Mercerization and Etherification of Mung Bean Pods

for the Production of Carboxymethyl Cellulose

Crisnuel C. Ramirez, Joniel A. Rebalde, Rachel G. Salvador, Aldous Fran D. Tabuzo
Chemical Engineering Department, College of Engineering and Technology,
Pamantasan ng Lungsod ng Maynila

INTRODUCTION
Carboxymethylcellulose (CMC) is an industrial polymer which is a chemically modified
derivative of cellulose with an ether structure. Given its good film forming properties and high
viscosity, it is used as an emulsifier, thickener, binder and stabilizer on a wide range of industries.
In the production of CMC, cellulose rich materials, like wood chips, plant stalks and leaves, is
reacted with alkali and chloroacetic acid. This involves two reaction stages; mercerization and
etherification. In the first stage, the raw material is treated with sodium hydroxide (NaOH) and
alcohol which yields to alkali cellulose. The alkali cellulose then reacts with monochloroacetic
acid, producing carboxymethyl cellulose. Cellulose can be found in different agricultural wastes
that are underutilized such as mung bean pods. Mung bean pod is a lignocellulosic material which
contain 37.2% cellulose which makes it a suitable raw material for the production of
Carboxymethyl Cellulose (CMC).
MATERIALS AND METHODS it achieved the right particle size. To achieve
quality and consistency of the material, the
The experimental method of converting
ground mung bean pods are passed through a
mung bean pods into carboxymethyl cellulose sieve
involves three (4) major processes. [1]
Preparation and conditioning of raw materials Cellulose Extraction
which includes drying, grinding and sieving. [2]
The ground mung bean pods are
Cellulose extraction which includes alkali
pretreatment and bleaching. [3] Conversion of pretreated with an alkali solution. The different
cellulose to carboxymethyl cellulose which parameters chosen for this process are type of
includes mercerization and etherification. And alkali, concentration of alkali, ratio of mung
lastly, [4] Purification which includes bean pods to alkali solution, temperature and
neutralization, alcohol washing, centrifugation, time of reaction. The mixture is filtered then
drying, grinding and sieving. The experimental washed. The pretreated alkali undergoes the
process flow diagram is shown in Figure 1. process of bleaching at elevated temperatures
to further delignify the material.
Preparation and conditioning
Conversion of cellulose to CMC
Mung bean pods are dried in an oven
at different time and temperatures. Then, it Bleached cellulose undergoes the
was ground in a blender at different times until process of mercerization. This is a
pretreatment process that converts alpha –
cellulose to alkali cellulose which is more
reactive to the monochloroacetic acid for
etherification. The etherification process is
shown in Figure 2.
Purification
As shown in Figure 2, the products of
etherification process have many impurities
that are undesirable for the researcher. This
can be removed by neutralization and alcohol
washing. In neutralization, different acids are
tested at different amounts. This removes the
sodium glycolate from the mixture. The
neutralized CMC undergoes the process of
alcohol washing which removes the sodium
chloride byproduct of the reaction. This yields
pure CMC which is refined through drying,
grinding and sieving. This ensures that the
product’s moisture content and particle size
are controlled to desirable values.

Figure 1: Experimental Process Flow Diagram

Figure 2: Etherification Reaction

 RESULTS AND DISCUSSION For the cellulose extraction, the best
alkali to be used for alkali pretreatment was
Table 1: Cellulose Extraction of Pretreated
NaOH with the concentration of 25%. The
Mung Bean Pods
optimum reaction temperature was 100°C and
Process Parameter Optimum
Condition the optimum reaction time was 90 minutes.
Type of alkali used NaOH Bleaching was done after alkali pretreatment.
Concentration of 25 % (w/w) The optimum ratio of crude cellulose to
alkali bleaching solution was 1:7 with an optimum
Mung bean pods to 1:7 concentration of 15%. The bleaching was done
alkali solution ratio
in 90 minutes. In the mercerization process, the
Reaction 100 ˚C
optimum ratio of the diluent to cellulose was 1:7
temperature
and the optimum ratio of cellulose to alkali was
Reaction time 90 minutes
1:3.
Cellulose to bleach 1:7
solution ratio After mercerization, etherification
Concentration of 15% should be done to convert the cellulose to the
bleaching solution desired product, carboxymethyl cellulose. The
Time 60 minutes optimum cellulose to MCA ratio was 1:1.2 with
Temperature 90 ˚C a temperature of 55°C and reaction time of 90
minutes.
Table 2: Conversion of Cellulose to CMC
Process Parameter Optimum RECOMMENDATION
Condition
Cellulose to Alcohol 1:7 For further improvement of the study,
Ratio the selectivity of the etherification reaction
Cellulose to NaOH 1:3 should also be considered. This is to account
Ratio for the amount of byproducts formed by the
Cellulose to MCA 1:1.2 reaction.
Ratio
REFERENCES
Temperature 55 ˚C
Time 90 minutes 1. Xu et. al., 2017; Synthesis of sodium
carboxymethyl cellulose using bleached
crude cellulose fractionated from cornstalk
The experiment for the different 2. Das et. al., 2015; Pretreatment Methods of
parameters were conducted and the optimum Ligno - Cellulosic Biomass: A Review
conditions for each parameter were taken. 3. Labbafi et. al., 2017; Synthesis and
During a dry run of these optimum conditions, Characterization of Carboxymethyl
the researchers have produced 71.30g of Cellulose from Sugarcane Bagasse
CMC from 250g of mung bean pods. This will 4. Arslan et. al., 2003; Production of
give us an overall conversion of 28.52%. carboxymethyl cellulose from sugar beet
pulp cellulose and rheological behaviour of
CONCLUSIONS carboxymethyl cellulose
The researchers were able to product 5. Wunna et. al., 2017; Effect of Alkali
carboxymethyl cellulose from mung bean pods Pretreatment on Removal of Lignin from
Sugarcane Bagasse
by the process of mercerization and
etherification. The optimum parameters were
identified using one – factor at a time method.