TOPIC:

Can you predict the

production of biofuel from
used Vegetable oil?
Production of Biodiesel from
Waste Vegetable Oil via KM
Micro mixer.

Done By:
Biodiesel from Waste Rahaf Awad (200302605)

Vegetable oil Abdelrahman Ramadan(200302611)

Biotechnology project Derar Taleb (200302610)

  Abstract:
Biodiesel production has received considerable attention in the past as a biodegradable and
nonpolluting fuel. The production of biodiesel by transesterification process employing alkali
catalyst has been industrially accepted for its high conversion and reaction rates. The use of
methoxide as a catalyst to perform the transesterification reaction into biodiesel in this work. The
effect of the most relevant variables of the process such as reaction temperature, molar ratio
between alcohol and oil, amount of catalyst and amount of free fatty acids fed with oil have been
analyzed. For this purpose, an ideal sunflower oil using lauric acid and palm oil, coconut oil also
used. The alcohol used was methanol. Fats and oils are chemically reacted with alcohol to
produce chemical compounds known as fatty acid methyester (Biodiesel). The production of
biodiesel from waste vegetable oils through its pretreatment followed by transesterification
process in presence of methanol was investigated using a KM micro mixer reactor. The
parameters affecting biodiesel production process such as alcohol to oil molar ratio, catalyst
concentration, the presence of tetrahydrofuran (THF) as a cosolvent, and the volumetric flow
rates of inlet fluids were optimized. The properties of the produced biodiesel were compared
with its parent waste oil through different characterization techniques.

 Introduction:
The idea of using alternative fuels has been widely spreading for many years
now as a replacement for fossil fuels. The importance of this idea came from
the large scale of utilization of fossil fuels in mechanical power generation in
various sectors, like agriculture, commercial, domestic, and transport
sectors, and also the fact of the continuous rise in fuels cost and their
eventual vanishment. The use of vegetable oils and their derivatives was
found to be one of the reasonable solutions. However, the direct use of
vegetable oils in diesel engines was found impractical due to several factors,
such as the high viscosity, acid composition, and free fatty acid content.
Accordingly, they require further modifications for effective use. Undergoing
transesterification reaction is the most favorable for decreasing oil’s viscosity
and producing so-called “biodiesel fuel”. Biodiesels are monoalkyl esters of
long chain fatty acid derived from renewable lipid feedstock. The interest of
this alternative energy resource is that the fatty acid methyl esters, known
as biodiesel, have similar characteristics of petro diesel oil which allows its
use in compression motors without any engine modification. However, using
vegetable oil to replace fuel caused the food versus fuel issue all over the
world. So the idea of using waste vegetable oil (WVO) has been introduced
as an economical solution which also gives a waste management solution.
Transesterification is a process of transforming triglycerides in vegetable oils
into a mixture of fatty acid esters using alcohol and catalyst to speed up this
reaction to the right side and to obtain high biodiesel yields. Methyl or ethyl

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esters are obtained, with much more similar properties to those of
conventional diesel fuels. The main byproduct obtained is glycerol. The most
common alcohol used for biodiesel production is methanol because of its
price and conversion rates. Other alcohols can be used too, such as plant
based ethanol, propanol, isopropanol, and butanol. In presence of excess
alcohol, the foreword reaction extends beyond the reverse reaction. Many
catalysts could be utilized in the process; however, it was confirmed that
transesterification is completed faster using an alkali catalyst. The
mechanism of transesterification shows some challenges regarding this
process, starting from the limitation of reaction rate by mass transfer
between the immiscible oil and alcohol besides the reversibility of the
transesterification itself which limits the conversion and consequently
increases the reaction time and cost.
These challenges of transesterification reaction happened to appear clearly
using conventional batch reaction processes. Many alternatives have been
proposed to undergo the reaction in a more effective way through improving
mixing rate, enhancing heat and mass transfer of the reaction, and
decreasing cost and time consumed. Accordingly, micro reactors were
utilized at the transesterification reaction holding the advantage of high
volume/surface ratio, short diffusion distance, fast and efficient heat
dissipation, and mass transfer. By this role micro reactors promote the
overall volumetric mass transfer coefficient of methyl esters due to the
increase of the specific interfacial area by decreasing the droplet size. This
eventually results in the increase of reaction rate for triglycerides. The KM
micro mixer has been tested for mixing two immiscible fluids and was found
superior over other mixers designs. Also it provides high throughput and
stable operation in a wide range of flow rate ratios for the two reactant
fluids. In this investigation, a KM micro mixer has been used as a micro
reactor for transesterification of waste vegetable oil with methanol in
presence of NaOH as catalyst. The influences of transesterification process
variables such as alcohol to oil molar ratio, catalyst concentration, volumetric
flow rate, and effect of an organic cosolvent presence were optimized.

 Materials and Method:

1. Materials
Waste vegetable oil was purchased from a local restaurant as a source of triglycerides for
transesterification reaction. The alcohol selected was methanol (99.8%, Sigma-Aldrich). Other
utilized chemicals for transesterification process are of analytical grades such as sodium
hydroxide (99%, Sigma-Aldrich), acetic acid (98%, Sigma-Aldrich), and tetrahydrofuran (ACS
GRADE, 99%, Right Price Chemicals).

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2. Waste Vegetable Oil Pretreatment
The waste vegetable oil (WVO) was first filtered to remove bits of food residues using a glass
Buchner funnel filtration system and then it was subjected to an acid catalyzed esterification
process in order to maintain free fatty acid content lower than 1%.
3. Experimental Setup
The KM micro mixer proposed for this investigation consists of 3 stainless steel plates, inlet,
mixing, and outlet plates holding fourteen micro channels fabricated for fluid streams.
Dimensions of the micro mixer are shown in Table 1. The mixer has 2 inlets for two different
reactant fluids. The fluids are transferred to the mixing plate through annular channels where
fourteen micro channels are present.

Micro channels are fabricated by Micro-Electric-Discharge Machining (μ-EDM). The stream of

each fluid was divided into half of the total number of micro channels. The two divided fluids
meet at the center of the mixing plate and are immediately mixed. The diameter of the mixing
zone was found to be 220 μm. Finally, the outlet plate has a hole for the exit of the mixed fluid at
the center of the plate; the exit fluid hole (200 μm) is smaller than the diameter of the mixing
zone to accelerate the mixing process.
The experiment is set as shown in Figure 1. The KM mixer is immersed in a water bath to
provide the required reaction temperature. Two syringe pumps (KD Scientific, KDS100, USA)
were used for feeding the inlet reactant fluids.

Figure 1

Schematic view of
the KM mixer system

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4. Biodiesel Production Process Using KM Mixer
Two reactant fluids were fed via syringe pumps into the designed experimental setup; the first is
the preheated oil at specific temperature, and the second is the mixture of methanol, sodium
hydroxide, and THF. The proper amount of sodium hydroxide was dissolved completely in
methanol to avoid clogging the micro channels at the KM mixer with solid particles. The amount
varied from 0.5% to 2% (wt/wt of oil) to elucidate the most suitable amount that attains the
highest biodiesel production yields. The reactants feeding rates were changed over a wide range
from 20 mL/h to 200 mL/h to investigate the influence of residence time on the biodiesel
production process. The reactants molar ratio was optimized to determine the most proper
mixing ratio. The KM mixer that includes the process reactants was maintained at specific water
bath temperature 70°C. The experiments were conducted three times to consider the
experimental error. At the KM mixer outlet, the product is collected after reaching steady state in
a beaker containing appropriate amount of acetic acid to neutralize the excess alkaline catalyst
and stop the reaction. The product of the reaction is placed in a separating funnel to be separated
into two clear phases. The biodiesel layer which represents the main product was separated as
upper light-colored phase, while the lower dark phase is mainly glycerol. The upper phase was
washed after separation with distilled water for excess catalyst and glycerol removal and then it
was heated up to 70°C to vaporize the excess solvent. The remaining main product was then
characterized using GC-MS analysis to confirm oil conversion and identify biodiesel production
yield.
5. Characterization of Produced Biodiesel
In order to characterize the quantity and the quality of the produced biodiesel several techniques
were utilized. The volume of biodiesel product was first measured and the volume yield
percentage was calculated according to the following:
%Volume Yield = (V of product/ V of oil fed) (100)

The fatty acid methyl esters (FAMEs) in the produced biodiesel were then characterized and
identified using gas chromatography-mass spectrometry (GCMS-QP2010 Ultra, Shimadzu,

%Biodiesel yield = (Fames %from GC analysis) (V yield)

Japan) fitted with 5MS column (30 m, 0.25 mm ID, 0.25 μm). GC-MS analysis mainly identifies
the quality and quantity of the produced biodiesel resembled in the methyl esters present in the
product sample. This analysis technique also gives the distribution area for each component in
the produced sample. Table below shows the GC-MS configuration used for biodiesel analysis.
The total yield from the biodiesel was finally calculated according to:
Thermal analysis of the prepared biodiesel and its parent waste oil was carried out using thermal
gravimetric analysis (TGA-50, Shimadzu, Japan) with a heating rate of 20°C/min under the flow
of nitrogen gas, starting from ambient condition
up to 800°C.

Table showing GC-MS configuration

 Conclusion:
This study investigated the use of KM micro
mixer in the production of biodiesel from
waste vegetable oil. The effects of methanol/oil molar ratio, catalyst concentration,
volumetric flow rates, and the presence of a cosolvent on the transesterification reaction were
examined. The study proved that the reaction can be completed giving higher percentage
yield of biodiesel that reached 97%. In order to characterize the biodiesel product, its quality
and quantity, GC-MS analysis has shown the characteristic peaks of FAMEs that ranged
between C16 and C18 methyl esters as main products with 98% yield. In addition, TGA and
FTIR analysis were used to differentiate between the produced biodiesel and its parent oil.
The results from both GC-MS and TGA methods were in good agreement regarding the
quantity. The study confirms that the proposed KM micro mixer designed with fourteen
micro channels was found effective for transesterification reaction completion. Thus, it can
be employed in biodiesel production introducing many advantages over the batch reaction
like time saving and higher yield and better conversion.

References:
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transesterification duration for biodiesel production from Nigerian palm kernel
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