COMBINED RESISTANCE AND OSMOTIC PRESSURE MODEL … · Large molecules bound by Vander Waals forces...

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International Journal of Advanced Research in Engineering and Technology (IJARET) Volume 5, Issue 5, May 2014, pp. 160–173, Article ID: IJARET_05_05_018

Available online at http://www.iaeme.com/ijaret/issues.asp?JType=IJARET&VType=5&IType=5

ISSN Print: 0976-6480 and ISSN Online: 0976-6499

© IAEME Publication

COMBINED RESISTANCE AND OSMOTIC

PRESSURE MODEL MODELS FOR

ULTRAFILTRATION USING DYE SOLUTION FOR

PREDICTION OF MEMBRANE FOULING IN SPS,

SPES, SPEEK AND NAFION MEMBRANES

B. Chirsabesan*, M.Vijay and S. Shanmugananthan

Department of Chemical Engineering, Annamalai University, Annamalai Nagar, India

*Corresponding Author, [email protected]

ABSTRACT

Experiments were performed in four poly electrolyte membranes (PEM) such

SPES, SPS, SPEEK and Nafion at optimized condition. The SPES, SPSf, SPEEK were

prepared with different ion exchange capacity. In the present study, Eosin B dye was

chosen for effective investigation of fouling, resistances due to pore blocking, pore

constriction, caking mechanisms. The understanding of both combined caking and

complete blockage model was the most useful for membrane performances. The

individual model prediction was investigated to provide good fits of all SPES, SPS,

SPEEK and Nafion membranes. The resistance series model was provided good fits of

a broad range of curves where the flux declines in a manner by cake filtration and

complete blocking. The osmatic pressure models models also provided good data fits

and may be applicable to systems where these models are consistent with the

experimentally observed fouling mechanisms.

Keywords: Dye solution, resistance series model, osmatic model, poly electrolyte

membranes (PEM)

Cite this Article: B. Chirsabesan, M. Vijay and S. Shanmugananthan, Combined

resistance and osmotic pressure model models for ultrafiltration using dye solution

for prediction of membrane fouling in SPS, SPES, SPEEK and Nafion membranes,

International Journal of Advanced Research in Engineering and Technology, 5(5),

2014, pp 160–173.

http://www.iaeme.com/ijaret/issues.asp?JType=IJARET&VType=5&IType=5

1. INTRODUCTION

Nowadays, when care of the environment is a major issue, it is tempting to assume that the

use of natural colours is an environmental friendly alternative to present-day practice. There

are several groups studying the use of natural dyes in modern dyeing industry (Angelini et al.

2003, Kamel et al. 2005). Some of the advantages of the use of this type of compounds are

the absence of toxicity upon humans, the use of sustainable sources and the fit into the natural

pathways of biodegradation of the released dye baths. According to the Colour Index dyes

Combined resistance and osmotic pressure model models for ultrafiltration using dye solution for

prediction of membrane fouling in SPS, SPES, SPEEK and Nafion membranes


can be classified on the basis of colour and application method. Various attractive forces have

the potential of binding dyes to fibres, and often more than one type of chemical bonding can

operate with the same dye-fibre combination. The dominant force depends on the chemical

character of the fibre and the chemical groups in the dye molecule. The types of bonds

established between the dye and the fibre, by increasing relative strength of the bond, can be:

Van der Waals, hydrogen, ionic or covalent (Guaratini and Zanoni 2000). According to the

application categories dyes can be classified as seen in Table 1.

Table 1 Application categories of dyes

Type of dye Characteristics Substrates

Acid

When in solution are negatively

charged; bind to the cationic NH3+

-

groups present in fibres

Nylon, wool, polyamide, silk, modified acryl,

paper, inks and leather

Reactive Form covalent bonds with OH

-, NH

-

or SH- groups

Cotton, wool, silk and nylon

Metal complex

Strong complexes of one metal ion

(usually chromium, copper, cobalt or

nickel) and one or two dye molecules

(acidor reactive)

Silk, wool and polyamide

Direct Large molecules bound by Vander

Waals forces to the fibre

Cellulose fibres, cotton, viscose, paper, leather

and nylon

Basic Cationic compounds that bind to the

acid groups of the fibre Synthetic fibres, paper and inks

Mordant

Require the addition of a chemical

that combines with the dye and the

fibre, like tannic acid, alum,

chromealum, and other salts of

aluminium, chromium, copper, iron,

potassium, and tin

Wool, leather, silk, paper, modified cellulose

fibres and an odized aluminium

Disperse Scarcely soluble dyes that penetrate

the fibre through fibres swelling

Polyester, polyamide, acetate, acrylic and

plastics, Paints, inks, plastics and textiles

Pigment

Insoluble, non-ionic compounds or

insoluble salts that retain their

crystalline or particulate structure

throughout their application

Cellulose fibres, cotton, viscose and wool

Azoic and Ingrain

Insoluble products of a reaction

between a coupling component and a

diazotised aromatic amine that

occurs in the fibre

Cotton, viscose, cellulose acetate and

polyester

Sulphur Complex polymeric aromatics with

heterocyclic S-containing rings Cellulose fibres, cotton and viscose

Solvent Nonionic dyes that dissolve the

substrate to which they bind

Plastics, gasoline, varnish, lacquer, stains,

inks, oils, waxes and fats

Fluorescence

brightners

Mask the yellowish tint of natural

fibres

Soaps and detergents, all fibres, oils, paints

and plastics

Food Non-toxic and not used as textile

dyes Food

Natural Obtained mainly from plants Food, cotton, wool, silk, polyester, polyamide

and polyacrylonitrile

B. Chirsabesan, M. Vijay and S. Shanmugananthan


Discharged wastewater by some industries under uncontrolled and unsuitable conditions

is causing significant environmental problems. The importance of the pollution control and

treatment is undoubtedly the key factor in the human future. Membrane technology has

emerged as a feasible alternative to conventional treatment processes of dye wastewater and

has proven to save operation costs and water consumptions by water recycling. Usually this

technique is applied as a tertiary/final treatment after biological and/or physical-chemical

treatments (Ciardelli et al. 2000, Marcucci et al. 2002). It has also been used to concentrate

and purify dyes in the manufacture of these compounds (Crossley 2002). Table 2 shows the

disadvantages according to different dye class

Table 2 Disadvantages of different dye classes

Dye classes Disadvantages

Azo groups

Their reductive cleavage of azo linkage is

responsible for the formation of toxic amines in

the effluent

Anthraquinone-based

dyes

It is most resistant to degradation due to their

fused aromatic ring structure and thus remains

coloured for a longer time in wastewater.

Basic dyes It has high brilliance and intensity of colours and

is highly visible even in a low concentration

Rose Bengal dye is extensively used in the printing, insecticides and in dying industries.

Aqueous solutions of Eosin B, Eosin Y, Eryhtrosin B, Ehidium Bromide, Giemsa Stain, Janus

Green B, Methylene Blue, and Trypan Blue were successfully decolorized. The reduction

after 24 h is reported to be 53%. Eosin B dyes blue can be degraded to some extent on

activated carbon and its surfactant based desorption. The efficacy of removal was higher for

dyes with low molecular mass, with lower flowrate and smaller particle size of the resin.

Quinoline Yellow (E104) are both sometimes referred to as quinoline yellow which has

created significant confusion when companies are formulating global products. For example,

the following countries accept either color for use in drug products: Argentina, Australia,

Canada, Bangladesh, Brazil, Chile, Hong Kong, Israel and Peru. For example, China, Korea,

India and Pakistan accept only quinoline yellow and Mexico and the Phillipines only accept

quinoline yellow. It is important that the specific regulations of the target countries be

evaluated before making a formulation decision. Hence we have taken up work on the

membrane For the ultrafiltration performance dye solution. The resistances effecting the

permeate flux like membrane resistance, concentration polarization resistance were

performed. The main motivation for the present work is colour removal and resistances

effecting the permeate flux during separation of dye aqueous solution using membrane

materials. Flux decline is the major problem in membrane system. Various models have been

developed to predict membrane flux behaviour during separation. All of them can be

classified into three broad categories: (a) osmotic-pressure-controlled models, (b) gel

polarization models, and (c) resistance-in-series models. In a typical membrane filtration

process the flux drops due to osmotic pressure, pore blocking, and gel layer growth may

coexist. The models for the quantification of flux decline due to above constraints are

available in the literature (Sarkar 2013)

2. EXPERIMENTS AND METHODS

Analytical grade reagents of NaOH, Na2CO3, K2Cr2O7, H2SO4, Na2SO4, CH3OH, KBr,

ferrous ammonium sulfate, ethyl acetateare used for all the analysis. Textile dye Quinoline

Yellow, obtained from pollution control division, Central Electrochemical research Institute,




Karaikudi, Tamilnadu.PES (3500) was received from Udel. Rose Bengal (C20H2Cl4I4Na2O5,

Mr: 1017.65) was procured from M/S Merck and the 0.01 M stock solution was the dye was

prepared in doubly distilled water. Eosin B dye (4´,5´-Dibromo- 2´,7´dinitrofluorescein di

sodium salt, colour index: 45400), chloroform, chlorosulfonic acid, methanol, and

dimethylformamide (AR grade) were obtained from S.D fine Chemicals, India, and were

used without any further purification.

2.1. Preparation of membranes

For the sulfonation of PS, 5g weight was dissolved in 50 ml of chloroform and the solution

was cooled to 0°C in ice bath. The mixture of chloroform (25 ml) and chlorosulfonic acid

(2.5 ml) was added drop-wise to above solution. After 30 min reaction was terminated by

addition of fivefold of methanol in the reaction mixture. Precipitate was collected, washed

thoroughly with methanol and dried at 50°C, which resultant material were SPS. Poly ether

sulfone 40g was dissolved in 1,2 - dichloroethane by heating the solution at a temperature of

85°C ± 5°C, for 2-3 h. The solution was then cooled to 4°C and 5 ml of chlorosulfonic acid

was added drop wise to the solution for about 15 minutes. This reaction mixture was

maintained at 4°C for 2 h. The 20 g of PEEK was dried in a vacuum oven at 100°C and then

dissolved in 500 ml of concentrated (95-98% H2SO4) sulphuric acid at 50-70°C under vigorous

mechanical stirring. The reaction time ranged from 5 to 6 h. The sulfonation reaction was

terminated by decanting the polymer solution into a large excess of ice-cold water under

continuous mechanical agitation and the polymer precipitate was filtered and washed several

times with distilled water until the pH was neutral. The recovered SPEEK was dried at room

temperature for 2 days, finally the polymer was dried in a vacuum oven at 80°C for 24 h, and

stored in a desiccator. The above procedure for preparation of membranes was reported in our

earlier work [Chirsabesan et al 2013a and Chirsabesan et al 2013b]

2.2. Film polarization model

This model was developed based on the film theory and mass balance principle about the

membrane. At steady state the convective flow through the membrane is balanced by solute

flux through the membrane plus diffusive flow from the membrane. Fig shows the

concentration profile near the membrane surface at steady state from the feed side. The

following equation expresses the material balance

�� 1

Where C is the concentration at a distance x from the membrane surface,� is the

permeate concentration and D is the diffusion coefficient of the solute.

Figure 1 Concentration profile near the membrane surface during steady state ultrafiltration



The boundary conditions are X=0 at C=��; X=δ at C=�

Where the boundary layer thickness is δ, � is the bulk solution concentration and ��is

the max value of the boundary layer concentration, which is the concentration at the

membrane surface. Integrating the above equation give

�� 2

Where, � � δ ⁄ is called the mass transfer coefficient .This model is called film

polarization model.

2.3. Osmotic pressure model

The osmotic pressure model is developed on the assumption that it can explain the flux

decline mechanism that limits the flux. A concentration difference between two solutions,

which are separated by a membrane, will cause an osmotic pressure difference. In order to

create osmotic equilibrium, water is induced to flow from the low concentration region to the

high concentration region. This reduces the convective flux generated by the operating trans

membrane pressure. As any other flows in nature, the permeate flow across the membrane is

governed by the free energy difference across the membrane. In addition, the coupling effect

between water and solute may reduce this energy difference, and the effective trans

membrane pressure may drop.

Originally, Kedem and Katchalsky (1958), using irreversible thermodynamics, derived

the relation:

�� = �(∆� − �∆�) 3

Where �� is the permeate flux, � is the membrane permeability, ∆π is the osmotic

pressure across the membrane [∆π= π (��) – π ( �)] and σ is the reflection coefficient of

solute across the membrane. The osmotic pressure effect on the permeate flux decline is

scaled by the parameter σ. The parameter measures the relative restriction of the membrane to

transmit the solute compared to the solvent, and varies between 0 for a freely permeable to 1

for a completely impermeable solute. � is an inverse function of membrane resistance which

includes both membrane and fouling resistance due to adsorption. Therefore the equation for

permeate flux is given by equation (4.8)

�� = ∆�� ∆!"(#�$#%) 4

Rf is assumed to be independent of pressure and stands to account for the effect of

adsorption.

2.4. Resistances-in-series model

The model has been used to predict the performance of ultrafiltration of different

macromolecule solutions. This model considers all the resistances involved in flux decline

such as membrane resistance, adsorption resistance, pore blockage resistance concentration

polarization resistances in series. Permeate flux can be given by equation (4.9)

��=∆&

"(#�$#'�$#() 5

Where, Rm is membrane resistance, Rcp is concentration polarization resistance, Ra is

adsorption resistance, Rp pore blockage resistance.




3. RESULTS AND DISCUSSION

3.1. Physical properties of membranes

Table 3 Thickness and porosity of the prepared membranes

Name of Polymer Thickness(mm) Porosity (%)

SPSf 0.25 59.2

SPEEK 0.25 62.5

SPES 0.25 60.0

Nafion® 117 0.25 52.5

The thickness and porosity of the prepared membranes are given in Table 3.1. The above

results have shown that SPEEK membrane is more porous than SPS, SPES and commercial

Nafion® 117 membranes. Hence, permeability and transfer of dye molecules was higher in

SPEEK membranes, when compared with other membranes. However, membrane resistance

differs according to membrane properties. The thickens of membranes plated main role in

solution diffusion. According to Fick’s law, mass transport influence by thickness of

membranes. In this study, the influence of resistance due to concentration polarization, cake

and gel layer on surface of the membranes affect the permeate flux and rejection properties.

3.2. Membrane resistance

It is the resistance offered by the membrane for the transport of particles. It should be

constant for a given feed solution. Membrane resistance can be determined by

)� = ∆&" *+

6

Where ∆� is the transmembrane pressure, )� is membrane resistance, μ is the viscosity

of the water, �� is pure water flux. The above equation shows that flux is a linear function of

pressure for a given feed solution and membrane. Membrane resistance can be determined

and shown in Table 4.

Table 4 Membrane resistance of the prepared membranes

Name of Polymer Membrane Resistance x 1013

(m-1

)

SPS 7.93

SPEEK 4.43

SPES 7.83

Nafion® 117 8.52

3.3. Concentration polarisation during dye separation with effect of pressure and

flux of all membranes

The ion exchange membarnes are responsible for solute aggregation commonly seen in high

pressur membrane process. The exchange groups present in SPS, SPES, SPEEK and Nafion

are induced the intermolecular exchanges between dye molecules result in exchanges and

propagate aggregate growth. The presence of a sulfone group has been shown to be necessary

to initiate exchanges of moclecues. Severe flux decline has been observed with dyes

containing amino acid groups. Consistent with this, decreasing the reactivity of the amino

group, for instance by increasing pH, reduced the severity of flux decline. During filtration,

there is an accumulation of retained colloidal particles at the membrane surface giving rise to

a concentration gradient of particles perpendicular to the membrane surface, known as

i. e xi. e x



concentration polarisation. This concentration gradient is the driving force for diffusion of the

particles back to the bulk, which at steady state, is in balance with the bulk movement of

particles to surface (Chanukya et al 2013). This layer of concentrated particles generates a

resistance to fluid flow, as a physical barrier or increased osmoticpressure which reduces the

effective transmembrane pressure.

Concentration polarisation is a reversible phenomenon that is controlled by the balance

between mass transfer towards and away from the membrane. This gives rise to the typical

flux-pressure correlation seen during ultrafiltrtion of Eosin B Dye dye solution (Figure 2.). At

low transmembrane pressures (TMP), flux and CP are both low, and flux is observed to

increase linearly with pressure (pressure-controlled region). Conversely, at high TMP, CP is

severe, and flux starts to highland with increasing pressure. Here, flux increases are only

possible if mass transfer properties are improved.

Figure 2 Effect of Pressure on permeate flux of dye solution of prepared membranes

3.4. Determination of permeate flux of dye solution through experiment at

different operating conditions and fitting a suitable mathematical model

This is a mathematical model based on resistance in series model considering membrane

resistance and concentration polarization resistance acting in series to the filtrate.

Mathematical model equation for permeate flux is given by

� ∆&",#�$- &�. / 7

In above equation z is given by (Bhattacharjee et al 1998)

0 1�2��2��3�24�2��5�24673�24�2�� 8

89 can be calculated from concentration polarization model given by

� = : ln =(24�2�)(2��2�)> 9

Substituting z in equation 5.4 gives

?* = "#�

∆& � "&�∆& @ =

13 A

2��2�24�2�B �

5�3

2424�2�CD> 10




Equation 5.7can be written as

?* E?F � EGD � EH 11

The above equation can be solved by least square method to find the constants a1, a2, a3.

Solving non-linear equation 5.8 by least square method the equations can be given by

E?∑FG − EG∑F. D + EH∑F = ∑(F. ?*) 12

E?∑F. D − EG∑DG + EH∑D = ∑ ?* . D 13

E?∑F − EG∑D + �EH = ∑ ?* 14

From Eqn. 5.6 & Eqn. 5.7 a1, a2, a3 can be given as

E? = "(2��2�)&�∆&3(24�2�) 15

EG = "5�246&�∆&3K24�2�L 16

EH = "#�∆& 17

From the above equations ��, : , )� can be calculated.

�� = "(2��2�)MN∆&3(24�2�) 18

: = MO&�∆&3(24�2�)"24P 19

)� = MQ∆&" 20

A mathematical model based on filtration theory coupled with resistance in series model

and gel polarization model has been developed in the present study. This work has been done

by using Eosin B dye solution. Permeation flux studies done through flat sheet dead-end

ultrafiltration set up at 50 psi and 300 rpm speed. In this present study permeate flux from

developed model and experiment was compared. Experimental data measuring flux and

volume of permeate up to that time at definite time interval of 15 min is given below.



Figure 3 Variation of inverse of flux of dye solution with time for SPS, SPEEK, SPES and Nafion

membranes

The inverse of flux of dye solution at the end of 205 min for all SPS, SPEEK, SPES and

Nafion is plotted in Figure 3. It is evident that the inverse of flux increases with time in

ultrafiltration. This indicates that the number concentration and size distribution become

wider with the initial feed surfactant concentrations leading to more severe pore blocking

(Huang et al 2012). Due to velocity, the permeate flux varies along the length, resulting in a

non-uniform solids concentration at the membrane surface. The ultrafiltration models

discussed to predict an area-averaged flux to determine the concentration at the membrane.

From Figure 3, the time-dependent fouling resistances are related to the flux and particle

deposition rate. For dye solution separation systems where membrane fouling is also

contributed by primary adsorption of dye solutes, the rate of dye molecules deposition may

also be modelled via resistance series model and osmotic pressure model. According to

present work, these models have yet to be applied to dye solution in UF system. In both

models, it was observed that resistance due to pore blocking dominated initially, while cake

resistance becomes more significant in the later stages of filtration.

Figure 4 Variation of volume of dye solution with time for SPS, SPEEK, SPES and Nafion

membranes




From Figure 4, it is evident that the volume of dye on surface of the membranes increases

with time almost linearly. The gel layer resistance is formed on all surfaces of the

membranes. However, the individual property, membrane resistance, porosity influenced the

formation of specific cake resistance and leading to more resistance to the solvent flux.

Further, the variation of gel layer resistance with all membranes to Eosin B dye at the end of

the experiment for different operating pressures. Figure 4 shows that the volume of dye

solution increases with the feed concentration. We note that the experimental results of the

variation of Rg with feed concentration are less conclusive.

Figure 5 Variation of permeate flux with time at different membranes at operating pressure 414 kPa

and Eosin concentrations of 1000 ppm

Figure 5 shows that flux decline with time and it attained steady state during the filtration.

The effects of dyes permeate flux and times are presented in Figure 5. The curves in Figure 5

clearly show the decline of the permeate flux during the operating time due to concentration

polarization (Salahi et al 2010). At the initial point of time, the flux is higher feed

concentration of eosin. The decrease in flux results in an increase in insolubilized dye. This

causes an increase in the rejection of the dye through the membrane. As a result, the transfer

of dilute water molecules suppressed in the dye concentration in the feed.

Figure 6 Variation of bulk layer concentration of permeate concentration on the eosin dye retention

with time at different membranes



The effect of the bulk layer concentration of permeate concentration on the eosin

retention is presented in Figure 6. Figure 6 shows that the retention of eosin increases with

concentration. This is quite obvious, as the number concentration, of build-up of the solutes

will be more with increasing concentration polarization, resulting into an increase of the

amount of the dye solubilized in the surface. This leads to an increase in the bulk layer

concentration of permeate concentration of dye (Zhang et al 2010). It is also clear from the

figure that the bulk layer concentration of permeate concentration is at a maximum for the

SPEEK membrane. This is due to porosity and resistance of the membranes.

Figure 7 J Vs ln(cb-cp) of SPS membrane

In ultrafiltration, accumulated solute (dye) particles provide additional resistance to fluid

flow when the permeation process. C to denote the excess number concentration of particles

in the polarization layer. The actual particle concentration is C, + C, where C, is the bulk

(feed) number concentration of particles (Cb). The distribution of permeation of accumulated

particles in permeated liquid (Cp) is influence the retention performances (Koyuncu et al

2013). This observation is shown in Figure 7.

Figure 8 J Vs ln(cb-cp) of SPEEK membrane




The direction of the permeate velocity is explained from the Figure 8 from the bulk to the

membrane, so that v(x) is always positive. The J value denoted the flow molecules from the

membrane surface. From Figure 8, It is clearly understand that effective applied pressure is

equal to the applied hydraulic pressure minus the osmotic pressure difference between the

bulk suspension and the permeate.

Figure 9 J Vs ln(cb-cp) of SPES membrane

From Figure 9, wall particle concentration of dye solution on SPES membrane surface

more striking, it is independent of the bulk particle concentration. From the R2 value, it is

noted that change in ratio of the wall particle concentration to bulk particle concentration.

Further, the wall particle concentration is assumed to be a constant independent of pressure

for dye molecules/particles (Purkait et al 2004). The particles, a cake layer of retained

particles will form between the concentration polarization layer and the membrane surface.

By 'cake' mean that the retained particles are packed so as to attain minimum porosity.

Figure 10 J Vs ln(cb-cp) of Nafion membrane

Hence, a model for the permeate flux was developed for cases where the additional

resistance of this cake layer is considered. This investigation in the work, and it is particularly

useful for ultrafiltration using dye solution separation and removal. Further, the bulk fluid

moves toward the membrane surface owing to the applied pressure. The magnitude of this



transverse flow of dye molecules is determined by the applied pressure, the membrane

resistance and the extent of concentration polarization. The R2 value of Nafion membrane is

0.8993. This value is lower when compared with other membranes. This may be due to

higher value of nafion membrane resistance is when compared with other membranes. The

permeate velocity in ultrafiltration varies along all membranes since the concentration-

polarization layer thickness over the membrane surface increases gradually along with

respective porosity and membrane resistance.

4. CONCLUSIONS

The understanding of dye removal, membrane science, and mathematical modelling can yield

new insights into the mechanisms of flux decline in dye separation using ultrafiltration. Past

three decades, significant advances towards modelling of ultrafiltration have been reported.

The quantification of rejection and membrane properties via thickness, porosity, membrane

resistance and pressure have revealed the importance of concentration polarization, fouling, c

and permeability on ultrafiltration flux. From the both resistance and osmatic model, it is

clearly do influence both bulk layer concentration and gel formation was observed. This is

important when taking into consideration as the operating pressure in ultrafiltration are of a

magnitude higher than cake layer formation. The effect on bulk layer concentration and gel

formation on SPS, SPES, SPEEK and Nafion membrane surface varied with individual

membrane properties.

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