Anode for oxygen release

FIELD: electricity.

SUBSTANCE: anode for oxygen release at high surge voltage comprises substrate from valve metal or ceramics, the first intermediate layer on the basis of valve metals oxides applied onto specified substrate, the second intermediate layer of platinum applied onto specified first intermediate layer, and outer layer that substantially consists of tin, copper and antimony oxides, besides specified second intermediate layer of platinum comprises from 10 to 24 g/m2 of platinum.

EFFECT: electrode made according to invention may be used as anode in treatment of sewage waters.

23 cl, 1 dwg, 1 ex

 

This invention relates to anodes for oxygen evolution at high overvoltage in aqueous solutions, for example, for the destruction of organics in wastewater. Anodic oxygen is a very common reaction when total water treatment and, in particular, in the processing of wastewater, when the content of organic or biological substances must be reduced to extremely low levels. The efficiency of the resulting oxygen in relation to the destruction of organic substances depends primarily on the anode potential of the selection, which should be as high as possible, preferably without having to use excessively high current densities. The benefits of oxygen evolution at high potential at the anode according to the invention can be used in other industrial processes, for example, in the field of organic electrosynthesis; however, the oxidation of organic impurities in aqueous solutions undoubtedly represents the most widespread and economically most important species of its application.

Anodes for oxygen evolution at high strain according to the prior art traditionally receive on ceramic substrates, for example based on tin dioxide, variously modified by other elements of the AMI, mainly in order to impart sufficient electrical conductivity; usually used for this purpose, the material is lead dioxide. Geometric constraints substrates of this type have led, however, to the development of electrodes with a high oxygen overvoltage on the basis of valve metals, which in the preferred version contains a substrate of titanium or a titanium alloy, a protective ceramic intermediate layer, for example, on the basis of the oxides of titanium and tantalum, and an outer layer with a low catalytic activity, in which the tin dioxide again represents the main component, usually in a mixture with other elements such as copper, iridium and antimony; an electrode of this kind, also includes auxiliary catalytic layer containing mainly the oxides of tantalum and iridium, disclosed in example 6 in WO 03/100135. Although the electrode according to WO 03/100135 able to provide attractive initial characteristics at the specified application because it produces oxygen at a potential slightly higher than 2 V At currents of 100 a/m2in sulfuric acid solution, and its service life is very unsatisfactory. In fact, even if the above-mentioned anode provided with an outer layer with a low catalytic activity, under normal industrial operating conditions, the potential of oxygen evolution who meet the tendency to suddenly drop for several hundred hours, together with the decrease in the efficiency of removal of organic impurities. Moreover, from the description of WO 03/100135 can immediately conclude that the method of manufacturing discussing electrode is very challenging for large-scale production due to the fact that it is necessary to apply a large number of alternating layers of two different precursors (in the given example - ten successive layers, each of the two layers of coating).

The aim of the present invention to provide an anode for oxygen evolution operating at high strain, approximately more than 2V (relative to the standard hydrogen electrode, BOO), at current densities not exceeding a few hundred a/m2to overcome limitations of the prior art while providing a longer service life in industrial environments.

Another objective of the present invention is to develop a method of making an anode for oxygen evolution at high strain characterized by simple applicability in industry.

According to the first aspect of the invention is the anode, obtained on a ceramic substrate or, preferably, on a substrate of titanium, titanium alloy or other valve metals, containing the first protective intermediate layer is the oxide of a valve metal, known in the art, the second protective intermediate layer based on a noble metal and an outer layer containing oxides of tin, copper and antimony.

In one preferred embodiment, the implementation of a substrate of titanium or titanium alloy, is activated in accordance with the invention, pre-attach a suitable profile roughness, for example, sandblasting and subsequent etching with sulfuric acid.

In another preferred embodiment, the first intermediate layer contains a mixture of titanium oxide and tantalum; in another preferred embodiment, the second intermediate layer on the basis of the noble metal includes platinum, more preferably in a quantity in the range between 10 and 24 g/m2.

The outer layer contains oxides of tin, copper and antimony, optionally in combination with other elements. The content of tin is preferably in the range between 5 and 25 g/m2the content of antimony is in the range between 0.4 and 2 g/m2and the copper content is in the range between 0.2 and 1 g/m2; in an even more preferred variant of realization of the tin is present in amount of at least 90% by weight of the total content of all metals.

According to another aspect of the invention lies in the method of manufacturing an anode for separation of oxygen is at high strain, includes sequential deposition of the first protective intermediate layer based on an oxide of a valve metal, a second intermediate layer on the basis of the noble metal and the outer layer containing the oxides of tin, copper and antimony, on a substrate made of ceramics or a valve metal. In one preferred implementation, the substrate made of titanium or titanium alloy, pre-treated to make it suitable profile roughness, for example, sandblasting followed by etching with sulfuric acid, as disclosed in 03/076693. However, there are other kinds of processing, for example, heat treatment or processing a stream of plasma or etching other corrosive reagents. In one preferred embodiment, the first intermediate layer is obtained by deposition precursors, for example, chlorides of titanium and tantalum, and their subsequent thermal decomposition, for example, between 450 and 600°C; the coating precursors can be carried out, as known in the art, through a variety of individual or combined methods, such as spraying, brush application or the application roller. In one preferred embodiment, the second intermediate layer receive thermal decomposition hexachloroplatinic acid in temp is the temperature of 400-600°C, in practice, however, can also be used and other forms of deposition of noble metals, for example, by electroplating techniques. When forming the second intermediate layer composition can be included predecessors and other precious metals, but particularly preferred is the presence of platinum.

In one particularly preferred variant of the implementation of the external layer is applied using a single solution containing the precursors of the oxides of tin, copper and antimony, for example, corresponding chlorides. This solution is applied in accordance with the prior art and preferably decompose between 450 and 600°C.

The anode according to the invention is able to release oxygen at high overpotential, i.e. at a potential of approximately 2 V (BOO), at current densities of several hundred a/m2and has a much longer lifetime than the lifetime of the anode according to WO 03/100135 or other anodes according to the prior art. Without the intention to connect the present invention to any specific theory, it can be assumed that in the case of WO 03/100135 anode has a tendency to the formation of cracks or fractures in the coating that exposes some areas, which, despite their limited extent, have a high content of iridium Il is the same in any case, significantly lower oxygen overvoltage. In the case of the anode according to the invention the possible formation of cracks or faults would lead to the exposure of rich platinum sites at which the overvoltage of the oxygen is still quite high.

The explanation of this kind seems reasonable data and shown in the accompanying figure.

The drawing shows polarization curves related to the release of oxygen at the anode according to the invention.

In particular, the curves in the drawing relate to the oxygen in the sodium sulfate at pH 5 and 25°C.

(1) the curve denotes the polarization related to the anode according to the invention; (2) - polarization curve related to the anode according to the invention, equipped with only two intermediate layers respectively on the basis of the oxides of titanium and tantalum and platinum-based; (3) curve of polarization related to the anode, provided with only a first intermediate layer on the basis of the oxides of titanium and tantalum and an outer layer on the basis of oxides of iridium and tantalum. In fact, the curve (2) simulates the behavior of the anode according to the invention, in which the outer layer of oxide of tin, copper and antimony has been completely destroyed, while curve (3) simulates the situation when the total destruction of the outer layer of the anode according to WO 03/100135.

The invention will be further explained by the example in no way intended to limit its scope, defined solely by the attached claims.

EXAMPLE

Titanium sheet mark 1 in accordance with ASTM B 265 size 45 cm × 60 cm and a thickness of 2 mm was subjected to blasting with corundum and protravel 25%sulfuric acid containing 10 g/l of dissolved titanium at a temperature of 87°C. this sheet was applied a solution containing the chlorides of titanium and tantalum, at a concentration of 0,11M Ti and 0,03M Ta, by electrostatic spraying, followed by rolling with a roller. The solution was applied in four stages to obtain the total gain applied material 0.87 g/m2with drying between one application stage and the next at 50°C for 10 min and then performing thermal decomposition at 520°C for 15 minutes

Thus was obtained the first intermediate layer, to which was applied a second intermediate layer consisting of 20 g/m2platinum. The application was carried out in three stages, causing the brush hexachloroplatinum acid, dispergirovannoyj in eugenol and subjecting to thermal decomposition, each layer of the coating for 10 minutes at 500°C.

Finally, put the outer layer, based on the solution of the chlorides of tin(IV) (94% by weight calculated on the total content of all metals), copper(II) (2% by weight calculated on the total content of all metals) and antimony (4% by weight calculated on the total retained the e all metals). The application was done with a brush in 16 stages, with cycles of drying at 50°C and decomposition at 520°C after application of each coating layer.

Thus obtained electrode according to the invention was tested on polarization when the oxygen in the sodium sulfate at pH 5 and 25°C; the results are presented in figure 1 as the curve marked (1). Figure 1 also shows the data on polarization, obtained under the same conditions with equivalent electrode that does not have the outer layer, and the electrode provided with the equivalent of the first intermediate layer and outer layer, containing 24 g/m2oxides of tantalum (35 mass%) and iridium (65 mass%). These data are presented on the curves, denoted respectively as (2) and (3).

In conclusion, the electrode according to the invention was subjected to the accelerated test of the life in which he had been exploited in conditions of oxygen evolution in sulfuric acid with a concentration of 150 g/l at 60°C and at a current density of 20 kA/m2. After 500 hours of such accelerated tests were measuring the potential of oxygen evolution in the sodium sulfate at pH 5 and 25°C at a current density of 500 A/m2: the measured potential was the result equal to 2.15 In (BOO). The anode produced in accordance with WO 03/100135 subjected to the same test, showed the potential of oxygen evolution of 1.74 In (BOO) under the same conditions.

<> As is obvious to a person skilled in the technical field this invention can be implemented in practice by other variations or modifications in relation to the presented examples.

The preceding description is not intended to limit the invention, which may be applied in accordance with different implementations without deviating from its scope and the volume of which is uniquely determined by the attached claims.

Everywhere in the description and claims of this application, the terms "include" and "comprise" and variations such as "may contain" and "contains", " does not imply the exclusion of the presence of other elements or additional components.

1. Anode for oxygen evolution at high strain containing a substrate of a valve metal or ceramic, the first intermediate layer on the basis of oxides of valve metals, deposited on said substrate, a second intermediate layer of platinum deposited on said first intermediate layer and the outer layer essentially consisting of oxides of tin, copper and antimony, in fact the second intermediate layer of platinum contains from 10 to 24 g/m2platinum.

2. The anode according to claim 1, in which said substrate of a valve metal made of titanium or a titanium alloy.

3. The anode according to claim 2, in which amanuta substrate of titanium or titanium alloy has a roughness profile, controlled through treatment, containing etching with sulfuric acid, which is not necessarily preceded by sandblasting.

4. The anode according to claim 1, in which the first mentioned intermediate layer contains oxides of titanium and tantalum.

5. The anode according to any one of the preceding paragraphs, in which the mentioned outer layer contains from 5 to 25 g/m2tin, from 0.4 to 2 g/m2antimony and from 0.2 to 1 g/m2copper.

6. The anode according to claim 5, in which the tin is present in said outer layer in an amount of not less than 90% by weight of the total content of all metals.

7. Anode for oxygen evolution at high strain containing a substrate of a valve metal or ceramic, the first intermediate layer on the basis of oxides of valve metals, deposited on said substrate, a second intermediate layer of platinum deposited on said first intermediate layer and the outer layer essentially consisting of oxides of tin, copper and antimony, in fact the outer layer contains from 5 to 25 g/m2tin, from 0.4 to 2 g/m2antimony and from 0.2 to 1 g/m2copper.

8. The anode according to claim 7, in which said substrate of a valve metal made of titanium or a titanium alloy.

9. The anode of claim 8, in which said substrate of titanium or titanium alloy has a roughness profile, controlled through the processing, containing etching with sulfuric acid, which is not necessarily preceded by sandblasting.

10. The anode according to claim 7, in which the first mentioned intermediate layer contains oxides of titanium and tantalum.

11. The anode according to claim 7, in which the aforementioned second intermediate layer of platinum contains from 10 to 24 g/m2platinum.

12. The anode according to claim 7, in which the tin is present in said outer layer in an amount of not less than 90% by weight of the total content of all metals.

13. A method of manufacturing an anode for oxygen evolution at high strain according to any one of claims 1 to 12, comprising applying a first intermediate layer based on an oxide of a valve metal on a substrate of a valve metal or ceramic, applying a second intermediate layer of platinum on said first intermediate layer, and the application of the outer layer containing the oxides of tin, copper and antimony.

14. The method according to item 13, in which said substrate is a substrate of titanium or titanium alloy with controlled roughness profile obtained sandblasting and subsequent etching with sulfuric acid.

15. The method according to item 13, in which the first mentioned intermediate layer is applied by at least one method selected from spray, brush and roller applications, based on the solution of the chloride is in titanium and tantalum, with subsequent thermal decomposition at a temperature in the range between 450 and 600°C.

16. The method according to any of PP-15, in which the aforementioned second intermediate layer of platinum is applied by thermal decomposition of a solution containing hexachloroplatinic acid, at a temperature in the range between 400 and 600°C.

17. The method according to item 13, in which the mentioned outer layer is applied in several stages, based on the solution containing the chlorides of tin, antimony and copper, followed by thermal decomposition at a temperature in the range between 450 and 600°C.

18. The method according to 14, in which the mentioned outer layer is applied in several stages, based on the solution containing the chlorides of tin, antimony and copper, followed by thermal decomposition at a temperature in the range between 450 and 600°C.

19. The method according to item 15, in which the mentioned outer layer is applied in several stages, based on the solution containing the chlorides of tin, antimony and copper, followed by thermal decomposition at a temperature in the range between 450 and 600°C.

20. The method according to clause 16, in which the mentioned outer layer is applied in several stages, based on the solution containing the chlorides of tin, antimony and copper, followed by thermal decomposition at a temperature in the range between 450 and 600°C.

21. Electrochemical the process, includes anodic oxygen at a potential higher than 2 In (BOO) at the anode according to any one of claims 1 to 12.

22. The process according to item 21, which includes industrial water treatment.

23. The process according to item 22, in which said processing includes removal of organicheskikh molecules from the wastewater.



 

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Electrolyzer // 2252921

FIELD: medical instrument making, namely apparatuses for preparing ecologically safe electrically activated water.

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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