CM Design and Characterization
CM Design and Characterization
I. INTRODUCTION
Membrane separation has become an important unit operation in water operation in water and wastewater
treatment. Different degrees of water quality can be obtained with removal of particles, dissolved organic compound, protein
and ions. However, two dominant areas are removal of organic compound in water clarification and osmotic desalination.
The overall principle in any membrane separation is sketch in figure.
1. Separation by size- the sieve effect: This requires porous membranes with rather large pores. Terms like macrospores,
mesopores and micro pores (figure 1.a.2) are used to describe the pore size in membrane for microfiltration ultra-
filtration and nanofiltration.
2. Separation by different in solubility and diffusivity of material: This principle is used in operations like reverse osmosis
and requires the membrane used to be dense (nonporous).
3. Separation by charge: An ion exchange membrane separates compounds of different charges. Ion-exchange membranes
are used in operation like electro dialysis and are generally nonporous.
The above table is a very qualitatively way to list of physical-chemical membrane properties. It is often difficult to
do otherwise with this kind of properties, but in the next section a tool to physical characterization will be presented and it
will make the classification more quantitatively.
Plant Engineers and plant operators demand, with respect to membrane installations, process stability, high
availability and low requirements for preliminary treatment and minimum need for support and maintenance.
In contrast to many polymer membranes the ceramic membranes are a perfect match for this demand due to their
extremely high chemical and physical stability, their outstanding separation characteristics and their long working life.
Ceramic materials are generally very stable chemically, thermally and mechanically, and in addition are frequently
bio inert. They are therefore ideal materials for many applications in the chemical and pharmaceutical industry or in water
and waste water processing.
The medium to be filtered flows through the channels of the membrane carrier. Particles are retained if their size
exceeds the radius of the membranes pores, building up the concentrate. The filtrate permeates through the pores and it is
subjected to subsequent process stages.
Many are the advantages deriving from the ceramic membranes use:
No ageing, long life and reliability.
High temperature stability.
Mechanical stability under large pressure gradient.
Stability over a large pH range.
0.3 – 100 efficiency in gas separation.
Ability to be backwashed and abrasion resistance (steam sterilization and high flash capability )
Incentive to bacterial action.
Can process highly viscous fluid.
Good control of pore dimension fouling.
They are ecologically friendly and more favorable than separation technologies.
No additives are necessary and the process temperature is not limited
Filtration with ceramics is a mild, highly selective process without phase transformation. Running costs are limited
by closed production cycles and continuous processes.
Disadvantages are:
Brittle character needs configuration supporting system.
Relatively high capital installation cost.
Relatively high modification costs in case of defects.
Sealing technology for high temperature application may be complicated.
Applications
Initially, ceramic membranes were used in waste water technology. Meanwhile, successful and possible applications
cover all industries where media were filtered.
Chemical industry :
- Product separation and cleaning.
- Concentration of polymer suspensions and metal hydroxide solutions.
- Separation of catalysts.
- Recovery of dyes and pigments.
- Desalination of products.
- Cleaning and recycling of organic solvents.
Weighing
Cone Blending
Extrusion
Natural Drying
Testing
Binders: Substances, which hold ceramic raw material and bodies together during the initial stage of processing, are called
binder.
1. Lignin has been used for tempering all type body fabricated by ceramic process it increases the strength of the weak body.
2. Tannic acid has long been employed to increase the particles of days, but it is not effective as extract in increasing the dry
strength.
3. Ordinary paraffin’s, with a small percentage of carnauba wax, is a good binder in some cases and can be molded cold with
a reduction in molding time.
600C to 700C
Solution
Filtration
Solution
SiC tube
Zirconium Oxide(ZrO2)
Zirconia is an extremely refractory material. It offers chemical corrosion inertness to temperatures well above the
melting point of alumina. The material has low thermal conductivity. It is electrically conductive above 6000 C and is used in
oxygen sensor cell and as the susceptor (heater) in high temperature induction furnaces. With the attachment of platinum
lead, Nernst glowers use in spectrometers can be made as a light emitting filament which operated in air.
Occurrence
The element occurred with a number of mineral deposits. Principally rutile ilmenites which are widely distributed in
earth crust and lithosphere and it is found in almost in all living things, rocks, water bodies and soil. The metal is extracted
from its principle mineral ore via kroll process or hunter process.
Sulphate process
Chloride process
Sulphate process
The sulphate process has been in existence for more than 70 years. The process is carried out in the following steps.
Hydrolysis
Calcinations
Dry milling
Chloride process
The chloride process was developed by du-pont around 1959. The main process steps are as follows,
A technical composition of sulphate & chloride process indicates that the chloride process gives a product which is in finer
in particle size, low in impurity &less waste products are generated. As a result more & more manufactures are shifting to
chloride process. Presently about 55% of titania is produced by sulphate process.
Density 4 gm/cc
Porosity 0%
Modulus of rupture 140 Mpa
Compressive strength 680 Mpa
Poisson’s ratio 0.27
Fracture toughness 3.2 Mpa.m-1/2
Shear modulus 90 Gpa
Modulus of elasticity 230Gpa
Micro hardness(HV 0.5) 880
Resistivity(250C) 1012 ohm.cm
Resistivity(7000C) 2.5×104 ohm.cm
Dielectric constant(1 MHz) 85
Dissipation factor(1 MHz) 5× 104
Dielecric strength 4 kV/mm
Thermal expansion(RT-10000C) 9×10-6
Thermal conductivity(250C) 11.7Wm/K
2. True density
True density is the mass per unit volume of a material including all forms of pores i.e. open and closed pores.
4. Water absorption
The water of absorption is expressed as the %age relationship of weight of water absorbed by the dry specimen.
Experimental procedure:
The specimen to be tested is kept in Dryer at 1100 C until it reaches constant weight, then dry weight (D) of the
specimen is noted down. Then the specimens are kept in boiling water for 2 hours, then they are allowed cooled to room
temperature and the saturated weight (W) of the test specimens are noted down, then the specimens are suspended in water
and the suspended weight (S) of the specimens are noted down and calculated using the formula given below.
Dry weight
SEM analysis
The scanning electron microscope (SEM) is a type of electron microscope that images the sample surface by
scanning it with a high- energy beam of electrons in a raster scan pattern. The electrons interact with the atoms that make up
the sample producing signals that contain information about the sample’s surface topography, composition and other
properties such as electrical conductivity.
The types of signals produced by an SEM include secondary electrons; back scattered electrons (BSE), characteristic
X-rays, light (cathodoluminescence), specimen current and transmitted electrons. These types of signal all require
specialized detectors for their detection that are not usually all present on a single machine. The signals result from
interactions of the electron beam with atoms at or near the surface of the sample. In the most common or standard detection
mode, secondary electron imaging or SEI, the SEM can produce very high –resolution images of a sample surface, revealing
details about 1 to 5 nm in size Due to the way these images are created, SEM micrographs have a very large depth of field
yielding a characteristic three – dimensional appearance useful for understanding the surface structure of a sample. This is
exemplified by the micrograph of pollen shown to the right. A wide range of magnifications is possible, from about x
250,000, about 250 times the magnification limit of the best light microscopes. Back- scattered electrons (BSE) are beam
electrons that are reflected from the sample by elastic scattering. BSE are often used in analytical SEM along with the
spectra made from the characteristic X-rays. Because the intensity of the BSE signal is strongly related to the atomic number
Permeability :
Permeability apparatus
Pressure difference
Where,
LMH= litre
m2.hr.
RESULTS
Sample No. Dry wt.(gms) Suspended Saturated Bulk density % Porosity % Water
wt.(gms) wt.(gms) (gm/cc) absorption
U –Uncoated samples
Inlet
pressure Permit flux LMH
Sample no Composition Area(m2) (kg/cm2) ml/min (l/m2.hr)
3 100% titania sol 0.00319 0.5 7 131.66
1 10 188.09
1.5 13 244.514
2 14 263.32
2.5 16 300.32
45gms of zirconia
oxynitrate + 300ml of
6 water 0.0046 0.5 8 104.35
1 11 143.48
1.5 15 195.65
2 17 221.74
2.5 21 273.913
Titania sol + 5%
titania
powder(50ml)+ 50ml
5 0f slurry 0.00319 0.5 16 300.47
1 20 375.59
1.5 28 525.82
2 41 769.95
2.5 44 826.29
Titania slurry+ 15%
13 sol 0.0032 0.5 9 168.75
1 12 225
1.5 17 318.95
2 23 431.52
2.5 26 487.8
200ml of zirconia
oxynitrate solution +
14 100ml of water 0.0046 0.5 22 286.96
1 34 443.28
1.5 40 521.51
2 42 545.45
2.5 45 586.70
200ml of zirconia
oxynitrate solution +
23 100ml of water 0.0032 0.5 24 433.99
1 25 452.08
1.5 32 578.66
2 34 614.83
2.5 37 669.08
200ml of zirconia
oxynitrate solution +
24 100ml of water 0.0031 0.5 22 425.78
1 28 541.90
1.5 30 580.61
2 32 619.31
2.5 34 658.02
SEM analysis:
1. TiO2 coated samples
References:
1. C.C. chen, M.M. Nasrallah, H.U. Anderson, Solid state ionics.(1994) 101-108
2. T. Okubo, T. Takahashi, M. sadakata, H. magaroto, J. Membr. Sci 118(1996) 151-157
3. J. Kimi, Y.S. Lin, J. Membr. Sci. 139 (1998) 175-183
4. Introduction to ceramics by ‘Singer and Singer’
5. Www.sciencedirect.com