Journal of Materials Education Vol.

31 (3-4): 157 - 166 (2009)

POLYMERIC FLOCCULANTS FOR WASTEWATER AND

INDUSTRIAL EFFLUENT TREATMENT

Witold Brostow1, Haley E. Hagg Lobland1, Sagar Pal2 and Ram P. Singh1, 3
1
Laboratory of Advanced Polymers & Optimized Materials (LAPOM), Department of Materials
Science and Engineering, University of North Texas, 1150 Union Circle # 305310, Denton, TX
76203-5017, USA; wbrostow@yahoo.com, haleyhagg@gmail.com; http://www.unt.edu/LAPOM/;
2
Department of Applied Chemistry, Indian School of Mines - Dhanbad, Dhanbad - 826 004, India;
sagarpal1@hotmail.com; 3 Indian Institute of Science, Education and Research (IISER), Pune,
India; singh.prakash.ram@gmail.com

ABSTRACT

The fact that water is the most important material used by mankind defines the importance of water
purification. Wastewater and industrial effluent treatment require removal of suspended solids for
purification and possible re-usage. The removal can be accomplished by gravitation (very slow), by
coagulation (dependent on electric charge situation) and by flocculation (not dependent on electric
charges and the fastest). Inorganic flocculants are used in very large quantities, they leave large
amounts of sludge and are strongly affected by pH changes. We describe the mechanism of
flocculation by polymers in ppm concentrations by strong solvation of the liquid by the flocculant,
thus pushing the solid particles outside the solvated domains. The solid particles aggregate in much
smaller regions then available to them. Polymeric flocculants cause formation of large cohesive
aggregates (flocs) and are inert to pH changes. Both natural and synthetic polymers are used as
flocculants. Natural polymers are biodegradable, are effective at large dosages and are shear stable.
Synthetic polymers are highly effective flocculants at small dosages and have high tailorability but
poor shear stability. Concern for environmental and ecological issues warrants the use of
biodegradable flocculants. Natural polysaccharides such as starch, guar gum, alginate, glycogen or
dextran can be used. Chemical modification of these polysaccharides to improve their flocculation
efficacy is possible, including grafting polyacrylamide branches on polysaccharide backbones and
insertion of cationic moieties on the backbones. We discuss flocculants based on polysaccharides
more in detail since they provide both shear stability and biodegradability. Since flocculants exist as
polymers in solution, their standard characterization is in terms of the radius of gyration; that radius
is related to the flocculation efficacy. Drag reduction (DR) is also related to flocculation since the
same polymeric agents cause both. DR is briefly described and the common mechanism of both
phenomena is explained. Possibilities of using recycled industrial water after flocculation as
agricultural water are pointed out. Such usage results in less contamination of the environment and
also in saving fresh water.
158 Brostow, Hagg Lobland, Pal and Singh

1. INTRODUCTION Water is used, among other applications, in

mineral processing, such as in bringing metal
Materials play a major role also in lowering ores in the form of water slurries from their
pollution and contamination of the environment. original location below the Earth surface to the
For this reason there are intensive research surface and also in subsequent transport.
activities in the areas of lowering toxicity of Movement of coal from its deposits in coal
industrial waste, lowering toxicity of exhausts, mines and the subsequent surface transport
confinement of contamination and recycling of similarly requires the use of water. It is for such
materials of many kinds – including water. So reasons that the problem of potable water is
far standard instruction in Materials Science and related to that of industrial water. Clearly less
Engineering (MSE) largely ignores these use of industrial water - or recycling some of it -
activities. A course on Environmental Protection will increase the supply of potable water.
taught at the Poznan University of Technology
by Paukszta and Garbarczyk1 is an exception. The effluents are highly undesirable and unsafe
Other exceptions are those metallurgical and to use. Wastewater contains solid particles with
ceramic engineering curricula which include a wide variety of shapes, sizes, densities and
mineral processing so that flocculation is at least composition. Specific properties of these
mentioned2. The present article represents a particles affect their behavior in liquid phases -
further step to remedy this situation. and thus the removal capabilities. Many
chemical and microbiological contaminants
found in wastewater are adsorbed on or incorp-
Effluent disposal is a major problem around the
orated in the solid particles. Thus, essential for
world. Growing along with the population
purification and recycling of both wastewater
growth, industries create environmental prob-
and industrial effluents is the removal of solid
lems and health hazards for the population.
particles.
Hence, environmental concerns and progressing
depletion of raw material resources behoove
As renewable raw materials, polysaccharides
scientists and engineers to develop materials
already play an important role as alternatives to
from renewable agricultural and plant resources
fossil raw materials - due to both their generally
to lower the extent of pollution of the environ-
non-toxic nature and the constantly rising global
ment.
demand for energy and raw materials. Poly-
saccharides are large organic molecules that
The world population is increasing – while occur in a variety of natural sources. Depending
availability of potable water is decreasing. Water upon the source, the polysaccharides contain
is essential for the survival of human beings – various impurities and also exhibit a variety of
not to mention modern industry. Although the molecular characteristics. However, by purifi-
earth consists of 75% of water, water for cation, grafting and cationization, useful
drinking, sanitation, agricultural and industrial products can be made – usable as flocculating,
processes is not easily available. According to drag reducing and viscosity enhancing agents3.
the United Nationals Organization Report of
2005, 1.2 billion people lack access to adequate
amounts of clean water and 2.6 billion people 2. METHODS OF REMOVAL OF SOLID
lack proper sanitation. This situation got only PARTICLES SUSPENDED IN LIQUIDS
worse since 2005 and necessitates recycling of
municipal wastewater and industrial effluents on The simplest process imaginable is by gravity.
a massive scale. To meet the requirements of Solid particles have higher densities than water.
potable, industrial and agricultural water, we However, fine particles with diameters on the
have to treat the wastewater, particularly the order of 10 µm will not settle out of suspension
municipal sewage sludges and slimes and by gravity alone in an economically reasonable
industrial effluents. amount of time. We note that particle sizes in

Journal of Materials Education Vol. 31 (3-4)

 Polymeric Flocculants for Wastewater and Industrial Effluent Treatment 159

emulsions are still smaller, 0.05 – 5 µm, hence how ppm concentrations of a flocculating agent
the removal of particles from emulsions (de- are sufficient. In Figure 1 we show a schematic
emulsification) is even more difficult. illustrating how one chain pervades a large
volume of the liquid.
The second process, still widely used, is
coagulation. Destabilization of colloidal
suspensions occurs by neutralizing the electric
forces that keep the suspended particles
separated4. The aggregates formed in the
coagulation process are small and loosely
bound; their sedimentation velocities are
relatively low – although higher than in gravity
separation. Given the nature of the process, the
results are strongly dependent on pH and its
variations.

Flocculation is caused by the addition of minute

quantities of chemicals known as flocculants.
Both inorganic and organic flocculants are in Figure 1. A section of a macromolecular chain in
use. Among the inorganic flocculants, salts of forming of a domain pervaded by a chain in the
multivalent metals like aluminum and iron are system of liquid + suspended solid particles. Liquid
applied most often - at high concentrations4. molecules are either solvated by the chain (shaded
Inorganic flocculants are used in very large area) or else are located inside a domain. Size of the
quantities, they leave large amounts of sludge domain is related to the polymer radius of gyration --
and are strongly affected by pH changes. as discussed in the text. When a flocculant is applied
and such domains then formed, the solid particulate
Organic flocculants are typically polymeric in
matter remains outside of the domains.
nature; by contrast to inorganic ones, they are
effective already in ppm concentrations. Both A measure of the pervaded volume is the radius
synthetic and natural water-soluble polymers are of gyration RG. The radius is the root-mean-
used as flocculants. square distance of the collection of atoms from
their common center of gravity:
In contrast to the process of coagulation, electric
charge manipulation is not the dominant RG2 = Σi mi ri2/ Σi mi (1)
mechanism of action in flocculation. In fact,
flocculation is possible without significant Here mi is the mass of the i-th atom while ri is
changes in the particle surface charges. As a the vector from the center of gravity to that
consequence, flocculation is not strongly affect- atom; the summations run over all atoms. As
ed by pH in a given medium, or by pH discussed by Lucas and her colleagues7 and also
variations. Moreover, flocculation is much more by Gedde8, there are several methods of
effective than coagulation since the so-called experimental determination of RG , including
flocs are larger and more strongly bound than light scattering and viscometry.
the aggregates obtained by coagulation. Thus,
among the possible options, flocculation is the With large solvent volumes pervaded by the
method of choice. macromolecular chains, solid particulates are
pushed outside the solvated domains such as
shown in Figure 1. This is the main mechanism
3. MECHANISMS OF FLOCCULATION of action of the flocculating agents. The solid
particles aggregate in much smaller regions now
Polymeric flocculants act by extensive available to them. Clearly higher molar mass of
solvation5. Here lies, first of all, an explanation the polymer results in larger or more solvated

Journal of Materials Education Vol. 31 (3-4)

160 Brostow, Hagg Lobland, Pal and Singh

domains. We shall return to this issue in a The surface charge explanation is in terms of
quantitative way later in this review when contamination of solid particles in solution by
looking at suspensions containing specific solids electrostatic adsorption of ions on their surfaces.
and flocculants used to treat them. We see why this cannot be a general mechanism
of flocculation. There are suspensions in which
It has been found that polymeric flocculants are
also drag reduction (DR) agents9, 10. The DR flocculation occurs while the electrostatic forces
phenomenon is used to advantage in oil pipeline are unimportant. Needless to say, in the pres-
conduits, oil well operations, flood water ence of ions we can have flocculation enhanced
disposal, fire fighting, field irrigation, transport by electrostatic adsorption of ions. The adsorp-
of suspensions and slurries, sewer systems, tion can cause repulsion between solid particles,
water heating and cooling systems, airplane tank attraction of counter ions into the vicinity of the
filling, marine systems. Most airplane pass- particles, and thus formation of an electrical
engers do not realize that filling their plane fuel double layer - a phenomenon known for a cen-
tank would take much more time without the use tury or so.
of DR agents. The importance of drag reducers
in saving human life during a fire can hardly be Since it was clear for a long time that the
overstated.
electrostatic mechanism cannot be operational in
We do have a joint explanation of flocculation a number of systems in which flocculation
and DR. The large volumes pervaded by occurs, as far back as 1952 a bridging mechan-
polymeric chains cause DR. In turbulent flow ism model of flocculation was developed by
the solvated domains such as seen in Figure 1 Ruehrwein and Ward11. One assumes that a
resist the eddies of turbulence and - not much single polymer chain forms a bridge between
affected - move along the flow. The only differ- two or more particles. The basics of this model
ence is in the shape; the domains in flow are have been subsequently refined, but the main
oval rather than static appoximately spherical points are unchanged; the loops and tails of the
ones. It has been demonstrated that solvation adsorbed polymer chain on one particle protrude
numbers obtained from ultrasound velocities are
into solution and get attached to a second solid
related to the DR efficacy; the larger the solv-
particle. The first problem with this model is that
ation number, the stronger is a given DR agent6.
Thus, a domain flows as a unit, with some it cannot explain how ppm concentrations of a
perturbation to its shape caused by the turbu- polymer are sufficient to cause flocculation.
lence along the way. Here we see the reason for Second, what would be the force pushing a
DR: individual solvent molecules solvated by macromolecular chain to get adsorbed on a
polymer chains are not ‘attacked’ individually second particle? But assume for the sake of
by eddies of the turbulence. When such an attack argument that such force exists, that anchoring
occurs, the solvent molecules defend themselves of a macromolecular chain on two distinct
collectively. The solvent molecules inside the suspension particles occurs somehow, conceiv-
domains (see again Figure 1) are protected even ably as a consequence of simple Brownian
more than those which by solvation are attached dynamics motions. Then a 'bridge' would result
to macromolecular chains outside. in doubling the mass of the suspension particle,
We now return to flocculation. Given the not more. The fact that flocs are much larger and
practical importance of this phenomenon, heavier than just twice the size of particles
various explanations have been advanced before before flocculation cannot be explained by the
the mechanism described in Ref. 5 was formul- bridge formation. Thus, we are left with the
ated. Two such explanations still mentioned on solvation model described in the beginning of
occasion are surface charge neutralization and this Section as the only one explaining the
bridging. We shall consider them in turn. totality of observed phenomena.

Journal of Materials Education Vol. 31 (3-4)

 Polymeric Flocculants for Wastewater and Industrial Effluent Treatment 161

4. CLASSES OF ORGANIC FLOCCULANT degradable and easily available from reproduc-

ible farm or forest resources. The bio-degrad-
The organic flocculants fall into two categories, ability of natural polymers reduces their shelf
namely natural and synthetic. The poly- life and needs to be suitably controlled. Their
saccharides, mainly starch and its constituents, required dosage is large and their solutions and
different types of gums, alginic acid, cellulose floc lose stability and strength respectively due
and its derivatives, dextran, glycogen etc. are to biodegradability. It is thus evident that all the
among the natural polymers used in flocculation. polymers whether natural or synthetic have one
Synthetic flocculants are broadly divided as or other disadvantages.
anionic, cationic and non-ionic categories. Poly-
acrylamide (PAM) and poly(ethylene oxide) In this situation, attempts have been made to
(PEO) are non-ionic. The majority of the cation- combine the best properties of both kinds of
ic groups of polyelectrolytes are derived by polymers by grafting synthetic polymers onto
introducing quaternary ammonium groups onto backbones of natural polymers after purifi-
the polymer backbone, although polymers cation2,14-28. Biodegradability is reduced because
containing sulfonium and phosphonium groups of a change in the original regular structure of
are used to a limited extent. The most commonly the natural polymer as well as the increased
used cationic polyelectrolytes are poly(diallyl synthetic polymer content. It is also observed
dimethyl ammonium chloride) (polyDADMAC). that grafting of shear degradable polymers onto
In the anionic group of polyelectrolytes, mainly rigid polysaccharide backbone provides fairly
two types of polymers are used; one type is shear stable systems.
polymers containing carboxyl functional groups
and the other containing sulfonic acid groups. A Cationic polysaccharides can be prepared by a
representative of the former is poly(acrylic acid) reaction of a polysaccharide with various
and its derivatives, of the latter poly(styrene reagents possessing positively charged groups
sulfonic acid) (PSSA). such as amino, imino, ammonium, sulfonium or
phosphonium groups. Cationized polysacch-
The extensive use of polymers as flocculants is arides are effective flocculants over a wide range
due to their distinct characteristic attributes12, 13. of pH. They are non-toxic and their biodegrad-
As already noted, polymers are convenient to ability can be controlled. They are being used
use and do not affect the pH of the medium. for sustained organic and inorganic matter in
They are used in ppm quantities - with obvious wastewater carrying negative charges. They are
consequences for the cost of flocculation. The also used as wet-end additives in paper making -
flocs formed are larger, stronger and settle more for controlling flocculation, retention and paper
easily than do the simple coagulation electro- strength. Introducing cationic groups onto starch
lytes. Flocculation efficiency of polymers gives good mineral binding properties; this is
increases with increasing molecular weight (we required for anchoring the mineral to the fibers.
shall return to this fact below). Large tonnage
use of inorganic compounds produces large Since we have concluded that synthetic poly-
amounts of sludge - a problem absent when mers grafted on natural ones provide the best
using polymeric flocculants. Among polymeric combination of properties, in Figure 2 we show
flocculants, the synthetic polymers can be tailor an example how graft polymerization can be
made by controlling the molecular weight, mol- initiated. Ceric ions provide here the initiator.
ecular weight distribution and chemical
structure. Thus, due to tailorability, synthetic Whether grafting has been successful one can
polymers can be very efficient flocculants. verify by a variety of techniques: Fourier-
transform infra-red (FTIR) spectroscopy,
However, the synthetic polymers in flow are not elemental analysis (C, H, N analysis), intrinsic
shear resistant. Natural polymers – including viscosity measurement29, thermophysical anal-
polysaccharides - are fairly shear stable, bio- ysis including determinations of glass and

Journal of Materials Education Vol. 31 (3-4)

162 Brostow, Hagg Lobland, Pal and Singh

C H2O H C H2O H
O O
OH + C e ( IV ) O H
O O
OH OH

C e ( IV )
C o m p le x
C H2O H
O +
OH H + C e ( III) + H
O C. C
H O
C o m p le x or
C H 2O H
O +
H H + C e ( III) + H
O C .C
O OH
F re e ra d ica l
F re e R a d ica l + V inyl M o no m e r G ra ft C o p o lym e r
C H2O H
O +
F re e R a d ica l + C e (IV ) H H + C e ( III) + H
O
C C
O O

AGU ( A G U) AGU
n

M M M M

C H2O H
O
AGU OH
O
OH

Figure 2. Initiation of graft copolymerization by ceric ions.

Journal of Materials Education Vol. 31 (3-4)

 Polymeric Flocculants for Wastewater and Industrial Effluent Treatment 163

melting transitions7,8,30-33, by several techniques

for determination of molecular weight and
radius of gyration7,8 and also by X-ray
diffractometry7, 34 when crystalline phases are
formed.

5. EVALUATION OF FLOCCULATION
EFFICACY

When flocculant is introduced into the

container, an interface is formed. Above it is
the supernatant liquid while below is the
suspension containing the contaminants. Under
the action of the flocculating agent, that is along
with the progress of the flocculation process,
that interface descends, until all contaminants
are settled at the bottom.

Two methods of flocculation efficacy determin-

ation are in use, a so-called jar test and a
settling test. In the jar test one adds the Figure 3. Jar test results in 0.25 wt. % silica
flocculant in solution form to the suspension. A suspension using several flocculants.
typical flocculant dose varies from 0.025 ppm
to 1 ppm. The system is stirred at a uniform
speed, first at a high speed such as 75 rpm for 2
minutes and then at a slow speed such as 25
rpm for 5 minutes. Afterwards, a settling time
of 10 min was allowed. At the end of the
settling period, the turbidity of the supernatant
liquid is measured with a turbidity meter. The
lower the turbidity, the better is the flocculant.
An example of results so obtained is shown in
Figure 3 (the symbols in the insert pertain to
different compositions of the flocculant).

Supporters of the settling test claim that their

test provides a higher accuracy than the jar test.
One reason is that the jar test results show
sometimes minima and/or maxima. The nature
of the solid suspension may also indicate which
test will perform better in a given situation.
Where flocs are widely dispersed, it may be
necessary to induce a velocity to suspended
solids to obtain larger flocs. In this case the jar
test is more appropriate. In the settling test one
typically employs a 100 ml. graduated cylinder
and stopwatch. First the suspension sample is Figure 4. Settling characteristics of a silica
placed in the cylinder and then polymeric suspension with addition of cationic glycogen (Cat
flocculant solution is added into it. The cylinder Gly) and several commercial flocculants.

Journal of Materials Education Vol. 31 (3-4)

164 Brostow, Hagg Lobland, Pal and Singh

is inverted a number of times for thorough flocculation described in the beginning of

mixing. After that the cylinder is set upright and Section 3. We now consider experimental
the height of interface between water and evidence in the light of the model. Several types
settling solid bed is measured over time. An of suspensions were investigated5,36, containing
example of such results is shown in Figure 4. in turn silica, iron ore, coal and manganese ore.
For each system the flocculation efficacy was
As can be seen in Figure 4, curves of the determined in terms of the settling velocity y
interface height as a function of time are linear, and the radii of gyration; a variety of polymers
except for fairly short final parts which are with different chemical structures was so
concave. The linear parts of such diagrams thus evaluated. The results are presented in Figure 5:
provide us with the settling velocities y which settling velocities vs. the radius of gyration.
are used as a measure of the flocculant efficacy
of an additive in a given suspension medium. Figure 5 demonstrates the validity of the
model5. Several flocculating agents were
applied to each suspension system. In each
6. PREDICTION OF FLOCCULATION such system application of a polymeric
EFFICACY flocculant with a higher radius of gyration
results in an increased settling velocity. This
As already discussed in Section 4, the idea is to can be represented by a relationship valid for
combine advantageous features of natural and each system:
synthetic flocculants. Thus for instance
y = a.RGb (2)
copolymers have been synthesized by grafting
flexible polyacrylamide onto a rigid polysacch- where a and b are parameters characteristic for
aride backbone. Grafted glycogen has shown a given suspension medium, that is both the
very good performance in flocculation27,28 dispersed solid phase and the majority liquid
because glycogen has a highly branched struc- phase. One can consider Eq. (2) as a quant-
ture and a high molecular weight. One of us itative formulation of the EAM discussed in the
has developed an Easy Approachability Model beginning of this Section.
(EAM)2. According to EAM, an increase in
branching, in molecular weight and in sub- Eq. (2) provides us with the desired capability
sequent grafting/ionic loading, the approach- to select efficient flocculating agents. Given a
ability of the contaminants towards the floccul- liquid system, we evaluate radii of gyration of
ant chains is enhanced – and so is the floccul- candidate polymeric flocculants. The larger the
ation efficiency. radius of gyration, the higher will be the
flocculation efficacy.
EAM helps in the choice of a flocculant,
While our primary concern is water
including a possible chemical modification of a
purification, Eq. (2) is general. The majority
given flocculant by grafting. A quantitative
liquid phase does not have to be water.
criterion would be still better. Discussing
flocculation mechanisms above, we have Flocculation experiments are not ‘colorful’. An
pointed out how interaction of solid particles instructional laboratory experiment is under
with polymeric chains affects the flocculation development.
efficacy. This fits with the discussion by
Kopczynska and Ehrenstein35 how important We began this article with stressing the need for
are properties of interfaces in multiphase water recycling. Water purified by flocculation
systems. However, one begins with a candidate cannot be used as potable – but it can be used as
polymer and the question is: will it serve well agricultural water. Whenever that is done,
as a flocculant ? equivalent amounts of fresh water are saved.
At the same time, rejection of un-purified water
The answer can be found in the mechanism of into the environment has been prevented.

Journal of Materials Education Vol. 31 (3-4)

 Polymeric Flocculants for Wastewater and Industrial Effluent Treatment 165

Figure 5. Flocculation settling velocity for several suspension media as a function of the radius of gyration of
the flocculating agent. While for silica suspensions we have only two experimental points, the data have been
sufficient to evaluate parameters in Eq. (2) and plot the curve.

ACKNOWLEDGEMENTS Mexico, Queretaro; Elizabete F. Lucas, Federal

University of Rio de Janeiro.
Some of our own research results discussed
above have been obtained with support from:
the Robert A Welch Foundation, Houston REFERENCES
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Journal of Materials Education Vol. 31 (3-4)