FORM 2
THE PATENT ACT, 1970
mum .I Ill 11
& 200000682
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule13)
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l.TITLE OF THE INVENTION:
A NON-BIOLOGICAL PROCESS FOR TREATING
CHEMICAL LABORATORY EFFLUENT RICH IN
DETERGENTS AND SOLVENTS.
2. APPLICANT
(a) NAME: GALAXY SURFACT ANTS LTD.
(b) NATIONALITY: An Indian Company incorporated under the Indian
Companies ACT, 1956
(c) ADDRESS: C-49/2, TTC Industrial Area, Pawne,
N avi Mnmbai — 400703
Maharashtra, India
3.PREAMBLE TO THE DESCRIPTION
The following specification particularly describes the invention and the manner in
which it is to be performed.
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FIELD OF INVENTION
The present invention relates to effluent treatment and in particularthe process for
treating the effluent generated from a chemical laboratory with variation in terms of
both the effluent quality and quantity. The present invention relates to process of
treating effluent streams having high concentrations of detergent, water miscible
solvents, traces of water immiscible solvents and other organic impurities.
The present invention also relates to setting up an effluent treatment plant having a
physicochemical process for a small industrial set-up/ chemical laboratory where
typical biological effluent treatment technologies faces several limitations such as
space constraint , obnoxious odor problems, un-adaptability to heavy and sudden
fluctuations in effluent volume and characteristics.
BACKGROUND OF INVENTION
With increase in awareness towards environmental and water pollution, stricter
environmental protection laws have been enacted by 'various environmental agencies
and pollution control bodies across the globe. Thus treatment of effluent has become
mandatory prior to its discharge in the receiving water bodies such as lakes, rivers
and ground water without adversely affecting the ecosystem. Because of such
scenario it has become imperative for even smaller industries to setup their own
effluent treatment systems. However for small industrial setups and chemical

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laboratories, the space and financial burden are the main bottlenecks for setting up
and running ETP plant, and thus it is essential that the effluent treatment system be as
compact and as cost effective as possible.
Effluent treatment by conventional means of biological effluent treatment processes
can be a challenging task for such small scale set-ups typically due to several
constraints such as limited land availability (large footprint) due to the need for large
aeration tanks and clarifier tanks, odor issues with biological sludge, scaling down of
ETP plant with treatment capacity of 3-5 KL/days, requirement of an ETP plant that
can be operated discontinuously with minimum treatment time and operator
intervention. Even though modern technologies such as membrane bioreactor (MBR)
have relatively much lower space requirements than conventional biological process,
but still it cannot be employed when the space constraint is a major bottle neck,
further MBR also has disadvantages such as issues of membrane fouling, high cost of
membrane etc. Further, an effluent having good amount of ethanol/ strong
preservativesl bactericidal components will not be effectively treated with the
biological processes due to its tendency to kill or inhibit microbial growth, which is a
key requirement for effluent treatment by biological process.
Majority of the commercially available detergents for cleansing purpose/laundry are
anionic. There are very few prior art which disclose the method to treat effluent
containing high concentrations of detergents, particularly by non-biological process.

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US patent 4005009 describes a method of treating waste water containing anionic
detergents and heavy metals, by using inorganic coagulant and cationic
polyelectrolyte through the foam separating process (froth floatation), thereby to
collect said surfactant and heavy metals as separated from water. The disclosed
method is reported to be suitable for waste water containing from 3 to 20 ppm of
heavy metals and from 1 to 20 ppm of anionic detergent.
A method for removing detergents from a wastewater stream by ultra-filtration
process has been described in PCT/US2006/001007, however such membrane based
separation process are very costly, especially the problem that arises due to
membrane fouling and high cost of membranes. Further the described ultra filtration
process decreases the detergent concentration to 100 ppm in permeate stream but it
also generate a reject stream having very concentrated solution of surfactant which
could have 10-50 times higher concentrations of detergents and Chemical Oxygen
Demand (COD) values compared to effluent, thus appropriate treatment of reject
streams remains a challenge to be solved and thus membrane based‘ detergents
separation process are not a commercially viable option for effluent treatment.
In view of the above requirements and challenges, recently a number of non-
biological processes of effluent treatment have been developed which are gaining
popularities includes advanced oxidation processes such as treatment with UV,
treatment with ozone, peroxide and hydrodynamic cavitation etc
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US patent 20090032471 discloses ozone and UV-based water treatment methods,
combined with peroxide treatment that can be used to remove a diverse range of
contaminants from water. However, it does not discuss treatment of detergent
containing effluent.
In the article published in J. Environ. Anal. toxicol.; 3(4), 2013, effluent containing
anionic surfactants is treated with Advanced Oxidation Processes (AOPs), wherein
about 50% anionic surfactants are removed by treating the effluent with lg/L
hydrogen peroxide. The drawback of the process is that it involves huge quantity of
hydrogen peroxide and results in only 50% reduction in detergent.
The inventors of the present invention have surprisingly developed a non-biological
process of effluent treatment which overcomes the drawbacks of the prior art and
which is suitable to treat effluent streams containing detergent concentrations of as
high as 5000 ppm and solvent concentrations of 1000 ppm.
OBJECT OF INVENTION
i) It is an objective of the present invention to establish a non-biological process
for treatment of effluent produced from chemical laboratory which contains
high concentration of solvents and detergents.
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ii) It is another objective of the present invention to develop a robust effluent
processing system which can treat the effluent with wide range of variation.
iii) Another objective of the present invention is to develop a compact effluent
system.
iv) Another objective of the present invention is to develop a system that can be
operated with minimal operator intervention.
v) It is another objective of the present invention to develop a process of treating
effluent streams having high concentrations of anionic detergents and
solvents.
vi) It is another objective of the present invention to develop an effluent treatment
plant that can be operated as an when required (no need of running it in
continuous mode).
SUMMARY OF INVENTION
The present invention describes a two step process for effectively addressing the
requirement of treating chemical laboratory effluent rich in detergents and solvents.
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The present invention relates to a method for treatment of detergent and solvent rich
effluent having Chemical Oxygen Demand (COD) up to 5000 ppm, comprising the
steps of i
i) Removal of detergents from effluent by employing use of inorganic precipitant
and cationic polymer at acidic pH;
ii) Degradation of solvents in effluent by using oxidants in combination with UV
irradiation;
wherein the COD is reduced to less than 500 ppm.
Deviation from the above specified sequence significantly reduces the efficiency of
the process.
By the present method, the detergent is removed by 90-95% and solvent removal is
50-65%.
Detergent herein refers to anionic surface-active agent having high cleansing activity.
DETAILED DESCRIPTION OF INVENTION
The present invention describes a two step non-biological process for effectively
addressing the requirement of treating chemical laboratory effluent rich in detergents
and solvents in a specific sequence. Deviation from the specified sequence
significantly reduces the efficiency of the process.
The present invention relates to a method for treatment of detergent and solvent rich
effluent having COD up to 5000 ppm, comprising the steps of

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i) Removal of detergents from effluent by employing use of inorganic precipitant and
cationic polymer at acidic pH;
ii) Degradation of solvents in effluent by using oxidants in combination with UV
irradiation;
wherein the COD is reduced to less than 500 ppm.
Chemical laboratory effluent:
All the chemical laboratories generally follow the standard practice of waste
management in which one of the basic segregation is based on physical nature where
solid wastes, semisolid wastes and liquid wastes are segregated depending on their
chemical nature (hazardous, non-hazardous, acid, base, corrosive etc). Solid and
semisolid wastes are discarded by sending it waste disposal bodies, government
authorized waste management agencies. The liquid waste is also generally segregated
as water miscible fraction and water immiscible fraction. Water immiscible
component is stored as solvent waste and is disposed appropriately. The water
miscible component is generally resulted from aqueous streams that are generated by
washing of glassware with detergents and by use of water miscible solvents which are
either used for accelerating drying of glass wares or which results as the waste
streams generated from High performance liquid chromatography (HPLC), such
waste is allowed to go in to the drainage and thus is subsequently collected as
effluent.

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The present invention discloses the method to treat chemical laboratory effluent
which is aqueous stream generated after appropriate segregation of chemicals and
which primarily consist of detergents, solvents and traces of organic contaminants.
Process:
The schematics of the equipment used and the process flow summary are given in
Figure I.
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:2 §
is :2
E 3
H! II
E D _
5 El Fecl, Caustic
A Polv
electrolyte
X X
Tankl Tankz 2
V/, ...... .' ,/''§:}
2-K.’ 5-r“5
Precipitated and Ferric hydroxide T m
coagulated sludge sludge reaiede “em
(com 500)
1,2 Cyclone separator
3,4 Bag filter (5 micron filter)
5 Activated carbon filter
6 Oxygen concentrator and ozone generator
7 Venturi injector
B Chemical oxidant, Activators
9 500 Liter Pressurized SS tank (Zbar) for mixing effluent with oxidants, activators
10 UV reactor
Fig.: I
The equipment primarily consists of three sequential treatment tanks having working
capacity of 1000 L each. Tank 1 and Tank 2 are open tanks equipped with mechanical
agitators and pH meters and chemical dosing pumps. Tank 3 is closed loop gas and
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liquid diffusion mixing chamber in which effluent is continuously recirculated with
oxidizing chemicals such as ozone and hydrogen peroxide which are injected
upstream to the mixing chamber. An Ultra-Violet (UV) reactor is also connected in
the loop.
. Step-I:
The first step includes precipitation of detergents by addition of an inorganic
precipitating agent in the range of fiom 500 to 1000 ppm at pH between 2-3. The
precipitating agent is selected from ferric chloride, ferric alum, alum, preferably ferric
chloride is used. The added ferric chloride reacts with anionic detergent and forms a
precipitate which is ferric salt of detergent, after sufficient mixing time.
FeC|3 + 3RArso',Na*—. Fe[RArSO3]3l + 3NaCl '
Fecl, + 3Rso,,'Na* _.. Fe[Rso,]3l + 3NaC|
FeC|3 + 3R(OCH2)nSO4'Na*__, Fe[R(OCH2)nSO ,1, l + 3NaC|
Addition of 1000 ppm of ferric chloride forms a heavy precipitate and can efficiently
remove surfactants in concentration range of 250- 5000 ppm (Figure 11)

Percent Reduction of SLE5 Activity using 1000ppm FeCl3
97.00
96.50 " "
9530 ) ..
95.50 1 »
95.00 ._:. .. ..
94.50 E
94.00 . ...
a-«cu-percent Reduction of
SLES Activity
93.50 .
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Reduction
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9100 ._....... W-.-
52.50 . .5 I1 ...-... _,__,_, ,....., .
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92 .00 ‘‘‘‘ ”
91.50 “ ’
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250 522 990 1980 5000
LES-1 mole Cuncentration (ppm)
Figure II
However, addition of 1000 ppm of ferric chloride increases the total dissolved solids
(TDS) beyond the desirable limits, particularly chloride content increases beyond 600
ppm which makes the treated effluent unsuitable to be discharged in water natural
bodies. While lower ferric chloride concentration may be desirable but are not
effective below the range of 900 ppm. To effectively precipitate detergents using
lower ferric chloride concentration, a cationic polyelectrolyte is added which
coagulates the finer precipitates to large aggregates that can be easily separated by
sedimentation, forced sedimentation (centrifugation, hydrocyclone separation) or
filtration or combination thereof. Preferably the process involves separation of larger
aggregates by hydrocyclone separation followed by filtration through micron size
filters to remove residual finer particles.
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The cationic polyelectrolyte is chemically polyacrylamide and is selected from
commercially available series of Zetag® cationic polymer powders (BASF). The
concentration of polyelectrolyte used is in the range of 1-15 ppm, preferably not
exceeding 10 ppm.
The precipitation and coagulation is carried out at a pH range of 2-3 which is resulted
by addition of ferric chloride. The pH of filtered effluent is then adjusted between 7-9
by addition of caustic or lime which results in to precipitation of excess ferric
chloride in the form of ferrous hydroxide, which is again subjected to sedimentation,
centrifugation or hydrocyclone separation process followed by filtration through sand
filter and then 5 micron size bag filter. The clarified effluent is then pumped through
activated carbon colunm which removes other organic contaminants from the effluent
except water miscible solvents.
Removal of the surfactants from effluent stream is essential prior to solvent removal
by oxidative degradation (Step H), since presence of surfactants generates foam
which severely decreases the efficiency of solvent removal process.
Use of ferric chloride in the concentration range of 700-800 ppm with the aid of 1-15
ppm of polyelectrolyte allows 90-95% surfactant removal of effluent having
detergent load of 200 ppm to 5000 ppm, without increasing the chloride content and
TDS beyond the acceptable limits.
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Step-II:
lln the second step, the effluent which is now devoid of detergent and other organic
contaminants and which mainly contains solvents is treated with oxidants such as
ozone or H202 or both, preferably in combination with UV irradiation and other
inorganic activators. The levels of such oxidants required for complete degradation of
solvents and other organic contaminants is calculated on the basis of
measured/predicted Chemical Oxygen Demand (COD) of the influent water.
In accordance with one aspect of the invention, effluent being treated comprise about
200-5000 ppm detergent, organic solvent content of 50- 400 ppm, COD levels of
about 300 -5000 ppm, pH of about 2-10.
In an embodiment, the anionic detergent include those surface-active or detergent
compounds which contain an organic hydrophobic group containing generally 8 to 18
carbon atoms and at least one water-solubilizing group selected from the group of
sulfonate, sulfate and carboxylate. Examples of suitable anionic detergents include
sodium salts of fatty alcohol sulfates, fatty alcohol ether sulfates and linear alkyl
benzene sulfonates.
In an embodiment, water miscible solvents are acetone, ethanol, methanol, isopropyl
alcohol, acetonitrile, or mixtures thereof.
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Advantages of the invention
1. Treatment of effluent containing high concentrations of detergent and
solvents.
2. Method for treating effluent in confined space by non-biological process.
3. Method to treat effluent from Chemical laboratories.
4. Low treatment time (few hours).
5. Discontinuous (batch wise) operation.
EXAMPLES
The present invention is now described by way of working on non-limiting
illustrative examples. The detail of the invention provided in the following examples
is given by the way of illustration only and should not be construed to limit the scope
of the present invention. Analytical techniques for measurement of anionic detergent
concentrations and solvent concentrations are well known for those who are skilled in
the art and thus detailed analytical procedures are not described here.
General Experimental Procedure:
The effluent (1000 L) is pumped in to tank 1 [Fig.1] followed by addition of
anhydrous ferric chloride (750 g) which is mixed with the effluent under mechanical
agitation using overhead stirrer at 1200 rpm for 10-15 min. Polyelectrolyte (log) is
then added and mixing continued for 5 minutes to allow coagulation of the
precipitated Fe-Detergent complex. The slurry of the coagulated Fe-Detergent

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complex is then pumped through cyclone separator [Fig.1 (l)] to remove coagulated
sludge while fine particulate matter is filtered through 5 micron size bag filter [Fig.1
(3)]. The clear filtrate is then pumped in to tank 2 [Fig.1]. Required amount of caustic
is added to make filtrate alkaline (pH 7-9). Precipitated ferric hydroxide is separated
by passing through cyclone separator [Fig.1 (2)] and bag filter [Fig.1 (4)]. The clear
filtrate is then passed through a column of activated carbon [Fig.1 (5)].
The outlet fiom activated carbon Column [Fig.1 (5)] is pumped in to a gas and liquid
diffirsion mixing chamber [Fig.1 (9)] in which effluent is continuously mixed with
oxidizing chemicals such as ozone [Fig.1 (6)] and hydrogen peroxide [Fig.1 (8)]
which are injected upstream toithe mixing chamber. A sufficient excess of oxidants is
maintained by bubbling ozone in the effluent at constant flow rate of 50 .- 100 g/hour.
Hydrogen peroxide is added in such a way that its concentration (in ppm) is half the
concentration of the measured or expected Chemical oxygen demand (COD) of the
effluent stream being treated. A UV reactor is connected in the recirculation loop
[Fig.1 (10)] which irradiates the effluent with high energy UV light of 254 nm. UV ~
treatment accelerates hydroxyl radical formation, which increases the degradation of
contaminants. Recirculation of the effluent in Tank 3 [Fig.1] is typically continued for
2-3 hours.
Data for the three trials is given in the examples cited below:

After stage 1
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Example 1 Influent After stage 2 % reduction
Treatment Treatment
Detergent concentration 1 12 25 25 77
(ppm)
Solvent concentration 120 95 50 58
(ppm)
COD (ppm) 560 265 175 69
Example 2 Influent After stage 1 After stage 2 % reduction
Treatment Treatment
Detergent concentration 21 0 20 1 5 93
(ppm)
Solvent concentration 250 247 ll 1 5 6
(ppm) .
COD (ppm) 851 568 275 68
Example 3 Influent After stage 1 After stage 2 % reduction
Treatment Treatment
Detergent concentration 880 75 70 92
(ppm)
Solvent concentration 450 440 154 66
(ppm)
COD (ppm) 3540 1 188 383 89
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We claim
1. A method for treatment of Chemical laboratory effluent rich in detergents and
solvents having Chemical Oxygen Demand (COD) up to 5000 ppm, comprising
the steps of
i) Removal of detergents from effluent by’ employing use of inorganic
precipitant and cationic polyelectrolyte at acidic pH;
ii) Degradation of solvents in effluent by using oxidants in combination with
UV irradiation;
wherein the COD is reduced to less than 500 ppm.
2. The method as claimed in claim 1 wherein the inorganic precipitant is ferric
chloride.
3. The method as claimed in claim 1 wherein the polyelectrolyte is chemically a
cationic polyacrylamide.
4. The method as claimed in claim 1 wherein the pH is between 2-4.
5. The method as claimed in claim 1 wherein the detergent contains anionic
surfactant
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6. The method as claimed in claim 1 wherein the solvents are water miscible
solvents such as acetone, ethanol, methanol, isopropyl alcohol, acetonitrile or
mixtures thereof.
7. The method as claimed in claim 1 wherein the oxidant is hydrogen peroxide,
ozone or combination thereof.
Dated this 28"‘ day ofNovember, 2014
Galaxy Surfactants Ltd.
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