MAPUA UNIVERSITY

School of Chemical, Biological, and Materials Engineering and Sciences

Experiment No. 1.3

Simple Distillation: Recycle waste from biodiesel production

Submitted By:

Date Performed:

Date Submitted:

Faculty In-charge
 School of Chemical, Biological and Materials Engineering and Sciences

I. Introduction

Distillation, a unit operation, is referred to the physical separation of two or

more components in a mixture with varying boiling point temperatures, by
boiling out the more volatile components (Kister, 1992). The principle of
distillation has applications in a laboratory and an industry scale, especially in
food and drug processing. This experiment aims to recycle biodiesel by
separating glycerol from water through simple distillation. To attain this, the
following sub-objectives are assigned: (1) to determine the mole percent
composition of the water-glycerol and methanol-water mixture, (2) to prepare
and understand the components and the concepts behind a simple distillation
setup, (3) to interpret temperature vs volume plots and boiling point curves, and
(4) to analyze the effect of atmospheric pressure to boiling point temperature.

II. Theory

Distillation is the separation process of different components in a liquid

solution depending on the component’s distribution between liquid to vapor
phase, which are present in both phases (Geankoplis, Hersel, & Lepek, 2018).
In process industries, this method is the most utilized and practical fluid
separation technique (Olujić, Jödecke, Shilkin, Schuch, & Kaibel, 2009). The
process of distillation is divided into two processes: evaporation and
condensation (Lagi & Chase, 2009). Upon heating the solution, the more
volatile component would turn into vapor first, and the less volatile component
would remain in the distillation setup (Lei, Li, & Chen, 2003). Also, boiling point
refers to the temperature at which the solution’s vapor pressure is the same as
the surrounding atmospheric pressure (Zubrick, 2016).

Glycerol is a polyol compound, naturally found in triglycerides which are the

fatty acid compounds (García, García-Marín, & Pires, 2014). Meanwhile,
methanol is colorless, transparent, and volatile liquid compound which is also
an acid-base neutral, non-corrosive, polar compound (Yang, 1994). The boiling
point of glycerol is around 253 to 307 °C while methanol is around 64.7 °C
(García, García-Marín, & Pires, 2014; Yang, 1994). Lastly, water is an inorganic
compound made of an oxygen atom and two hydrogen atoms which exists in
three states: solid, liquid, and vapor phases (Eisenberg & Kauzmann, 2006).
With its chemical composition, it is known to have a melting point of around 0
°C and a boiling point of around 100 °C (Eisenberg & Kauzmann, 2006).

III. Methodology
 School of Chemical, Biological and Materials Engineering and Sciences

The chemical or reagent needed for this experiment was the biodiesel waste
or the glycerol-water mixture. Moreover, the apparatus or equipment utilized
for the distillation setup were a condenser tube, a heating mantle, hose for
cooling water, a laboratory jack, a thermometer, 3 pcs. of 100 mL volumetric
flasks, and a 250 mL volumetric flask. The summarized step-by-step procedure
for simple distillation was presented in Figure 1.

Figure 1. Process Flow Diagram for Simple Distillation

IV. Results

The plot of the volume of distillate collected as the temperature rise in the
distillation set-up containing the water-glycerol solution was displayed in
Figure 1 while for the methanol-water solution was shown in Figure 3. Also,
the boiling point composition curves for each of the sample mixtures was
presented in Figure 2 for the water/glycerol mixture and in Figure 4 for the
methanol/water mixture.
 School of Chemical, Biological and Materials Engineering and Sciences

Figure 1. Temperature vs Volume of Distillate Plot of Water-Glycerol

Mixture

Figure 2. Boiling Point Curve of Water-Glycerol Mixture

Figure 3. Temperature vs Volume of Distillate Plot of Methanol-Water

Mixture
 School of Chemical, Biological and Materials Engineering and Sciences

Figure 4. Boiling Point Curve of Methanol-Water Mixture

V. Discussion

In summary, the experiment was able to separate water from the water-
glycerol mixture but was not able to separate methanol from the methanol-
water mixture through distillation. It is because, looking at Figure 1, the volume
of the distillate both plateaued at 100 °C and 300 °C which were around the
boiling point temperature of water and glycerol, respectively. It means that the
water was first evaporated and condensed in the set-up and after the water
was gone, glycerol was then distilled at a different temperature. While, in
Figure 3, it is also observed that at 290 °C most of the water was already
evaporated and no water exists at the liquid phase. We can say that the water
in the mixture evaporated while the glycerol remained liquid.

The otherwise cannot be said for the methanol-water mixture. That is

because, the plot of the distillate volume per temperature in Figure 2 indicated
that there is no specific temperature at which the volume of the distillate
increased. It is shown that as the temperature increased both the methanol and
water component in the mixture was evaporated and condensed in the
experiment. It is because the boiling points of the components are very close
to each other, which the boiling point temperature for water is around 100 °C
and around 64.7 °C for methanol. It can also be said that no component is
relatively more volatile to the other.

After performing the experiment, it can be concluded that the mole percent
of the water-glycerol mixture and the methanol-water mixture was determined
from the moles of the solute and the moles of the solution, which were used as
one of the variables or components of the boiling point composition curves.
 School of Chemical, Biological and Materials Engineering and Sciences

Also, the experiment was also successful in providing knowledge on how to

build a simple distillation set-up, on how the distillation process work, and what
are concepts and theories behind distillation. Lastly, we were able to interpret
boiling point curves and analyze how pressure and temperature affect the
boiling points of substances or mixtures.

VI. References
a

Eisenberg, D., & Kauzmann, W. (2006). The Structure and Properties of Water
(1st ed.). Oxford: Oxford University Press.

García, J. I., García-Marín, H., & Pires, E. (2014). Glycerol based solvents:
synthesis, properties and applications. Green Chemistry, 16, 1007-
1033. doi:10.1039/c3gc41857j

Geankoplis, C. J., Hersel, A. A., & Lepek, D. H. (2018). Transport Processes

and Separation Process Principles (5th ed.). London: Pearson
Education, Inc.

Kister, H. Z. (1992). Distillation Design (1st ed.). New York: McGraw-Hill, Inc.

Lagi, M., & Chase, R. S. (2009). Distillation: Integration of a historical

perspective. Australian Journal of Education in Chemistry, 70, 5-10.

Lei, Z., Li, C., & Chen, B. (2003). Extractive distillation: A review. Separation &
Purification Reviews, 32(2), 121-213. doi:10.1081/spm-120026627

Olujić, Ž., Jödecke, M., Shilkin, A., Schuch, G., & Kaibel, B. (2009). Equipment
improvement trends in distillation. Chemical Engineering and
Processing: Process Intensification, 48(6), 1089-1104.
doi:10.1016/j.cep.2009.03.004

Yang, B. L. (1994). Physical and Chemical Properties and Handling Aspects.

In W. -H. Cheng, & H. H. Kung, Methanol Production and Use (pp. 23-
50). New York: Marcel Dekker, Inc.

Zubrick, J. W. (2016). The Organic Chem Lab Survival Manual: A Student's Guide
to Techniques (10th ed.). Hoboken: John Wiley & Sons, Inc.

VII. Appendices
 School of Chemical, Biological and Materials Engineering and Sciences

Calculating for Mole Percent of Water

moles of solute
%mole = mole fraction x 100% = x 100%
moles of solution
4 moles H2 O
= x 100%
4 moles H2 O + 1 mole glycerol
= 80 %