Department and Institution: Chemical, Metallurgical and Materials Engineering

The following proposal is submitted for registration of the degree Master Of Engineering
(MEng) In Chemical Engineering

Research Topic: Purification of crude glycerol from the biodiesel

production using waste cooking oil, Process optimisation using simulation
software (DWSIM)

Names: Xaba Nosizwe

Student Number: 222892678

Email address: [email protected]

Supervisor: Dr Shongwe

Co-Supervisors: Mr Mosesane & Ms Boinotlo

ABSTRACT

The world population is heavily relying on fossil fuels as a source of energy, resulting in
concerns of over depletion. Biomass meets different energy needs such electricity generation,
vehicle fuels as well heating purposes. Biomass conversion technologies into bioenergy and
biofuels must be modernized to be sustainable. Biodiesel has desirable properties which
makes it a feasible substitute to the fossil fuels. In this study, the biodiesel will be produced
from a waste cooking oil collected from the campus cafeteria through transesterification
reaction. Surplus of crude glycerol has increased due to an increased demand in the biodiesel
production, necessitating the research of sustainable processes that could convert the crude
glycerol into higher value-added products. The study intends on closing the loop in the
sustainability of the biodiesel production .In this work, waste cooking oil is trans esterified to
produce biodiesel, and the glycerol produced is purified. With modest lab apparatus, studies
will be carried out first, and once the ideal level of purity has been established, the
computational model will be used to optimize the vacuum distillation of glycerol purification.
1.0 INTRODUCTION

1.1 BACKGROUND

The energy markets worldwide heavily depend on fossil fuels, which are subjected to
depletion. The rapid growth of renewables is mostly driven by the rising global concern on
global warming related issues (Iqbal et al 2021). A lot of research work has been done into
advancing the technologies of converting biomass into biofuels(Jeswani,Chilvers and Alzapic
2020).

Biomass conversion technologies commonly used are grouped into two categories, thermal
and chemical. Thermal conversion technologies makes use of heating methods to convert
biomass, gasification process is used to produce syngas and pyrolysis to produce tar or bio-
oil. Chemical conversions make use of chemical reagents to convert biomass into liquid
fuels , anaerobic digestion to produce bio-gas and transesterification to produce
biodiesel(Quaver and Ahmed 2017).

Vegetable oil has received a lot of attention as a renewable energy resource that can help
reduce greenhouse gas emissions. Although pyrolysis, dilution with liquid hydrocarbon, and
emulsification can all be used to convert vegetable oil to fuel oil, transesterification with
methanol is the most practical method(Tan et al 2023).

Transesterification is a chemical process that uses a low-molecular-weight alcohol (typically

methanol) to convert vegetable oils and animal fats into methyl esters and glycerol in the
presence of a catalyst. Factors that influence transesterification are the reaction temperature,
alcohol type, molar ratio of alcohol to vegetable oil, catalyst type, amount of catalyst, mixing
intensity, and FFA content of the vegetable oils(Lee 2015).

It is reported that approximately 10% of crude oil is produced as a byproduct in a

transesterification reaction to produce the biodiesel oil. Potential glycerol applications which
have been discovered in order to ensure that the economic viability of biodiesel production as
a whole is improved (Moklis et al 2023). Crude glycerol has properties which makes it not
suitable to be directly used as a fuel in diesel engines. Therefore, converting it into
oxygenated fuel through etherification reaction to be used as a fuel additive will ensure that
the biodiesel production is sustainable (Cakmak & Ozcan 2020)
1.2 PROBLEM STATEMENT

The world’s ever-increasing energy demand has influenced the usage of biofuels with
biodiesel gaining more popularity due to its favourable properties. During the
transesterification reaction ,10wt% of glycerol is produced with 90wt% of biodiesel.
An increase in biodiesel production will lead to an increase in surplus of glycerol
which is very costly to safely dispose of .Crude glycerol cannot be used as fuel
additives on engines it needs to be refined and purified first.

1.2.1 Sub-Problems

1. Edible feedstocks are expensive and threatens the population’s food

security.

2. Glycerol is highly sensitive to heat and its compounds easily split into water
and quickly decomposes when put through separating units.

3.The purity of glycerol during vacuum distillation is affected by different

factors including internal velocities inside the vacuum, packing columns

1.3 HYPOTHESIS

1.The purity of the glycerol increases with each purification step

2.Vacuum distillation is the most energy efficient method of achieving highest purity
of glycerol
1.4 RESEARCH OBJECTIVES

1.4.1 Main Objective

The main objective of this research is to purify the glycerol which is a by-
product of biodiesel production and use the computational modelling
tools( DWSIM) and simulation techniques optimize the purification process
and improve purity.

1.4.2 Sub-Objectives

1. To characterize the biodiesel produced from transesterification reaction.

2. To obtain chromatographic analysis of crude glycerol before purification
and after the purification

3. To study the effects of different factors on the purity of glycerol in a

vacuum distillation simulation.

4. T compare the percentage purity obtained from experimental data and the
data obtained from DWSIM results.

1.5 DELIMITATIONS

At this point of the study no limitations have been discovered.

1.6 INNOVATION

The literature has shown that several alternatives to purify has been exploited and the
goal of achieving the desired purity was never met. This study will explore the
sequence of low cost and energy efficient routes to increase the glycerol purification.

1.7 Significance of the study

 This work intends on exploring easiest and energy efficient methods of purifying the
glycerol obtained from the biodiesel production. A computational simulation
( DWSIM ) will be used to optimize the operating operations of the vacuum
distillation in purifying glycerol.

2.0 LITERATURE REVIEW

2.1. INTRODUCTION

Many different sources produce waste cooking oil, including large industrial users like power
plants and manufacturing firms, as well as residential homes, dining establishments, and food
factories. Urban areas produce large amounts of waste cooking oil, which are currently
disposed of primarily in landfills (Joshi 2023). In the automobile industry, biofuels have
gained increased attention as a viable alternative to gasoline and diesel fuels (Ritchie 2020).
Vegetable oils and animal fats are used to make biodiesel, a renewable fuel for diesel
engines. These feedstocks can create a variety of biofuels, including biodiesel, bio alcohols,
and biogas. (Azad 2023). In this research, attention will be focused on waste cooking oil as
the feedstock for biodiesel production

A byproduct of the transesterification process that yields biodiesel is glycerol. It is also

referred to as glycerin, 1,2,3-propanetriol, or glycerol chemically. When transesterification is
aided by a homogeneous alkali catalyst, water, inorganic salts, soaps, fatty acids, and methyl
esters are the main contaminants that end up in the glycerol. (Tan 2023). Simple distillation is
unable to extract glycerol because it retains water in a stable chemical combination. As a
result, the majority of anhydrous glycerol is produced from pure glycerol that has undergone
water removal procedures. Purified glycerol is defined as glycerol that is 99 percent pure or
above (Vavra 2021).The conventional technique for analysing glycerol quantitatively
involves titrating a standard sodium hydroxide solution. Impurities can cause a shift in the
titration curve's end point, which will impact the accuracy of the result.

Sustainable and economic method for glycerol purification and production of value-added
products is highly desired. Among current glycerol purification technologies, distillation is
the most commonly used technique (Lima 2022).The use of computational simulation to
improve glycerol purification operating conditions has been the subject of extensive research
recently. One possible result of the simulation model's application would be its ability to
monitor the impact of various operational parameters and provide "what if" answers in order
to optimise the distillation process for the purification of glycerol (Silva 2023).

2.2. REVIEW OF PUBLICATIONS IN THE LITERATURE

2.3.1. Review of Literature on Problem Definition and Formulation

The world global energy demand is expected to steadily increase in the next coming decades.
The increase in energy demands poses a huge threat on the environment resulting from the
carbon emissions (Kour et al 2019).The main sources of air pollution are vehicles used for
transportation ,followed by emissions from manufacturing plants as reported by Qiang et al
2020. For the purpose of ensuring global energy stability and security, scientist’s focus is
more on discovering the alternative reliable energy sources with biodiesel being the most
preffered biofuel due to its desirable properties.There are different feedstocks that can be
used in the biodiesel production, grouped into the first, second and third generation
feedstocks.

The world food organization has put in strict restrictions to the usage of edible oils as main as
main feedstocks in biodiesel .The extensive use of edible oils threatens the food security
worldwide and mostly in developing countries.(Ramli et al 2017).

According to the department of Energy in SA(2016), about 99000 litres of waste cooking oil
is produced by resturants,fast food outlets and households per month in South Africa.The
huge portion of this amount is not correctly disposed and therefore contribute directly to
environmental pollution(Langaniso et al 2022). The waste management technologies has
evolved through the years ,and waste cooking oil is recycled to be used in the production of
biodiesel fuel.If a kilogram(g) of waste is recycled, about 2,8kg of carbon emission is
reduced and this contributes immensely to the green environment(Attari 2022).

Biodiesel production via transesterification produces 10wt % of glycerol as a by-product. For

every one ton of biodiesel produced, 10 kg of glycerol is glycerol is produced (Raman et al
2019).The increase in the demand of biodiesel production results in excess surplus of
glycerol.The glycerol that is produced from thr biodiesel has low commercial value because it
contains impurities such methanol,salt,oil and other organic matter(. Gholami et al
2014).More research has been made around the valorisation of crude glycerol as well as
different methods to turn it into high-value chemicals.

In an adsorption study conducted by Anza et al, bentonite was used in purification of

glycerol. The bentonite was 1,5M sulphuric acid and the purity obtained was 89,5 wt
%.Several studies has shown the membrane technology to purify glycerol to be the most
exciting option because it requires low energy and also easy to operate ,however it is
impossible to optimize the technology in an industrial scale (Dhabhai 2024).For a glycerol to
be effectively purified , the purity must be 99.77w/w% , therefore it is very important to
reduce the cost of this phase as much as possible.The optimization of vacuum distillation will
ensure that the performance is enhanced and higher glycerol purity is achieved(Braga 2023).
Setyaningsih 2017 produced triacetin which can used as an additive through esterification of
glycerol with acetic acid using lewatit catalyst. The highest glycerol conversion reported
from this study was 66,7 % with 3% catalyst weight while the lowest being 56.28 % with 2%
catalyst weight.

2.3.2. Review of Literature on your topic (Material, process, application)

Transesterification is a chemical process that uses a low-molecular-weight alcohol (typically

methanol) to convert vegetable oils and animal fats into methyl esters and glycerol in the
presence of a catalyst. Factors that influence transesterification are the reaction temperature,
alcohol type, molar ratio of alcohol to vegetable oil, catalyst type, amount of catalyst, mixing
intensity, and FFA content of the vegetable oils (Lee 2015).

Babel et al (2016) successfully carried out transesterification of waste cooking oil using
KOH as a heterogenous catalyst through the microwave with the assistance of conventional
heating .An overall biodiesel yield obtained was 91,3% with following reaction conditions :
catalyst kept at 5wt% ,the alcohol toil ratio at 12:1 and a reaction temperature at 40 ℃.In an
optimization carried out by Hamza et al 2021 to obtain the maximum biodiesel yield it was
found that the transesterification must be carried out on the following conditions : the catalyst
weight percent must be 1wt% , with the reaction temperature kept at 18 ℃ for 60
minutes .The biodiesel yield obtained was 99,1 %.The feedstock used in this study was
soybean.
Several options for purification of glycerol includes the treatment with ethanol and activated
carbon, using the membrane technology as well as using vacuum distillation in an atmosphere
with the highest purity obtained from the distillation method(Pott 2014).Pitt 2019 used three
step method of glycerol purification ,neutralisation followed by liquid-liquid extraction and
finally vacuum distillation .The glycerol was characterised after each purification step and it
was observed that the glycerol purity improved each time it was characterized.

A study was conducted by Olivera 2022 whereby ASPEN Plus was used to improve the
purification of glycerol. An additional heat exchanger in the vacuum separator component
accounts for an increased mass flow of 40%. The study indicated that the temperature from
the separator as well the feed flow has an impact on the mass flow. An increase in these will
results in an increased flow. The overall purity of 99.7% was achieve

3.0 METHODOLOGY

3.1 RESEARCH APPROACH

For this study, a quantitative research approach will be used as it is more scientific and
rational. With the literature support, standardized experimental procedures has been
developed. A laboratory bench scale will used for conducting all the experiments as per the
study’s objectives. A surface response methodology will be used to verify the reliability of
the data,

3.2 MATERIALS AND SITE SELECTION

Titration to determine free fatty acids (FFA)

Filter the waste vegetable oil to remove any impurities, and heat the oil at 100 for 60 min to
ensure that there are no water droplets. Using Erlern Meyer flask add 1 g of oil sample with
10 ml of isopropyl alcohol. Add 4 drops of a phenolphthalein indicator. Now begin with
titration using KOH as a titrant and as soon as purple pink color occurs measure the end
point. Using the equations below, the FFA % was then calculated. Titration will be performed
three times and the therefore the average will be calculated. If the value is 1,5 % then
transesterification reaction will be carried out.

Transesterification

A phenolphthalein will be used as an indicator during the titration of the waste cooking oil in
order to determine the amount of FFA present in the oil sample produce the biodiesel, the
transesterification reaction will be carried out using waste cooking oil as feedstock, with
methanol in a presence of KOH as a catalyst. The potassium hydroxide is chosen for this
reaction because it is heterogenous and therefore it does not need to separate from the product
chemically, also it can be re-used. Other laboratory apparatus includes glass beakers, stirrer,
weigh boats, condenser, pipes and double neck round bottom flask for building up the reactor
system. The oven will also be utilized for heating samples

Glycerol Purification

Titration will be the first to determine the amount of acid needed to neutralise the glycerol
residue. The main reason for neutralizing the residual is to promote the separation of salts and
soaps in the glycerol. In the titration ,1g of phosphoric acid will dissolved in 50ml of distilled
water. Bromophenophtalein will be used as an indicator. The end point will only be realised
when the solution changes from the blue colour to yellow. Therefore, the amount of acid
needed to neutralise glycerol will be determined.

The second step following the titration will be the neutralisation of glycerol by the addition of
phosphoric acid. The salt will be formed from neutralisation and in order to remove the salt,
liquid-liquid extraction method will be used. A 2l reactor with a stirrer and a heat source will
be used. The glycerol will first be heated to 60 degree Celsius then acid added with a stirring
speed of 40rpm for 30 minutes.

Vacuum filtration will be used the next step to remove the salt from the phosphoric acid. The
neutralised glycerol mixture will be kept at 60 degree and poured onto balloon flask and
allowed to settle over 24hrs. The mixture will be separated into two liquids phases with the
top being the liquid free of fatty acids and will be discarded and the bottom will be the
glycerol with decanted traces of potassium phosphate salts.

vacuum is the last purification step. It will be conducted at 120 degree Celsius to remove the
water and salts from glycerol

A vacuum distillation set up will be used for the glycerol purification. A round bottom flask
will be used as a receiving medium. The rest of the apparatus will be connected to the set up
to have a complete vacuum distillation set up. The apparatus needed for the this set up
include: condenser, thermometer, clamps, y-adapter, tygon tubing

Process Simulation
An open source simulator called DWSIM will be used for the simulation of the vaccum
distillation unit .DWSIM has a component library which is registered with accordance to the
UNICAF methodologies.

3.3 RESEARCH METHODS

3.3.1. Design of Experiments (DOE)

Central Composite Design with 5 level point will be used for this study. Different factor
which affect the purity of glycerol includes PH, reaction time, stirring speed, reaction time
, H 2 S O4 dosing. The design expect will be used for the analysis of variance, response
surface. The mathematical model for the experimental design will be selected on the basis p-
value

3.4 CHARACTERISATION

Gas Chromatography will be used to obtain the fatty acid profiles of the FFA present in the
glycerol. The FAME analysis will also be done to confirm the formation of soaps during
saponification.

To determine the presence of different functional groups, present in the purified glycerol, and
Infrared Spectroscopy analysis will be carried out. The spectra will be generated from the
experimental data. The crude glycerol will be compared to the purified glycerol.

3.5. DATA COLLECTION

Experiments will be carried out for the purpose of collecting data for this study. With the help
from the literature the experiments procedures have been lined out to gather preliminary data.
The data will be recorded and analysed.
For the simulation part of this study, the thermodynamic packages WILSON and NRTL will
be used to obtain simulation input data.

6. BUDGET AND PROJECT TIMELINE

6.1 Project Timeline

6.2 Project Budget

Material Price
CHEMICALS
Isopropyl alcohol
Phenolphthalein
Potassium hydroxide
Phosphoric acid
Bromophtalein
LABORATORY APPARATUS
Erlenmeyer flask
 Glass beakers
Weigh boats
Condenser
Pipes
Round bottom flask
Clamps
Tygon Tubing
Thermometer

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