Alexandria Engineering Journal (2015) 54, 1265–1272

H O S TED B Y

Alexandria University

Alexandria Engineering Journal

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REVIEW

Purification of crude biodiesel using dry washing

and membrane technologies
I.M. Atadashi *

Adamawa State University, P.M.B 25, Mubi, Nigeria

Received 20 July 2014; revised 4 August 2015; accepted 20 August 2015

Available online 11 September 2015

KEYWORDS
Abstract Purification of crude biodiesel is mandatory for the fuel to meet the strict international
Biodiesel; standard specifications for biodiesel. Therefore, this paper carefully analyzed recently published lit-
Water washing; Dry eratures which deal with the purification of biodiesel. As such, dry washing technologies and the
washing; Biodiesel most recent membrane biodiesel purification process have been thoroughly examined. Although
membrane purification of biodiesel using dry washing process involving magnesol and ion exchange resins pro-
purification vides high-quality biodiesel fuel, considerable amount of spent absorbents is recorded, besides the
skeletal knowledge on its operating process. Further, recent findings have shown that biodiesel
purification using membrane technique could offer high-quality biodiesel fuel with less wastewater
discharges. Thus, both researchers and industries are expected to benefit from the development of
membrane technique in purifying crude biodiesel. As well biodiesel purification via membranes has
been shown to be environmentally friendly. For these reasons, it is important to explore and exploit
membrane technology to purify crude biodiesel.
2015 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an
open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-
nd/4.0/).

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1266
2. Biodiesel dry washing process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1267
3. Membrane separation process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1268
3.1. Biodiesel organic membrane separation process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1269
3.2. Removal of impurities from biodiesel via ceramic membrane process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1269
3.3. Membrane fouling and cleaning process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1270
3.3.1. Membrane fouling process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1270
3.3.2. Membrane cleaning process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1270
4. Successes and failures of biodiesel refining techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1271

* Tel.: +234 8037874859.

E-mail address: atadashimusa1@yahoo.com.
Peer review under responsibility of Faculty of Engineering, Alexandria
University.
http://dx.doi.org/10.1016/j.aej.2015.08.005
1110-0168 2015 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
242 I.M. Atadashi

5. Conclusions and recommendations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1271

Acknowledgment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1271
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1271
Purification of crude biodiesel 243
1 [8], as well as substantial undergoing operation should be done
. reduction in PM, HC and transesterification to give in a sufficiently large
CO emissions [9]. Typically, biodiesel. This is often container (at most two-
I biodiesel could signifi- accomplished by heating the thirds full) which is closed
n cantly reduce unburned total filtered oil to approximately but not sealed [17,20].
t hydrocarbons (THCs), and 120 C. At this In addition, quite a
r car- bon monoxide (CO) temperature dissolved or number of feedstocks
o (28–46%) while carbon suspended water will boil are being
d dioxide (CO2), and nitric off. When the water boils, it explored and exploited in
u oxides (NOx) (6.95– spatters (chemists refer to order to lessen the cost of
c 17.62%) emissions may it as ‘‘bumping”). To producing biodiesel fuel.
t prevent injury, this Presently tremendous efforts
be slightly increased by
i are being made to develop
1.46–5.03% [10,11]. In
o feedstocks such as microalgal
addition, biodiesel fuel offers
n oil to produce biodiesel.
engine performance similar
to the one of petroleum Microalgae clearly provides
It is worthy to mention diesel fuel [12]. It is also to several advantages compared
that development of a great extent biodegradable to plant oils including much
renewable fuels has recently in the soil as well as in the higher production of
become important because freshwater. Further, under biomass com- pared to that
of the limitations of non- aerobic or anaerobic of land plants, and a number
renewable fossils fuels, conditions, 90–98% of the of species can have up to
which include best part of biodiesel is 20–50% triglycerides,
contamination of the mineralized within 21–28 whereas less fertile
environment, short supply days [13]. agricultural land is sufficient
of petroleum products, Biodiesel, composed of to achieve biomass [21].
increase in the prices of saturated and unsaturated Furthermore, microalgal oil
petroleum products, long- chain fatty acid alkyl has the potential to
considerable increase in esters is derived from animal produce higher biodiesel
global energy demands, fats, refined and unrefined yields with about 25%
dwindling fossil fuels vegetable oils through reduction in production cost
reservoirs and greenhouse transesterification and [22].
effects causing global esterification processes Biodiesel is mostly
warming [1–5]. Conse- [8,14–16]. Vegetable oils are produced through
quently, different produced from numerous transesterification reaction.
approaches are being oil seed crops. While all Transesterification is a
explored and exploited to vegetable oils have high process involving reaction
circumvent these problems; energy content, most between triglyceride and
some of these approaches require some processing to alcohol in the presence of a
include development of ensure safe use in internal catalyst to produce ester
renewable energies such combustion engines. Some and glycerol. The molecular
as wind energy, geothermal of the sources of vegetable weight of a typ- ical ester is
energy and biofuels. oil include sunflower, roughly one-third that of
Biofuels, in particular cottonseed oil, and soybean typical oil molecule and
biodiesel has been found oil. Vegetable oils and their therefore has a much lower
to be a good esters are found to be viscosity. To complete the
replacement to petro-diesel. promising alternatives as transes- terification process
This is because biodiesel fuel for diesel engines [17]. stoichiometrically, 3:1 M
provides quite a number of Several researches have ratio of alcohol to
advantages among others shown that waste cooking triglycerides is needed.
including renewability, oil (WCO) is a promising However in practice, higher
biodegradability, regional feed- stock in biodiesel ratio of alcohol to oil ratio
and agriculture production [18]. Thus, is generally employed to
development, and lower biodiesel production cost ensure comple- tion of the
gaseous emissions [6,7]. might be considerably reaction [17].
Besides, renewable reduced by 60–90% when After transesterification,
resources such as fats and WCO is employed in its the ester can be separated
vegetable oils, when production [19]. If waste from glycerol by simple
converted to biodiesel fuel vegetable oil is used, it is gravitational sedimentation
take away more carbon- filtered to remove dirt, and the ester has to be
dioxide from the charred food, and other washed to remove traces of
atmosphere dur- ing their non-oil materials often alkali [23]. Biodiesel is
production than is added to found. Water is removed conventionally purified using
it by later combustion. because its presence causes water and dry washing
Therefore, it lessens the the triglycerides to technolo- gies. Water could
increasing carbon-dioxide hydrolyze to give salts of eliminate the remaining
content of the atmosphere the fatty acids instead of sodium salts and soaps
 244 I.M. Atadashi
formation; this is due to so as
their water solubility [24].
Although water washing is
efficient, it is associated with
prob- lems such as increase
in production time and cost
of produc- tion, and
difficulty in removing
biodiesel from water.
Besides, use of water in
the purification of crude
biodiesel could result in
increase in wastewater
discharges, thereby caus-
ing severe environmental
effects due to high pH
values, high contents of
biological oxygen demand,
and chemical oxygen
demand [25]. Thus to
overcome these problems,
dry washing technique by
means of magnesol powder,
ion exchange resins, and
acid clay, etc. was then
introduced to substitute
the water washing
technology. Even though
dry washing tech- nique is
used commercially, its
chemistry is not yet
understood [26–28].
Additionally, because of the
importance of glycerol in
biodiesel production,
glycerol is also refined
before it is being used for
its conventional
applications in food,
cosmetic and
pharmaceutical industries.
Recently glycerol is used as
carbon feedstock in
surfactants, polymers,
fermentations, lubricants
and intermediates and as
animal feed [25].
At present, quite a
number of researches are
being con-
ducted in the development
of membrane technology
for the purification of crude
biodiesel. These researches
are been embarked upon due
to the difficulties
encountered with biodie- sel
water and dry washing
processes. The researches on
biodie- sel purification via
membrane systems have
provided promising results,
with less water being used
[29–31]. For this reason,
exploration and exploitation
membranes are imperative
Purification of crude biodiesel 245
 246
to find a suitable replacement for the conventional biodiesel
separation and washing processes. Hence, this work was ana-
lyzed and reported on the purification of crude biodiesel using
dry washing and membrane technologies.
2. Biodiesel dry washing process
Dry washing is another most regularly used technology in the
dynamics of biodiesel purification process. This process is
achieved via application of adsorbents such as Amberlite,
purolite, cellulosics, Magnesol, Trisyl, activated carbon, acti-
vated fiber, and activated clay. Adsorbents comprise of basic
and acidic adsorption sites and can easily attract polar sub-
stances, which include glycerol and methanol etc. [32]. To
make the process more effective and efficient, a filter unit is
provided as depicted in Fig. 1. The process is operated at
65 C and refining process is completed in 20–30 min [6].
During dry washing, both glycerides and total glycerol are
reasonably reduced to appreciable levels. The dry washing
procedure is waterless, improves fuel quality, is simple to
incorporate into existing plant, reduces washing time and zero
waste-water, minimizes total surface area coverage of wash
tank, and saves space [32]. It was found by [33], that dry wash-
ing procedure for the refining of crude biodiesel decreases cost
of production and lowers production time. The process offers
quality biodiesel and because no water is added, the possibility
of achieving water content below 500 ppm as specified by
ASTM D6751 is significantly high. It is worthy to note that,
in water washing process, fuel water content is mostly higher
than 1000 ppm, hence rendering water removal costly, compli-
cated, and time-consuming [33]. As well, samples of esters pre-
pared from waste frying oil (WFO) were refined by means of
rice husk ash (RHA) at varying concentrations of 1%, 2%,
3%, 4% and 5% (w/w), which were then compared with refin-
ing techniques; commercial adsorbent Magnesol 1% (w/w)
and conventional acid solution (1% aqueous H3PO4). Rice
husk ash with a concentration of 4%, presented excellent result
in removing impurities in biodiesel as compared to other con-
centrations. The high adsorption capacity of impurities is as a
result of high concentration of silica in its composition and the
presence of meso and macropores can. Hence, the rice husk
Residual
Unrefined alcohol
biodiesel Removal
Mixing
(65 o C for
20-30min)
Figure 1 Schematic diagram of biodiesel dry washing technology [26].
I.M. Atadashi
ash, which is a by-product of rice processing, appears as a sub-
stitute material to refine crude biodiesel [34].
It was commented by [35], that ion exchange resin and mag-
nesol powder are pioneered to replace water washing process.
Dry washing processes are easily adopted industrialized plants.
The use of magnesol to refine biodiesel requires thorough
mixing and needs 1.5–3 wt.% of biodiesel. Consequently,
magnesol was used to refine biodiesel produced from soybean
and grease, and it was found that both physical and chemical
properties of the fuel met the required specification designed
by ASTM D6751 and EN 14214 [36]. The polar compounds
are attracted by magnesol, therefore effectively removing
impurities such as metals, alcohols, di-glycerides, glycerol
and soap. Furthermore filtering of biodiesel mixture is easily
achieved via cloth filter of size 5 lm, with 1 lm nominal filter
used to perform final filtration process. Biodiesel is finally pol-
ished via filter (0.45 lm or 0.55 lm) prior to being applied as
diesel engine fuel. In addition, application of magnesol to
refine biodiesel was performed by [37], and the products
obtained were found to offer properties similar to the values
specified by ASTM D6751. Similarly, magnesol was employed
by [38], to refine crude biodiesel with different concentrations
of 0.25%, 0.50%, 0.75% and 1.00% at a temperature of
60 C, by means of a batch reactor. The reactor of size
200 ml immersed in a water bath was used for the purification
process. Biodiesel samples were removed from the reacting ves-
sel at an interval time of 10 and 20 min, but 30 min was the
standard time for the washing process. Thus the intermediate
products were removed via a centrifuge. Separation of the final
biodiesel product was performed using a Buchner funnel and
water ejector. Consequently, biodiesel with free glycerol con-
tent of 0.03% and methanol content of 0.51% was recorded.
It important to note that, when magnesol bag is opened, care
must be taken to re-seal the bag as tightly as possible since
magnesol is hygroscopic. Thus masks must be used to handle
magnesol, in view of the fact that the powder is very fine
[38]. Nonetheless magnesol is limited because little is known
about its performance and its catalytic efficiency [32]. In a sim-
ilar study by [39], magnesol was efficiently used to eliminate
numerous impurities in esters produced from used cooking
oils. The magnesol used was effective in removing methanol,
Adsorbent
(Magnesol/ion
exchange resins),
ac vated carbon
Refined
biodiesel
Filter
Pump
Spent
Adsorbent
glycerol and soaps chromatography column contact time was after methanol and water
formation. For the 0.50– with internal diameter 1 cm 720 min. The experiments stripping, silica refining
1.00 wt.% of magnesol , and a height of 15 cm by means of silica gel as enabled the removal of
methanol and Soaps which was packed with adsorbent were carried out glycerides and traces of
formation were reduced by glass wool. The column was in a vacuum (0.21 bar) with FFA from biodiesel, hence
around 98% and 67–92% then filled with a bed of 2 g stirring at a tem- perature of fulfilling the EN 14214
respectively, The glycerol of activated car- bon. 90 C for 90 min. The limits for glycerides, FFA
reductions were lower which Subsequently, crude results showed that glycerol and methyl ester contents
range from 15% to 55%. biodiesel samples were was almost completely [34].
Magnesol with a passed through the removed and a significant Another suitable
concentration of 1.00 wt.% adsorbent bed of the reduction of glycerides was adsorbent used for the
and 600 rpm provided the column with a flow rate of made by the adsorption purification of biodiesel is
best results. The 15 drop/min. Biodiesel with process. Such process Purolite (PD206), which is
international standard, EN high yields and allowed the eradication of a dry polishing media
14214 was met in terms of physicochemical properties water washing steps, purposely designed to
density, acid value, free was obtained after refining consequently minimizing eliminate impurities in
glycerol, methanol, triglyc- via activated carbons wastewater effluents issues. biodiesel [42]. Although
erides and mono-glycerides besides, the limits specified Further, purolite (PD206) is sold as
contents. In the same way an by ASTM D6751 for ion exchange resin; the
investigation by [28] biodiesel fuel were achieved. suppliers do not promote
employed adsorbent to In addition, the spent its revitalization since it is
refine crude bio- diesel and activated carbons used for acting as adsorbents. The
the results obtained from the biodiesel refining process use of ion exchange resins
magnesol 1% and silica were regenerated and for the refining of biodiesel
2% were 61 ppm of reused. The results obtained samples was investigated by
soap, 500 mg kg 1 of showed compared to the [38], at a time of 2 h for
water, other methods the activated removal of glycerol and
0.17 mg KOH g 1 for acid carbons regenerated methanol and established
number, 0.03% of free presented biodiesel with bet- that ion exchange resin can
glycerol and 0.22% of ter fuel properties as well as proficiently decrease
methanol. The results higher yields. glycerol to a level of 0.01 wt.
obtained for free glycerol In addition, biodiesel % and significantly
were above the specified silica refining was reported eliminate soap; however,
minimum by ASTM D6751 to offer easy and efficient metha- nol is not effectively
standard. procedure for removal of removed. The results
In another investigation, glycerides and FFA showed methanol content of
biodiesel was refined via impurities in crude biodiesel 1.14%, and this value is
activated carbon, activated [34]. Hence, silica gel was more than the value pro-
clay, activated fibers, and experimented in the vided by EN14214. Besides,
acid clay. As well, glycerol adsorption of glycerol and little soap adsorption points
was employed as a solvent monoglyc- erides. The values to a restriction for
to remove contaminants obtained indicated efficiency feedstocks having higher
from biodiesel. and robustness of content of soap forma- tion
Furthermore, biodiesel is adsorption of glycerol and [7,35]. Ion exchange resins
effectively purified with clay monoglycerides. provide excellent
grain size that ranged Consequently, purification performance in the
between 0.1 mm and 1.5 of biodiesel was carried out eradication of water,
mm. Better biodiesel through a settling sep- glycerol, removal soap, salt
purification process is arator and a silica and catalyst, and it is also a
achieved via clay with adsorption unit as an waterless process [42]. But,
smaller grain size. However alternative to the cur- rently its ability to remove
removal of spent adsorbent used water washing methanol is low [6].
proves more cumbersome. technique. In this sense,
When the size of clay grain different adsorbents such as 3
is larger, purifi- cation diatomaceous earth, .
process is inferior but impregnated activated
separation after the carbon and bleaching using M
treatment becomes simple. activated carbon were e
Usually, activated carbons utilized to refine biodiesel m
are mostly employed as produced from chicken oil b
adsorbent for the removal containing high degrees of r
of excess color in bio- diesel acidity. The process was a
carried out at an ambient n
[40]. In another study [41],
e
purified crude biodiesel temperature in a gas-tight
using activated carbons was autoclave with stirring. The
prepared from spent tea loading of the adsorbent s
waste. They used a was 0.3–5 wt.% and the e
p inert gases and aqueous
a solution. Therefore
r application of membrane
a technology in treating
t nonaqueous fluids is an
i area that is being newly
o explored [45]. The
n membranes used for the
pressure driven sep- aration
p processes, are reverse
r osmosis (RO),
o ultrafiltration (UF), and
c microfiltration (MF).
e Further separation using
s membrane is mainly a size
s exclusion-based pressure-
driven process, and the
Module configurations separation of components is
include among others based on shapes and the
tubular, hollow fiber, spiral sizes or weight of the
wound and rotating devices particles. During separation
and flat plate. Tubular pro- cess, the performance
modules are commonly of membrane is affected by
applied where it is beneficial interactions between
to have a turbulent flow membrane surface and
regime, for instance, in the components of the feed,
concentration of high solid veloc- ity of flow,
content feeds. The temperature, pressure, and
membrane is cast inside of membrane composition
a porous support tube [46].
which is often housed in a Membranes are classified
perforated stainless steel into organic and inorganic
pipe. Individual modules mem- branes. Inorganic
contain a cluster of tubes membranes such as
in series held in a stainless ceramic membranes have
steel permeate shroud. The great potentials toward
tubes are generally 1–6 m in aiding purification processes.
length and 10–25 mm in Inorganic membranes
diameter. Tubular modules (Al2O3, TiO2, ZrO2, SiC)
are cleaned without are presently
difficulty and a good deal
of operating data exists for
them. Their major
disadvan- tages are the
fairly low membrane
surface area [37].
The separation of
solution components via
membrane is achieved by
restricting the passing of
unwanted material via a
semi-permeable barrier in a
selective manner [43]. The
trans- portation using
membrane is affected by
diffusion of individ- ual
molecules, temperature or
pressure gradient and
concentration difference
[44]. In the refining of
water, gas sep- arations and
protein separations,
membrane technology has
played a critical role, but
industrial use of membrane
technique has limited
separations to relatively
given much attention for been superior to organic membranes
in terms of increased resistance to fouling, long lifetime, nar-
rower pore size distribution, mechanical, thermal and chemical
stability, resistance to microbial degradation, high flux, and
high porosity [46]. The organic membranes include polysul-
fone, polyamide, polycarbonate and a number of additional
highly developed polymers. Most of these synthetic polymers
comprised of improved resistance to microbial degradation
and chemical stability [26]. It was commented by [47], that
polyacrylonitrile (PAN) is asymmetric and porous membrane
which joins high permeation rate and high selectivity, but poly-
meric membranes may swell up, which result in either instant
swelling or long-term pore-size changes. Therefore, application
of polymeric membranes in solvent could lead to short life
span [48].
3.1. Biodiesel organic membrane separation process
Membrane technology has been playing a vital role in the refin-
ing of various products. Consequently, hollow fiber membrane
extraction (polysulfone) was used to remove impurities in
biodiesel. The hollow fiber membrane with the following
dimensions: length: 1 m, diameter: 1 mm, was filled with
distilled water and immersed into the reactor at a temperature
of 20 C. The unrefined biodiesel was transferred into the hol-
low fiber membrane with a low rate of 0.5 ml/min, and pressure
of 0.1 MPa [49]. Subsequently the crude biodiesel was passed
over heated sodium sulfate and then properly filtered [50]. This
procedure successfully decreased the loss of yield during the
refining process and avoided formation of emulsion during
the washing step. Further biodiesel purity of about 90% was
obtained and the physicochemical properties met the ASTM
standards [51]. The results obtained showed that membrane
extraction is very promising toward purifying biodiesel sam-
ples. It was found by [52], that membrane technique can be
employed in refining crude biodiesel without involving water
washing process. The membrane systems could enhance
treatment of effluents, and valuable products recovery, hence
minimizing their atmospheric harmful effects and offering solu-
tions to many ecological problems commonly faced during the
refining of crude biodiesel. The polyacrylonitrile (PAN)
membrane was tested at 25 C in order to eliminate glycerol,
methanol, water, and soap. With the addition of little amount
of water, removal of glycerol from biodiesel was considerably
increased and glycerol content as low as 0.013 mass% was
obtained, which is lower than the value (0.020 mass%) specified
by ASTM D6751 standard.
3.2. Removal of impurities from biodiesel via ceramic membrane
process
Recently, ceramic membrane technique is employed in separat-
ing and purifying biodiesel samples, particularly removal of
glycerol from biodiesel. Biodiesel was produced by [53], by
means of ethyl transesterification of degummed soybean oil
and evaluated use of micro- and ultrafiltration with ceramic
membranes to remove glycerol from biodiesel. Tubular a-
Al2O3/TiO2 membranes with average pore diameter of 0.2,
0.1 and 0.05 lm and 20 kDa were used to perform the experi-
ments. The experiments were performed using the following
conditions: temperature of 50 C, transmembrane pressures
(TMP) of 1.0, 2.0 and 3.0 bar, and mass concentrations of
acidified water of 10%, 20% and 30%. The separation process
was effectively carried out using mass concentration of 20%
acidified water; however, a sharp reduction of flux over the fil-
tration time was noticed which was attributed to the fouling of
the retained phase on the membrane surface. At a mass con-
centration of 30% the aqueous phase containing glycerol was
observed to permeate through the pores of the membrane.
Further, addition of 10% of acidified water, promoted reten-
tion of aqueous phase containing glycerol which yields biodie-
sel with glycerol content below 0.02 wt.%, besides the fouling
on the membrane was significantly reduced. The separation of
glycerol through ultrafiltration was advantageous since it elim-
inated the settling step and led to reduction of the amount of
water required for washing. The properties of biodiesel pro-
duced met the standards provided by ASTM D6751 for com-
mercialization. In a similar study [29], it was noted that
removal of free glycerol from crude biodiesel is a most critical
factor. This process was effectively performed using microfil-
tration with tubular Al2O3/TiO2 ceramic membranes, which
involved average pore size of 0.2, 0.4, and 0.8 lm, and filtra-
tion area of 0.005 m2. Fig. 2 shows schematic diagram of the
micro and ultrafiltration experimental unit. The samples of
biodiesel were microfiltered at a temperature of 60 C, and
transmembrane pressures of 1.0, 2.0, and 3.0 bar. For the feed
solution with 5% ethanol, the lowest flux decline rate and
99.6% glycerol retention were recorded. The technique involv-
ing refining of biodiesel appears to be efficient, thus offering
high quality biodiesel [2], as well as minimizing energy usage
[54]. In another study [55], biodiesel was refined using a cera-
mic membrane with a pore size of 0.02 lm in order to achieve
biodiesel fuel that meets both ASTM D6751 standard specifi-
cations. The membrane system used in the refining process
was effectively developed and the process variables which
include temperature, flow rate and transmembrane pressure
were examined. The interaction between various process vari-
ables was well understood using central composite design
(CCD) coupled with Response Surface Methodology (RSM).
The best operating conditions were found to be temperature,
40 C, flow rate, 150 L/min and transmembrane pressure,
2 bar. These conditions provided permeate flux of 9.08
2
(kg/m h), with corresponding potassium value of 0.297 mg/L
and free glycerol value of 0.007 wt.%; these values are quite
lower than those specified by ASTM D6751 standard specifica-
tions. The membrane system also presented biodiesel with
physical properties that are comparable to those of ASTM
D6751 and EN 14214 standards. These showed that ceramic
membrane with pore size 0.02 lm could provide high-quality
biodiesel. In another similar study [56], membrane reactor
(tube length: 1200 mm, pore size: 0.05 lm, surface area:
0.022 m2, internal diameter: 6 mm, and external diameter:
8 mm) was employed in producing biodiesel. The reactor is
particularly useful for its capability in retaining the unreacted
triglyceride, which led to the achievement of high-quality
biodiesel. The main advantage of the process is the achieve-
ment of free triglyceride esters. In another investigation [57],
micro- and ultrafiltration techniques were proposed to be used
in removing impurities from biodiesel. At different transmem-
brane pressures, the biodiesel mixture was filtrated in a
dead-end process and using membranes of different pore sizes.
Permeate fluxes obtained showed that greater pore sizes as well
as greater transmembrane pressures enable greater fluxes. The
Figure 2 Schematic diagram of the micro and ultrafiltration experimental unit [29].
properties of the produced r brane fouling include the temperatures, while using
biodiesel such as viscosity, o use of more hydrodynamic hydrogen peroxide, chlorine,
density, and acid values met c control affected by pulsated caustic, steam sterilization
the international legislation e feed flows or non-planar and/or ozone and strong
for biodiesel quality. The s membrane and the inorganic acids. These
process of water washing s application of further membranes can also be
and membrane separa- tion The degree of membrane perturbations at the back-pulsed, which is
considerably reduced the fouling is dependent on the membrane surface such as essentially a permeate flow
amount of soap present in proper- ties of the process continuous or pulsated reversal technique to decrease
the biodiesel. But, the feed and on the nature of electric fields [37]. fouling and to increase
proposed microfiltration the membrane employed. filtration efficiency. Back-
process could not efficiently Therefore membrane 3 pulsing is an in situ
reduce the free glycerol fouling is firstly controlled . technique for the cleaning of
content compared to water by careful choice of 3 membrane by periodically
washing. Also, the membrane type. Secondly, a . reversing the permeate flow
ultrafiltration membrane of good choice of module 2 by applying pressure to the
30 kDa could not reduce design offers appropriate . filtrate side. In this manner,
biodiesel glycerol content to hydrodynamic conditions permeate liquid is forced
the international legis- lation for the particular M back through the membrane
for free glycerol content. application. Equally, e to the feed side. This
However, the ultrafiltration process feed pretreat- ment m permeate flow reversal
membrane of 10 kDa is also essential. When b dislodges deposited
provided biodiesel with membrane fouling occurred, r foulants, which are then
glycerol content that is less the permeation rate can be a carried out of the
than 0.02 wt.%. Addition substantially restored n membrane module by the
of water in the raw bio- through back- flushing of e tangential flow of retentate,
diesel enhanced removal of the membrane. or which may re-deposit on
glycerol via membrane Nevertheless, this is rarely c the membrane surface later
filtration. Furthermore, totally effective; thus, l on [13,37,59]. The cleaning
production of high purity chemical cleaning is e process is more efficient
biodiesel using tubular eventually required. On a when using
ceramic membrane system start-up of a process, a n transmembrane pressure
was further validated i of
reduction in membrane
n
experimen- tally [58]. permeation rate to 30–10% 0.45 bar. It was suggested
g
of the pure water that an efficient way to
3.3. permeation rate after a clean and recover permeate
Membran few minutes of operation is p flux of a ceramic membrane
e fouling common for ultrafiltration. r that is submitted to crude
and o soybean oil ultrafiltration, is
Such a quick decrease may
cleaning c
be even more intense for by using only hexane. In this
process e
microfiltration. This is often way it can help to the
s
followed by a more steady understanding of the
s
3 decrease throughout behavior of the cleaning
. processing. More recent During membrane cleaning process of degumming of
3 approaches to the control process, components are crude oil using ceramic
. of mem- removed physically, membranes [60].
1 chemically or hydraulically.
. A module is temporar- ily
out of order, when the
M cleaning process is
e performed. As a result,
m dead-end management is a
b discontinuous process. The
r length of time that a module
a performs filtration is called
n filtra- tion time and the
e length of time that a
module is cleaned is called
f cleaning time. In practice
o one always tries to apply
u the lowest possible cleaning
l time and make filtration
i time last as long as
n possible. In addition,
g ceramic membranes are
ideal for in-place chemical
p cleaning at high
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