July 19, 1960 F. D.

GIBSON, JR 2,945,791
INERT LEAD DIOXIDE ANODE AND PROCESS OF PRODUCTION
Filed March 5, 1958 3. Sheets-Sheet l
Pb(NO3)2
Cu(NO3)2·3H2O
FIG. I. Ni(NO3)2'6HO
H2O
Hect

Heot Hydrophilic Colloid

Lead Dioxide
Effluent Anode

n-Amyl Alcohol Neutralizing Tank Lead Oxide

DeCont Underflow

Distillotion Cake To Wolste

Clean And Neutro

Hydrophilic Colloid Residue

ind Woter
Cooling Wo Condenser |
To Wolste

INVENTOR
Fred D. Gibson, Jr.

34.72% e/ ATTORNEY
 July 19, 1960 F. D. GIBSON, JR 2,945,791
INERT LEAD DIOXIDE ANODE AND PROCESS OF PRODUCTION
Filed March 5, 1958 3. Sheets-Sheet 2

INVENTOR
Fred D. Gibson, Jr.

BY Joy
ATTORNEY
July 19, 1960 F. D. GIBSON, JR 2,945,791
INERT LEAD DIOXIDE ANODE AND PROCESS OF PRODUCTION
Filed March 5, 1958 3. Sheets-Sheet 3

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INVENTOR
Fred D. Gibson, Jr.

ATTORNEY
 United States Patent Office 2,945,791
Patented July 19, 1960

2
bon electrode using a specifically formulated lead nitrate
electrolyte and a certain sequence of operating conditions.
Heretofore, lead dioxide has been deposited from lead
2,945,791 nitrate electrolytes on base substrate materials such as
INERTLEADDIoxIDE ANODE AND PROCESS platinum, platinum clad tantalum, and tantalum for use
OF PRODUCTION as anodes. In other instances, attempts have been made
to electrodeposit lead dioxide on conductors such as
Fred D. Gibson, Jr., Box 797, Henderson, Nev. graphite. Such attempts in the production of anodes
Filed Mar. 5, 1958, Ser. No. 719,224 have not been successful because of the lack of the ad
O herence of the lead dioxide deposit to the graphite anode,
11. Claims. (C. 204-57) the weak structure of the deposit, and the lack of com
plete coverage of the deposit over the graphite anode.
I have discovered that all of these difficulties in de
positing lead dioxide from lead nitrate electrolytes can be
My invention relates to the electrodeposition of lead 15 overcome by varying the current density of the anode
dioxide (PbO), and more particularly to the electro from a high of 75 to 150 amperes per square foot for the
deposition of lead dioxide in such a form and on such a first one to five hours of electrodeposition to a low of 20
base substrate material as to be usable as an insoluble to 60 amperes per square foot for the remaining hours
anode in certain electrolytic processes. of electrodeposition. The cathode current densities should
In the past, lead dioxide has been electrodeposited from . 20 be about 1.5 to 3 times the corresponding anode cur
solutions containing lead salts, but invariably these de rent densities. In depositing the lead dioxide coating on
posits were not suited for electrochemical use as an inert graphite, it is desirable that the edges of the anodes be
or insoluble anode because they suffered from one or rounded as sharp points or angular edges tend to form
more of the following defects: (a) the lead dioxide deposit trees or nodules of the coating. Before starting, it is ad
was non-uniform and non-adherent to the electrode sur 25 vantageous to have present in the lead nitrate aqueous
face; (b) the lead dioxide coating was too porous and electrolyte about 4 grams per liter of free nitric acid, as
too coarse; (c) the lead dioxide deposit would not with this improves the throwing power or coverage of the
stand the normal abuse associated with the routine han anode. In addition, it dissolves sodium fluoride in the
dling in the commercial plant; and (d) the active life of electrolyte. The graphite electrode should be soaked in
the electrode was drastically shortened due to excessive 30 water for about 24 hours before immersion in the elec
anode plate corrosion particularly above the solution level trolyte. A graphite electrode is normally quite porous
at the electrical bus connection. and these pores are filled with air. By soaking in water,
The consistent lack of reliability of lead dioxide coat preferably preceded by vacuum treatment, any contained
ings and the expense involved in their preparation has air and gas is displaced by the water, thus inhibiting the
compelled the industry to use platinum anodes which rep 35 formation of pinholes in the lead dioxide coating.
resent a considerable original investment, suffer from When installed in the electrolyte, all wires are con
"platinum losses in processing, and the platinum anodes nected to the graphite substrate before the electrode is
require a high power input and manifest a lower efficiency immersed in the electrolyte and the current is immediately
, than that obtained by the anodes of my invention. turned on to avoid any battery action which might cause
One of the principal objects of my invention is to pro 40 an undesired deposit on the graphite anode. The elec
vide a process for the production of tenacious, adherent, trolyte should be agitated to wipe any adhering bubbles
: uniform, stress-resistant lead dioxide coatings on carbon off of the graphite base. The voltage employed will de
and graphite electrodes of various shapes which do not pend on the amount of applied current and may vary
manifest the defects of prior processes. from 1.9 to 3.5, using an acid lead nitrate bath as an
Another object of my invention is to provide an inert 45 electrolyte. The electrical connection is made directly
and insoluble anode which can be successfully used in to the graphite base plate above the solution level. By
the electrolytic production of chlorine, chlorates and per proceeding as above outlined, a lead dioxide deposit is
chlorates from aqueous solutions without deterioration produced having the characteristics of a fine crystalline,
. . of the anode: or contamination of these electrochemical
products. randomly oriented structure, hard smooth surface, high
50 tensile strength, and strong adherence to the graphite or
It is an object of the present invention to provide a carbon base substrate. The lead dioxide coated graphite
process for the electrodeposition of lead dioxide from an anode can be used directly in the electrolytic production of
aqueous solution containing lead nitrate on a base sub chlorine, chlorates or perchlorates without any further
strate material such as graphite or carbon, treatment.
It is a further object of the present invention to pro 55 For the purpose of the present invention, the lead ni
vide such a process wherein the lead dioxide is electro trate bath may be prepared as follows: Anhydrous lead
deposited in such a form as to be usable as an insoluble nitrate is dissolved in water to produce a liter of an
anode in certain electrolytic processes and more particu aqueous solution having a concentration of 200 grams of
larly the electrolytic production of sodium chlorate, sodi lead nitrate per liter of solution. The aqueous solution
um perchlorate and chlorine. 60 also contains the following compounds in the following
It is a still further object to provide a process for the concentrations: 10 grams per liter of cupric nitrate: 10
preparation and control of aqueous solutions used in the grams per liter of nickelous nitrate; 0.75 gram per liter
electrodeposition of lead dioxide. of a surface active agent of the alkyl phenoxy polyoxy
These and other objects of my invention are achieved ethelene ethanol class; 0.50 gram per liter of sodium fluo
65 ride; 4 grams per liter of nitric acid.
by depositing lead dioxide on a prepared graphite or car This bath will produce the desired dense type of PbO
 2,945,791
3 4.
coated graphite electrode. The cathode may be made of trical connections 9 and 10 lead to a power source for
a suitable metal such as copper, stainless steel, nickel, the Supply current to the anode 1 and cathodes 2, re
platinum or the like. It is advisable to deposit the PbO2 spectively. For agitating the electrolyte there is a glass
in one operation without current interruption. In addi enclosed magnet 5 operated by a 110 volt magnet motor 6.
tion, it has been found that moderate agitation of the Referring to Fig. 2, the cell arrangement is the same
electrolyte aids in the production of complete coverage as shown in Fig. 3. For feeding nitrate solution to the
of the anode and reduces the nodulation. Nodular de cell tank 4 there is a feed solution tank 12 with a valved
posits are undesirable and my process produces few, if pipe 13 discharging solution into the cell tank 4. For
any, nodular deposits. The PbO2 deposit will be found discharging solution from the cell tank 4 to a neutralizing
to be compact, hard, dense, smooth, tenacious, adherent tank 14, there is a siphon 5 which discharges into a pipe
to the electrode, and the crystals will be randomly i6 and then into the tank 14. An agitator 17 is op
oriented. erated by the motor 18. The amyl alcohol 19 separates
Satisfactory coatings have been used having thickness out and is decanted through the siphon 20 to a still for
from about a thirty-second of an inch to about one-half reuse and for removal to waste of the surface active
an inch. I prefer a coating thickness of about a sixteenth 5 agent residue. The underflow from tank 14 is returned
to three-sixteenths of an inch. to the system through a pipe 21 to a filter 23 by a force
The function of the surface active agent is to raise the pump 22. The filtered neutral solution is returned to
oxygen overvoltage at the anode, inhibit gassing and in the feed tank 12 for delivery to the cell tank 4.
prove the throwing power of the nitrate bath, resulting The flow sheet Fig. 1 with legends represents the se
thereby in a compact lead dioxide deposit. Without the 20 quence and character of operations as just described with
surface active agent, the lead dioxide deposit tends to be respect to Fig. 2. . . .
Spongy and porous. It functions in the same manner as Referring to Figs, 3 and 5, there is shown one form
natural hydrophilic colloids such as gelatine, dextrine, of cathode in which annealed copper wire 2a is wound
gum arabic, soluble starch, etc. across a plexiglass supporting plate 2b. Other forms of
During the electrodeposition of the lead dioxide, the 25 well known similar cathodes may be used and are readily
surface active agent in the electrolyte is altered as the available. Apertures 2c in the plate 2b and 1a in the
result of electrolysis in the presence of nitric acid. These graphite anode receive rods for supporting the anode and
altered products interfere with electrodeposition resulting cathode in proper position in the cell tank 4. The angu
in time in a porous, non-adherent, non-uniform lead di lar edges of the graphite anode are rounded at 1b and
30 the bottom end 1c is cut in a half circular shape.
oxide plate and ultimately the total lack of deposition.
A part of this difficulty can be overcome by allowing the The following Examples I and II illustrate my process
neutralized cell effluent to stand neutral for more than for production of a lead dioxide anode.
24 hours before reuse. This allows a portion of the EXAMPLE I
altered products to recombine in the original form of the 35 A liter of aqueous electrolyte was prepared containing
surface active agent. However, this treatment is not com the following compounds in the concentration shown for
pletely effective and over a period of time certain of the each:
permanently altered products build up in concentration Grams per liter
to a point where the solution is not usable and must be
thrown away. 40
Pb(NO3)2 ---------------------------------- 200
In order to maintain the plating solution so that it will Cu(NO3)2.3H2O ----------------------------- 10
consistently produce close textured crystalline smooth Ni(NO3)2.6H2O ----------------------------- 10
PbO2 coats completely covering the graphite or carbon NaF --------------------------------------- 5
anode, I have found that the solution can be regenerated Surface active agent -------------------------- .75
as it leaves the cell as effluent by treating it with a small HNOs -------------------------------------- 4.
45
amount of n-amyl alcohol, i.e., about one liter of alcohol This solution was contained in a cell tank and heating
for four liters of solution and adding sufficient lead oxide and agitation of the solution was started. On reaching
to neutralize the contained nitric acid. The alcohol re a temperature of 72° C., a graphite anode and copper
moves substantially all of the residual surface active cathodes were installed and electrodeposition started. The
agent and its altered products and permits unlimited re anode was prepared for electrodeposition by smoothing
use of the solution. When the solution is allowed to and cleaning with sandpaper, followed by soaking in dis
stand, the surface active agent and its altered products tilled water for 24 hours. The edges of the graphite base
being immiscible with the solution, stratify out and can were rounded and the bottom end cut in a half-circular
be removed by decantation. In starting electrodeposition shape. Electrical connection was made to both electrodes
of the lead dioxide with a freshly prepared solution, and 55 before immersion in the electrolyte.
on return of the regenerated solution to the cell, a fresh Feed solution was started at the same instant electro
amount, as above specified, of the surface active agent deposition was initiated and was continuous thereafter at
is added to the solution. The solubility of the amyl alco a rate sufficient to maintain an acid concentration of ap
hol in the nitrate bath is about 1% by weight. proximately 4 grams per liter and a lead nitrate concen
Reference is made to the drawings for a more com 60 tration of approximately 190 grams per liter. The feed
plete disclosure of the invention in which Solution was neutralized effluent from a previous run, free
Fig. 1 is a flow sheet of a complete cyclic operation; of Surface active agent and containing approximately
Fig. 2 is a diagrammatic elevation of a plant arrange 1.15% by weight of n-amyl alcohol. Along with the
ment; neutralized feed solution sodium fluoride and surface
Fig. 3 is a vertical section of a cell for depositing lead 65 active agent were added at the rate of .5 gram and .75
dioxide; gram respectively per liter of feed solution.
Fig. 4 is a diagrammatic top plan view of a cell of the Effluent from the cell was neutralized with lead oxide
type showing in Fig. 3; and thoroughly mixed with n-amyl alcohol. On settling,
Fig. 5 is a diagrammatic vertical section at right an the alcohol containing substantially all of the surface
gles to Fig. 3, showing the cathode in fragmentary form. 70 active agent and altered products separated from the ni
Referring to Figs. 3 and 4, is the graphite anode and trate Solution. This alcohol layer was decanted and then
2 are the cathodes. For controlling the temperature of distilled to recover the alcohol. The cleaned neutral so
the electrolyte 7 there are submerged 110 volt electric lutions containing approximately 1% by weight of al
resistance heaters 3. Reference numeral 8 indicates the cohol was filtered and returned to the electrolytic cell as
level of the electrolyte 7 in the cell tank 4. Suitable elec 76 feed solution and the above cycle repeated.
 5 6
-Table I covered with a smooth, compact, firmly adherent layer
OPERATING CONDITIONs of EXAMPLE I of lead dioxide free of cracks and pinholes.
Electrolyte: The use of my PbO graphite anodes in the electro
Pb(NO3)2....
9NO).3HO chemical production of chlorine, chlorates and perchlo
Ni(NO)6HO rates is illustrated in the following Examples III, IV
See active ag and V. - . .
EXAMPLE I
"Aode: 136" x 30 untreated graphite, surface cleaned, edges rounded, The lead dioxide coated graphite anode, prepared as
tried Solution 21'giving available plating area of approximately
C., inches. above, was used as an anode in the electrolysis of an
Cathode: Two sections each containing 2064 dia, soft annealed copper O aqueous sodium chlorate solution to produce a sodium
Wire Wound across 7.5'x 24' Plexiglas
area of approximately 142 sq. in. plates so as to give an immersed perchlorate solution. Subsequent to the electrodeposi
9ell:12' diax 24' high Pyrexiar tion of the lead dioxide and before use in this operation
Spacing: 2' between cathode surface and anode surface
Temperature: 729-82 C. no further treatments of any kind were made to the
"Feed solution: anode. The same electrical connection to the uplated
Pb(NO3)2.----------------------------------------------gipil. 200 5 top portion of the graphite base was utilized in both
9(NO3)2.3H2O. ---g.pl.- 10 the electrodeposition of the lead dioxide and the electrol
Ni(NO3)2.6H2O.----------------------------....- - - - - E. 10
n-Amlalcohol.-------------------- -Percent by weight ysis of the sodium chlorate solution.
'Additives: -
Surface active agent of alkyl phenoxy polyoxyethelene ethanol A nearly. Saturated aqueous solution of sodium chlo
rate was prepared from technical grade sodium chlorate.
. 5 20
class-------------------------------------- - - - - - - - - - -gipl.- .75
NF--------------------------------------------------gip.l.. The solution was purified of chromate by precipitation
with barium chloride and filtered. Approximately .5
Current density------ 1st 60 min..... Next 90 min.
Anode........... 101 Amps.) 50.5 Amps.)
Next 180 min.
24 Arnps.f gp.l. of NaF was added to inhibit cathode reduction.
Sq. ft. sq. ft. sq.ft. The electrolysis was carried out in a 12' dia. x 24'
Cathode.------...- 213 Ampsi 106.5 Amps.1 high Pyrex jar in which the anode and two type 316
50.6Amps.f

|
-
' -- ... Y't
Applied current
Voltage-----
"Feed rate
sq. ft.
- 210 Amps
3.5---
108 cc.
2.38---
54 cc.fm
Sq. ft.
105 Amps
sq. ft.
50 Amps.
25
stainless steel cathodes were immersed. The electrolyte
was cooled by water flowing thru glass coils placed with
in the cell. The electrolyte was agitated by means of
magnetic stirrer. During the first 6 hours of electrolysis
Current efficiency: 98%
Time: 5.5 hours 30. hydrochloric acid was added in order to maintain a pH
At the end of 5% hours electrodeposition was stopped. of 5.0electrolysis
to 6.8. No further acid additions were required.
The anode was removed from the cell and thoroughly The was stable and continuous and continued
washed with water to remove the drag-out. That por until the electrolyte was nearly free of chlorate. The
lead dioxide coated graphite was untouched and unat
tion of the graphite immersed in the plating solution was tacked and no contaminants were transferred to the sodi
found to be completely covered with a very smooth, 35
compact, finely crystalline, firmly adherent layer of lead um perchlorate therefrom. The external electrical con
nection was preserved and no difficulty was indicated at.
dioxide free of cracks and nodules. - that point. The cumulative current efficiency of 75.5%
EXAMPLE II was greater than the 60 to 70% usually encountered in
I proceeded as in Example I, above, except that neither 40 commercial sized platinum anode perchlorate cells. The
average voltage of 4.75 was also considerably lower than
the electrolyte nor the feed solution contained n-amyl
alcohol. The anode was a 3’ diameter by 14' long the usual 6.5 to 6.9 recorded in platinum anode perchlo
rate cells.
rod of untreated graphite with the lower end rounded in Table III
a spherical shape.
Table II OPERATING CONDITIONS OF EXAMPLE III
45. Electrolyte:
OPERATING CONDITIONS OF EXAMPLE.II Initially
Electrolyte:
Pb(NO3)2------------------------- 200
'CCNO3)2.3H2O.-------.
Ni(NO3)2.6H2O.--
10()
Surface active agent .75 50
'ENO 4.
NaF. .5
Anode: 3’ dia. x 14' long graphite rod, 9.5' immersed. Effective area NaF.-- 5
approximately 90 sq. in. Anode: Lead dioxide coated graphite produced in Example I-20'.
Cathode: 273' x.064' dia. soft annealed copper wire strung vertically immersed. Effective area approximately 285 square inches.
between two 7' dia. Plexiglas plates (birdcage effect) to give an effec Cathodes: Two type 316 stainless steel sheets each 8' x 22' immersed.
tive area of approximately 55 sq. in. Effective area approximately 166 square inches each.
55 Spacing:
Cell:12' dia. x 12' high Pyrexiar 112 inch between cathode surface and anode surface
Spacing: '2' between cathode surface: and anode surface Cell: 12' dia. 24' high Pyrex jar
Woltage: 4.75
Temperature: 73°-92 C.
Feed solution: Applied current: 285 amperes
Pb(NO3)2-----------------------------------------------g.p.l.. 200 Current density:
g.p.l.-- 10 Anode:------------------------------------------amp.fsq. in--
Ni(NO3)2.6E20---------------------- sar saw - - narra a w n n n ing.p.l.. 10
60 Cathode----------------------------------------amp./sq. in... .86
Additives: Cumulative current:
Efficiency------------------'m a ri was a saw as ses - w - a - - - - aspercent. 75.5
Surface active agent of alkylphenoxy polyoxyethelene ethanol Time--------------------------------------------------hours.- .4
class--------------------------------------------------g.p.l ,75
NaF---------- l ,5 pH: 5.0–6.8
Temperature: 38-45 C.
Applied current....... 1st 3 hrs. 55 Amps.... Last 3 hrs. 35 Amps. 65 EXAMPLE IV
Current density:
Anode.-------------
Cathode -
88 Amps.fsq. ft.--------
158 Amps.sq. ft -
56 Amps.fsq. ft.
101 Amps. Iso.ft. The lead dioxide coated graphite anode prepared as
...Voltage----- --3:--------- 2.35 above was used as an anode in the electrolytic produc
Feed rate------------- 33 ccfmini---- -- 20 cc/min. tion of sodium chlorate from a sodium chloride solution.
As in Example III, no further treatments of any kin
Current efficiency: 95% 70 were made to the anode before this use.
Time: 6 hours
An aqueous solution was prepared from technical grade
At the end of electrodeposition the anode was removed Sodium chloride and sodium chlorate with a composition
from the cell and thoroughly washed with water to re of approximately 450 grams per liter sodium chlorate
move the drag-out. That portion of the graphite im and 90 grams per liter sodium chloride. ...5 gram per
mersed in the electrolyte was found to be completely 75 liter sodium fluoride was added to inhibit cathode reduc
 2,945,791
7 8
tion. The cell and auxiliary equipment used in the pre Having thus described my invention, what I claim as
vious example were also utilized for this operation. The new and desire to secure by Letters Patent is:
concentration of sodium chloride in this electrolyte was 1. In the process of electro-depositing a lead dioxide
not permitted to go below 80 grams per liter. The elec coating on a graphite anode, the electrolyte consisting
trolyte composition was regulated by continuously re essentially of an aqueous acid solution of lead nitrate
moving sodium chlorate from the bath by concentration in a conceneration, and at a temperature that will deposit
by evaporation and selective crystallization, and return - lead dioxide on the graphite anode and a surface active
ing the depleted solution for electrolysis. An amount agent, the improvement comprising varying the anode
of salt equivalent to the sodium chlorate removed was current density for at least two successive periods of
added to the recirculated solution. A pH of 6.0 to 6.8 10 electro-deposition, the anode current density varying from
was maintained by the periodic addition of HCl. about 75 to 150 amperes per square foot for the prior
Table IV period of electro-deposition to about 20 to 60 amperes
per square foot for the succeeding period of electro
OPERATING CONDITIONS OF EXAMPLE IV deposition, to completely cover the graphite anode with a
Feed solution: 15 compact, hard, dense, smooth coating having randomly
oriented crystals firmly bound to the graphite base.
2. The process of claim 1, in which the cathode current
density is about 1.5 to 3 times the corresponding anode
current density.
20 3. The process of claim 1, which produces a lead di
Anode: Same as in Example III. oxide coating having a thickness from about a thirty
Dathode: Same as in Example III.
Spacing: Same as in Example III. second of an inch to about one-half an inch.
Cell: Same as in Example III. 4. The process of claim 1, in which the lengths of
Voltage: 4.0.
Applied current: 285 amperes
Current density: Sane as in Example III. the periods of time of electro-deposition vary, the length
pH: 6 to 6.8. 25 of the prior period of time being substantially shorter
Temperature: 38° to 45° C. than the length of the succeeding period of time.
Current efficiency: 90%--. 5. The process of claim 1, in which the lengths of
No perceptible attack or loss of lead dioxide was ob - the periods of time of electro-deposition are about the
served after prolonged use. In this operation the anode Sac
current density was five times as great as that obtainable 30 6. The process of claim 1 in which the current density
with a graphite anode and in addition there was no of the anode varies from about 75 to 150 amperes per
destruction and hence no graphite or lead compounds square foot for the first one to five hours of electro
were transferred to the electrochemical sodium dioxide deposition to a low of about 20 to 60 amperes per square
product. foot for the remaining hours.
EXAMPLE V 35 7. The process of claim 1 in which the surface active
The anode prepared as above was used as an anode agent is of the alkyl phenoxy polyoxyethylene ethanol
in the electrochemical production of chlorine from a so class.
dium chloride solution. A saturated solution of sodium 8. The process of claim 1 in which the spent solution
chloride was used as an electrolyte. The anode and 40 is regenerated by dissolving therein about 1% by weight
cathode compartments were separated by an asbestos of n-amyl alcohol.
diaphragm and each compartment was sealed from the air 9. The process of claim 4, in which the anode current
by Plexiglas covers. Chlorine formed at the anode was density of the prior period of electrodeposition is about
drawn off and absorbed in caustic soda. Hydrogen and twice that of the succeeding period of electro-deposition.
caustic were formed at the cathode. The caustic soda 10. The process of claim 5, in which the current den
was continuously removed as a 14% solution. This 45 sity of the prior period of electro-deposition is about
effluent from the cathode chamber was replaced by an one and a half times that of the succeeding period of
equivalent volume of salt solution which percolated thru electro-deposition.
the diaphragm from the anode chamber. This salt so 11. An anode for use with corrosive electrolytes hav
lution was in turn replaced by fresh feed to the anode 50 ing a graphite base, and having electrolytically deposited
chamber. A temperature of approximately 95 C. was thereon a massive coating of lead dioxide completely
maintained in the cell by means of two quartz type im covering the immersible active portion of the anode, the
mersion heaters. Periodic inspection of the lead diox coating being smooth, compact, hard, firmly bound to
ide anode showed both the plate and the graphite to be the base, with randomly oriented crystals and produced
unattacked and unchanged. by the process of claim 1.
Table V References Cited in the file of this patent
OPERATING CONDITIONS OF EXAMPLE W
UNITED STATES PATENTS
Electrolyte: Saturated sodium chloride solution
Anode: Same as in Example IV 2,846,378 Hoffman --------------- Aug. 8, 1958
Cathode: 2 sections 4' thick 6' x 24' iron sheets im 60 2,872,405 Miller et al. ------------ Feb. 3, 1959
mersed 20'. Effective area 120 sq. inches each. FOREIGN PATENTS
Cell: Same as in Example IV with the addition of an
asbestos diaphragm located between the anode and 456,082 Great Britain ------------ Nov. 3, 1936
cathodes.
Spacing: Same as in Example IV 65 OTHER REFERENCES
Applied current: 143 amperes
Voltage: 3.0 "Journal of the Electrochemical Society,' vol. 105
Current density: 0.5 ampere per square inch (February 1958), pages 100-101; and vol. 104 (July
Current efficiency: 98% 1957), pages 448-449.
Temperature: 95° C. 70