Journal of Mechanical Engineering and Sciences (JMES)

ISSN (Print): 2289-4659; e-ISSN: 2231-8380; Volume 7, pp. 1115-1126, December 2014
© Universiti Malaysia Pahang, Malaysia
DOI: http://dx.doi.org/10.15282/jmes.7.2014.10.0108

PERFORMANCE EVALUATION OF CERAMICS MICROFILTRATION

MEMBRANE FOR WATER TREATMENT

F.T. Owoeye1, A.P. Azodo1* and S.B. Udo2

1
Mechanical Engineering Department
Federal University of Agriculture
Abeokuta (FUNAAB),P M B 2240, Abeokuta, Nigeria.
E-mail: [email protected], [email protected]
Phone: +2348060601776
2
Metallurgical Department, Yaba College of Technology
Yaba Lagos, Nigeria.P.M.B. 2011, Yaba, Lagos

ABSTRACT

Ceramic membranes are especially suitable for processes with high temperatures and
harsh chemical environments or for processes where sterilizability of the membrane is
important. The main objective of this work is to determine the evaluation of four
different ceramic membranes with different material compositions. Ceramic disc type
microfiltration membranes were fabricated by the mould and press method from
different percentage compositions of clay, kaolin, sawdust and wood charcoal. The
fabricated membranes were sintered at a temperature of 1100°C and characterized by an
X-ray diffractometer and optical scanner. Compressibility tests and physical properties
of the membranes were also examined. It was observed that, as the percentage
composition of kaolin increased from 0 to 80% and the percentage composition of clay
decreased from 80 to 0% respectively, the compressive stress of all the sample
membranes increased, with an increase in compressive strain from 1.8 to 2.4. Sample A
had the highest value of compressive stress from 1.8 to 2.2 compressive strain, but
sample B had the highest value of compressive stress of 150MPa at a compressive strain
of 2.4. Optical micrographs of all membranes showed the presence of uniformly
distributed pores and no cracks were seen around them. It was concluded that, with
increasing percentage of kaolin and decreasing percentage of clay, there was a decrease
in porosity and water absorption, as well as a decrease in the mechanical properties of
the fabricated membranes.

Keywords: Membranes; physical properties; X-ray diffractometer; kaolin; sintered.

INTRODUCTION

Ceramic membranes are especially suitable for processes with high temperatures and
harsh chemical environments or for processes were sterilizability of the membrane is
important. These ceramics were made of animal fat and bone mixed with bone ash and a
fine claylike material. Primitive ceramics were made of basic earthen materials like clay
and were burnt in domes. Ceramics is the materials science and engineering of inorganic
or nonmetallic solids. Traditional ceramic raw materials include clay minerals such as
kaolinite, aluminium oxide (alumina), carbides and silicates [1]. Membrane processes
have been increasingly gaining importance in recent decades as separation techniques,
since they offer several advantages over traditional methods (like precipitation or

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liquid–liquid extraction), such as set-up and handling simplicity, low time consumption,
including a relatively cheap technology and they are environmentally respectful. Most
membrane processes can be performed at room temperature and are carried out
continuously. Furthermore, it must be considered that membranes can be prepared to
have a wide range of different sizes from macro to micro. As a consequence, some
membrane processes have already been applied at industry level; and certain of them,
for instance, water treatment (including water desalination), food purification and
biomedical purposes (blood dialysis), are even industrially consolidated [2-4].
Membranes may be divided, according to their composition, into organic or inorganic
ones, the former (organic polymeric membranes) being mainly used in all commercial
applications. Therefore, the discussion in this study essentially refers to polymeric
membranes. A membrane applied for removing colloidal particles in liquid is usually
semi-permeable. Its pore range of 0.1–20µm is suitable for water treatment, which
allows one component of a mixture to permeate the membrane freely, while hindering
permeation of other components [5, 6]. The membrane separation process is based on
the presence of semi-permeable membranes. The principle is quite simple; the
membrane acts as a very specific filter that will let water flow through, while it catches
small particles and other substances, where the performance is enhanced by the pressure
difference, either applied pressure or vacuum. Membrane filtration can be used as an
alternative to flocculation, sediment purification techniques, adsorption (sand filters and
active carbon filters, ion exchangers, extraction and distillation) and sand [2, 7, 8].
Microfiltration often serves as a critical step in ensuring final product integrity.
Microorganism removal is essential to beverages in which contamination can lead to
consumer illness, as well as to those beverages susceptible to microbial spoilage
mechanisms. The microfiltration process uses porous membranes to separate suspended
particles with diameters between 0.1 and 10μm [9, 10]. Beverages that are not in danger
from microbial contamination may undergo microfiltration for general particulate
removal to ensure the aesthetic quality of the final product. Microfiltration serves many
auxiliary functions throughout the beverage industry in addition to final product
filtration. Ensuring process water quality can be crucial to general plant cleaning and
sanitation regimens. Gases such as carbon dioxide are being used in many product
formulations. Bulk or point-of-use filtration of these gases is often important to
maintaining product quality. Selective use of microfiltration can lead to a faster, easier,
and more economical process. Brewers can use microfiltration both for lees recovery
and as an alternative to pasteurization. Wineries may use microfiltration for titrate
removal [11]. Whiskey makers can remove chill haze using a filtration step. Ceramic
cross-flow systems allow the cleaning and reuse of caustic solution. Each plant’s
individual processes, even within the same industry, may have their own uses for
microfiltration [12]. The bottled water and wine industries are the largest beverage
microfiltration users in terms of spending. They are followed by the beer, spirits, and
soft drink industries. Other industries that use microfiltration include juice, sports drink,
energy drink, coffee and tea, oils, as well as various liquid or semi-liquid product or
component producers. The ceramic membranes have found many applications in the
food, beverage, biotechnological and pharmaceutical industries as well as in the
petrochemical industry, environmental control, electronic industry, gas separation and
other process industries [2, 13-17]. Ceramics are the most compatible products with
their qualities of being free from decay caused by gradual natural impacts like
corrosion, erosion, abrasion and thermal shocks [18]. Advantages of ceramic
membranes include stability towards high temperature, high pressure and resistance to

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chemical attack [19, 20]. It is commonly agreed that the key factor for the correct
development and application of polymeric membranes is the control of their polymeric
morphology. Therefore, many efforts have been made within recent decades to find the
relationship between membrane preparation, membrane morphology and membrane
performance [11]. In that sense, membrane characterization has become fundamental for
the optimization of membrane process design, as membrane features, such as nature,
thickness and porosity, govern the process behaviour. The best results, that is, the most
unfailing outputs, are encountered when combining different membrane characterization
techniques [21]. This research work is aimed at the determination and evaluation of four
different ceramic membranes with different material compositions. It also focuses on
the fabrication of membranes from natural raw materials, as well as the investigation of
mechanical and physical properties of the produced membrane discs.

MATERIALS AND METHOD

The raw materials that were used for this research work are represented in Figure 1. The
major materials constituents were clay and kaolin, while sawdust acted mainly to aid the
porosity of the membranes and was burnt off during firing. Wood charcoal also gave
room for little porosity, but mainly helped the fabricated membrane to be fired. Water
was added to make paste. Table 1 shows the percentage composition of the raw
materials used in fabrication of the membranes. Four membranes of different
constituents were produced: sample A contained 80% clay, 0% kaolin, 10% sawdust
and 10% charcoal. Sample B contained clay, kaolin, sawdust and charcoal at 60%, 20%,
10% and 10% respectively. Sample C contained 20% clay, 60% kaolin, 10% sawdust
and 10% charcoal, while sample D contained 80% kaolin, 10% sawdust, and 10%
charcoal with no clay content.

RAW MATERIALS

Main Materials Additives Solvent (Water)

Clay Kaolin Sawdust Charcoal

Figure 1.Graphical representation of the raw materials.

Table 1.Percentage composition of the raw materials.

Samples Clay % Kaolin % Sawdust % Charcoal %

A 80 0 10 10
B 60 20 10 10
C 20 60 10 10
D 0 80 10 10
.

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Steps in Production of Membrane

Slurry preparation: The main components of slurry used for the fabrication of ceramic
membranes are inorganic powder, organic additives and solvent. In the selection of the
inorganic powder, important factors are particle size and distribution, as well as the
shape of the particles. They have an effect on the porosity, pore size and pore size
distribution of the final product.

Grinding: This involves the process of breaking the large particles of raw materials into
small pieces.

Milling: Milling is the process by which materials are reduced from a large size to a
smaller size. Milling may involve breaking up cemented material (in which case
individual particles retain their shape) or pulverization (which involves grinding the
particles themselves to a smaller size). Milling is generally done by mechanical means,
including attrition.

Sieving: A process by which un-milled materials are separated from fined/powder

forms.
Batching: Batching is the process of weighing the raw materials according to their
recipes and preparing them for mixing, weighing different powdered raw materials in
different percentages to make up the batch composition for different membranes.

Mixing: Mixing occurs after batching and is performed with various machines such as
dry mixing ribbon mixers [22].

Addition of water: Water is added to the mixed powders gradually in order to avoid
over-softening of the contents.

Fabrication: Four pair membranes were fabricated by means of mould and press
methods. The produced membranes were dried for some days and later sintered at a
temperature of 110oC. Details of the processing steps of the membranes are displayed in
Figure 2.
Raw materials

Grinding Forming/Fabrication

Milling Drying

Sieving
Firing

Batching
Assembly/Testing

Mixing

Figure 2. Sequential path for membranes preparation/production.

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Determination of Mineral Composition of the Membranes

The minerals compositions of all powder samples were determined in the laboratory of
the Research Institute, Engineering Materials and Development Institute, Abeokuta,
Nigeria. The mineralogical data were determined on each sample powder using Radicon
MD-10, version 2.00 X-ray diffractometry equipment withCuKα radiation at exposure
time of 1200/1200 seconds with Lambda: 1.5418 and a Beta filter used for all the
samples. The diffractometer is an apparatus used to determine the angles at which
diffraction occurs for powdered samples.

Optical Testing

The micrographs of all the fired samples were determined by an optical testing machine
with model number 702907.

Determination of Physical Properties of the Membranes

Bulk Density

The bulk density of the fired membrane samples was determined by displacement of
water from the beaker using the Archimedes principle. The weights of all membrane
samples were measured in air using a Digital Electronic Scale model JCS-A
Gallenkomp. The experimental set-up included the mass of the beaker partially filled
with water, with and without the cut-up samples immersed in water one after the other.
The difference gave masses of water displacement, according to the Archimedes
principle. The mass of water displaced can be easily related to the volume of water
displaced, as the density of water is known as 1000kg/m3. Thus, the bulk density in
g/cm3 is given in terms of mass sample measured in air and the volume displaced by the
membrane as shown in Eq. (1).

Mass in air (g)

Bulk density (g/ml)  (1)
Volume of water displaced (ml)

Percentage of Water Absorption by the Membranes

Water absorption measurements were carried out according to BS EN 12808 – 5:

(2008). Cut-up samples of fired membrane were measured using a Digital Electronic
Scale model JCS-A Gallenkomp as initial weights of the membranes. The measured
membrane samples were then soaked in water in a beaker for 24 hours at room
temperature in the Mechanical Engineering laboratory. As the samples were immersed
in water, air bubbles were observed as the pores in the samples were filled with water.
After the lapsed time, the samples were removed from the beaker and allowed to dry by
removing the excess water on the surfaces using a dry napkin prior to weighing as wet
weight, and the percentage of water absorption was calculated as shown in Eq. (2).

Wet mass (g) - Mass in air (g)

Water absorption (%)  100 (2)
Mass in air (g)

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Percentage Apparent Porosity of the Membranes

For calculation of the percentage apparent porosity, all the samples were measured in
order to get the initial weight (weight in air). They were suspended in water individually
with string and air bubbling was observed. The weight of each suspended sample was
measured. The samples were also soaked in water for 24 hours, after which the weights
were measured. The percentage apparent porosity was determined as shown in Eq. (3):

Soaked mass (g) - Mass in air (g)

Apparent porosity (%)  100 (3)
Soaked mass (g) - Suspended mass (g)

RESULTS AND DISCUSSION

Chemical Composition of Clay

From the percentages of chemical composition of the clay material, alumina and silica
are found to be the major constituents with other minor constituents, while the
percentage of manganese (II) oxide [23] could not be determined. The loss on ignition
(LOI) corresponds to water vapour from hydroxide reaction in the clay minerals, the
burning out of organic matter and the carbonate decomposition in CO2 and oxide in the
minerals, as shown in Table 2.

Table 2.Chemical composition of clay.

Clay SiO2 TiO2 Al2O3 Fe2O3 MnO MgO CaO P2O5 K2O Na2O LOL
contents
Composition 46.4 1.69 34.0 2.49 ND 0.04 0.02 0.04 0.08 0.03 17.7
%

Figure 3. Compressive stress against compressive strain.

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Compressibility Test

Figure 3 shows the compressive stress against compressive strain of the produced
membranes. Generally, the compressive stress of all the sample membranes increased
with increase in compressive strain from 1.8 to 2.4. Sample A had the highest value of
compressive stress at 1.8 to 2.2 compressive strain, but sample B attained the highest
overall value of compressive stress of 150MPa at compressive strain of 2.4. The
relationship between compressive stress and strain showed that the fabricated
membranes have the ability to withstand external loads during the operation that is the
filtration technique [24].

Physical Properties of the Membranes

The apparent porosity of the membranes examined, as shown in Table 3, decreased from
samples A, B, C to D with values of 170.05, 165.71, 161.9 and 153.10% respectively.
The water absorption of the membranes also decreased in value from samples A to D in
a narrower range (48.92 to 46.52%). Bulk densities of the fabricated membranes
increased from samples A, B, C to Dwith values in order of 33.01, 34.09, 34.93 and
35.82g/ml.

Table 3. Apparent porosity of the membranes.

Samples Apparent porosity (%) Water absorption (%) Bulk density (g/ml)
SP A 170.05 48.92 33.01
SP B 165.71 48.56 34.09
SP C 161.9 47.11 34.93
SP D 153.10 46.52 35.82

Q-quartz, A-alumina, V-vermiculite

Figure 4. X-ray diffraction pattern for membrane A.

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Mineral Compositions of Membranes

The crystalline phases in the fired fabricated membranes, as shown in Figures 4 to 7,

were identified using an X-ray diffractometer, a Radicon MD10.00UM, Version 2.00.1 using
CuKα radiation at 40Kv/40mA from 12°<2θ<73°, with exposure time of 1200/1200sec.
Figure 4 shows the diffraction pattern for membrane A containing quartz, alumina and
vermiculite. In quartz, it had the highest peak of 0.75 × 102 pulses and 25.0o at 2θ, while
the vermiculite had a peak of 0.2 × 102 pulses and 40.0o at 2θ. Alumina had its highest
peak of 0.1 × 102 pulses and 60.0o at 2θ. Alumina, montmorillonite, quartz, vermiculite
and silica are the minerals contained in membrane B, as shown in Figure 5. Alumina
and quartz had their highest peaks of 0.1 × 102 pulses and 40.0o at 2θ and 0.3 × 102
pulses and 17.5.0o at 2θ respectively. Montmorillonite had its highest peak of 0.25 × 102
pulses and 55.0o at 2θ, while vermiculite had its highest peak of 0.25 × 102 pulses and
65.0o at 2θ. The highest peak of 0.25 × 102 pulses and 37.5.0o at 2θ was produced by
silicate. Figure 6 shows the diffraction pattern of fabricated membrane C, which
contained quartz and kaolin. Kaolin had its highest peak of 0.7 × 102 pulses and 17.7o at
2θ, while the quartz had the highest peak of 0.25 × 102 pulses and 20.0o at 2θ. Figure 7
shows that the diffraction pattern for membrane D contained the presence of kaolin and
carbon with highest peaks of 1.3 × 102 pulses and 25.0o at 2θ and 0.3 × 102 pulses and
36.0o at 2θ. It also contained vermiculite and montmorillonite [25].

A-alumina, M-montmorillonite Q-quartz, V-vermiculite, S-silica

Figure 5. X-ray diffraction pattern for membrane B.

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Q-quartz, K-kaolin

Figure 6. X-ray diffraction pattern for membrane C.

K-kaolin, C-carbon, V-vermiculite, M-montmorillonite

Figure 7. X-ray diffractometer pattern for membrane D.

Optical Micrographs of the Membranes

Figure 8 shows the optical micrographs of the four fabricated membranes A, B, C and D
respectively, with the lens of the machine set at a magnification of 100. It was noticed
generally in all the four membranes that the magnifications of 100 were dark. It was
also observed that all the membrane surfaces were neat, without any traces of cracks.

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M: X100 M: X100

(a) Membrane A (b) Membrane B

M: X100 M: X100

(c) Membrane C (d) Membrane D

Figure 8. Optical micrograph

CONCLUSIONS

This research work has been able to make use of natural resources or raw materials that
are highly available with low cost of extraction from their natural deposits. The total
cost of production of these membranes is much less than procuring synthetic or already
made materials for the production of membranes that perform the same function. Also,
this project work has enabled us to fabricate effective and functional membranes from
different constituents of raw materials for water treatment. The optical micrographs of
all the membranes showed the good quality of the clay and kaolin materials used in the
production of the membranes, as there were no cracks on any of the membranes, despite

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the high firing temperature of 1100oC. The addition of kaolin content in the mixture of
all the sample membranes prepared reduced the physical properties of the percentage of
porosity and that of water absorption, while only the bulk density of the sample
membranes increased with an increase in the percentage of kaolin content. It was
concluded that, with an increasing percentage of kaolin and a decreasing percentage of
clay, there was a decrease in porosity and water absorption, as well as a decrease in the
mechanical properties of the fabricated membranes. Further research should be carried
out to investigate the performance of ceramic nano-filtration membranes for water
treatment.

ACKNOWLEDGEMENTS

Our special gratitude to the entire staff of the Mateng Water Filtron Abeokuta for
allowing us to make use of their equipment for the fabrication of the membranes.

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