MICROCRYSTALLINE CELLULOSE: EXTRACTION AND ANALYSIS

Transcription

1 MICROCRYSTALLINE CELLULOSE: EXTRACTION AND ANALYSIS I. Lokshina 1, S. Lugovskoy 2, К. Melisbekova 3, S.O. Karabaev 1,3, I. Gainullina 1, E. Andreeva 3 1 Kyrgyz national university, Kyrgyzstan 2 Ariel University, Ariel, Israel 3 Kyrgyz Russian Slavonic university, Kyrgyzstan Abstract Microcrystalline cellulose (MCC) was extracted from cotton waste. Moisture and ash content were defined, morphology of surface, IR-spectra, X-ray diagram of sample of microcrystalline cellulose were studied. Key words Microcrystalline cellulose (MCC), moisture, ash content, IR-spectra, X-ray diagram, morphology of surface. Introduction Width and a variety of fields of application of materials on the basis of cellulose and its derivatives are connected with possibility of the directed change of their properties first of all due to use of chemical reactions with participation of functional groups and communications of a polymeric chain. Cellulose and its derivatives are widely applied in various industries. One of such materials is microcrystalline cellulose (MCC). MCC unlike other cellulose materials has the maximum degree of crystallinity and density. MCC is the purest form of natural cellulose. A number of its unique properties allowed to use it in the pharmaceutical, food, cosmetic industry [1]. Now they become aggravated environmental problems do actual researches on synthesis of new ion-exchange materials, including on the basis of cellulose and its derivatives. Experiment and discussion In work as initial raw material used cotton lint (the II grade). It is cotton down, short fiber (to 15 mm), a fibrous cover of seeds, remaining on a seed after ginning. It is used for production batting, the packing and absorptive materials. Cotton lint contains not cellulose components - fats and wax (0,5-1%), plant substances of albumen nature, pectin substances (2%), lignin (2-3%), its ash content to 1-2%. Process of extraction of microcrystalline cellulose from lint represents multistage cleaning and chemical processing of raw materials, which purpose is extraction the qualitative final product of MCC. Cleaning of plant impurity was carried out manually (combed out, chose), then carried out whitening of raw materials, by wet steeping in solution of "whiteness" for the 24th hour, with the subsequent washing and drying. The raw materials prepared thus were used for extraction of MCC. 101

2 Methodic of MCC extraction. Raw material s weighed amount (in the ratio 1:5) was immersed in the beginning to boil solution of hydrochloric acid (concentration of 2,5 M). Reaction was carried out during 90 minutes at a solution boiling temperature. Then cellulose mass was pressed, washed out the desalted water before neutral reaction and negative reaction to chloride ion and dried [2]. The exit of powder made about 90%. MCC was dried, and then sifted through a sieve with openings with a diameter of 0,25 mm (no more than 60 meshes). The extracted MCC represents white, easily loose insoluble powder without taste and a smell, isn't toxic. The moisture and ash content of MCC sample were defined using the methods described in [3-4]. Values of moisture and ash content are W а =3,8%; А а =0,4%, suitably. Morphology of surface of microcrystalline cellulose sample (MCC) was researched by Scanning electronic microscope of JEOL company (Japan Electron Optics Laboratory) JSM 6510 using secondary electrons detector (SEI). Suitable photographs are presented on the Fig. 1. As follow from figure MCC is the product of soft hydrolysis. MCC represents the cellulose fibers which broke up to parts. Fibers are collected in aggregates bunches. Fibers look like anisodiametric particles of needle type.. 102

3 Fig.1.Photographs of microcrystalline cellulose sample separated from cotton waste (II sort lint) At the same time, also the microcrystalline structure of MCC is well visible. Thus, data of MCC morphology of surface confirm the destruction of amorphous fraction of cellulose fibers by means of hydrolysis, and cellulose material turns into a highcrystal preparation, containing a small amount of the microcrystals connected by chemical bonds, having various extent of aggregation, including separate microcrystals of cellulose. Length and diameter of microcrystals differ and have the sizes from 1 to 100 microns. IR-spectrum of MCC sample. Research of IR-spectrum was made with the help of Varian IR- Furie spectrometer in standard KBr based tablets in proportion 1:300 and in the spectral range of cm

4 Absorbance δ (см-1) Fig. 2 IR-spectrum of microcrystalline cellulose Analyzing a spectrum of the microcrystalline cellulose, it is possible to tell that existence of a wide indistinct band in the field of 3348 cm -1 testifies to a large number of various types of hydrogen bonds, formed by OH groups and stabilizing certain conformations of macromolecules. In the field 2901cm -1 the band of symmetric and asymmetric valent vibrations of CH 2 groups lies, and ledges on a band speak about cotton cellulose. In the field cm -1 frequencies of deformation vibrations of CH 2 and CH groups are located and also angular deformation vibrations of C-O-H. Intensive bands in the field cm -1 are characteristic for cyclic mono saccharides and correspond to valent vibrations of S-O and the C-C ring structures. Absorption bands in the field cm -1 can be carried both to the pulsation vibrations of a piranoz ring, and to deformation vibrations of C-H. Distinct bands in the fields 2901 and 1431cm -1 testify to that the sample is characterized by high degree of orderliness of macromolecules [5]. Splitting of a band of absorption of deformation vibrations of OH - groups at 1374cm -1 also can testify to removal at hydrolysis of fragments of cellulose connected by weak hydrogen bond and inclusion remained OH- groups in stronger intermolecular hydrogen bond. In other words character of a spectrum of MCC testifies to removal of amorphous part of polymer and formation in it new crystal zones, that will well be coordinated with earlier provided data on MCC surface morphology. X-ray analysis of MCC sample was made by difractometer Panalytical X Pert Pro (Philips) at the wave length λ=0.154 nm. As seen from fig.3 X-ray spectrums have the view of broad line (halo). 104

5 Fig.3 X-ray analysis of microcrystalline cellulose It is typical for amorphous materials. However, existence of peaks testifies to presence at a sample of structural formations. In other words, it is possible to conclude that the received sample of MCC has a crystal lattice with high degree of orderliness. It grants the right to apply to it the term "microcrystalline cellulose" or cellulose with "limit" degree of polymerization [6]. Conclusion. MCC was extracted from cotton waste (lint, sort II). Moisture and ash content of received sample correspond to preparations of MCC from cotton. Morphology of surface, IR-spectrum, radiograph of sample of MCC allow to say that the pure highcrystal sample of MCC is extracted. REFERENCES 1. Battista O.A. Microcrystalline cellulose. Cellulose and its derivatives / Under edition N. Baykls, L. Segal. - M.: Mir, V.2.- P Copyright certificate (USSR) Method of extraction of powdery cellulose / R.I. Sarybaeva, T.V. Vasylkova B.I Obolenskaya А.V., Shegalova V.P., Akim G.L.,. Akim A.L, Kossovich N.L., Emelyanova I.Z. Practical works on chemistry of wood and cellulose. - M.: Forest industry, P Klimova V.A. Principal micromethods of analysis of organic compounds. М.: Chemistry, p. 5. Zhbankov R.G. Infrared spectra of cellulose and its derivatives. Minsk: Science and technik, p. 105

6 6. Microcrystalline cellulose / G.A. Petropavlovsky, N.E. Kotelnikova // Wood chemistry P