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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
ID: IJTSRD39943 | Special Issue on Innovative Development of Modern Research Page 56