Durban University of Technology

Department of Chemical engineering

Title: Biodiesel Test rig








Authors full names and student numbers
Hermenegildo Bernardo Sacagica 21334144
Jeusa Rosria De Oliveira Manuel 21334141
Llia Rossana Carvalhda Da Costa 21334137

21/07

Submitted in partial fulfillment of the requirements for Chemical Process Design III in the
Department of Chemical Engineering, Durban University of Technology
i

Preface
The present project, Biodiesel test rig, was carried out at Durban University of Technology,
Steve Biko Campus, S3 level 01. The project was supervised by Mrs Nirvana Naidoo at
chemical Engineering laboratory. This project contains information about the biodiesel test
rig and biodiesel full scale plant that may be implemented at the university. The
instrumentation of the rig has been addressed, as well as some considerations about the cost.





















ii

Declaration
We hereby declare that the project report entitled Biodiesel test rig submitted to Durban
University of Technology is a record of original work done by us, under the guidance of Mrs
Nirvana Naidoo, Chemical Engineering Department. Any ideas taken from other sources will
be acknowledged as such.
Student names Student numbers Signatures
Costa L.R.C. 21334137
Manuel J.R.O. 21334141
Sacagica H.B. 21334144



















iii

Acknowledgements
First off all we would like to thanks God for giving us the strength and motivation for the
completion of the report. We want also to thank our lecturer Mrs Naidoo for her guidance and
supervision. Finally we would like to express our special gratitude to our parents and friends
who have willingly helped us out.






















iv

Abstract
Biodiesel production is worthy of continued study and optimization of production procedures
because of its environmentally beneficial attributes and its renewable nature. At Durban
University of Technology large amounts of oil used for frying foods are discarded each year
into sewage systems. Thus, it adds to the cost of treating effluent or pollutes waterways. The
objective of this project is to design a test rig to process 1kiloliter of used cooking oil per day.
into fuel grade biodiesel and consider aspects related to the feasibility of the production of
biodiesel from waste oils in an attempt to help reduce the cost with fuel and reduce waste and
pollution coming from waste oils. A small scale biodiesel 0.5m
2
and 0.62m test rig was used
to determine the optimum parameters to design a full scale plant. Residence time and reaction
temperature were investigated. The achieved results were analyzed and a set of
recommendations was proposed. All the runs were done at an oil/ ethanol ratio of 5 : 7,
refined sunflower oil was used for the experiment, and the results were assumed to be the
same as that of cooking oil. From the obtained results, the optimum process conditions was
achieved on 2 hours run and 50
0
C. From the optimum parameters the requirements of the
full scale plant were found to be:
A reactor vessel of 0.21 m
3
capacity 0.37m diameter
Oil container 8.33*10
-5
m
3

Ethanol container 1.167*10
-4
m
3

A pump of 20 Watts
A double pipe heat exchanger consisting of two 1.9 m long tube connected by 180
bend with an outer diameter of 21.3 mm and inner diameter of 17.1 mm

PVC pipe with approximate total length of 8m

One industrial thermometer
Net power requirement of 320.64 Watts
The full scale plant was design for an approximate area of 6 m
2
. The running cost will be
approximately R per day. The project was considered to be feasible, as it will minimise the
cost with diesel for a long term period at the university. Will reduce the cost with waste
disposal and some profits can be obtained from sale or transformation of the glycerin into
usable products. Furthermore, the biodiesel production is environmentally friendly, as it will
reduce the carbon foot print and toxic gases emissions (SOx, NOx and Cox).
For the construction of the rig goggles and hard hat must be used to avoid injuries.





v


Table of content
Preface ..................................................................................................................................................... i
Declaration .............................................................................................................................................. ii
Acknowledgements ................................................................................................................................ iii
Abstract .................................................................................................................................................. iv
1.Introduction .......................................................................................................................................... 1
2.Literature review .................................................................................................................................. 2
2.1. Biodiesel .......................................................................................................................................... 2
2.1.1.Biodiesel Production ...................................................................................................................... 2
2.1.2.South Africa specifications for diesel and biodiesel ...................................................................... 4
2.1.2.1.Biodiesel specifications............................................................................................................... 4
2.1.2.2.Diesel specifications ................................................................................................................... 7
2.2.Theory ............................................................................................................................................... 8
2.2.1.Operating principles and relevant theory of each unit operation of the constructed test rig. ......... 9
3.Material and Methods ........................................................................................................................ 11
3.1.Equipment ....................................................................................................................................... 11
3.1.1.List of materials used for the test rig ............................................................................................ 11
3.1.2.Piping and Instrumentation Diagram of the test rig ..................................................................... 12
3.1.3.Engineering drawing of key components ..................................................................................... 13
3.1.4.Diagrams/photos describing the equipment ................................................................................. 14
3.2.Procedure ........................................................................................................................................ 16
3.2.1.Residence time test: ..................................................................................................................... 16
3.2.2.Reaction temperature ................................................................................................................... 16
3.3.Analytical ........................................................................................................................................ 16
4.Data Analysis and Evaluation ............................................................................................................ 18
5.Full scale plant Design ....................................................................................................................... 22
5.1.Full scale plant requirement ............................................................................................................ 22
5.2.Operational method ......................................................................................................................... 22
5.3.Process and Instrumentation Diagram of the full scale plant .......................................................... 23
5.4.Cost benefit analysis ....................................................................................................................... 24
5.5.Safety aspects .................................................................................................................................. 24
vi

6.Conclusion ......................................................................................................................................... 26
7.References .......................................................................................................................................... 27
8.Appendices ......................................................................................................................................... 28

List of tables
Table 1 - Requirements for biodiesel according to SANS 1935(edition 2, 2011) .................................. 4
Table 2 - Diesel specifications according to SANS 342:2006 (edition 4, 2006) .................................... 7
Table 3- Residence time ........................................................................................................................ 18
Table 4-Reaction temperature ............................................................................................................... 19
Table 5- Raw data ................................................................................................................................. 28

List of figures
Figure 1- Block diagram of a complete biodiesel rig ............................................................................ 10
Figure 2- Block diagram of a the biodiesel test rig ............................................................................... 14
Figure 3- Entire test rig picture ............................................................................................................. 14
Figure 4- Oil and alcohol lines .............................................................................................................. 15
Figure 5- Reactants container ............................................................................................................... 15
Figure 6-Reactor vessel ......................................................................................................................... 15
Figure 7-Pump ...................................................................................................................................... 15
Figure 8- Double pipe heat exchanger .................................................................................................. 15
Figure 9- Biodiesel yield versus residence time ................................................................................... 18
Figure 10 - Chart of Biodiesel Final Volume versus Temperature ....................................................... 19











1

1. Introduction
In order to safeguard the environment and protect people from inhalation of toxic substances,
several strategies for cleaner burning are being developed and implemented.
Exhaust products from petroleum, especially diesel is regarded as being carcinogenous and
toxic in nature, since they contain polycyclic aromatic hydrocarbons. Apart from these
reasons, there has also been a rise in the prices of petroleum products, which means rise in
electricity and fuel. Emissions of greenhouse gases associated to the energy consumption
leading to catastrophic environmental consequences.
The department of Chemical Engineering at DUT has implemented strategies like cleaner
production, sustainable development, Green Engineering, process integration, waste
minimisation, etc. The main goal is to replace diesel with biodiesel. Used cooking oil from
the university cafeterias and large scale kitchen operation in the Hotel school is to be
converted to fuel grade biodiesel. Biodiesel is an alternative fuel produced by trans-
esterification of the vegetable oil or animal fat. It can be blended with traditional petroleum
diesel or used directly in diesel vehicles. The reaction to produce biodiesel is as follow:


In this project a biodiesel test rig was built to accommodate the initial test work. The
objectives for the project were set out to be:
To run and commission the biodiesel test rig
To conduct an extensive feasibility study to determine economic, environmental and
social benefits for this project.
Use experimental data results to design a biodiesel plant that can process 1 kilolitre of
used cooking oil per day.

This work was worthy being done because it can contribute for:
Reduction in NOx, SOx, Cox emissions, since biodiesel is cleaner fuel.
Reduction in purchases of fossil fuel derived diesel- cost saving.
Reduction in carbon foot print
Reduction in waste disposal costs.




2

2. Literature review
2.1. Biodiesel
Any fuel that has appropriate properties can be used to fuel a diesel engine. If the properties
of the alternative fuel match the properties of the fuel that the engine is designed to run, it can
be used in the engine without any modification. Biodiesel is the most suitable alternative fuel
for diesel engines, because it can be used on an unmodified engine and due to the fact that it
is considered a sustainable fuel source.
Biodiesel can be used in pure form (B100) or blended with petroleum diesel at any
concentration. Most part of the world uses a system known as the "B" factor to state the
amount of biodiesel in any fuel mixture:
100% biodiesel is referred to as B100
20% biodiesel, 80% petrodiesel is labelled B20
5% biodiesel, 95% petrodiesel is labeled B5
2% biodiesel, 98% petrodiesel is labeled B2
Blends of 20% biodiesel and lower can be used in diesel equipment with no, or only minor
modification. Using biodiesel (B100) in pure form may require certain engine modifications
to avoid maintenance and performance problems.
2.1.1. Biodiesel Production
Biodiesel refers to a diesel-equivalent, long-chain alkyl esters that are produced by reacting
lipids with an alcohol in a presence of a catalyst. It is defined by the World Customs
Organization (WCO) as a mixture of mono-alkyl esters of long-chain (C7-24) fatty acids
derived from animal fat or vegetable oil. Despite being energetically benignant, direct use of
straight vegetable oils in fuel engines is not advisable. Due to the high viscosity (about 11 to
17 times higher than diesel fuel) and low volatility, they do not burn completely and may
form deposits in the fuel injector of diesel engines. Furthermore, a highly toxic substance
(acrolein) is formed through thermal decomposition of glycerol (Schuchardt, 1998). Different
methods of biodiesel production have been reported. These includes: trans-esterification
(Ma and Hanna, 1999), blending of oils, microemulsion and pyrolsis. This report will be
focus on trans-esterification method which is suitable for waste oil applications
Trans-esterification: involves stripping the glycerine from the fatty acids with a catalyst
such as sodium or potassium hydroxide and replacing it with an anhydrous alcohol that can
be methanol or ethanol. The resulting product is then centrifuged and washed with water to
cleanse it of impurities. This results in methyl or ethyl ester (biodiesel) and glycerol, a
valuable by- product used in making cosmetics, soaps and numerous other products. Trans-
esterification from oil/fat includes:
Acid-catalyzed trans-esterification.
Base-catalyzed trans-esterification.
3

Enzymatic conversion (lipase-catalyzed).
Non-catalytic conversion (supercritical process.
Ultra-and high in-line and batch reactors.
Ultrasonic reactor method
Acid catalyzed method
Acid catalysis is used when free fatty acid content is greater than 1 percent in the feedstock
because using base catalyst undesired product can be produced such soap that prevent the
separation of ester, glycerol and wash water. It has been proved that is possible to produce
ethyl esters from cooking oil using acid catalyst. Strong acid such as sulfuric and phosphoric
acid are used in most of the cases. The advantage of using it is the absence of alkali metals in
the system because it may avoid the formation of soap. And the disadvantages are:
- The trans-esterification reactions of triglycerides take days for completion.
- Are used large amount of strong acid which may be more expensive.
Base catalyzed method
It is one of the cheapest methods used to produce biodiesel. Is highly recommended to use
less than 0.1 percent of free fatty acid, 0.1 percent of moisture and 10 ppm (part per million)
of phosphorous content. High level of free acid content can cause side reaction and produce
soap which reduces the actual yield. Palm oil and fat from animal are not suitable to produce
biodiesel due to its high free fatty acid on the other hand there are some sources commonly
used that are: Canola, soybean, cottonseed, palm kernel and sunflower.
The bases catalysis most used are sodium hydroxide (NaOH), potassium hydroxide (KOH)
and sodium methoxide (CH
3
ONa). They react easily with water and free fatty acids. The
disadvantage of using base catalysis is the reminiscent soap formation.
Lipase-catalyzed method
Good yield is obtained when lipase is used as raw material to produce biodiesel. Although
this method has many advantages over the traditional base catalyzed method but cost and
instability of lipase limits the industrial applications. And also methyl acetate is used instead
of methanol because it inactivates the catalyst.
Supercritical process
Is a continuous process in which supercritical methanol is used at high pressures and
temperatures. It is a non-catalytic process where a rapid and spontaneous reaction between oil
and methanol occurs. The process has the advantages of allowing water in the feedstock since
it is vaporized due to high pressure and temperatures, the reaction take less time and there is
no possibility of forming soap. However the energy cost is very high.


4

Ultra-and high-shear in-line and batch reactors
The reaction occurs when small droplets of oil and methanol are mixed in the shear zone of
the reactor. This process has the advantage of producing high volume of biodiesel in short-
time, and the velocity of catalyst is increased because of the small droplets size.
Ultrasonic reactor method
The trans-esterification process is carried out by heating and mixing the components in the
ultrasonic reactor using ultrasonic waves. The advantages of this process are:
- Energy input, temperatures and reaction time are reduced by the use of ultrasonic
reactor.
- Many thousands of barrels per day in industrial scale are produced using
ultrasonic equipments.
As the major part of the biodiesel worldwide comes from virgin vegetable oils, base-
catalyzed method is the most used being the cheapest process when treating virgin vegetable
oils. It requires low temperatures and pressures and produces over 98% conversion yield as
long as the starting oil hasa low percentage in free fatty acids (Refaat, Attia, Sibak, El
Sheltawy and ElDiwani, 2008, 75-81).
2.1.2. South Africa specifications for diesel and biodiesel
2.1.2.1. Biodiesel specifications
The biodiesel specifications in South Africa are accomplished through the rules specified in
what is called SANS 1935. This is a combination of different tests and values that must be
achieved by the biodiesel before being considered good for use examining some important
chemical and physical properties. A basic test for biodiesel involves some of the properties
such as viscosity, water content, acidity, free glycerol, density, appearance, total glycerol and
flash point, and certain requirements can be achieved.
Table 1 - Requirements for biodiesel according to SANS 1935(edition 2, 2011)
Properties Requirements Units Test Method
Methyl ester amount 96,5 % (m/m) EN 14103
Copper strip corrosion (3hrs at 50
)
Class 1 Rating ISO 2160
Density at 15 860-900 kg/cm ISO 3675
Oxidation stability at 110 6 Hrs EN 14112
Kinematic viscosity at 40 3,5 5,0 mm
2
/s ISO 3104
Acidity 0.5 mg KOH/g EN14104
Flash point 120 ISO 3679
Iodine value 140 g I/100g EN 14111
Sulphur content 10 mg/kg ISO 20846
Linolenic acid methyl ester 12 % (m/m) EN 14103
Carbon residue (on 10% distillation 0,3 % (m/m) ISO 10370
5

residue)
Polyunsaturated methyl esters 1 % (m/m) -
Cetane number 51 - ISO 5165
Methanol content 0.2 % (m/m) EN 14110
Sulphated ash content 0,02 % (m/m) ISO 3987
Monoglyceride content, % mass
fraction
0.8 % (m/m) EN 14105
Water content, % mass fraction 0,05 % (m/m) ISO 12937
Diglyceride content, % mass
fraction
0.2 % (m/m) EN 14105
Total contamination, mg/kg 24 mg/kg EN 12662
Triglyceride content, % mass
fraction
0.2 % (m/m) EN 14105
Free glycerol, % mass fraction 0.02 % (m/m) EN 14105
Data taken from
(http://www.greendiesel.co.za/index.php?option=com_content&view=article&id=18&Itemid
=45)
Copper strip corrosion: this test is used to indicate the presence of acids and corrosive
metals. There are some components making part of the engine may be attacked by acids if
consist of copper or bronze.
Density: is used to indicate the degree of completion of reactions.
Oxidation stability: indicates the storage time of a product before it can react with oxygen
molecules and form peroxides.
Kinematic viscosity: is a test which measures the ability of liquids to flow. It is very
important around the injector nozzles and the fuel pump as if the fuel has a high viscosity it
can cause some strain on the fuel pump and therefore, it can lead to failure.
Acidity: measures acidic groupings in the final product. The acids can be produced from the
acids that were used during the initial process and not removed, and from the acids present in
the free fatty acids.
Flash point: gives the ignition temperature of a fuel. It can be used to provide right
information about how to handle it safely and its hazardous while stored. Also it is used to
determine the fuel capacity to burn in a combustion cycle for an engine.
Iodine value: shows the number of double bonds present in biodiesel. If iodine value is high
the cetane number is reduced and, consequently reduces the performance of the engine.
Sulfur content: great sulfur levels are present in crude oil and some sulfur oxides are prone
to be formed during combustion processes and harm the environment. In the engine
combustion cylinder they form acids that contribute to metal corrosion but some sulfur is
needed to provide the fuel pump and injectors lubrication.
6

Linolenic acid methyl ester and polyunsaturated methyl esters: these are the name of two
tests which indicate the completion of the reaction of production of biodiesel from oils
providing the amount of fatty acids for a certain sample of fuel.
Carbon residue: shows the amount of carbon that deposit in the engine during fuel
combustion process and most of the carbon is formed by the presence of high levels of
glycerin.
Cetane number: is a parameter that helps in the determination of the fuel ignition time delay.
In biodiesel the cetane number depends upon the feedstock that is used in its production, so if
it is too low it can cause engine clatter, some difficulties when running the engine, exhaust
smoke and if it is too high it results in smoking because the fuel will burn before it mixes
with air.
Methanol content: this will show the fraction of the methanol that has not been reacted after
the transmethylation process.
Sulfated ash content: this test gives the amount of metals such as potassium, zinc, tin,
magnesium, sodium, barium and calcium found in the fuel. Ash can be formed from materials
found in three distinct forms residual catalyst, soluble metallic soaps and abrasive solids.
Ash formation will cause wear of injectors, pistons and the fuel pump.
Monoglyceride, diglyceride and triglyceride contents: it measures the amount of material
that remains un-reacted in the biodiesel. This test is most used by producers examining the
efficiency of the process as the final fuel can contain glycerin and cause carbon deposition.
Water content: dissolved water can be present in fuels and is responsible for failure in the
engines due to cause corrosion, rust, erosion and so on.
Total contamination: it gives an overview of other type of contaminants that may be found
in the fuel. An example, are the waxes that can block the filter if found in high levels.
Free glycerol: it shows the amount of glycerin that was converted effectively. However,
some of it can remain in the biodiesel after processing and deposit into the bottom of the
storage tanks causing filter blocking and therefore, pump failure.






7

2.1.2.2. Diesel specifications
South African National Standard (2006: 3-7) states that the diesel specifications are achieved
by the rule SANS 342:2006 (edition 4). It is also a combination of tests but specifies two
types of diesel fuel that are the low sulfur type and the standard type.
Table 2 - Diesel specifications according to SANS 342:2006 (edition 4, 2006)
Properties Requirement Test method
CF1
a
CF2
b
Sulfur content for:
a) Standard type,
mg/kg, max.

b) Low sulfur type,
mg/kg, max.

500


50

-


-
ASTM D2622 or
ASTM D5453
IP336, ASTM
D4294

ASTM D2622 or
ASTM D5453
IP336
Biodiesel content
(FAME), %volume
fraction, max.
5 -
Polyaromatic
hydrocarbons, %
mass fraction, max.

Uncontrolled

8
IP391, ASTM
D2425; EN 12916
Cetane number,
min.
45 51 ASTM D613 or
IP41
CF1
a
= Clean fuels 1 (no longer permitted after 28 February 2017)
CF2
b
= Clean fuels 2
Data taken from (http://s04.static-shell.com/content/dam/shell-
new/local/country/zaf/downloads/pdf/others/southafrican-national-standard2.pdf)
Sulfur content: sulfur is a very common element in diesel and gasoline. During the
combustion processes water vapor is formed and can combine with sulfur producing sulfuric
acid. Besides being a great environmental pollutant, sulfuric acid is very corrosive causing
wear on cylinder liners and valve guides, and therefore engine failure.
Biodiesel content: FAME contains low percentage in oxygen therefore has a lower energy
content possibly affecting performance and the consumption of the fuel. It also shows a very
low oxidation stability and this can contribute for bacterial growth.
Polyaromatic hydrocarbons: they are very common elements present in crude oil
containing high internal energy but low combustion properties that contribute to their low
auto-ignition and formation of very small particles and these particles can be harmful to the
public health and for the environment. (Republic of South Africa, 2011:17).
Cetane number: indicates how fast the fuel auto ignites. If a fuel shows a high cetane
number, it will have carbon emissivity reduced and a high positive impact to the
environment. (Republic of South Africa 2011: 18)

8

2.2. Theory
As above said biodiesel is a fuel made from natural sources - animals and plants - through
trans-esterification reactions. It can be used as an alternative way in diesel engines that use
organic materials as a fuel reducing hazardous emissions to the atmosphere compared to
usual diesel when burned. Also reduces tailpipe pollutants mostly from old diesel cars and
lessens greenhouse effect. Consequently, biodiesel study is becoming relevant because it can
be obtained from renewable organic materials and mainly for its positive impact for the
environment. Other points can be achieved for example, its production decrease the
dependence on imported fuels contributing for the countrys economy and available jobs.
The trans-esterification reaction is an equilibrium reaction where the products are formed by
mixing reactants. However, the presence of a catalyst considerably accelerates the
equilibrium (Ma and Hanna, 1999). The stoichiometric ratio requires 1 mol of a triglyceride
and 3 mol of the alcohol. However, an excess of the alcohol is used to increase the yields of
the biodiesel and to allow its phase separation from the glycerin to be formed (Schuchardt,
199). The maximum biodiesel yield could be obtained by optimizing the process variables
that affect the yield and purity of biodiesel. The extent of trans-esterification and side
reactions depends upon the type of, catalyst formulation, catalyst concentration, feedstock,
alcohol-to-oil ratio and reaction temperature. Moisture content and free fatty acid in the
reactant mixture are also in biodiesel production. Any fatty acid source can be used to prepare
biodiesel, but in the scientific articles reviewed, trans-esterification reactions have been
studied for many vegetable oils such as sunflower (Vicente, 2004), rapeseed (Jeong and Park,
1996), fish oil (El Mashad, 2006), soybean (de Oliveira, 2005), safflower (Meka, 2007),
canola (Singh, 2006) and palm (Darnoko and Cheryman, 2000; Cheng, 2004). Since the
prices of edible vegetable oils, like soybean oil, are higher than that of diesel fuel, waste
vegetable oils and non-edible crude vegetable oils as, Pongamia pinnat, Jatropha and tigernut
oil have been considered as potential low priced biodiesel sources. Biodiesel made from these
feedstocks was predicted to be more economical than the biodiesel produced from refined
vegetable oil. Meanwhile, it has proved to perform similarly (Pinto, 2005). The free fatty acid
and moisture content are fundamental for determining the viability of the vegetable oil trans-
esterification process. To complete the alkali-catalyzed reaction, a free fatty acid (FFA) value
lower than 3% is needed (Dorado, 2002). Used oil will have a higher percentage of free fatty
acids (FFA) produced from hydrolysis of triglycerides at high temperatures during the frying
process. Before the trans-esterification process, these free fatty acids must be removed with a
base or pre-processed with acid esterification to esters (Van Gerpen, 2005). The oils used in
trans-esterification should be essentially anhydrous (0.06% w/w). The presence of water
causes hydrolysis of some of the produced ester, with consequent soap formation. Soap
formation reduces catalyst efficiency, increases viscosity, leads to gel formation and makes
the separation of glycerin difficult (Guo and Leung, 2003).
9

2.2.1. Operating principles and relevant theory of each unit operation of
the constructed test rig.
A unit operation is a fundamental step required in a process that involves chemical
transformation or physical change. For example: decantation, filtration, chromatography,
distillation, crystallization, dialysis, osmosis and so on.
In Chemical engineering unit operations are divided in five classes:
Fluid flow processes, including fluids transportation, filtration, and solids
fluidization.
Heat transfer processes, including, condensation, evaporation and heat exchange.
Thermodynamic processes, including gas liquefaction and refrigeration.
Mass transfer processes, including, distillation, extraction, gas absorption, drying,
and adsorption.
Mechanical processes, including, crushing and pulverization, solids transportation
and screening and sieving.
Chemical engineering unit operations also fall in the following categories which involve
elements from more than one class:
Combination (mixing)
Separation (crystallization, distillation, , chromatography)
Reaction (chemical reaction)
In addition, there are some unit operations which combine even these categories, such
as reactive distillation and stirred tank reactors.
The biodiesel test rig was composed of the following unit operations: A reactor tank and a
double pipe heat exchanger.
Reactor vessel: this was a cylindrical plastic vessel with a small hole on top for temperature
control, a top reactants entrance and a bottom discharge. This is where essentially the
reactants are mixed continuously on a cycle created by the pump.
Heat exchanger: As we know the oil is viscous and dense and because of that the system can
process slowly and influence the final yield. To overcome this problem a double pipe heat
exchanger was used on the biodiesel test rig. The heat exchanger was composed of one inner
pipe (copper) where hot water was circulating and the outer pipe (PVC) where cold oil was
passing through. Heating the oil enhanced the surface area and the contact between oil and
catalyst solution making the cycle faster and effective in each run set for the experiment.
After the cycle was completed the product was allowed to decant and the biodiesel separated
from the glycerin. Decantation is summarized by time the more you leave it decanting the
more the particles of the desired mixture settle down.
10

For the presented test rig was used refined sunflower oil/ethanol at a ratio of 5:7. As clean oil
was used for the test, filtration of the oil was unnecessary. The mass of the catalyst (Sodium
hydroxide 3%) was found from its concentration and volume of ethanol. The following
equation was used:

Where:
(g)
(mol/l)
(g/mol)
(l)
A complete biodiesel rig should have the following structure:

Figure 1- Block diagram of a complete biodiesel rig
This process uses a reactor tank with a stirrer to ensure a homogeneous mixture and the
reaction occurs at 60-80C. Due to high FFA (free fatty acid) content present a special pre-
treatment by esterification is done and applied an effective recovery system for excess
methanol. The final mixture is separated either by decantation or centrifugation and then both
of them are washed with water in the ester washing system and glycerol washing system. To
ensure that the fatty ester is completely finished the oil phase is neutralized with phosphoric
acid. As can be seen from the diagram above, fatty acids and glycerol are recovered at the
end of the process by adding acid to soap splitting system and using a flash distillation or film
evaporation for methanol recovery in the glycerol water mixture.
11

3. Material and Methods
3.1. Equipment
3.1.1. List of materials used for the test rig
The rig was built using the following materials:


PVC (Polyvinyl chloride) pipe approximate total length of 2,65m
4 ball valves
2 plastics nozzles
Screws
12 elbows(90)
3 T junctions
Water Pump
Conical plastic reactor vessel
Reactor holder
2 Reducer
1 Thermometer
Copper pipe
2 Container
Wood
Driller


















12

3.1.2. Piping and Instrumentation Diagram of the test rig










































13

3.1.3. Engineering drawing of key components


























14

3.1.4. Diagrams/photos describing the equipment
The constructed biodiesel test rig can be summarized in the following diagram:




















Figure 2- Block diagram of a the biodiesel test rig

















Refined sunflower oil
Ethanol/sodium
hydroxide mixture

Reactor Vessel

Pump

Heat Exchanger

Product Container

Figure 3- Entire test rig picture
15








































Figure 5- Reactants container
Figure 4- Oil and alcohol lines
Figure 6-Reactor vessel Figure 7-Pump
Figure 8- Double pipe heat exchanger
16

3.2. Procedure
The method used for this experiment was the base catalyzed.
3.2.1. Residence time test:
1. Exactly 700 ml of ethanol was poured in a volumetric flask.
2. 0.84g of solid catalyst (sodium hydroxide) was weighed and then added to the
ethanol flask. The mixture was shaken for about 40 minutes until the solid dissolved
completely.
3. The alcohol mixture was placed in the rig container and closed (the container must be
closed to avoid any absorption of moisture).
4. 500 ml of oil was measured using a beaker and poured in the rig oil container.
5. The hot water valve was opened. The reactor vessel was kept at 40
0
C by manipulating
the heater.
6. The oil valve was opened.
7. The pump was plugged and the oil was allowed to heat.
8. The Alcohol mixture valve was opened.
9. The recycle valve was opened.
10. The reactants were allowed to mix continuously on a cycle. The pump works as a
stirrer, transferring the mixture to the heat exchanger and sending it back to the
reactor.
11. After 1 hour, the pump was switched off and the product collected.
12. The same procedure was done for 2 hours, 3 hours and 4 hours runs.
13. The products collected on each run decanted and the biodiesel separated from the
glycerin. The volume of the biodiesel produced was recorded for each run.
3.2.2. Reaction temperature
For reaction temperature the procedure was the same but for the first run the
temperature was kept at 35
0
C, second at 40
0
C, then 45
0
C, 50
0
C and 55
0
C, for the
other runs. Each run was done in 2 hours. The volume of the biodiesel was recorded
for each run.
3.3. Analytical
The flow rate of hot water was measured using a small container and clock watch. In 10
seconds was collected 120 ml of hot water.
The instruments used to measure and analyse the data are:
1000ml volumetric flask
1000ml graduated cylinder
500ml beaker
Spatula
Digital scale
Watchglass
17

4 Plastic bottle
Thermometer
The volume of oil and alcohol was measured with graduated cylinder. The amount of product
produced was collected in the plastic bottle, and allowed to settle down. The biodiesel was
poured in the graduated cylinder and the volume recorded. Care must be taken when
measuring the volume because is not easy to read accurately the value of the volume when
the operator does not place well his eyes on the meniscus.
The amount of catalyst was measured using the digital scale. The watchglass was placed into
the scale and bottom Tare pressed. Using the spatula the required amount of sodium
hydroxide was taken from bottle. The catalyst bottle must be kept closed to avoid any
moisture. The result on scale were taken with an error of +or -0.01.
The temperature on the reactor vessel was monitored by the thermometer. The volume of
biodiesel may be inaccurate because of difficulties on kept the temperature constant. When
the temperature on reactor was above required, cold water was added to the heater. When the
temperature was below, the heater temperature was increased.
















18

4. Data Analysis and Evaluation
During this design project, namely, development of a processing plant to convert used
cooking oil to biodiesel, the raw data below described was obtained. In each study on
residence time and temperature dependence, respectively, several runs were done. Repeated
observations were made under similar conditions to evaluate and estimate the magnitude of
the experimental error and also to obtain sufficient data for conclusions in terms of trends.
Table 3- Residence time
Runs Temperature () Time (hr) Biodiesel Final Volume (ml)
1 40 1 730
2 40 2 770
3 40 3 694
4 40 4 580


Figure 9- Biodiesel yield versus residence time
From the above table and chart, it can be observed a non-linear relationship between
biodiesel product yield and residence time. At one hour period, a volume of 730 ml of
biodiesel was produced, as the time is increased to 2 hour, the volume rises to 770 ml and at
the period of 3 and 4 hour, the volume decreases to 694 ml and 580 ml respectively. The
maximum biodiesel production was therefore obtained at 2 hours run.
Freedman (1986) observed an increase in fatty acid esters conversion with an increase in
reaction time. According to his study, reaction is slow at the beginning due to mixing and
dispersion of alcohol and oil. After that the reaction proceeds very fast. However the
maximum ester conversion is achieved within < 90 min. Further increase in reaction time
does not increase the yield product i.e. biodiesel/mono alkyl ester (Leung and Guo, 2006;
Alamu, 2007). Besides, longer reaction time leads to the reduction of end product (biodiesel)
due to the reversible reaction of trans-esterification resulting in loss of esters as well as soap
formation (Eevera, 2009; 1998).
0
100
200
300
400
500
600
700
800
900
1 2 3 4
B
i
o
d
i
e
s
e
l

F
i
n
a

V
o
l
u
m
e

(
m
l
)

Time (hr)
Biodiesel yield versus residence time
19

The trend obtained is therefore in accordance with theory. The maximum biodiesel
production was obtained at 2 hours run, which is acceptable, and the lowest yield was
obtained at 4 hours run as expected. Generalizing, the biodiesel product yield increases for a
residence time up to 2 hours. From values higher than 2 hours the product yield decreases.
Table 4-Reaction temperature
Runs Temperature () Time (hr) Biodiesel Final Volume (ml)
1 35 2 756
2 40 2 770
3 45 2 782
4 50 2 800


Figure 10 - Chart of Biodiesel Final Volume versus Temperature
In temperature dependence, all runs were done in a constant time of two hours. In total four
runs were done, ranging from 35
0
C to 50
0
C. From above table and chart, it can be observed
that the relevant final product production increases when temperature is slightly increased. At
a temperature of 35
0
C the product yield was 756 mL, at 40
0
C and 45
0
C, the product yield
was 770mL and 782 mL, respectively. Finally, 800 mL was obtained when working with a
temperature of 50
0
C. An increase of 8-14 mL product yield was observed.
According to literature investigated higher reaction temperature increases the reaction rate
and decreases the reaction time due to the reduction in viscosity of oil. On the other hand,
Leung and Guo (2006) and Eevera, (2009) found that an increase in reaction temperature
beyond the optimal level leads to decrease of biodiesel yield, because higher reaction
temperature accelerates the saponification of triglycerides. Usually the trans-esterification
reaction temperature should be below the boiling point of alcohol in order to prevent the
alcohol evaporation. The range of optimal reaction temperature may vary from 50c to 60c
depends upon the oils or fats used (Leung and Guo, 2006; Ma and Hanna, 1999; Freedman,
1984).
730
740
750
760
770
780
790
800
810
35 40 45 50
B
i
o
d
i
e
s
e
l

F
i
n
a
l

V
o
l
u
m
e

(
m
L
)

Temperature ( C)
Biodiesel yield versus reaction temperature
20

The trend observed is once again in accordance with theory. The maximum biodiesel
production was obtained at 50
0
C, which is within the optimal range, and the minimum
biodiesel production was obtained at 35
0
C, a value below the optimal range. In general the
product yield increases with an increase in temperature up to a working temperature of 60
0
C.
Slightly increase in temperature may account to an increase in production, but can lead to
critical working conditions.
Relevant considerations
Higher biodiesel yield would be expected on both experiments. Some sources of error were
found when collecting the product. Not the entire product was successfully removed from the
rig, as a considerable fraction remains within the pipes and heat exchanger.
The optimum process conditions are therefore defined as 2 hours residence time and 50
o
C
working temperature. The results obtained can be applied for cooking oil, which will have
more advantages in terms of costs.
Some of the advantages of using biodiesel as a replacement for diesel fuel are:
Renewable fuel, obtained from vegetable oils or animal fats
Low toxicity, in comparison with diesel fuel.
Lower emissions of contaminants: carbon monoxide, particulate matter, poly- cyclic
aromatic hydrocarbons, aldehydes.
Degrades more rapidly than diesel fuel, minimizing the environmental consequences
of biofuel spills.
Lower health risk, due to reduced emissions of carcinogenic substances.
No sulfur dioxide (SO2) emissions.
May be blended with diesel fuel at any proportion; both fuels may be mixed during
the fuel supply to vehicles.
Excellent properties as a lubricant.
It is the only alternative fuel that can be used in a conventional diesel engine, without
modications.
Used cooking oils and fat residues from meat processing may be used as raw
materials.
Disadvantages of the Use of Biodiesel:
Slightly higher fuel consumption due to the lower caloric value of biodiesel.
Higher freezing point than diesel fuel. This may be inconvenient in cold climates.
It is less stable than diesel fuel, and therefore long-term storage (more than six
months) of biodiesel is not recommended.
May degrade plastic and natural rubber gaskets and hoses when used in pure form,
in which case replacement with Teon components is recommended.
It dissolves the deposits of sediments and other contaminants from diesel fuel in
storage tanks and fuel lines, which then are ushed away by the biofuel into the
21

engine, where they can cause problems in the valves and injection systems. In
consequence, the cleaning of tanks prior to lling with biodiesel is recommended.
It must be noted that these disadvantages are signicantly reduced when biodiesel is used in
blends with diesel fuel.
In this small project for the biodiesel production were used, ethanol, virgin sunflower oil and
caustic soda as catalyst. Ethanol can be purchased at R 150/2.5L, 500 g of caustic soda at R
208 and virgin sunflower oil 16 R/L. Some other points must be taken into account when
producing such as the electricity and water costs. Economic viability of proposed solution
was conducted and found that it can be slightly expensive to produce biodiesel rather than
buying the conventional diesel at R 13.45/L. However, this project is feasible and
environmentally-friendly. The demand of diesel on fossil fuels dependent processes produces
harmful gases that contribute to greenhouse effect and harms the public and environmental
health; consequently replacing it by biodiesel will be a worthy investment as it is a cleaner
fuel.




























22

5. Full scale plant Design
5.1. Full scale plant requirement
For the full scale plant design the optimum conditions of 2 hours and 50C were defined, and
from that the following requirements of the plant was established:
A reactor vessel of 0.21 m
3
capacity and 0.37 m diameter.
Oil container 8.33*10
-5
m
3

Ethanol container 1.167*10
-4
m
3

A pump of 20 Watts
A double pipe heat exchanger consisting of two 1.9 m long tube connected by 180
bend with an outer diameter of 21.3 mm and inner diameter of 17.1 mm

PVC pipe with approximate total length of 8m

One industrial thermometer
Net power requirement of 320.64 Watts
All the specified requirements were set for an approximate area of 6m. The capacity of the
reactor vessel was obtained by dividing 1000000 ml of oil that will be processed per day to
total number of runs 12 (each run takes 2 hours) to complete. The Plant will hold only one
reactor vessel to produce biodiesel. The height of the reactor was assumed to be 2 m and the
diameter of it was calculated which is 0.37 m. The diameter of the pipe and was taken of the
pump specifications.
As it is a batch process, two containers (oil and ethanol solution container with 83.3 ml and
116.7 ml respectively) will be used to supply the reagents to the reactor vessel on each run.
The scale up of double pipe heat exchanger was based in the practical manual which consists
of two 1.9 m long tube connected by 180 bend with an outer diameter of 21.3 mm and inner
diameter of 17.1 mm. Detailed calculations are beyond the scope of the project. The net
power requirement was found from the heat exchanger duty and pump requirement.
5.2. Operational method
1. Measure 116.7 ml of ethanol in a volumetric flask.
2. Weigh 140g of sodium hydroxide and place into the ethanol volumetric flask.
Shaken the volumetric flask until the catalyst dissolves completely.
3. Measure 83.3 ml of used cooking oil and place it in the rig oil container.
4. Open the hot water valve.
5. Open the oil valve.
6. Plug the pump.
7. Open the alcohol valve.
8. After two hour, switch off the pump and collect the product.
9. Repeat the same procedure for two hours and proceed until 12 runs are completed.

23

5.3. Piping and Instrumentation Diagram of the full scale plant


























24

5.4. Cost benefit analysis
The purpose of this experiment is to design a full scale biodiesel plant that can process one
kilolitre of used cooking oil per day. For this, cost benefit analysis must be performed. It is a
tool that helps to calculate and compare benefits and costs of a project.
From the obtained results, the best yield product was obtained using a temperature of 50
0
C
for two hours then these are the set optimum biodiesel conditions. So for the plant to be able
to process one kilolitre of used cooking oil per day, twelve runs will be fed each having two
hours of duration. It means that we will be using 140 grams of caustic soda, volumes of
116.666,67 mL of ethanol and 83.333 mL of oil based on the given initial ratio, therefore
an approximated total volume of 200.000 mL will be used in each run.
Plant requirements:
- A current cooling water requirement of 50 kl /hr.
- A power requirement of 320 kWh enough to process one kilolitre of used cooking oil
and for heating purposes.
Cost factors
relating to the
project
Cost Required per
day
Total cost per
day
Diesel R 13,92 / L 2500 L R 34800
Ethanol USD 450 / metric
ton
*

1400L R 5300
Caustic soda USD 180 / ton
*
1680 g R 3.22
Water R 14,59 / kL 50kL R 730
Electricity (excl. vat) R 195,60 / kWh 60 kWh R 11736
*
USD 450 approximates R 4797.35 based on current exchange rate
*
USD 180 approximates R 1918.96 based on current exchange rate

To produce biodiesel fuel, it will be encountered the costs on ethanol, caustic soda and on
services such as water and electricity supply. By the end of a day, the university would have
spent R 34800 on buying diesel and R 29532 if producing its own fuel. Therefore, it would
save approximately R 5230 and be beneficial to universitys pocket and for the environment.
5.5. Safety aspects
Most plants face very common problems. In biodiesel plants, methanol and catalysts become
the most hazardous materials seriously affecting plant safety; usually methanol makes up
75% to 80 % of total material. It is very inflammable and its vapors can be explosive
depending on concentrations, therefore indoor units should be well ventilated. Methanol
escaping to operating area can occur due pump seal failures, worn hoses, poor
instrumentation connection and some other incidents. Personnel must be trained to identify
any potential chemical and mechanical hazards. Use of the hard hat and goggles is
compulsory.
25

All plant must be maintained in a safe condition, once it is ready to operate all equipment
should be evaluated and safety information reviewed to reduce future leaks and failure.
Temperature and pressure must be kept under operational limits, if exceed relief systems
must be used. Equipment installation methods must be reviewed as well. In case of fire, steps
should be taken to protect most affected areas such as the storage tank, pump, heat exchanger
and others. All electrical installation must be reviewed for meeting the right requirements.
A plant to operate safely, operator training is a necessary investment. They must be familiar
with start-up, shut-down procedures and need to understand the mechanics and chemical
reactions which are associated with the facility. Understanding the basics of each process is
very important allowing the operator to respond to problems that may arise. All personnel
must use the proper safety equipment required at all times and have caution when handling
certain chemicals.


















26

6. Conclusion
Biodiesel has becoming an important alternative fuel to diesel engine because of its eco-
friendly benefits and from renewable nature. The trans-esterification method is the more
applied, and it is affected by residence time, reaction temperature, oil/ethanol ratio and
catalyst concentration.
The optimum process conditions were found to be 2 hours residence time and 50
o
C working
temperature. The results obtained can be applied for cooking oil, which will have more
advantages in terms of costs. From the optimum conditions the full scale plant design has the
following requirements:
A reactor vessel of 0.21 m
3
capacity and 0.37 m diameter.
Oil container 8.33*10
-5
m
3

Ethanol container 1.167*10
-4
m
3

A pump of 20 Watts
A double pipe heat exchanger consisting of two 1.9 m long tube connected by 180
bend with an outer diameter of 21.3 mm and inner diameter of 17.1 mm

PVC pipe with approximate total length of 8m

One industrial thermometer
Net power requirement of 320.64 Watts
Hard hat and goggles must be used on construction of the rig.













27


7. References
Biodiesel basics (online). 2014. Available: http://www.biodiesel.org/what-is-
biodiesel/biodiesel-basics (Accessed 25 June 2014).
Biodiesel production (online). 2014. Available:
http://en.wikipedia.org/wiki/Biodiesel_production (Accessed 25 June 2014).
Biodiesel standard (online). Available: http://www.green-
diesel.co.za/index.php?option=com_content&view=article&id=18&Itemid=45 (Accessed 02
July 2014).
Dunford, N.T. Biodiesel production techniques (online). Available:
http://www.fapc.biz/files/factsheets/fapc150.pdf (Accessed 25 June 2014).
FAME (online). 2014. Available: http://en.wikipedia.org/wiki/Diesel_fuel#FAME (Accessed
30 June 2014).
How to make biodiesel (online). Available: http://www.wikihow.com/Make-Bio-Diesel
(Accessed 25 June 2014).
Vitek, J. and Kalibera, T. n.d. R3 Repeatability, reproducibility and rigor (poster online).
Purdue University, USA and University of Kent, UK. Available:
https://www.cs.purdue.edu/homes/jv/pubs/r3.pdf (Accessed 28 June 2014).
Refaat, A. A.; Attia, N. K.; Sibak, H. A.; El Sheltawy, S.T.; ElDiwani, G. I., (2008).
Production optimization and quality assessment of biodiesel from waste vegetable oil. Int. J.
Environ. Sci.Tech. (online), 5 (1), 75-82. Available:
http://www.ijest.org/jufile?c2hvd1BERj0xOTQ=&ob=19df3d3c5a22d0678a9432aedb792f07
&fileName=full_text.pdf (Accessed 28 June 2014)
Republic of South Africa. 2011. Discussion document on the review of fuel specifications and
standards for South Africa. Government Gazette number 34089: 8 March (online). Available:
http://www.energy.gov.za/files/esources/petroleum/March%202011/1-34089%208-
3%20Energy.pdf (Accessed 30 June 2014).
South African National Standard. 2006. Automotive diesel fuel (online). Available:
http://s04.static-shell.com/content/dam/shell-
new/local/country/zaf/downloads/pdf/others/southafrican-national-standard2.pdf (Accessed
30 June 2014).
Sulfur contents in fuel (online). Available:
http://www.cdxetextbook.com/fuelSys/emission/types/sulfurcontent.html (Accessed 30 June
2014).

28

8. Appendices
Table 5- Raw data
Test rig VARIABLES VALUES
Diameter of tube
Capacity of reactor vessel 2672 ml
Mass catalyst 0.84 g
Power pump rig 200.64 W
Height reactor 42 cm
Scale up Plant
design
Full capacity reactor 210 L
Power pump out rig 300.96 W
Power pump in system 20 W
Diameter tube
Height reactor 2 m
Flowrate mixture (biodiesel +ethanol soln) 1500 L/H

CALCULATIONS
Full capacity of the test rig reactor vessel

D = 9 cm measured
H = 42 cm measured

Power required for the pump out of the rig

29

Mass of catalyst

Scale up calculations
Full capacity of reactor vessel is 200L
If 1000000 ml of Oil is processed in one day and we got 12 runs each run 2h, then:
1000000/12= 83333.3 ml of oil in each run or

If 500 ml Oil 700 ml ethanol
83333.3 ml oil
X=116666.67 ml ethanol
Full capacity is 83333.3 ml oil + 116666.67ml ethanol = 199999.97 ml mixture
Full capacity = 200 L or 210 L (10 L of extra space)
Scale up of Power required out of the rig
If 200.64 W 0.5
X 0.75

X= 300.96 W
Scale up of mass of catalyst
700 ml 0.84 g
30

116.7 ml x
X=140 g
Power required for the pump in the system
Assuming the height which is 2 m high the diameter can be calculated by using the following
equation:

210 L =0.21 m
3