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International Journal of Nanoscience And Nanotechnology

International Journal of Nanoscience and Nanotechnology, 2016, 1(1),14-17

SNVS Murthy et al., Page No.14

A narrative synthesis and characterization of Cellulose Nano fibers from jute fiber SNVS Murthya, Tentu Nageswara Rao*b, Tentu Manoharanaiduc, S Seshammad and K.Paramesware

aDepartment of Chemistry, DLR PG College, G. Mamidada, AP India. bDepartment of Chemistry, Krishna University, Machilipatnam, AP, India .

cDepartment of Nuclear Physics, Andhra University, Visakhapatnam, AP, India. dDepartment of Bio Chemistry, AN University, Guntur, AP, India.

eDepartment of Pharmacy, JNTU, Hyderabad, Telangana, India. Email: tentu6581@rediffmail.com

…………………………………………………………………………………………………………………………. Abstract: Cellulose can be obtained from fibers of plant tissues. Normally the natural fibers are composed through glucose and it's far insoluble in water due to its ß (1-4) bonds and interactions of hydrogen bonds between the glucose chains. Jute fiber is a wealthy source of fibers and it may be purified to achieve monocrystalline cellulose which might be used for the elaboration of natural nanoparticles. Amorphous areas of cellulose can be functionalized with different chemicals to improve some of its purposeful residences, which may be beneficial to broaden new nanomaterials. The goal of these paintings turned into to synthesis and characterizes cellulose nanofibers from jute fiber through chemical remedy the usage of mineral acids, alkaline and inorganic salts accompanied through mechanical remedy and disintegration techniques. To obtain and separate the cellulose nanofibers; the cellulose changed into purified and hydrolyzed through manner of warmth, sonication and ageing. Scanning electron microscope (SEM), transmission electron microscope (TEM) and x-ray diffraction (XRD) have been used to symbolize morphology, distribution and length. It became found to be distribution of length with maximum 45 ± 10 nm and fluctuated from five to 80 nm with a logarithmic distribution. XRD look at became evaluated for crystalline houses of jute fiber cellulose nanofibers on contrast with acknowledged well known microcrystalline cellulose as reference. This paintings confirmed that it became viable to synthesize cellulose nanofibers from jute fiber, and its characterization evidenced amorphous and crystalline areas in addition to nanofibers with triclinic structure. Key words: Cellulose, Cellulose nanofiber, Jute fiber, FESEM, TEM, XRD, EDS, FTIR, CCNF, BCNF …………………………………………………………………………………………………………………………. Introduction A billionth of a meter is known as Nanometer. Which is having less than 100 nm in a dimensional is considered as Nanosize. Nanotechnology is thriving quicker with application in all the fields. Materials in Nanoform having different property camparsion with the bulk material due to its large surface area. Cellulose is a most plentiful natural bioresources and renewable. A French scientist Anselme Paymen has discovered cellulose in 1838, he has isolated the cellulose from plant tissues and he determined the cellulose formula (C6H10O5)n. Cellulose is a bio polymeric substance and abundant in natural eco system. Plant tissues were consisted with hemicellulose, lingo cellulose, lignin and pectin. Cellulose is a polysaccharide, which is containing number of hydroxyl groups produce strong intermolecular hydrogen bonds in its structure, it can be reacted with various reagents and gives its derivatives which is having valuable properties like cellulose ester and cellulose ether. Certain bacteria and small sea animals are produced cellulose (samir et al., 2005). Cellulose based biopolymer were prepared from the cellulose rich materials were used in preparation of biocomposite. Cellulose having a strong affinity and hydrogen bonding through the Vander Val’s force to itself, hence cellulose is very stable and insoluble in water and most of the solvent, soluble in some of the

reagent like dimethyl formamide, cadium ethylenediamine (cadoxen), cupriethylenediamine (CED) and N-methylmorpholine N- oxide. Cellulose is a long chain molecule when its breakdown into small chain molecules or glucose units by cellulolysis process are called as cellodextrins. Cellodextrins are soluble in water and most of organic solvent. The physical and chemical properties of cellulose and its chemical reactivity and behavior are strongly influenced due to the arrangement of the hydroxyl group and hydrogen bonding with related to each other to the fiber axis. Native cellulose is arranged by sequence like amorphous region and crystalline region, when it undergoes chemical reaction amorphous region could get wrecked and crystalline region was isolated. Cellulose in its nano form has greater potential in emerging medical and environmental applications. Cellulose fiber has contributed to its use in paper and other fiber based composite materials in adsorbents, textile industry, cosmetics and medical. The aim of this study is to prepare cellulose nanofibers from jute fiber through the top down process. The crude cellulose fiber was separated from the jute fiber. The crude fiber was treated with acids, alkali and the mixture of NaOCl – HCl followed by dialysis, mechanical treatments like ball milling, sonication and dissolution. The resulting cellulose fibers was dried and isolated. Cellulose fiber

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size and properties were characterized by Transmission Electron Microscope (TEM), Field Emission Scanning Electron Microscope (FESEM) and X-Ray Diffraction (XRD) analysis. Energy Dispersive X-ray Spectroscopy (EDS) is a technique for identifying the elements present in the sample. The FT-IR is an analytical technique for studying the cellulose nano fiber characterization and chemistry of the cellulose. The functional group of cellulose was confirmed with Fourier transform infrared spectroscopy (FTIR) spectra by comparing the stretching and bending of functional groups. The obtained cellulose nanofibers are used in the preparation of absorbents, membranes, biosensors, biocomposites, protective clothing and biomedical application. Materials and methods Materials The jute fiber was collected from local agriculture farm. Chemicals such as Nitric acid, Hydrochloric Acids, Sodium hydroxide, Sodium hypochorite and liquid nitrogen were supplied from Merck specialties Pvt Ltd., India. These chemicals were pure and analytical grade chemicals, used directly without any purification. A 2.5 N sodium hydroxide solution was prepared by weighing 40 g of sodium hydroxide into a 500-ml glass bottle and diluted with 500-mL distilled water. A 2.5 N hydrochloric acid solution was prepared by adding 103.3-mL of concentrated HCl into a 500-ml glass bottle and diluted with 500-mL distilled water. A 2.5 N Nitric acid solution was prepared by adding 78.8-mL of concentrated HNO3 into a 500-ml glass bottle and diluted with 500-mL distilled water. Methods jute fiber was cut into small pieces and dried in sunlight, ground well using a homogenizer. The pulp was washed with water and dried in temperature

controlled oven at 60°C for 18 hours. The pulp was transferred in to soxhlet apparatus with the mixture of acetone and distilled water 1:1 ratio, to minimize the unwanted wood extractive. Around 20 g of dried pulp was weighed into a 250-mL round bottom flask and added 125 ml of 2.5 N sodium hydroxide solutions. The pulp was soaked in 2N sodium hydroxide for 24 hours at room temperature. Then the pulp was washed with plenty of distilled water, after which is the same was soaked with 2.5 N HNO3 acid for 48 hours. This was followed by digestion for 48 hours at 60°C with 2.5 N sodium hydroxide. After NaOH treatment the pulp was washed well with plenty of water and digested using 2.5 N HNO3 at 60°C for 48 hours. The resulting pulp was washed with distilled water until the pH attain neutral and dried at 60°c in temperature controlled oven for 18 hours. In this step most of water soluble materials, lignin, pectin and chlorophyll were removed, leaving behind the cellulose. Mechanical Treatment - Ball Milling Ball mills are used to grind the materials that are soft, medium hard to extremely hard, brittle or fibrous. The instrument has three modules, a grinding chamber (A), a grinding bowl (B) with balls and a threaded spindle with three point grip (C). The grinding bowl is placed on a disc (D) inside the grinding chamber. The threaded spindle is placed firmly on the grinding bowl, it is made of agate material. The bowl is also provided with a removable lid (G). The pretreatment pulp was milled by ball milling instrument (Model - Ball Mill PM 100, Make – Retsch Germany) with several times up to get a fine powder. After the Mechanical treatment the resulting cellulose was characterized with Fluorescence microscope (Zeiss) and the images was presented below. Figure 1 represents the obtained from jute fiber

Figure 1 Microscope image for jute fiber after mechanical treatment with ball milling The pretreated dried pulp was digested with the mixture of 10 % wt sodium chlorite and 100 mL of 2.5 N Hydrochloric acid controlled temperature at 60°C for 24 hours to break down the long chain molecule into a cellodextrins. When the cellulose treated with mixture of sodium hypochlorite and hydrochloric acid, intermoleculer hydrogen bonding gets breakdown and size of the chain was reduced. The resulting pulp was washed repeatedly with plenty of distilled water until the solution getting pH neutral and the pulp dried in a

temperature controlled oven at 50°C to dryness. The dried pulp was ground well by gradual addition of liquid nitrogen using a mortar in a fuming hood. Dissolution The cellulose fibers were mixed with 0.1 N sodium hydroxide, sonicated for 2 hours then the pulp was washed with distilled water by centrifugation and the pH maintained with neutral. Dried pulp was taken into a 100-mL stoppered conical flask and 50 ml of distilled water was added and stir with magnetic pellet for 48

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hour and dried at 50°C upto dryness. The dried pulp was ground well by gradual addition of liquid nitrogen thrice. The resulting fiber was investigated for FESEM analysis and XRD. Result and Discussions The resulting cellulose material was investigated by FESEM Analysis (Model – Quanta FEG 200, FEI, Netherlands). The operated accelerated maximum voltage is 30 KV and minimum is 200V, it has three modes, High Vacuum, Low Vacuum and

Environmental SEM. The Cellulose size and property was characterized by FESEM analysis at high resolution. The specimen was deposited on the electron microscope grids, operated at an acceleration voltage at 10 kv with SE mode and observed. The obtained FESEM image shows that the cellulose is in the form of fibrous and width of the range is 20 nm to 80 nm. FESEM image of CNF obtained by jute fiber represents the Figure 2 represents obtained from the jute fiber.

Figure 2 SEM image of Cellulose Nanofiber prepared from jute fiber

XRD Characterization X-ray diffraction analysis helps to understand crystallinity and amorphous nature of cellulose nanofibers. Microcrystalline cellulose sourced from merck specialities, Mumbai was used as reference for XRD characterization. The X-ray dirractision is a Panalytical XPert Pro XRD with both powder mode and GI Attachments. The patterns are detected on XPert High Score Plus software. Figure 3 to Figure 4 shows XRD patterns of microcrystalline (reference), jute fiber cellulose nanofiber respectively. From the micro crystalline cellulose XRD characteristics, sharp peak resolved which is indicative of crystalline in nature (Figure 3, 2 θ = 22.83°). The XRD characteristics of

microcrystalline cellulose nanofiber and jute fiber cellulose nanofiber are 2 θ = 22.49° and 22.78° (Figure 3 and Figure 4) respectively, and the peak was broad which is indicative of amorphous nature. The peaks are broad on the nanomaterials, which is indicates more of amorphous content in the nanomaterials ( thygesen et al. 2005). It could be more important due to having crystalline and amorphous regions, it will generate a more reactivity with the other chemicals to achieve the nano material functionality (ClaudiaE. Ponce). It was observed clearly that material obtained from jute fiber has a partial amorphous and crystalline nature. The crystallinity is directly proportional to the tensile strength of the material.

Figure 3 XRD pattern for the microcrystalline cellulose counts

Position [°2Theta] (Copper (Cu)) 20 30 40 50 60 70 80 900

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International Journal of Nanoscience and Nanotechnology, 2016, 1(1),14-17

SNVS Murthy et al., Page No.17

Figure 4. XRD pattern for jute fiber Cellulose Nanofiber counts Energy dispersive X-ray Analysis (EDS) EDS is a analytical technique to identify the elements and elemental composition present in the sample. The EDS analyses are integrated characteristics of the SEM. The EDS spectrum peaks of CCNF and BCNF corresponding to the energy levels for which the carbon and oxygen. The comparison of carbon and oxygen elements sigma weight percentage, the carbon elemental sigma weight percentage is higher than the oxygen elemental sigma weight percentage in both CNF and BCNF, higher sigma weight percentage in a EDS spectrum is the more concentrated element in the spectrum. From this it can be concluded the carbon is likely slightly high compared to oxygen in the CNF as well as BCNF. Elemental analysis of cellulose nano fibers were confirmed with the EDS results. The prepared cellulose Nanofibers posses skeleton of only the carbon, oxygen and hydrogen. The chemicals associated with chemical treatment were not detected in the final cellulose Nanofibers, which has been confirmed by EDS analysis. FT-IR spectroscopy Analysis

The properties of the CCNF and BCNF were characterized by FT-IR using a fourier transform infrared spectrophotometer, model -8400S, shimadzu. The analyses were carried out by the KBr pellet technique. The samples were prepared by mixing the 2 mg to 3 mg of sample with approximately 250 mg of KBr in to a mortar and ground well. The KBR pellets were prepared in a specified device under vacuum and under a pressure of … The scanning range was from 400 to 4000 cm-1 . Figure 8 and Figure 9 represents the FT-IR spectra for the CCNF and BCNF. The Strong dominant broad peaks in the region from 3700 to 3000 cm-1 are due stretching vibration of –OH groups. The C-H stretching in methyl and methylene groups range between 2800 to 3000 cm-1. (Bodirlau, 2007). Figure 8 represents the FT-IR spectra of CCNF and Figure 9 represents the FT-IR spectra of BCNF.

The strong broad absorption peaks at 3354 cm-1 indicates the –OH stretching band (hydroxyl group), absorption peak at 2902 cm-1 indicates the aliphatic C-

H stretching band, absorption peak at 1061 cm-1 indicates the C-O-C bending (ester functional group), the further absorption peaks at 1325 and 1371 cm-1 indicates the C-H bending, absorption at 1433 cm-1 indicates the CH2 bending, absorption at 1163 cm-1 indicates the -OH bending. Conclusions

This study is to demonstrate that Cellulose Nanofibers can be synthesized from the jute fiber through a simple method like pretreatment, mechnical treatment, chemical treatment followed by dissolution. The obtained cellulose nanofibers size and properties were characterized by SEM, XRD, EDS and FTIR analysis. The results are shows that the synthesized nanofiber diameters are within range between 30nm – 90 nm with the length of few microns. The results indicate that the cellulose naonofiber synthesized from jute fiber can be useful in preparation of absorbents, membranes, biosensors, biocomposites, protective clothing and biomedical application. Acknowledgements We are thankful to Dr. Silpa, IIT, Madras for her invaluable support and encouragement. References 1. Sain, M., Panthapulakkal, S. Ind. Crops Prod. 23, 1-

8, 2006. 2. Thygesen, A. Oddershede., Cellulose. 12, 563-

576,2005. 3. Isci, G.N.Demirer, Renewable energy, 32, 750-

757,2007. 4. J. Zhang et al. carbohydrate polymer 607 -611,2007 5. D.J. Gardner, Journal of adhesion science and

technology 22, 545-567,2008. 6. Claudia E. Ponce, Jorge Chanona, Synthesis and

characterization of cellulose nanoparticles obtained from agave waste by electron microscopy and X-ray diffraction .

Position [°2Theta] (Copper (Cu))20 30 40 50 60 70 80 90

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