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DOI: 10.32434/0321-4095-2020-129-2-36-43
Electrolysis of sodium chloride solutions on Ti/Pt anodes under current reversal conditions
38 ISSN 0321-4095, Voprosy khimii i khimicheskoi tekhnologii, 2020, No. 2, pp. 36-43
polarization in the region of hydrogen evolution. Such forms on a platinum surface even in rather highly
state hereinafter will be referred to as a reduced state. concentrated NaCl solutions. Therefore, the potential
A layer of phase oxides is formed on the surface of shifts by almost 500 mV to the anode region and the
platinum with the anodic polarization in the region selectivity with respect to the products of Cl– ion
of oxygen evolution. This state hereinafter will be oxidation changes: the CE of hypochlorite decreases
referred to as an oxidized state. Oxidation and surface and the CE of chlorate increases [12].
reduction occurs almost instantly in a supporting The data obtained after the cumulative
electrolyte (for example, in 1 M HClO4 or 1 M electrolysis of 1 M NaCl solution are given in Table 1.
NaClO 4) at the current densities higher than In order to reduce the influence of the growth of
10 mA cm–2. A previously reduced Ti/Pt surface pH value from the initial 5.5 to 8.5–9.0 during the
during anodic polarization remains in a reduced state electrolysis, the initial solution was made alkaline
for a long time, if more than 0.5 M chloride ion is (pH 8.5). To decrease the reduction rate of ClO–
present in the solution. Chronopotentiograms on a and HClO on the cathode, the electrolysis was carried
previously reduced Ti/Pt sample in a 1 M NaCl out at a minimum rate of electrolyte mixing and at
solution at various anode current densities are shown the ratio of cathodic to anodic current densities of
in Fig. 1. An increase in potential more than 1.3 V 4:1 [15]. The electrolysis duration was 60 min, which
characterizes the transition of the surface to the does not exceed the time within which the surface
oxidized state. Therefore, the previously reduced was in the reduced state at 20 mA cm–2 (Fig. 1). As
platinum surface with an anodic polarization at follows from the results of the experiment, on the
80 mA cm–2, 40 mA cm–2 and 20 mA cm–2 remains reduced surface, the CE of ClO– is 10–12% higher
in the reduced state for 700, 1500 and 3000 seconds, than on the oxidized one and is more than 80%.
respectively. This allows obtaining quasi-stationary The CE of ClO3– is almost 2 times higher on the
current-voltage curves on the reduced Ti/Pt surface. oxidized sample than on the reduced one and is
A series of curves recorded in a galvanostatic 16% at 16 mA cm–2.
mode are shown in Fig. 2. Curve 1 was obtained on As one can conclude from the obtained results,
the oxidized surface of the sample, then the surface it is possible to increase the CE of hypochlorite up
was reduced and curve 2 was recorded; further, curve to 80–85%. In addition, it is possible to reduce the
3 was obtained on the oxidized and finally curve CE of chlorate up to 5–8%, however the duration
4 was recorded on the newly reduced surface. The of the electrolysis on the reduced surface is limited
reproducibility of the curves indicates the and significantly decreases with increasing current
reproducibility of the surface during sequential density. The need for reducing the surface every time
oxidation/reduction of the surface of the sample. As before the electrolysis almost negates the practical
one can see from Fig. 2, the surface state significantly value of the above results. It should be also noted
affects the polarization of the electrode in the that solutions of 0.15–0.45 M NaCl are used in
presence of Cl– ions. At 10 mA cm–2, the change in practice to prepare hypochlorite solutions by direct
polarization is 430 mV, which indicates the membraneless electrolysis. The transition time of the
electrocatalytic nature of the Cl– oxidation. reduced surface to the oxidized state significantly
Unfortunately, a layer of phase oxides gradually decreases in low-concentrated solutions of NaCl.
15
1.8
42 31
1.7
1 2 3
E / V (vs. Ag/AgCl)
430 mV
1.6 10
j / mA cm -2
1.5
1.4 5
1.3
1.2
0
0 1000 2000 3000 4000 1.1 1.2 1.3 1.4 1.5 1.6 1.7
Fig. 1. Chronopotentiograms recorded on reduced Ti/Pt Fig. 2. Steady-state polarization curves recorded on Ti/Pt in 2
electrode at ja=80 (1), 40 (2) and 20 (3) mA cm–2 in 1 M NaCl M NaCl. The curves numbering is explained in text
Table 1
Current efficiencies of NaClO and NaClO3 during one-hour electrolysis in 1.0 Ì NaCl on Ti/Pt
For instance, the transition time is 1200 s in 0.3 M (Fig. 5). The chronopotentiograms obtained on the
solution, whereas it is only 80 s in 0.15 M at oxidized surface of Ti/Pt in 0.15 and 0.3 M NaCl
20 mA cm–2 (Figs. 3 and 4). It is possible to refuse solutions by cathodic current polarization are shown
the procedure of the pre-treatment of the anode and in Figs. 6 and 7. As the concentration and the cathode
conduct the electrolysis with any duration on the current density increase, the surface reduction time
reduced surface by performing the electrolysis under decreases too. However, the transition time to the
current reversal conditions. reduced state does not exceed 15 s and 5 s even in
It is possible to realize reversible electrolysis in 0.15 M NaCl at jc=–10 mA cm–2 and –20 mA cm–2,
«asymmetric and symmetric» modes. When carrying respectively. A decrease in current density to
out the process in an asymmetric mode, the main 5 mA cm–2 increases the reduction period up to
electrolysis is performed at low anodic and high 100 s in 0.3 M NaCl (Fig. 6, curve 4). It should be
cathodic current densities (Sa>Sc, jc>40 mA cm–2) taken into account that the reverse current density
in order to decrease the reduction of hypochlorite at must be at least 10 mA cm–2 to ensure a rapid
the cathode. A short current reverse occurs after a reduction of the anode surface (up to 15 s) when
predetermined period to reduce the anode surface. carrying out the reversible electrolysis in asymmetric
In this way, it is correct to start the electrolysis with mode. When performing reversible electrolysis in a
the cycle of anode reduction. For the implementation symmetric mode, the reversal time is determined by
of a symmetric method, the electrodes must be the the transition time of the anode to the oxidized state
same and equal in their area. The reverse of the under these conditions of electrolysis. The service
current is done at regular intervals. life of such electrolysis cells is significantly increased
The cycle time of the anode polarization can because the anode workload is distributed alternately
be determined by recording the E vs. t dependences to both electrodes.
on a previously reduced anode at a given current The CE of hypochlorite of 80% with a
density, solution concentration, and hydrodynamic sufficiently low CE of chlorate (5–6%) is observed
electrolysis conditions. It should be noted that the at the electrolysis of 1.0 M NaCl under the current
time spent by the anode in the reduced state increases reversal conditions on Ti/Pt. Compared to standard
as the intensity of mixing of the solution increases electrolysis, an increase in CE of ClO– is almost
1.8 1 2 3
1.7
1.6 4
1 2 3
E / V (vs. Ag/AgCl)
E / V (vs. Ag/AgCl)
1.6
1.5
1.4
1.4
1.3
1.2 1.2
Electrolysis of sodium chloride solutions on Ti/Pt anodes under current reversal conditions
40 ISSN 0321-4095, Voprosy khimii i khimicheskoi tekhnologii, 2020, No. 2, pp. 36-43
1.8
0.5
1.7
E / V (vs. Ag/AgCl)
E / V (vs. Ag/AgCl)
2 1 3 4
1.6 0.0
4
1.5
-0.5
1.4 3
2
-1.0 1
1.3
1.2 0 5 10 15 20
0 100 200 300 400
t/s
t/s
Fig. 7. Chronopotentiograms recorded on oxidized Ti/Pt
Fig. 5. Chronopotentiograms recorded on reduced Ti/Pt electrode at jc=–40 mA cm–2 (1), –30 mA cm–2 (2),
electrode at ja=20 mA cm–2 in 0.15 M NaCl. Rotational –20 mA cm–2 (3) and –10 (4) mA cm–2 in 0.15 M NaCl
velocity of mixer (rpm): (1) – 0 (without mixing), (2) – 660,
(3) – 1400 and (4) – 2000 time of the reduced surface to the oxidized state in
0.15 M NaCl is 90 s and 10 s at the current density
of 20 mA cm–2 and 40 mA cm–2, respectively. The
0.5 electrolysis in reverse polarity mode at 20 mA cm–2
4 with a minute period of current direction reversal
E / V (vs. Ag/AgCl)
Table 3
Current efficiencies of NaClO and NaClO3 at electrolysis of 0.15 M NaCl at Ti/Pt electrodes in different modes
Table 4
Current efficiencies of NaClO and NaClO3 at electrolysis of 0.3 M NaCl at Ti/Pt electrodes in different modes
and low CE of chlorate (5%) were observed in the usual mode at 20–40 mA cm –2 , the CE of
reverse polarity mode with 300-second reverse time. hypochlorite does not exceed 26 and the CE of
Thus, the electrolysis in reverse polarity mode allows chlorate is at least 21%. Carrying out the electrolysis
solving the problem of chlorate accumulation during in reverse mode allows increasing the CE of
the synthesis of sodium hypochlorite for medical hypochlorite up to 39% while reducing the CE of
and veterinary purposes by electrolysis of isotonic chlorate to 5%. An increase in the concentration of
0.9% NaCl solutions on Ti/Pt electrodes. NaCl to 0.3 M improves the performance of reverse
An increase in the concentration of sodium electrolysis even more significantly. In this case, CE
chl oride in the initial sol utio n to 0.3 M of ClO– reaches 78% and CE of ClO3– decreases to
simultaneously with electrolysis in reverse polarity 2%.
mode on Ti/Pt allows obtaining high-purity solutions Thus, platinized titanium electrodes with
of sodium hypochlorite with a CE of the target 2 mg cm –2 platinum content can be used in
product up to 78% and practically free of chlorates diaphragmless flow and accumulative electrolysis cells
(Table 4). for the electrolysis of low concentration NaCl
Conclusions solutions in order to obtain highly pure NaClO
The electrolysis of 1 M NaCl solutions on a solutions. In this case, the electrolysis must be carried
previously reduced surface of Ti/Pt in diaphragmless out under the current reversal conditions, the period
electrolysis cells allows synthesizing sodium of which is determined in accordance with the
hypochlorite with the current efficiency of more than specified electrolysis parameters (current density,
80%, the current efficiency associated chlorate being NaCl concentration and hydrodynamic conditions).
less than 10%. The use of these concentrated
solutions is not always advisable. In the course of
electrolysis, the platinum surface gradually transforms REFERENCES
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Estrela C.R.A., Barbin E.L., Spano J.C.E., Marchesan M.A., ÅËÅÊÒÐÎË²Ç ÐÎÇ×ÈͲ ÍÀÒÐ²É ÕËÎÐÈÄÓ ÍÀ Ti/Pt
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ëåí³é ïîâåðõí³ Ti/Pt åëåêòðîäó ñïîñòåð³ãàºòüñÿ ï³äâèùåííÿ
countries / Dell’Era A., Zuccari F., Santiangeli A., Fiori C.,
âèõîäó çà ñòðóìîì ã³ïîõëîðèòó äî 80–85% ³ ìîæëèâå çíèæåí-
Micangeli A., Orecchini F. // Energy Convers. Manag. –2013. – íÿ âèõîäó çà ñòðóìîì õëîðàòó äî 5–8%. Îäíàê òðèâàë³ñòü
Vol.75. – P.446-452. åëåêòðîë³çó íà â³äíîâëåí³é ïîâåðõí³ îáìåæåíèé ³ çíà÷íî çìåí-
5. A review of chlorine evolution mechanism on øóºòüñÿ ç³ çá³ëüøåííÿì ãóñòèíè ñòðóìó. Íåîáõ³äí³ñòü â³äíîâ-
ëåííÿ ïîâåðõí³ ïåðåä êîæíèì åëåêòðîë³çîì ôàêòè÷íî çâîäèòü
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íàí³âåöü ïðàêòè÷íó ö³íí³ñòü íàâåäåíèõ âèùå ðåçóëüòàò³â. Âò³ì,
Yoon J. // Korean Chem. Eng. Res. – 2015. – Vol.53. – P.531- ÷àñ ïåðåõîäó â³äíîâëåíî¿ ïîâåðõí³ â îêèñëåíèé ñòàí çíà÷íî çìåí-
539. øóºòüñÿ â íèçüêî-êîíöåíòðîâàíèõ ðîç÷èíàõ NaCl (íà ïðàêòèö³
6. Cornell À., Hakansson Â., Lindbergh G. Ruthenium based çàçâè÷àé äëÿ îäåðæàííÿ ðîç÷èí³â ã³ïîõëîðèòó ïðÿìèì áåçìåì-
áðàííèì åëåêòðîë³çîì âèêîðèñòîâóþòüñÿ ðîç÷èíè 0,15–0,45 Ì
DSA in chlorate electrolysis–critical anode potential and reaction
NaCl). Òàê, íàïðèêëàä, ÷àñ ïåðåõîäó ñòàíîâèòü 1200 ñ â
kinetics // Electrochim. Acta. – 2003. – Vol.48. – P.473-481. 0,3 Ì ðîç÷èí³ ³ ò³ëüêè 80 ñ â 0,15 Ì çà 20 ìÀ ñì-2. Á³ëüø òîãî,
7. Adams B., Tian M., Chen A. Design and electrochemical ìîæíà â³äìîâèòèñÿ â³ä ïðîöåäóðè ïîïåðåäíüîãî îáðîáëåííÿ àíîäà
study of SnO2-based mixed oxide electrodes // Electrochim. Acta. ³ çä³éñíþâàòè åëåêòðîë³ç áóäü-ÿêî¿ òðèâàëîñò³ íà â³äíîâëåí³é
ïîâåðõí³, ïðîâîäÿ÷è åëåêòðîë³ç â ðåæèì³ ðåâåðñóâàííÿ ñòðóìó.
– 2009. – Vol.54. – P.1491-1498.
ßêùî çä³éñíþâàòè åëåêòðîë³ç 0,15 Ì NaCl â çâè÷àéíîìó ðå-
8. Active Ti/SnO2 anodes for pollutants oxidation prepared æèì³ çà 20–40 ìÀ ñì–2, òî âèõ³ä çà ñòðóìîì ã³ïîõëîðèòó íå
using chemical vapor deposition / Yao P., Chen X., Wu H., ïåðåâèùóº 26%, à âèõ³ä çà ñòðóìîì õëîðàòó ñòàíîâèòü íå ìåíøå
Wang D. // Surf. Coat. Tech. – 2008. – Vol.202. – P.3850-3855. 21%. Çä³éñíåííÿ åëåêòðîë³çó â ðåâåðñèâíîìó ðåæèì³ äîçâîëÿº
ï³äâèùèòè âèõ³ä çà ñòðóìîì ã³ïîõëîðèòó äî 39% ç³ çíèæåííÿì
9. On the electrolysis of dilute chloride solutions: Influence
âèõîäó çà ñòðóìîì õëîðàòó äî 5%. Çá³ëüøåííÿ êîíöåíòðàö³¿
of the electrode material on Faradaic efficiency for active chlorine, NaCl äî 0,3 Ì çíà÷íî ïîêðàùóº ïðîäóêòèâí³ñòü ðåâåðñèâíîãî
chlorate and perchlorate / Neodo S., Rosestolato D., Ferro S., åëåêòðîë³çó. Ó öüîìó âèïàäêó âèõ³ä çà ñòðóìîì ClO– çá³ëüøóºòü-
De Battisti A. // Electrochim. Acta. – 2012. – Vol.80. – P.282- ñÿ äî 78%, à âèõ³ä çà ñòðóìîì ClO3– çìåíøóºòüñÿ äî 2%.
291. Êëþ÷îâ³ ñëîâà: ïëàòèíà, ïëàòèíîâàíèé òèòàí, àíîä,
íàòð³þ ã³ïîõëîðèò, õëîðàò, ðåâåðñèâíèé åëåêòðîë³ç, ðåâåðñ
10. Czarnetzki L., Janssen L.J.J. Electrochemical oxidation
ñòðóìó.
of hypochlorite at platinum anodes // Electrochim. Acta. – 1988.
– Vol.33. – P.561-566.
11. Electrochemical chlorine evolution at rutile oxide (110) ELECTROLYSIS OF SODIUM CHLORIDE SOLUTIONS
ON Ti/Pt ANODES UNDER CURRENT REVERSAL
surfaces / Hansen H.A., Man I.C., Studt F., Abid-Pedersen F.,
CONDITIONS
Bligaard T., Rossmeisl J. // Phys. Chem. Chem. Phys. – 2010. –
Vol.12. – P.283-290. D. Girenko, O. Shmychkova, A. Velichenko *
12. Girenko D.V., Velichenko A.B. Synthesis of low Ukrainian State University of Chemical Technology, Dnipro,
Ukraine
concentration solutions of sodium hypochlorite in an electrolyzer
with undivided electrode space // Voprosy Khimii i Khimicheskoi
*
e-mail: [email protected]
Tekhnologii. – 2018. – No. 4. – P.82-91. An increase in the current efficiency of hypochlorite up to
80–85% and a possible decrease in the current efficiency of chlorate
13. Electrodeposition of Ni 2+ -doped PbO 2 a nd
up to 5–8% are observed if the electrolysis of NaCl occurs on a pre-
physicochemical properties of the coating / Shmychkova O., reduced Ti/Pt electrode surface. However, the time of the electrolysis
Luk’yanenko T., Amadelli R., Velichenko A. // J. Electroanal. on a reduced surface is limited and significantly decreases with
Chem. – 2016. – Vol.774. – P.88-94. increasing current density. The need for the reduction of the surface
every time before the electrolysis almost negates the practical value
14. Girenko D.V., Gyrenko A.A., Nikolenko N.V.
of the above results. The duration of the transition from the reduced
Potentiometric determination of chlorate impurities in surface to the oxidized state can be appreciably decreased in low-
hypochlorite solutions // Int. J. Anal. Chem. – 2019. – Vol.2019. concentrated solutions of NaCl (0.15–0.45 M NaCl solutions are
– Article No. 2360420. commonly used in practice to prepare hypochlorite solutions by direct
membraneless electrolysis). For instance, the duration of the transition
15. Girenko D.V., Velichenko A.B. Selection of the optimal
is 1200 s and only 80 s in 0.3 M and in 0.15 M solutions, respectively
cathode material to synthesize medical sodium hypochlorite (at 20 mA cm–2). Moreover, it becomes possible to refuse the procedure
solutions in a membraneless electrolyzer // Surf. Eng. Appl. of the pre-treatment of the anode and conduct the electrolysis at any
Electrochem. – 2018. – Vol.54. – P.88-95. duration on the reduced surface under current reversal conditions. If
the electrolysis of 0.15 M NaCl is performed in a «usual» regime at
20–40 mA cm–2, then the current efficiency of hypochlorite does not
Received 26.11.2019 exceed 26% and the current efficiency of chlorate is at least 21%. It
is shown that carrying out the electrolysis under current reversal
conditions allows increasing the current efficiency of hypochlorite up
to 39% while reducing the current efficiency of chlorate to 5%. An
increase in the concentration of NaCl to 0.3 M improves the
performance of reverse electrolysis even more significantly. In this
case, the current efficiency of ClO– formation increases to 78% and 9. Neodo S., Rosestolato D., Ferro S., De Battisti A. On
the current efficiency of ClO3– formation decreases to 2%. the electrolysis of dilute chloride solutions: influence of the
electrode material on Faradaic efficiency for active chlorine,
Keywords: platinum; platinized titanium; anode; sodium
hypochlorite; chlorate; reverse polarity electrolysis; reverse current. chlorate and perchlorate. Electrochimica Acta, 2012, vol. 80,
pp. 282-291.
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Chemistry, 2019, vol. 2019, article no. 2360420.
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based DSA® in chlorate electrolysis–critical anode potential and 15. Girenko D.V., Velichenko A.B. Selection of the optimal
reaction kinetics. Electrochimica Acta, 2003, vol. 48, pp. 473-481. cathode material to synthesize medical sodium hypochlorite
solutions in a membraneless electrolyzer. Surface Engineering and
7. Adams B., Tian M., Chen A. Design and electrochemical
Applied Electrochemistry, 2018, vol. 54, pp. 88-95.
study of SnO2-based mixed oxide electrodes. Electrochimica Acta,
2009, vol. 54, pp. 1491-1498.
Electrolysis of sodium chloride solutions on Ti/Pt anodes under current reversal conditions