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Enhanced electrochemical
oxidation of anionic
surfactants
a b b
Homg G. Leu , Sheng H. Lin & Tze M. Lin
a
Environmental Protection Bureau, Taoyuan
County, Taoyuan, 330, Taiwan, ROC
b
Department of Chemical Engineering, Yuan
Ze University, Neili, Taoyuan, 320, Taiwan,
ROC
Published online: 15 Dec 2008.

To cite this article: Homg G. Leu , Sheng H. Lin & Tze M. Lin (1998): Enhanced
electrochemical oxidation of anionic surfactants, Journal of Environmental
Science and Health, Part A: Toxic/Hazardous Substances and Environmental
Engineering, 33:4, 681-699

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J. ENVIRON. SCI. HEALTH, A33(4), 681-699 (1998)

ENHANCED ELECTROCHEMICAL OXIDATION OF


ANIONIC SURFACTANTS
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Key Words: Anionic surfactants, electrochemical oxidation, hydrogen peroxide

Homg G. Leu1, Sheng H. Lin2* and Tze M. Lin2


1
Environmental Protection Bureau
Taoyuan County, Taoyuan 330, Taiwan, ROC
2
Department of Chemical Engineering
Yuan Ze University
Neili, Taoyuan 320, Taiwan, ROC

ABSTRACT

The surfactant wastewater treatment by electro-chemical oxidation with or without

peroxide hydrogen was investigated. The two anionic surfactants studied here were

alkylbenzene sulfonate (ABS) and linear alkylbenzene sulfonate (LAS), both of them

being widely used in the household and industrial detergents. Experiments were cond-

ucted to examine the effects of pH, electrolyte concentration, time of electrochemical

oxidation, power input and amount of hydrogen peroxide (H2O2) on the surfactant remo-

val and other water quality parameters. Optimum operating conditions were experimen-

tally determined. The enhanced version of electrochemical oxidation (i.e. with addition of

hydrogen peroxide) was found to be significantly more efficient than that without.

681

Copyright © 1998 by Marcel Dekker, Inc.


682 LEU, LIN, AND UN

INTRODUCTION

Domestic wastewater is one of the major pollution sources adversely impacting

receiving water body in many developing countries around the world. In the domestic

wastewater produced by the households, surface active agents or surfactants invariably

exist in significant amount due to detergents used for all kinds of washings (Ainsworth,
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1994). In fact, surfactants have also been widely used in textiles, fibers, food, paints,

polymers, plant protection, cosmetics, Pharmaceuticals, mining, oil recovery and pulp

and paper industries (Hellston, 1986).

As noted by Swisher (1987), a large number of surfactants, including the anionic types

employed in the present study, are not easily biodegradable. Due primarily to econo-mic

reasons, it is not possible to use easily biodegradable surfactants in all household and

industrial applications. Pretreatment methods of surfactant wastewater thus need to be

developed which allow safe uses of refractory types of surfactant (Swisher, 1987). In the

past decades, ozonation and other advanced chemical oxidation has been suggested and

investigated by many researchers for pretreatment of refractory surfactants (Suzuki et al.,

1978; Nakis, 1980; Medley and Stover, 1983; Nakis et al., 1985, 1987; Pelizzetti et al.,

1989; Brambilla et al., 1993; Adams et al., 1994, 1996). Those investi-gators had found

mat the biodegradability of those refractory surfactants can be consider-ably enhanced by

ozonation or photocatalytic treatment.

Although effective in improving the biodegradability of refractory surfactants, ozo-

nation or photocatalytic oxidation is a relatively costly method. Alternative chemical tre-

atment methods which are as efficient and yet less expensive to implement would be

highly desirable. A method with a potential of meeting these requirements and deserving

attention is the electrochemical method. This method employs electric energy to oxidize
ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 683

pollutants in the aqueous solution. During the electrochemical oxidation process, bypo-

chorite is generated which, being a strong oxidant, accounts mainly for oxidation of

pollutant by the process. Hence it would be of much practical and academic interest to

look into surfactant wastewater treatment by electrochemical oxidation. In fact, the

electrochemical oxidation process has also been employed successfully to treat various
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industrial wastewaters in many previous investigations (Matis, 1980; Cenkin and

Belectsen, 1985; Camninellis and Pulgarin, 1993; Leffrang et al., 1995; Lin and Peng,

1995, 1996; Lin and Wu, 1996; Polcaro and Palmas, 1997). The purpose of this study is

to employ electrochemical oxidation process in conjunction with chemical coagulation in

treating the wastewater containing anionic surfactants. Experimental tests were carried

out to examine the effects of operating variables on the oxidation efficiencies of the

process and to facilitate determination of optimum operating conditions.

MATERIALS AND METHODS

The experimental apparatus for electrochemical oxidation is shown in Figure 1. The

electrolytic cell was a 1.5 liter pyrex beaker equipped with a magnetic stirrer. Two pairs

of anodic and cathodic electrodes (cast iron plates) situated approximately 1.5 cm apart to

each other and dipped in the surfactant wastewater. The total effective surface area of

electrodes was 22.6 cm2. The current input was controlled by an ammeter and the total

power consumption was integrated and registered by a power integrator. In each run,

approximately 1 liter of sample surfactant wastewater was placed in the electrolytic cell.

In the enhanced oxidation test runs, a desired amount of hydrogen peroxide (H2O2) was

added to the electrolytic cell before the electrical current was turned on. Addition of H2O2

was found to be highly beneficial for the electrochemical process in improving the waste-
684 LEU, LIN, AND LIN

1. D. C. Power Supply
ECS b o < ¿I».
2. Digital Ammeter
?®ñ
±t 3. Power Integrator
4. Parallel Cast Iron Anodes
5. Parallel Cast Iron Cathodes
6. Magnetic Bar Stirrer
7. Sampling Port
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8. Electrolytic Cell
9. Digital Magnetic Stirring Controller

FIGURE 1

Experimental Setup.

water quality. During the electrochemical treatment (with or without) of surfactant waste-

water, a small amount of iron was continuously dissolved into the wastewater from the

cast iron electrodes. The dissolved iron when combined with OH" would form many

small floes during the electrochemical process. The floes were difficult to settle out of

waste-water because of their small sizes. This phenomenon was observed frequently in

the present study. Presence of small floes in wastewater would interfere with COD, NTU,

color absorbance and metal ion measurements. To overcome the floe settling problem,

centrifugation of all samples for 5 min would suffice. On the other hand, chemical

coagulation of the wastewater after the electrochemical treatment using a low dosage of

50 mg/1 PAC (polyaluminium chloride) followed by 1 mg/1 polymer was observed to be

equally effective. Test runs using both methods for all samples after electrochemical

oxidation yielded practically the same results. Hence centrifugation was adopted for

convenience for small samples (i.e. less than 10 ml). In case of large samples, like the
ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 685

wastewater sample which needed further ensuing treatment, chemical coagulation was

employed. The surfactant concentration and NTU of wastewater samples were

determined by the standard methods (APHA, 1992). Fe concentration was measured

using a GBC 932 atomic absorption spectrophometer (GBC Scientific Equipment, Ltd.,

Victoria, Australia).
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Two surfactants considered here were of anionic type. They were alkylbenzene

sulfonate (GR grade ABS), obtained from Ferak Laborat GmbH, Germany, and linear

alkylbenzene sulfonate (GR grade LAS), obtained from E. Merck GmbH, Germany. Both

ABS and LAS are sulfonated alkyl sodium salt, but the former has many side chains on

the alkyl group while the latter has a linear alkyl group only. This may account for the

greater biodegradability of LAS than ABS. Regardless of its lower biodegradability, ABS

is still widely used in various household and industrial detergents due to its lower cost.

However, LAS has been gaining wider acceptable lately. In the present studies, the ABS

and LAS concentrations were limited to a maximum around 10 mg/1 due to the fact that

beyond that concentration level, foaming in the aqueous solution would be a severe

problem. Furthermore, past experiences of the present authors in monitoring the water

quality of seriously polluted streams revealed no more than 10 mg/1 of any kind of surf-

actants under most practical circumstances.

RESULTS AND DISCUSSION

Performance Characteristics of Electrochemical Oxidation

The mechanism of electrochemical oxidation in the aqueous system is a rather

complex process (Pletcher and Walsh, 1990). It is generally believed that there are two

possible important mechanisms involved in the oxidation process: electro-flotation and


686 * LEU, LIN, AND UN

electro-oxidation. Oxidation and reduction of the electrochemical process occur, respec-

tively, at the anode and cathode (Pletcher and Walsh, 1990). With sufficient power

supply, the surfactant molecules are decomposed into small molecule or end products at

the anode. Electro-flotation occurs at the cathode due to evolution of chlorine and/or

hydrogen. Generation of the gases can be easily detected by the gas bubbles observed in
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the test runs and the pungent smell of chlorine gas.

The sample surfactant solution for the present electrochemical oxidation was pre-

pared by mixing an appropriate amount of anionic surfactant with deionized water. The

conductivity of the sample surfactant solution was observed to be lower than 300 jimho/

cm which is insufficient for effective electrochemical oxidation of organic pollutants22.

To remedy this deficiency, addition of appropriate amount of table salt was found to be

highly efficient for this purpose. Figure 2 demonstrates the increase in conductivity of the

surf-actant wastewater as a function of salt concentration. The relation appears to be

linear with a slope of 1.4, implying that for an increase of 1 mg/1 in salt concentration,

there is a conductivity increase in the surfactant solution by 1.4 junho/cm. According to

Krstajic and Nakic (1987), the added chloride ion in the aqueous solution will be first

converted anodically to chlorine which is in turn transformed to hypochloric acid

following the reaction sequence:

2 Or— >Cl 2 + 2e

Cl2 + H2O —> HC1 + HCIO

The hypochloric acid (HCIO) is a strong oxidant. This may account for the strong effect

of salt concentration on the ABS and LAS removal as displayed in Figures 3(a) and 3(b),

respectively. Note that 0.01 M of NaCl is equal to 584.5 mg/1 which is in turn equivalent

to 818 lunho/cm according to Figure 2. Figure 3(a) indicates that for a salt concentration
ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 687

5000
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1000 2000 3000 4000


-l
Salt Concentration, mg-I

FIGURE 2

Conductivity of aqueous solution vs salt concentration.

exceeding 0.05M (equivalent to about 4,100 |imho/cm conductivity), its effect on the

ABS removal becomes relatively small, achieving a 92% ABS removal after 30 min of

electrochemical oxidation which is excellent. The effect of salt concentration on the LAS

removal is shown in Figure 3(b). This figure shows a different removal characteristics of

LAS from that of ABS. After 30 min of electrochemical oxidation, the LAS removal was

increased by 25.5% from 43% to 68.5% as the salt concentration was increased from

0.0 IM to 0.03M. However, as the salt concentration was increased by ten times from

0.03M to 0.3M, the LAS removal was only improved by 22.5%, being elevated from

68.5% to 91%. The smaller increase of LAS removal as a function of the salt concentra-

tion indicates that a NaCl concentration greater than 0.03M will be necessary for

effective electrochemical oxidation of LAS.


688 LEU, LIN, AND LIN

>
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O
u

oo
CD

0.1 MNaCI
O 0.07 MNaCI
• 0.05 MNaCI
(a) A 0.03 MNaCI
A 0.01 MNaCI
I
12 IS 24 30
Time, min
ü 0.30 MNaCI
• 0.15 MNaCI
0.09 MNaCI
0.05 MNaCI

12 18 24 30

Time, min

FIGURE 3

ESect of Salt Concentration of the Surfactant Removal with 2.5 A Current.


ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 689

Figures 4(a) and 4(b) demonstrate the changes in surfactant concentration, turbidity

(NTU) and power consumption during the electrochemical oxidation process for ABS

and LAS, respectively. The power supply seems to increase nearly linearly with treatment

time due to constant power input. It is of interest to note in both figures that a fast

decrease in surfactant concentration was accompanied by a rapid increase in NTU. This


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was caused by the increasingly large number of floes generated during the

electrochemical oxidation period. Those small floes remained suspended due to mixing

action and were rapidly removed by chemical coagulation.

The pH effects on the surfactant removal, power consumption and the final pH of

aqueous solution are shown in Figures 5(a) and 5(b) for ABS and LAS, respectively, after

15 min of electrochemical oxidation. Figure 5(a) reveals that there is relatively little

initial pH effect on the ABS removal. The LAS removal is seen in Figure 5(b) to increase

steadily with initial pH below pH 5 and after that the initial pH effect becomes rather

small. The initial pH effect on the final pH of the aqueous solution is relatively small,

being varied between 8 and 11. The two figures however show a rather strong initial pH

effect on the power consumption. The decrease in power consumption was caused by a

decrease of voltage in the power supply with increasing initial pH as observed in the test

runs. From the above observations, it could be concluded that an initial pH about 7 or

above would be optimum for the electrochemical oxidation of surfactant wastewater.

Performance Characteristics of Enhanced Electrochemical Oxidation

As mentioned earlier, the electrochemical oxidation of pollutant was due primarily to

generation of a strong oxidant (hypochloric acid) in the aqueous solution. During the

electrochemical oxidation process, a certain amount of Fe ion was continuously dissolved

into the aqueous solution from the iron plate electrodes (Pletcher and Walsh, 1990). The
690 LEU, LIN, AND UN

10
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FIGUKE4

The Surfactant Concentration, Power Consumption and NTU as a Function of Time with
0.07M NaCl for ABS and 0.09M for LAS Oxidation.
ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 691

100
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FIGURE 5

Effect of pH on the Surfactant Removal, Final Solution pH and Power Consumption with
2.5 A Current and after 15 min of Oxidation.
692 LEU, LIN, AND LIN

Fe ion can be beneficially utilized if hydrogen peroxide (H2O2) is externally supplied. The

rationale is mat simultaneous presence of Fe ion and H2O2 in the aqueous solution will

produce Fenton-like reaction which is itself a strong oxidation process for pollution

abatement (Lin and Peng, 1995). Hence addition of a small amount of H2O2 will enhance

the electrochemical oxidation process. Figures 6(a) and 6(b) demonstrate the effect of
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H2O2 on the efficiencies of ABS and LAS removal, respectively, by the electrochemical

oxidation. The two figures clearly shows the advantage of 100 mg/1 HiO2 addition. With

15 min of enhanced electrochemical oxidation, the ABS and LAS concentrations

decrease much more rapidly than that without H2O2 addition. Furthermore, addition of

100 mg/1 H2O2 delays the time for rapid NTU increase from the starting time to

approximately 8 min, at that time the surfactant concentration was already rather low.

Thus the overall quality of surfactant wastewater treated by enhanced electrochemical

oxidation is signifi-cantly better than that treated without H2O2.

To determine the optimum its amount required by enhanced electrochemical oxi-

dation, the amount of H2O2 was varied between 50 and 200 mg/1 in Figures 7(a) and 7(b)

for ABS and LAS treatments, respectively. Figure 7(a) shows that a large improvement in

the ABS removal was realized as the H2O2 concentration was elevated from 50 mg/1 to

100 mg/1. But beyond that the improvement with increasing H2O2 dwindled considerably.

Figure 7(b) demonstrates the effect of H A on the LAS removal. It is clear in this figure

that the optimum amount of H2O2 occurs at 150 mg/1 for LAS. This is higher the 100 mg/1

H2O2 for ABS shown in Figure 7(b).

Pertaining to Figures 7(a) and 7(b), the changes in the surfactant and residual H2O2

concentrations and NTU are displayed in Figure 8(a) and 8(b) for ABS and LAS, respec-

tively. It is noted in Figure 8(a) that after 8 min of electrochemical oxidation, the ABS
ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 693

10 30
I

^ \
(a)

v
\
\ \
M~^_ - — • ' *


1 NTU-> - 20
" \ /
I 6 1
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\\ /
- \^ /
- 10
/ A • Electrochemical _
) /
f A 0 Electrochemical/H202
2 -
/ ^ t 4 - ABS Cone.

i 1 , 1 , 1 ,
o 12 18 24 30
Time, min
100
ABS Removal
0»)

2
¿
A • Electrochemical
A O Electrochemical/HjOj

6 12 18 24 30

Time, min

FIGURE 6
Surfactant Removal for Electrochemical Oxidation versus that of Enhanced Version with
150 mg/1 H A and 2.5 A Current.
694 LEU, UN, AND LIN
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>
o

i
00
ffl
<

6 8 10 12 14 16
Time, min
FIGURE 7

Effect of the Amount of H2O2 on Surfactant Removal with 2.5 A Current.


ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 695

30 -i 100

•s,

1
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Î
20

o -Jo
6 8 10 12 14 16
Time, min
30 - , 160

l&-

120.
20

80
¿
o
O "3
CO

40Î Î

0 2 4 6 8 10 12 14 16
Time, min

FIGURE 8

The Surfactant Concentration, NTU and Residual Amount of H2O2 in the Solution as a
Function of Time with 100 mg/1 H2O2.
696 LEU, UN, AND LIN

and residual H2O2 concentrations level off while NTU starts a rapid rise. Hence this can

be deemed as a good time to terminate the electrochemical oxidation process and is

accepted as the reaction time for ABS wastewater treatment. The same optimum

oxidation time is reflected in Figure 8(b) for LAS wastewater treatment. It should be

noted that the opti-mum oxidation time does not seem to be affected by addition of H2O2.
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An important operating variable of electrochemical oxidation process is the current

density which is defined as the current input divided by the surface areas of electrodes.

Since the surface area of electrodes for the present study was fixed at 148.5 cm2, the 2.5

A current input employed in the previous figures was equivalent to 16.8 mA/cm2. Figure

9 displays the effect of current density on the surfactant removal, reaction time and power

consumption. The current density shown in this figure is equivalent to the current input

between 1.5 and 3 A. It is observed here that the big changes of these parameters occur

between 10 and 16.8 mA/cm2. After that, the improvements become much smaller and

hence 16.8 mA/cm2 (or 2.5 A current input) can be considered as the optimum power

input.

CONCLUSIONS

The electrochemical oxidation process could only proceed when the conductivity of

surfactant wastewater is sufficiently high. To maintain high conductivity of surfactant

wastewater, addition of table salt (or other electrolytes) was found necessary. A salt

(NaCl) concentration greater than 0.05M amply met this requirement and would con-

siderably facilitate the electrochemical oxidation of surfactant wastewater. With proper

salt concentration, the electrochemical oxidation of surfactant wastewater proceeded very

rapidly and reached a maximum surfactant removal in about 8 min. Addition of a small
ELECTROCHEMICAL OXIDATION OF ANIONIC SURFACTANTS 697

100 30

Surfactant . 4.0
Removal
1
20
O.
E
Power —> 3.0
c
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2.0
<s

12 14 16 18 20 22 24
2
Current Density, mA/cm

FIGURE 9
Effect of Current Density on the Surfactant Removal, Reaction Time and Power
Consumption with 100 mg/1 H2O2.

amount of hydrogen peroxide (larger than 100 mg/1 NaCl) was found to significantly

enhance the electrochemical oxidation, leading to an improved surfactant removal and

overall water quality of treated surfactant wastewater. However, addition of hydrogen

peroxide did not seem to affect the optimum operating condition stated below. For

efficient electrochemical oxidation with or without hydrogen peroxide, the optimum

operating conditions include: 0.05M NaCl, 16.8 mA/cm2 current density (or 2.5 A

current), pH 7 and 8 min of treatment time.

ACKNOWLEDGMENTS

The authors are grateful to Environmental Protection Bureau of Taoyuan County, Taiwan

for the financial support of this project.


698 LEU, LIN, AND UN

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