Method of fabrication of electrode for electrolysis of water solutions of alkali metal chlorides

FIELD: metallurgy.

SUBSTANCE: method of fabrication of electrode for electrolysis of water solutions of alkali metal chlorides consists in preliminary treatment of electrode titanium base surface, in application coating onto it, where coating consists of thermo-decomposed compounds of titanium, iridium and ruthenium; further the method consists in their succeeding thermal treatment in oxidising atmosphere and in producing electro-catalytic coating containing oxides of titanium, iridium and ruthenium; also surface of electro-catalytic coating is additionally treated with 20-25% water solution of hydrogen peroxide by means of sputtering it at amount of 80-140 g/m2 and successively heat treated at temperature of 450-480°C.

EFFECT: raised resistance of electrode, increased service life.

5 cl, 4 tbl

 

The invention relates to the field of electrochemical productions, specifically to the technology of the manufacturing process and regeneration economicallyactive electrode used as the anode in the electrolysis of solutions of chlorides of alkali metals, for example upon receipt of chlorine, caustic soda, sodium chlorate, hypochlorite.

Known electrode for electrochemical processes, containing electroconductive base of titanium or tantalum, which is applied to the active coating consisting of oxides of the platinum group metal and a mixture of metal oxides containing titanium oxide, or tantalum and at least one oxide of the alloying metal selected from the group of tin, silver, chromium, lanthanum, aluminum, cobalt, antimony, molybdenum, Nickel, iron, tungsten, vanadium, phosphorus, boron, beryllium, sodium, calcium, strontium, lead, copper, bismuth. The oxide of the alloying metal is taken in an amount of 0.1-50% by weight of titanium dioxide or tantalum pentoxide. The content of the platinum group to the rest of the metal oxide coating is 20:100-85:100. [U.S. patent No. 3948751]. The disadvantage of this electrode is the low resistance of the anodized coating and high stress on the cells.

Known electrode for electrochemical chlorine and alkali, contains the basis of a valve metal coated with AK is active coating of a mixture of oxides of tin, ruthenium and titanium, with ingredients taken in the following ratio, % mol.:

The ruthenium dioxide -15-30
Titanium dioxide -25-55
Dioxide tin -30-60

The active coating of the electrode has a high content of tin, which reduces its catalytic properties. [Patent SU # 1468970].

Known electrode for electrochemical processes, containing current-carrying substrate of the film-forming metal coated with a coating consisting of oxide or mixture of oxides of noble metals: platinum, iridium, rhodium, palladium, ruthenium, rhenium, osmium. The coating may additionally contain an oxide or mixture of oxides of base metals: manganese, lead, chromium, cobalt, iron, titanium, tantalum, zirconium and silicon in amounts of less than 50% by weight of oxide or mixture of oxides of noble metals. [Patent SU # 416925].

The disadvantage of this method of manufacture of the electrode is in its low resistance.

Known electrode for electrolysis of an aqueous solution of a halide of a metal containing conductive base of the valve metal coated on its surface asset of the second mass, containing iridium oxide, an oxide of a valve metal and an oxide of a base metal in the following ingredients mol%.:

The iridium oxide -5-75
Oxide of a valve metal5-70
Oxide of tin -20-70

The base electrode is made of titanium, tantalum, niobium, zirconium, or their alloys. [Patent SU # 1056911]. The operation of the electrode in saline is associated with increased solubility of iridium with its high content and high content of tin oxide affects the electrocatalytic properties of the coating.

Closest to the invention to the technical essence and the achieved result is an electrode for electrolysis of aqueous solutions of alkali metal chlorides containing the base of a valve metal coated with a coating of a mixture of oxides of titanium, iridium and ruthenium. [Patent SU # 1401072]. The disadvantage of this electrode is the lack of resistance of the electrode.

The objective of the invention is the increased resistance of the electrode.

The technical result achieved achieved using the invention is to increase the service life of the electrode.

P the set task is solved by the method of manufacturing the electrode for electrolysis of aqueous solutions of chlorides of alkali metals, which includes pre-processing the surface of the titanium bases electrode, application of a coating of terrorislamic compounds of titanium, iridium and ruthenium, with subsequent heat treatment in an oxidizing atmosphere to obtain electrocatalytic coating containing oxides of titanium, iridium and ruthenium, namely its characteristic, which is that the electrocatalytic surface coating further treated 20-25%aqueous solution of hydrogen peroxide spray it in the quantity of 80-140 g/m2followed by heat treatment at a temperature of 450-480°C.

In addition, the feature of the proposed method is that the heat treatment in an oxidizing atmosphere is carried out at a temperature 370-480°C, and the surface electrocatalytic coating of hydrogen peroxide and its subsequent heat treatment carried out at least once. Furthermore, the electrocatalytic coating contains oxides of titanium, iridium and ruthenium in the following ratio of components (wt%): the titanium oxide - 50-52, iridium oxide - 30-32, the ruthenium oxide - 17-19. And besides, electrocatalytic coating further comprises oxides of tin and cobalt in the following ratio of components (% weight): titanium oxide - 48-51, iridium oxide - 28-31, ruthenium oxide - 16-18, tin oxide - 2-3, cobalt oxide - 05-1,5.

Example

For titanium base electrode, pre-last shot blasting, degreasing and etching, is applied coating solution is a mixed solution of the following terrorislamic components: hexachloroiridium acid, gidrooksilirovania trichloride and titanium.

Coating solution prepared from the original solutions:

An aqueous solution of hydrochloride ruthenium (Ru (OH)Cl3) with a concentration of 120-180 g/l aqueous solution of titanium trichloride (TiCl3) 190-250 g/l and an aqueous solution hexachloroiridium acid with a concentration of 100-150 g/l

Coating solution containing in addition to the above components, compounds of tin and cobalt, obtained by dissolution of the salt in it cobalt dvuhgolosnogo 6-water and salt tin tetrachloride 5-water.

Coating solution is applied on the working surface of the electrode layer by sputtering in an electrostatic field and with the consumption of one layer 33-44 ml/m2, 1.33-1.78 g/m2the basic substance by applying an active coating in the amount 9-12 layers.

After applying each layer, the electrode is subjected to the heated drying air for 5-10 min, and then heat-treated at a temperature of 370-400°With the first 3-4 layer, and subsequent layers at a temperature of 400-480°C.

Multilayer coating the above coating is of astora on the surface of the electrode makes it possible to obtain electrodes with an electrocatalytic coating on the content of oxides of metals: a mixture of oxides of titanium, iridium, ruthenium at a ratio (wt%): 50-52:30-32:17-19, respectively; and a mixture of oxides of titanium, iridium, ruthenium, tin and cobalt at a ratio, wt%: 48-51:28-31:16-18:2-3:0.5 to 1.5, respectively

Next on the working surface of the electrode cause a 20-25%aqueous solution of hydrogen peroxide spray in an amount of 80 to 140 g/m2and conducting heat treatment at a temperature of 450-480°C.

According to the above method of manufacturing the electrode with the application of the active coating was made 6 samples with the same catalytic coating, wt%: TiO2- 51; IrO2- 31; RUO Li2- 18.

Sample 1 after applying the catalytic coating by the above method was not treated with hydrogen peroxide, respectively, did not conduct additional heat treatment.

Sample 2 was treated with hydrogen peroxide once with a subsequent heat treatment.

Sample 3 was treated with hydrogen peroxide with the corresponding heat treatment 2 times, 4 sample 3 times, 5 sample 4 times, 6 sample 5 times.

The resistance of the electrodes (samples) were evaluated for performance durability (definition of weight loss) by the method of variable polarity and amalgamation and measurement of anode potential in the conditions of chlorine electrolysis at different current densities. Characteristic values obtained in the tests are shown in table 1.

The essence of Yoda variable polarity and amalgamation is as follows: the test sample at the current density of 100,000 a/m 2in the sodium chloride solution with a concentration of 300 g/l is subjected to variable anodic and cathodic polarization for 40 minutes and Then the lower electrode 30 with the sodium amalgam with a concentration of 0.2% wt.. After these tests, the electrode is washed in distilled water, dried and determine weight loss

Measuring the potential of the anode is carried out in conditions of chlorine electrolysis, the concentration of sodium chloride solution of 300 g/l, 60°C, pH 3.5 to 4.0, the current density of 5000, 7500 and 10000 a/m2.

Table 1
FeaturesSamples
123456
The potential of the anode under the conditions of electrolysis of NaCl solution at the current density, a/m2
is the
50001,3751,3501,3451,3301,3301,330
75001,3901,3751,3551,3401,3401,340
100001,4151,3901,3701,3501,3501,350
Weight loss electrocatalytic coating, determined by the method of variable polarity at current density of 10000 a/m2and amalgamation in the NaOH solution, mg/cm2
0,450,250,150,090,090,09

In addition, they made a further 12 samples. Composition active coating of fabricated samples corresponds to the data described in table 2.

Table 2
Samples
TiO2(wt%)IrO2% weightRUO Li2% weightSnO2% weightCoOsub> 2% weight
1 and 1* (prototype)51,130,718,2--
2 and 2*52,029,015,04,00
3 and 3*50,030,5of 17.02,00,5
4 and 4*49,529,5of 17.52,51,0
5 and 5*51,028,019,002,0
6 and 6*45,027,015,07,05,0
Samples 1, 2, 3, 4, 5, 6 after application of the active coating is not subjected to the treatment with an aqueous solution of hydrogen peroxide.
Samples 1*, 2*, 3* 4*, 5*, 6* treated with a solution of hydrogen peroxide in a single layer and made further heat treatment.

The resistance of the electrodes (samples) were assessed by wear (on the definition of weight loss) by the method of variable polarity and amalgamation and measurement of anode potential in the conditions of chlorine electrolysis at different current densities. Characteristic values obtained in the tests are shown in tables 3 and 4.

Table 3
Samples
Features123456
The potential of the anode under the conditions of electrolysis of NaCl solution at the current density, a/m2
50001,3751,3951,3801,3751,4001,395
75001,3951,4101,3951,3951,4151,410
100001,4101,4251,4151,4101,4201,425
Weight loss electrocatalytic coating, determined by the method of variable polarity at current density of 10000 a/m2and amalgamation in the NaOH solution, mg/cm2
0,450,480,420.420,500,52

/tr>
Table 4
FeaturesSamples
1*2*3*4*5*6*
The potential of the anode under the conditions of electrolysis of NaCl solution at the current density, a/m2
50001,3651,3901,3701,3601,3851,390
75001,3801,3951,3801,3701,3901,395
100001,3901,411,3951,3851,4001,405
Weight loss electrocatalytic coating, determined by the method of variable polarity at current density of 10000 a/m2and amalgamation in NaOH solution
0,250,320,250,230,350,39

As can be seen from the results, carried out in table 1, the triple surface treatment of the electrode with hydrogen peroxide, followed by additional heat treatment improves the electrocatalytic properties of the anodized coating and, consequently, the operating characteristics of the electrode, subsequent processing does not lead to a significant change in the quality of coverage.

The authors of the proposed technical solution, further studies were commissioned by known methods, in which it is established that the surface of the anode after application of the electrocatalytic coating of hydrogen peroxide with subsequent heat treatment promotes the densification electrocatalytic layer and leads to the exclusion of micro-cracks, porosity and friability of coverage.

The advantage of the proposed method of manufacture of the electrode is the improvement of qualitative characteristics of the electrode: the improvement of wear resistance electrocatalytic coating and reducing the anode potential. Increasing iznosostoikosti coating of the electrode will extend the commercial operation of the electrodes to 24 months.

1. A method of manufacturing the electrode for electrolysis of aqueous solutions of alkali metal chlorides, including pre-processing the surface of the titanium bases electrode, paid the Deposit on her cover of terrorislamic compounds of titanium, iridium and ruthenium with subsequent heat treatment in an oxidizing atmosphere to obtain electrocatalytic coating containing oxides of titanium, iridium and ruthenium, wherein the electrocatalytic surface coating further treated 20-25%aqueous solution of hydrogen peroxide spray it in the quantity of 80-140 g/m2followed by heat treatment at a temperature of 450-480°C.

2. A method of manufacturing the electrode according to claim 1, characterized in that the heat treatment in an oxidizing atmosphere is carried out at a temperature 370-480°C.

3. A method of manufacturing the electrode according to claim 1, characterized in that the surface treatment electrocatalytic coating of hydrogen peroxide and its subsequent heat treatment of the electrode is carried out at least once.

4. A method of manufacturing the electrode according to claim 1, wherein said electrocatalytic coating contains oxides of titanium, iridium and ruthenium in the following ratio of components: titanium oxide 50-52 wt.%; the iridium oxide 30-32 wt.%; the ruthenium oxide 17-19 wt.%.

5. A method of manufacturing the electrode according to claim 1, wherein the electrocatalytic coating further comprises oxides of tin and cobalt in the following ratio, wt.%: oxide titanium 48-51, iridium oxide 28-31, ruthenium oxide 16-18, tin oxide 2-3, cobalt oxide 0.5 to 1.5.



 

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Electrolyzer // 2252921

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SUBSTANCE: electrolyzer includes two electrodes (one electrode of stainless steel and other electrode of carbon); bridge type voltage rectifier; electric circuit plug; membrane; second doubled membrane - cover, for example of tracing paper or canvas; glass vessel; low-resistance voltage divider with taps; array of light emitting diodes with additional resistors whose number corresponds to that of taps; housing of electrolyzer. Plug is connected with inlets of bridge type voltage rectifier; negative outlet of voltage rectifier is connected with electrode of stainless steel. Second positive-polarity outlet of voltage rectifier is connected through low-resistance voltage divider with taps to carbon electrode arranged in second membrane-cover. All cathode ends of light emitting diodes with additional resistors are connected in parallel and they are connected with positive outlet of voltage rectifier; second ends of said diodes are connected with respective taps of low-resistance voltage divider.

EFFECT: possibility for displaying information concerning activation degree of water at preparing it for medical purposes, preparation of ecologically safe anolyte.

2 dwg

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