight ratio (BMR) was 12:1 and the weight ratio of the balls with 10, 5 and 2 mm diameters was 5:4:3. In the preliminary experiments, it is found that high rotation speed resulted in very low nanocellulose yield. Thus, in this study, a relative low rotation speed of 300 rpm was selected. The ball milling was carried out for 0.5, 1, 2, and 3 h at room temperature in order to investigate the effect of ball milling time. The pretreated cellulose materials are defined as Ball-milled Cellulose Paper (BMCPPx3 ) or Ball-milled Cellulose Powder (BMCPDx4 ) corresponds to the type of material, while x is the ball milling pretreatment time (x = 0.5, 1, 2, or 3 h). Nanocellulose was extracted from two kinds of general cellulose feedstocks, i.e., cellulose paper and cellulose powder, by coupling planetary dry ball milling with mild acid hydrolysis. The effect of ball milling time on the yield and properties of nanocellulose obtained by mild hydrolysis in lower concentration (47 wt%) of sulfuric acid was investigated in details. The obtained nanocellulose was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). It is found that the crystallinity and crystal size of ball-milled cellulose decreased with the increase of ball milling time, and the mild acid hydrolysis of the ball-milled cellulose resulted in the crystallinity and thermal stability of nanocellulose at the high temperature range increased but without any changes of chemical structure. It indicates that the appropriate ball-milling of cellulose feedstock could be benefit for the mild hydrolysis process for the production of high quality nanocellulose with high yield. Acid hydrolysis was performed by using a low concentration of sulfuric acid aqueous solution (47 wt%). 8.8 mL of acid/1 g of cellulose materials was used in each case. The reaction temperature was controlled at 45 °C with a water bath and the mixing speed was set at 600 rpm The reaction time is fixed at 90 minutes. The sulfuric acid hydrolysis was stopped by adding 10-fold cold distilled water (4 °C). The suspension was centrifuged at 8500 rpm for 10 minutes to get the precipitates and simultaneously remove out the excess acid. The precipitate was then suspended in distilled water, followed by centrifugation. This process was repeated until the neutral pH was achieved. Subsequently, the suspension was frozen in freezer at -30 °C, then dried in freeze-dryer. The dried product was stored in vacuum for further characterizations. The obtained products are defined as Nanocellulose from cellulose materials; Nanocellulose from cellulose paper (NCCPP5), Nanocellulose from cellulose powder (NCCPD6), Nanocellulose from ball-milled cellulose paper at x h of ball milling pretreatment time (NCBMCPPx), and Nanocellulose from ball-milled cellulose powder at x h of ball milling pretreatment time (NCBMCPDx) [32]
Reinu E. Abraham , Cynthia S. Wong and Munish Puri investigated that Enrichment of Cellulosic Waste Hemp (Cannabis sativa) Hurd into Non-Toxic Microfibres. In this study a largely available lignocellulose feedstock hemp (Cannabis sativa), obtained as an industrial waste, was used for cellulose extraction. The extraction of cellulose microfibres from hemp biomass was conducted by alkaline treatment and an acidification process. The extracted cellulose microfibres were characterised using Fourier-transformed infrared spectroscopy (FTIR), Scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and X-ray diffraction (XRD). The viability of the study was determined by growing human fibroblasts on the preparation which resulted in being non-toxic; indicating its potential in preparing biological scaffolds. Upon enzymatic hydrolysis of the cellulose microfibre using cellulase from Trichoderma reesei, a maximum of 909 mg/g of reducing sugars were obtained, which endorses its suitability for biofuel production. [33]
Zhong-Xuan Bian, Xia-Ran Miao, Jin-You Lin, Feng Tian, Feng-Gang Bian, Hui Li investigated that Extraction and structural investigation of jute cellulose nanofibers. Cellulose nanofibrils (CNFs) are a type of natural nanomaterials extracted from plants and animals that have expanding applications in numerous areas benefiting from their inherent properties of renewability, biodegradability, and sustainability. For energy consumption reduction, CNFs were extracted from raw jute fibers, which were not pretreated in a hot alkali or acid solution, by TEMPO mediated oxidation. Synchrotron radiation wide-angle scattering was performed to realize the crystallization of the CNF crystallites; Fourier transform infrared spectroscopy, transmission electron microscopy, and fieldemission scanning electron microscopy were used to characterize the changes in chemical groups and visualized morphology of CNFs. The simplified preparation and shortened cycle should further help the study of the structure–function relationship of jute CNFs subjected to chemical modification [34]
R. Faiz Listyanda, Kusmono, Muhammad WazizWildan, and Mochammad Noer Ilmaninvestgated that Extraction and characterization of nanocrystalline cellulose (NCC) from ramie fiber by sulphuric acid hydrolysis. Nanocrystalline Cellulose (NCC) is a nano-sized material produced by the removal of amorphous regions on cellulose fibers through acid hydrolysis. In recent years. The effect of sulphuric acid concentration on the characteristics of NCC was investigated in this work. The cellulose was isolated from the ramie fibers (Boehmeria Nivea) through some chemical treatments including de-waxing in soxhlet apparatus, bleaching, and alkali treatments. NCC was extracted from isolated cellulose with sulphuric acid hydrolysis. The sulphuric acid concentrations was varied by 41, 44, 47, and 50%. The characterization of NCC were conducted through Fourier Transform Infrared Ray (FTIR), X-ray Diffraction (XRD), and Transmission Electron Microscopy (TEM). The results show that the shorter length of NCC was found with increasing higher sulphuric acid concentration. However, the crystallinity was decreased at higher sulphruric acid concentration. Based on the XRD analysis, the highest crystallinity index (90.7%) was obtained at the sulphuric acid concentration of 41% [35]
Júlia G. Vieira, Guimes Rodrigues Filho, Carla da S. Meireles, Fernanda A. C. Faria, Dayane D. Gomide, Daniel Pasquini investigated that Synthesis and Characterization of Methylcellulose from Cellulose Extracted from Mango Seeds for Use as a Mortar Additive. Methylcellulose was produced from the fibers of Mangifera indica L. Ubá mango seeds. MCD and MCI methylcellulose samples were made by heterogeneous methylation, using dimethyl sulfate and iodomethane as alkylating agents, respectively. The materials produced were characterized for their thermal properties (DSC and TGA), crystallinity (XRD) and Degree of Substitution (DS) in the chemical route. The cellulose derivatives were employed as mortar additive in order to improve mortar workability and adhesion to the substrate. These properties were evaluated by means of the consistency index (CI) and bond tensile strength (TS) tests. The methylcellulose (MCD and MCI) samples had CI increased by 27.75 and 71.54% and TS increased by 23.33 and 29.78%, respectively, in comparison to the reference sample. Therefore, the polymers can be used to produce adhesive mortars [36].
2.1.11 Tempo Oxidation
TEMPO Oxidation TEMPO induced oxidation produces a TEMPO (or another related mixture like TEMPO / NaClO2 / NaClO) in water. The solution is placed in TEMPO. TEMPO (2,2,6,6-tetramethyl-1-oxyl) is melted, while NaBr melted in H2O by adding NaClO to the oxidation mechanism as primary oxygen. The TEMPO reagent will be moved to N-oxoammo- nium salt (R1R2N ? = O) under some cases in order to catalyst for more reactions. Then, return the cata- lyst to the form of TEMPO of sodium hypochlorite and sodium Bromide. In addition, surface hydroxyls groups are majorly moved to carboxylate groups during thisin which C6 hydroxyl groups present with a higher reactivity than C2 and C3. Actually, this reaction occurs in external amorphous areas of cellulose fibres which imply negative surface nanocellulose that leaves the crystalline structure almost intact. NaCl is subsequently by-product of this process. Significantly, both acidic and primary con- ditions can be used in the reaction Hirota et al. illustrate a case with acidic pH. The oxidation structure for 4-acetamide-TEMPO/NaClO2 on the un-dried wood cellulosic material at 60 oC tempera- ture and pH 4.8 was studied up to 1 to 5 days. The outcomes in terms of NCC were developed with 67 to 77% by mechanically processing of oxidizing result (4 – 7 nm width and 100–200 nm long). Liu et al. have seen in another study in a simple pH status. Compared to the nanocellulose characteristic attained with acidic hydrolysis of the corncobresi- due, the TEMPO-intermediated oxidation of TEMPO/NaBr/NaClO at pH 10.5 has good results [37].
2.1.12 Refining
Conventional refining is a suitable physical process to deal with processing of nanocellulose. Many scien- tists employed a variety of machines to process the cellulose pulp and manufacture NFCs, for example the disc refiner and a PFI mill. Refining typicallyincreases the area and thickness of the fibres and decreases its size (because of the cutting effect and superficial fibrillation). Fibre slurry is main- tained in disc refiners by an intersection of spinneret and blade discs. Groove and bar that protected discs endure repetitive stresses that contribute to the for- mation of nanocellulose. Likewise, the head holding bars are pushed on one side of the case during the process of a PFI mill. Inside a PFI mill, fibres centrifugation occurred among the internal cylinder and the external sheet which revolve at varying speeds but in the same direction, resulting in mechanical power. Rotating bars also have an effect on fibres. As a result, fibrillation both internally and externally, thus reducing the fibre volume. Importantly, gener- atednanofibres bear a considerable quantity of water through processes like PFI mills (or valley beaters). As a result, the volume and emissions issues during storage and management cause problems. Meanwhile, cellulosic matrix among constant and moving hones is received in grinders, which rotate in around 1500 rpm to reduce fibre stresses. In reality, the primary layer composition as well as hydrogen bonding are tearing down for production of nanocellulose. Though, in the process of fibrilla- tion, excessive routes could be needed. Notably, expenses of NFC output could increase in terms of the energy usage of PFI plants. Spence et al. declared a beating of 3 h valley needs energy of 2 mWh/ton. Lee and Mani140 are both wasting 3.5 mWh/ton energy about the 20,000 rounds in a PFI mill. However, stretching fibres on a beater in the valley seem in contrast with a grinder more energy efficient. In addition, it may be caused by the pro- duction of sporadic pressure force in a fibre straightening blade in valley. In comparison, disc refiner energy consumption is smaller as com- pared to homogenizer andmicrofluidizer. Improving the energy intake technology is also criti- cal for decreasing of manufacture costs[38].
2.1.13 Ultrasonication
Using ultrasonic methods, mixing, microfluidization, biological treatment hominization, hydrolysis erup- tion of gas, ionic fluids and TEMPO-mediated oxidation is the motorized process used in study by the researchers alone or in combination with other nanocelluloses techniques. Thebenefit of this approach is that hydrodynamic ultra- sound forces make microscopic gas (cavitation) bub- bles leading to mechanical oscillation. This power disrupts the cellulose–fibres’ interaction force that finally generate nanocellulose. Since it is gen- erated by proving of excessive heat development, the heat transformation is normally regulated by hybrid pool. In a Chen et al. research, they find out that the natural structure, crystalline assembly and thermal strength of cellulose can be changed simply by ultrasonication, which only induces structural chan- ges to nanocellulose output. Yang et al. have reported ultrasonication conservation of cellulose biocompatibility and cellulose biodegradability, can performed without of chemical reagents. Moreover, such type of approach considered more advanta- geous in biomedical and drug arguments. The key elements influencing to procedure can be cellulose concentrations, time and ultrasonic strength. Frone et al. found that the increase in ultrasound time and power could decrease the fibre size and improve production quality. Similarly, Chen et al have found that increasing suspension cellulose concen- tration caused more crystallinity index of finer nanofibres. Rohaizu and Wanrosli further noted that increase in NCC output yields by 39% relative to a non-assisted process with TEMPO-assisted oxida- tiontechnology [39].
2.1.14 Radiation
A process of nanocellulose processing assists the use of radiation, in which mainly involve microwave, ultraviolet radiations, gamma rays and electrons beams radiations. Radiation treatment with higher amounts (200 to 300 KGy), through eliminating large portions of macromolecules, may create nanocellu- lose. But there is a very poor output yield (to1.0%), which means that for this reason the radiation ther- apy alone is inadequate. Researchers then merged this method with another physiochemical procedures. The results suggest that b-radiation penetrates the bulk fibre, while UV light interrelates more selectively to cellulose. UVs at 253.7 nm have enough strength for every chemically bonded cellulose, In addition, this strength (112 kcal/mol) poses a smaller value than b-rays in various orders of magnitude. Moreover, they found out in production process of samples, ultraviolet rays just permeate the amorphous areas. It has been established that the electron beam radiation can regulate nanocellulose molecular mass as well as crystalline structure in production processes[40].
3. Materials and Methods
3.1 Materials
The sample of Arachis hypogaea peel was collected from local village. In this study, this raw material was used to extract cellulose. Here, Sodium Hydroxide (scientific chemical ltd, Tongi Bazar 97%), Sodium chlorite (science lab, Dhaka), Glacial acetic acid (Hat-khula, Dhaka 100%), Hydrochloric acid (Mirpur -1, Dhaka 99%), all reagents were used without further purification[41].
3.2 Methods
3.2.1 Alkali treatment
The alkali treatment was performed to purify the cellulose by removing lignin and hemicellulose fromArachis Hypogaea peel. The ground Arachis Hypogaea peel was treated with an alkali solution (4 wt% NaOH). The mixture was transferred into a round bottom flask and treatment was performed at reflux temperature for 2hr at 60°C. Theph in the range of 9-10 was reached. The mixture was allowed to cool and was filltered using excess distilled water. Following alkali treatment, the bleaching process was completed by adding a buffer solution of acetic acid, sodium chlorite and distilled water at reflux 60°C for 2h. Here Ph in the range of 5-5.5 was reached. The mixture was allowed to cool and was filtered using excess distilled water.
4. Result and Discussion
4.1 Characterization of particles
4.1.1 Moisture content
Fiber samples with different degrees of water retting were kept in the open air at room temperature and 55-65% RH for one week. Then, after drying in an oven to a constant weight, weights of wetted (Ww) and oven-dried (Wa) samples were measured. Moisture content percentage (Mc%) of the fiber was calculated using Equation –
4.1.2 Moisture Regain
Fiber samples with different degrees of water retting were kept in the open air at room temperature and 55-65% RH for one week. Then, after drying in an oven to a constant weight, weights of wetted (Ww) and oven-dried (Wa) samples were measured. Moisture regain percentage (Mc%) of the fiber was calculated using Equation –
4.1.4 X-ray diffraction (XRD)
X-ray diffraction was used to determine the crystallinity of the rice husk fibres after different treatments. Each material in the form of milled powder was placed on the sample holder and levelled to obtain total and uniform X-ray exposure. The samples were analysed using an X-ray diffractometer (D8-Advance Bruker AXS GmbH) at room temperature (RT) with a monochromatic CuK radiation source (l = 0.1539 nm) in the step-scan mode with a 2θ angle ranging from 10◦ to 50◦ with a step of 0.04 and scanning time of 5.0 min. To characterize the crystallinity of the different samples, the crystallinity index CrI, was determined based on the reflected intensity data following the segalmethod.
Where l002 is the maximum intensity ofthe (0 0 2) lattice diffraction peak and lam is the intensity scattered by the amorphous part of the sample. The diffraction peak for plane (0 0 2) is located at a diffraction angle around 2 = 22◦ and the intensity scattered by the amorphous part is measured as the lowest intensity at a diffraction angle around 2θ = 18◦.
4.1.5 Fourier transform infrared ray (FTIR)
FTIR was used to examine the changes in the cellulose surface caused by contact with Arachis Hypogaea nanoparticles. FTIR spectra of commercial cellulose and cellulose- Arachis Hypogaea composite were investigated with Thermoset Scientific Nicolet iS50 equipped with a liquid-nitrogen-cooled MCT detector. The spectra were observed in the absorption mode at ambient conditions 4000-500 cm -1 wavenumber range.
4.1.6 Scanning electron microscope (SEM) analysis
The surface morphology of cellulose and cellulose- Arachis Hypogaea composite particles were analyzed by SEM S-4800 (Hitachi, Japan) with retaining 5kV operational voltage. The chemical element of the cellulose- Arachis Hypogaea composite was analyzed using energy-dispersive X-ray spectroscopy on SEM.
4.1.7 Thermogravimetric Analyzer (TGA)
The thermal stability of the sample was determined by TGA analysis using the thermogravimetric analyzer SDT-Q600, NETZSCH (Germany). Specifically, 5 mg of the powdered samples were analyzed under N2 flow at a rate of 20 mL/min, temperature range of 25–500 ℃, and heating rate of 10°C/min.
4.2 Results Analysis
4.2.1 XRD analysis
The crystalline characteristics of commercial cellulose powder and synthesized cellulose-Arachis Hypogaea composite were investigated using XRD, as shown in Fig. 2. From the diffractogram in 2a, the peaks of cellulose powder exhibited peaks at around 16˚, 22˚& 35˚.
Here, we got crystallinity 72.22%.
4.2.2 FTIR analysis
The FTIR absorption spectra were analyzed to identify changes on the cellulose surface during the synthesis process. The spectrum of the cellulose powders showed a broad peak at around 3270 cm -1 and 2890 cm -1 that corresponded to stretching of the O-H and C-H of polysaccharides A small peak was identified at 1645 cm -1, corresponding to the vibration of water absorption by the cellulose. A sharp absorbance band at 1034 cm -1 characterized the C-O stretching vibration of primary alcohol. The band was recognized at 890 cm -1 that referred to C-O-C vibrations belonging to the β-1, 4 glycosidic linkage. The position and intensity of mentioned bands could be influenced due to changes in intra or intermolecular hydrogen bonds, and hence the modifications in the surface groups may occur [42].
4.2.3 Thermogravimetric Analyzer (TGA)
Thermogravimetry curve is used for the measurement of heat weight. In this process, weight of the substance is taken as y-axis, temparature is taken as X-axis. In thermogravimetry curve , horizontal portion is that portion at which there is no change in mass occur. From 25˚ -250˚ the mass of cellulose was almost unchanged. Pyrolysis is the portion of graph at which with the increase of temperature the mass of substance fast pyrolysis occurred at 250˚ to 360˚. Procidial decomposition temperature started at which the temperature started at which the temperature decomposition. Besides, final decomposition temperature at which decomposition stop. Here, the procidial decomposition temperature was 260˚ and final decomposition temperature was 360˚C. The reaction interval at which the temperature range reaction occur. The reaction interval shows 100˚c. Besides the thermal stability shows 360˚c to 500˚C.
4.2.4 SEM Analysis
SEM was performed to determine surface morphology of the extracted cellulose. After the Final process, cellulose were average diameter 30 nm. The changes which occurred upon performing the final processing step. It is assumed that the surface of extracted cellulose is rough. The most obvious reason for clumping between cellulose particles was the presence of strong intermolecular hydrogen bonds. The SEM findings were in accordance with the results of reported that cellulose obtained from the acid hydrolysis had an irregular shape and size. The hydrolytic breakage of the glycosidic bond during acidification, which results in the breakdown of amorphous areas, was also linked to the tiny cellulose particle size.
4.2.5 Moisture Content
We first took a weight of the powder. The powder weight was 1.23 grams, then put it in the oven machine, after running the machine at 105°C, we got its weight of 1.05 grams, which was running for 20 minutes.
4.2.6 Moisture Regain
We first took a weight of the powder. The powder weight was 1.23 grams, then put it in the oven machine, after running the machine at 105°C, we got its weight of 1.05 grams, which was running for 20 minutes.
4.2.7 Cellulose Content
Cellulose content was determined by extracting holo- cellulose with the aqueous sodium hydroxide (17.5%) for 5 h before quenching the reaction with ice. The obtained white powder was washed with copious amount of water until filtrate becoming neutral. The initial mass was 4.20 grams and the obtained white powder mass was 2.15 grams. The cellulose content was calculated using Eq.
Where, M3 was the obtained white powder mass, M was the initial sample mass.
4.3 Limitations of the study
During the sample testing we faced many problems especially during the SEM test. We did not get the perfect result as we wanted in Dhaka University. It was not possible to re-test because the cost of testing was very high.
5. Conclusion
This study provided a quick overview of cellulose extraction & different application methods. In this way, cellulose is characterized from Arachis Hypogaea peel effectly by three step process: Alkali treatment, Bleaching by and acid hydrolysis by HCl. Before stirring, dry weight was taken and moisture content was calculated as 14.88 %. After Stirreing extraction, cellulose content was 51% extraction of cellulose nanocrystals from Arachis hypogaea peel was evaluated for the first time. The chemical composition, morphological, FTIR and XRD results confirmed that removal of hemicellulose and lignin from Arachis hypogaea peel. In the textile industry, powder cellulose ethers can be used as sizing, leveling, and thickening agents of textile pulp. Cellulose ethers such as sodium carboxymethyl cellulose and other varieties can be used as sizing agents.
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Founder & Editor of Textile Learner. He is a Textile Consultant, Blogger & Entrepreneur. Mr. Kiron is working as a textile consultant in several local and international companies. He is also a contributor to Wikipedia.
