Journal of Scientific & Industrial Research

Vol. 61, January 2002, pp 53-60

Chemical Industry Wastewater Treatment Using Adsorption

A K A Rathi*
Technica l Advi ser (Chemi ca l), Government of Gujarat, Industries Commiss ione rate,
Udyog Bhavan, Gandhinagar 382017

and

SA Puranik
VVP Engineering Co llege, Rajkot 360 005

Received: 3 1 July 200 I; accep ted: 02 November 200 I

In a typical wastewater treatment fl ow sheet used by several industrial units in Indi a. various stages of treatment
include primary treatment. foll owed by secondary treatment . and terti ary treatment. The concentrati on of total dissolved
solids increases durin g neutrali zation of the wastewater with acid/ alkali durin g primary treatment. which adversely affects
the activity of microorgani sms durin g biological treatment. The present stud y aims at demonstrating that adsorption as th e
Iirst stage of treatment shall increase efficiency of the subsequent bi ological treatment. Experiments were carried out on
different wastewater sampl es from chemical pl ants on adsorbents viz. acti vated carbon. bentonite. and lignite. The
effecti veness of adsorben ts in th e removal of refractory orga nics by way of reducing chemical oxygen demand and colour is
evaluated. The results of COD red uction are fitted into diffe rent models ava ilab le in literature including the new model Rat"i
Puranik eq uation . which requires least experimentati on for predicting COD values.

Introduction were reviewed 2. The use of activated carbon in water

A wide ran ge of adsorbents (granulated as we ll
as finely powdered) including activated carbon , clays,
bentonite, tly as h, alumina, magnes ium ox ide, ferric
oxide, silica, saw du st, zeo li tes , and activated
anthrac ite vo lcanic ash soil s are used in wastewater
treatment for the removal of heavy metals, and
di ssolved organic compound s whi ch res ult in the
reducti on of COD, BOD, and colour. For treatin g
wastewater from multiproduct chem ical plants
containing organic chemi cal substan ces in varying
co mpositi on and concentration, which are difficult to
degrade biologicall y, adsorption process I in
combinati on with other processes is cons idered ve ry
effective in reducing COD and colour.
Adsorbents in industrial wastewater
with adsorptive properties of adsorbents ,
carbon, inorgani c adsorbents and
app li cati ons of activated carbon adsorpt ion
*Auth or for correspondence
Tcl: 079 3225837. Fax : 079 3225S2S. c-mail: env @ic.guj .nic.in
and wastewater treatment, includin g the increasin gly
important role of adsorption" for removal of specific
target compound s or classes of compound s from
. water and wastewater containing complex organi c
substance mi xtures has also been reviewed. The
wastewater was biologically treated , and the residual
BOD and COD were removed further with activated
carbon~ . Powdered acti vated carbon and granular
acti vated carbon) were used for the terti ary treatment
of wastewater from a petrochemical plant. It was
inferred th at low COD and colour removal
effici encies were due to the presence of organic
co ll oids. whi ch were not adsorbed by the carbon.
Granu lated carbons prod uced colourl ess efflu ent from
the am ber-coloured intluent. The results of removal
treatment of phenols and cyanides6 by adsorption by acti vated
ac ti vated ca rbon in a pilot-plant were presented. Some
effici ent ind ustrial act ive carbons were used as adsorben ts in
processes phenol and pyridine? removal processes and in
adsorption of resins and oi ls from coki ng plant
wastewater. It was observed that phenols were more
easil y adsorbed than pyridines. It is reported that
54 J SCIIND RES VOL 6 1 JAN UA RY 2002
anionic, cation ic, or nonionic polyelectrolytes or clay
minerals 8 did not inhibit adsorption of phenol on
activated carbon. The phenol concentration In
wastewater 9 was reduced to less th an 0 .5 mg/L by
pass ing the wastewate r through a three-s tage-
adsorbing tank , each stage pac ked with activated
carbon.
More than 80 per cent COD re mo val was
obtained from wastewater containing be nze ne
derivatives. carboxylic acids, pesticides. a nd pheno ls
by sequential adsorption on sorbe nts combination of
activated anthracite PorolasT ion exchange resin
activated a nthracite 10. M agnesium oxide con tai nin g
ll
adsorbents are reported to have been used for th e
treatment of wastewater from pulp manufac turing
plants.
Physico-
Waste
pH Chemical!
Water
Adjustment .. Biological
Treatment
~
Conventional flowsheet
Wastewate r contain in g hea vy metal s was treated
with fly as h ' 2 from coal combu st ion. resu lting in a n
increase in pH to more than 8, a decrease in COD .
and re moval of the meta ls . Me thods for reducing
concentrat ion of surface-active agents in industri al
wastewater 13 were examined and it was observed that
adsorption on coa l gua ra nteed a satis fac tory
concentration reduction for the ca rboxy li c and
alkylsulphate surfacta nts but not the ami ne. which
was best removed by adsorpti on on benton ite. The
performance of wood c h arcoa l' ~ for the re mova l or
DDT from the aq ueous phase was in vest igated. Th e
influence of pa rti c le s ize, pH , and the time of contact.
which affect th e sorption process, was studi ed in
batch experiments.
Adsorption 15 was e mpl oyed to re move organic
impuntles fro m wastewater con tallllllt! sodium
ch loride 5-15, sodium carbona te 1.5. and sodium
nitrate O. I per cent and monochlorobenzene 0 .3.
polyamines 0.3 , 4,4' diaminodiphenylmethane 0. 3.
and toluenediamine 2 mg/L for subsequent salt
recovery. The efficie ncy of the organi c impurity
re mova l from isocyanate manu fac ture was obse rved
to be 90 per ce nt. The remaining sodium c hloride and
sodium carbonate were recovered and reused in soda
manufacture .
Methodology
The conventiona l flow sheet of wastewater
treatment used by most of the nndu "trial unit s,
in c ludes primary treatme nt , followed by secondary
and tertiary treatme nts.
During prim ary treatme nt , neutralizati o n of the
wastewater res ults into increase o f salts (total
di ssolved sa lts). Salts in hi gh concentration inhibi t
biological act ivi ty ' 6, a nd may cause a n increase in
non settleable suspended so lids in the treated
wastewater I? The tlow sheet g iven sub equ e ntl y is,
the refore,proposed, wherein adsorpti on with
Treatecl
.. Adsorption wdSte
Wolter
in ex pensive adsorbe nts could be emp loyed , pr ior to
the conve nti ona l primary treat me nt for in c reas in g
effic ie ncy of th e biologica l treat me nt.
This is expected to reduce refractory orga ni cs
(CO D) as well as BOD of the wastewate r
substantially a t the first stage of waste wat e r treatme nt
itself, facil itating further treatme nt. From multi -stage
production processes used in the producti on of
organic c he mic a ls, wastewater stream is li ke ly to
contain several organic as we ll as Inorganic
substances includin g products . inte rmed iates. side
prod ucts , byprod uct s and unreacted raw materia ls.
The industri a l wastewate rs being hi ghl y com ple x and
vary ing widely in th e adsorbability o f the compounds
present l ?, th e detailed analys is of s uc h wastewater
strea ms and stud y of their adsorpt io n on d i fferent
adsorbenrs was very compl ex . It was, therefo re.
decided to cons ide r COD as the measure of organi c
so lutes. The colour of the wastewater was a lso
measured . These parameters (COD and colou r)
reflect the practical aspects of wastewater treat men t
on the industrial scale. T hu s. such a stud y should be
of much relevance to the industry in sel ecting cost-
 RATHI & PURANIK : CHEM ICAL INDUSTRY WASTEWATER TREATMENT
Waste
Water . pH
... Adsorption Adjustment
Proposed flowsheet
effective wastewater treatment techniqu e for
complying with the statutory regulation s. The
approach fo ll owed in the evaluati on of adsorption
performance of different adsorbents viz. acti va ted
carbon, bentonite, and li gnite in the treatment of
wastewater is thu s based on detection of COD and
colour (optical density) in the wastewater with
varying degree of treatment. Thi s approach is entirely
different from that followed by many of the
researchers who prepare wastewater samples from
known solutes in the laboratory and carry out
chemi cal analysis of the treated sampl e.
.J
The COD determination IX is a meas ure of the
oxygen equivalent of that portion of the organic
matter in a sample that is susceptible to oxidation by
a strong chemical oxidant. It is an important, rap idl y
measured parameter for industrial wastewater studies
and for control of wastewater treatment processes .
The dichromate reflux method was used for the COD
determination because it has advantages over other
oxidants in oxidizabi lity, applicabi lity to a wide
variety of samples and ease of manipulation . The
colour absorbance was measured as optical den sity in
the UV visible ran ge, with the help of
spectrophotometer at the wavelength of maximum
absorbance. The measurements were done on neat
undiluted wastewater samples. In the cases, where
the absorbance readings went beyond the scale the
samples were diluted and the same dilution factor was
app lied to treated samples also.
Experimental Procedure
For the contact time experiments, eleven
wastewater samples from different production plants
were collected in labeled carboys and the carboys
were then sealed. These plants included dye
intermediates (H-acid , dihydroxydibenzanthrone.
dibenzyl oxybezaldehyde, dibenzanthronyl, and
benzanthrone crude; sample nos. I to 5. respectively),
55
Physico-
Treated
~
Chemical!
Bi ological ~ waste
Treatment water
two from ethanol (before and after biogas generation ;
sampl e no. 6 and 7), one from drug intermed iate
(diet hyl malonate; sample no. 8), two from a complex
manufacturing vat dyes and intermediates (before and
after neutrali zation ; sa mple no. 9 and 10). and one
from a complex manufacturing various dyes and
intermediates; sample no. 11 ). These samples were
taken directly from the process plant streams, before
these had any chance of getting mixed with any other
streams. In most of the cases these were concentrated
streams, often referred as mother liquor. While
carryin g out experimental stud ies on the wastewater
from each carboy the sample was analyzed for pH .
colour and COD. Then 500 mL of sample was taken
from the respective carboy in a cylindrical tlask. 2. 5 g
activated carbon (AC) was added into the flask and
magnetic stirrer was started. 5-10 mL sample was
drawn every 15 min from this mass, filtered on filter
paper and the fi ltrate analyzed for pH, colour and
COD. At the end of 2 h, the stirring was stopped and
the experiment was term inated. The experiments were
repeated wit h 5 g bentonite (WP) as well as 5 g
li gnite (BP). All the experiments were carried out at
room temperature of around 32 0 C. The properties of
adsorbents used are given in Tab le I .
Results and Discussions
Performance ofAdso rben ts
The performance of different adsorbent s used in
wastewater treatment with respect to COOl colour
red uction has been analyzed by considering the
fo llowing graded scale:
Performance Per cent reduction in
COOl colour
Effective >40
Moderately effective 20- 40
Not effective < 20
56 J SCIINO RES VO L 61 JAN UA RY 2002

Table 1- Prope rties of adsorbents

Activated carbon Bentonite Li gnite
..
Appearance Fine hlack powder. free from Fine white powder. free Fine black powder.
gritt y matter from gritt y matter free from gritty ma tt er
Ac idity! alkalinity 3g boiled in 60 mL water should pH : 8.76
give a neutral and co lourl ess
tiltrate
Mo isture. per cent by oven at 100" C 5 10.2 10 - 20
Volatile matter. per cent 30 - 35
Fixed carbon. per ce nt 20 - 22
Ad sorption on kerosene, mLiI 00 g 28
Porosity, per cent 19.5
Melting point, "c 1550
Specil1c surface. sq m! g 220
Refracti ve index 1.502
Ash content , per cent. 2-3 12 - 20
Oecolourization capac it y. per ce nt 40
Parti cle size. mi cron 10 - 100 10 - 100 10 - 100
Mesh size. per cent
-BS 72: 100
-BS 100 90 \

+BS 100 0.45

-BS 100 + BS 200 27 .22
-8S 200 + BS 300 11 .77
-8S 300 60.56

COD Reduction fo r wastewater from H-acid. BP is e ffectiv e for

The COD reduction by the three adsorbe nts over
time for sample nos. I to 5 and 6 to II is plotted in
Figure I and 2, respecti ve ly. It can be observed that
for COD reduction , AC is effecti ve for wastewate r
from H- acid , dihydroxydibenzanthrone, e th ano l
(before biogas recovery) a nd di ethyl malonate, a nd
moderate ly effecti ve for wastewater from the plants
manufacturing dibenzanthronyl , benzanthrone crude
and e th anol (after bi ogas recove ry), a nd the com p lex
manufacturing vat d yes and the ir intermediates. AC is
not effective for wastewate r from dibe nzy l
oxybenzaldehyde. WP is effecti ve for was tewate r
d ihydroxydi be nzanthrone, e tha nol (bot h befo re and
after biogas generati on) and from diethyl ma lo nate.
and the complex m anufacturin g differe nt dyes (other
than vat) and intermediates, a nd moderately effective
for dibenzyl oxybeza ld ehyde, dibenzanthronyl a nd
benzanth rone crude, and the complex manufacturing
vat dyes a nd th e ir intermediates. WP is not effective
wastewate r from dihydroxydiben zanthrone a nd
e tha nol (both before a nd after bi ogas gene.rat iun). a nd
the complex ma nufacturin g diffe rent dyes (othe r than
vat) a nd inte rmedi ates, a nd moderately effecti ve for
dibe nzanthron yl, benzanthrone crude and di et hyl
mal o nate, and the complex ma nufacturi :lg vat dyes
and their inte rmed iates. BP is no t effect iv" for H-acid
and dibenzyl oxybenza lde hyde.
Thu s the performance of all the three adsorbe nts
is compa rab le for red ucin g COD of the was tewater
from the plants ma nufacturing dih ydroxy-
dibenzanthron e, dibenzyl oxybenzaldehyde, diben-
zanthro nyl. benzanthron e crude and e th anol (both
before a nd after biogas recovery ). AC is obse rved to
perform be tter than both WP a nd BP for wastewater
from H-acid . In the case of wastewa ter from diethyl
malo nate p lant , the performance of AC and WP is
comparable. and better than BP. The performance of
WP a nd BP is comparable for mi xed wastewater from
 RATHI & PURANIK: CHEMICAL INDUSTRY WASTEWATER TREATM ENT 57

- - --_._----- _ ._ ---- --- - - -- - 1

--+--lAC ...-lWP -.-1I1P -M-2AC _+_2WP __ 2SP -+-3AC -2WP -3BP - :- ~c ':.j-. 4WP -'\- 48P
-+t-- SAC - lII- &WI' ___ _
0.8

0.5

~
1"
8U 0.3

0.2 .r_ ;'j ' -

0.1

Figure I - COD red uction over time

--+--SAC _+_SWP -'-6BP ~7AC -+-7WP --+--7BP -+-SAC -8WP -SBP ..., - SAC
-Jc"' gWp -H' - 10AC "":r. .. 1OWP -",- 1011P -- -i- llAC -llWP -11BP
-'-A- IIBP
0.6

0.5

I 0.4

I"
0.3

0.2

0 .1

0.25 0.50 0.75 1.00 1.25 1.50 1.75 2.00

t,h

Figure 2 - COD red uction over time

the compl exes manufac turin g di fferent dyes and the ir
intermediates and it is better th an AC for wastewater
fro m the compl ex manufac turin g d ifferent dyes (other
th an vat) and intermedi ates.
CoLour Reduction
For colour reducti on, AC is fo un d to be
effecti ve fo r wastewater of dihyd roxydibenzanth ro ne .
d ibenzyl oxybezalde hyde. di benzanthronyl and
benzanthrone crude, and the compl ex manu fac tu ring
vat dyes and the ir intermedi ates, and it is mode rately
effecti ve for ethano l (both before and after biogas
recovery. W P is effecti ve for wastewater of dibenlyl
oxybezaldehyde and moderate ly effect ive for
dihydroxyd ibenzanthrone, benzanthrone crude and
eth anol (both before and after biogas recovery ). and
the complex manu fac turing different dyes (other than
vat) and intermediates. WP is not effective fo r
58 J SCIIND RES VOL 61 JANUARY 2002

wastewater from dibenzanthronyl, and the complex """'"

manufacturing vat dyes and their intermediates. BP is
effective for wastewater from dihydroxy-
dibenzanthrone and benzanthrone crude dibenzyl
oxybezaldehyde, and the complex manufacturing vat
dyes and their intermediates, and is moderately
effective for and ethanol (both before and after biogas
recovery), and the complex manufacturing different
dyes (other than vat) and intermediates.
It may thus be observed that the performance of
all the three adsorbents is comparable in reducing
colour from the plants manufacturing ethanol. AC is
better than WP and BP, and BP is better than WP in
the case of wastewater from the other plants . ....", ul4RP
Comparing the cost of adsorbents used in the ...... 300000 _
100000
experiments, it is found that activated carbon is about Exper1_1 coo, mill L
ten-times expensive than either bentonite or lignite .
The spent activated carbon or lignite, considering Figure 3 - Experimental and estimated COD-AC
their calorific value, could be disposed easily and
gainfully along with coal in boilers. The adsorbate

/
organic matter from wastewater would also contribute
to calorific value to some extent. At high
temperatures in the boilers, large molecules of
organic adsorbate would get disintegrated into
harmless non-toxic small molecules like carbon
dioxide and water, and the statutory authoriti es may
permit this. Thus , spent activated carbon and lignite
have the advantage of easy and safe disposal; and
lignite has the cost advantage over activated carbon.

Comparison of Models
The COD values at differen t durations were
predicted, using the following mode ls available In
"WM Pl4RP
literature:
tOOOOO 200000 300000 400000 5(0000 iOOOOO
Weber and Morri ' s equation (Eq. I) Experimental COO, mgI L

(C;-C)/ Ci = m I to.5 + c I' .. . ( I ) Figure 4 - Experimental and estimate d COD-WP

Lagergren equation (Eq. 2)

log (C - Ceq) =m2 t + c2 . . . . (2) COD Equilihrium Prediction
It may be seen that Eq.(2) requires data on the
Rathi Puranik equation 19 (Eq. 3) eq uilibrium value of the COD for the p rediction of
... (3) COD at a given time. necessitating expe riments for
log (CODRT) = m t + c.
eac h system. Eq.(3) does not require equ ilibri ull1
The values of COD predicted from these three value of COD for predicting COD of a give n system
models at differen t durations are compared with the at any time. In fact, Eq.(3) can predi ct equ ilibriull1
experimental COD values in Figures 3 to 5, for three value of COD. COD eq uilibrium va lues so predicted
adsorbents . It may be observed that Eq. 3 predicts the are compared with the experimenta l values in
COD with least errors as compared to the other two Figure 6. It may be observed that the predicted values
models. are in agreement with the expe rimental va lu es
 RATHI & PURANIK: CHEMICAL INDUSTRY WASTEWATER TREATMENT
"""" ]
~,
) I
1
- j
, I
Q
o
I 1I0000
0--.0 .
I o
I
Ex~ coo, mgI L
Figure 5 - Experimental and estimated COD-BP
obtained at the end of 2 h of each experiment, in most
of the cases, which are considered to be equilibrium
values.
Conclusion
Rathi Puranik model, represented by Eq.(3) , can
be used to predict COD at any time in a given system,
using adsorption for wastewater treatment. This
model requires two data points, whereas other mode ls
available in literature require detailed experi-
mentation on a given system. Thus, Eq.(3) can be
used to predict COD values of a sample in a given
system at any time with least experimentation. This
model can also predict equilibrium values of COD.
The prediction of COD and COD equilibrium values
will be useful in the design of adsorption systems.
Considering the rate of reduction of COD
obtained for different adsorbents, effecti veness and
cost of the adsorbents , and ease of disposal of spent
adsorbents, suitable adsorbent or a combination of
adsorbents could be se lected for optimizing th e cost
of wastewater treatment. The performance of lignite
is observed to be comparable with that of activated
carbon. Lignite is, therefore, considered to be cost-
effective adsorbent in reducing COD as well as
colour from wastewater. This study will be useful to
chemical manufacturers, especially the small and
medium enterprises in the deve lopin g countries.
having limited resources 20 in resolving water
pollution problems economically.
Sl)
1I0000 1
150000 1
t,_ 1
...l
; .
'C 1
j
Q
o
i-I
-1
I e AC .WP .l BP
30000 60000 90000 120000 150000 1I0000
ExperimenbolCODequllibrium. mgl L
Figure 6 - COD equilibrium valucs
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US A) 1980.315
m - Slope o f the strai ght line log CODRT
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