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International Journal of Trend in Scientific Research and Development (IJTSRD)
                             Special Issue on Innovative Development of Modern Research
                                    Available Online: www.ijtsrd.com e-ISSN: 2456 – 6470

               Synthesis of Carboxymethyl Cellulose from Powder and

                  Microcrystalline Cellulose in Isopropyl Alcohol and

                                               Ethanol Medium

                                Yuldoshov Sh. A, Goyipnazarov I. Sh, Nishonova S. R,
                                   Sarymsakov A. A, Karabaeva B. S, Azizova M. A
             Institute of Polymer Chemistry and Physics Academy of Sciences of Uzbekistan, Tashkent, Uzbekistan

        ABSTRACT                                               (degree  of  crystallinity  of  22%,  degree  of  polymerization
        Synthesis conditions of different substituted water-soluble   420, particle size of 100 microns) were collected from the
        carboxymethyl cellulose (CMC) based on microcrystalline   production  part  of  Institute  of  Polymer  Chemistry  and
        and  powder  cellulose  in  isopropyl  alcohol  and  ethanol   Physics, Uzbekistan. Chemicals used during the studywere
        medium are studied. Samples of water-soluble CMC with a   sodium   hydroxide   (Tianye   Chemicals,   China),
        degree  of  substitution  of  0.38-0.40  based  on     monochloroacetic acid(Azko Nobel Industrial Chemicals B.V.,
        microcrystalline and powdered cellulose  were obtained.   The  Nitherlands),  ethanol  (China),  etc.  All  chemicalsused
        Also,  by  the  one  stage  carboxymethylation  of  cellulose   were of reagent grade and used without further purification.
        samples were obtained CMC samples with high degree of
        substitution.                                          2.2.  Synthesis of carboxymethyl cellulose
                                                               10 g of the cellulose-containing feedstock is treated with 60

        KEYWORDS:  microcrystalline  cellulose,  powder  cellulose,   ml  of  ethyl  alcohol  and  dispersed  for  15  minutes.  With
        carboxymethyl cellulose, etherification, degree of substitution,   stirring, 40% NaOH solution is added. The alkaline treatment
        ethanol, isopropyl alcohol.                            process is carried out for 90 minutes at a temperature of
                                                                 0
                                                               16 C.  Then  a  solution  of  monochloracetic  acid  (MCA)
        1.  INTRODUCTION                                       dissolved  in  60  ml  of  ethyl  alcohol  is  added  by  vigorous
        Carboxymethyl  cellulose  (CMC)  is  the  product  of  the   stirring for 15 minutes at 16°C. After that, the temperature of
        interaction of alkaline cellulose with monochloracetic acid or   the reaction mixture rises to 550°C and the esterification
        its sodium salt [1-5].                                 reaction is carried out for 3 hours. The product is filtered off
                                                               on  a  glass  filter  and  washed  with  aqueous  ethanol.  The
        Obtaining  of  CMC  from  cellulose  involves  two  stages  of   product is dried at 60-70°C to a certain humidity.
        chemical  reactions  [6-7].  The  first  stage  is  the  alkaline
        treatment of cellulose and the second stage is the reaction of   2.3.  Characterization
        carboxymethylation of alkaline cellulose with an alkylating   2.3.1.  Measurement of CMC yield
        reagent.                                               CMC yield was measured based on a dry weight basis. The
                                                               net  weight  of  dried  CMC  was  divided  by  the  weight  of
        Depending  on  the  type  of  raw  cellulose,  production   cellulose to get the yield value [12], as follow:
        technology,  CMC  is  produced  on  an  industrial  scale,
        characterized  by  the  degree  of  substitution  (DS)  and  the   CMC yield (%)=  (Weight of prepared CMC (g)) ×100
        degree of polymerization (DP). Currently produced CMC has            (Weight of driyed cellulose (g))    (1)
        above DS = 0.6 and DP = 400 [8].
                                                               2.3.2.  Determination of degree of substitution
        Depending on the number of carboxymethyl groups, CMC   To  determine  the  degree  of  substitution,  0.5  g  of  dried
        grades are subdivided into low (≥0.5), medium (0.55–0.85)   sodium CMC was ashed gently between 45  and 55 ◦C for 24
                                                                                                         0
                                                                                                  0
        and highly substituted (≤0.9) grades. CMC samples with a   h, and then dissolved in 100 mL of distilled water. 20 mL of
        degree of substitution greater than 0.9 are called polyanionic   this solution was titrated with 0.1 N sulphuric acid using
        cellulose  [9-11].  Traditional  CMC  acquires  the  ability  to   methyl  red  as  an  indicator.  After  the  first  end  point,  the
        dissolve in water at a degree of substitution above DS = 0.5.   solution was boiled and titrated to as harp end point. The
        We  have  studied  the  possibilities  of  obtaining  low-  and   carboxymethyl content was calculated from the degree of
        highly substituted water-soluble samples of CMC based on   substitution [13], as follow:
        microcrystalline cellulose (MCC) and powder cellulose (PC)   DS=   (0.162×B)
        by the suspension method.
                                                                      (1-0.08×B)                   (2)
        This method allows to obtain products with a high degree of
        substitution and a uniform distribution of carboxymethyl   B=   (0.1×b)
        groups along the cellulose macromolecule, which leads to an         G                      (3)
        improvement  in  the  physicochemical  and  operational
        properties of CMC.                                     where, b is the volume (in mL) of 0.1 N sulphuric acid and G
                                                               is the mass of pure CMC in grams.
        2.  Materials and methods
        2.1.  Material
        Materials  MCC  (degree  of  crystallinity  of  83%,  degree  of
        polymerization 280, particle size of 100 microns) and PC


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