CN107142496A - Active masking liquid of a kind of internal layer and preparation method thereof - Google Patents
Active masking liquid of a kind of internal layer and preparation method thereof Download PDFInfo
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- CN107142496A CN107142496A CN201710229449.9A CN201710229449A CN107142496A CN 107142496 A CN107142496 A CN 107142496A CN 201710229449 A CN201710229449 A CN 201710229449A CN 107142496 A CN107142496 A CN 107142496A
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- internal layer
- masking liquid
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/097—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds comprising two or more noble metals or noble metal alloys
Abstract
The invention discloses active masking liquid of a kind of internal layer and preparation method thereof, internal layer activity masking liquid includes solvent, solute and stabilizer, and the solvent is made up of n-butanol, isopropanol, and the solute is made up of ruthenium trichloride, chloro-iridic acid, butyl titanate and analysis oxygen killer；Concentration of metal ions in the active masking liquid of the internal layer is 0.3 0.4mol/L, and solvent is 10 with stabilizer volume ratio:1.It can promote that hypochlorite generator's electrode oxygen evolution potential is high, analysis oxygen speed is small, the active masking liquid of electrode life length internal layer the invention provides a kind of.Another object of the present invention is to provide a kind of preparation method of the active masking liquid of internal layer, the preparation method step is simple, easily operation, is easy to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of hypochlorite generator's electrode, and in particular to a kind of active masking liquid of internal layer and its preparation side
Method.
Background technology
With the continuous shortage of the constantly contaminated and water resource of water resource on the earth, sterilization water process seems more and more heavier
Will, sodium hypochlorite is prepared in situ compared with other disinfection technologies, it is with the obvious advantage, but hypochlorite generator's electricity in the market
Pole service life is short, and equipment occurs as soon as the situation of electrode failure in operation 1-2 or so, so that replacing electricity out of service of having to
Pole, therefore, electrode failure not only increase the cost of equipment, and have delayed the normal operation of hypochlorite generator, cause
Huge economic loss.The basic reason of electrode failure is that electrode oxygen evolution potential in electrolytic process is too low, analyses oxygen excessive velocities,
The oxygen of generation readily penetrates through coating and generates nonconducting TiO with titanium-based precursor reactant2, so that matrix passivation, electrode failure.
The content of the invention
In order to overcome the deficiencies in the prior art, hypochlorite generator can be promoted it is an object of the invention to provide one kind
Electrode oxygen evolution potential is high, analysis oxygen speed is small, the active masking liquid of electrode life length internal layer.
Another object of the present invention is to provide a kind of preparation method of the active masking liquid of internal layer, preparation method step letter
Single, easily operation, is easy to large-scale industrial production.
Realize that the purpose of the present invention can reach by adopting the following technical scheme that：
A kind of active masking liquid of internal layer, including solvent, solute and stabilizer, the solvent are made up of n-butanol, isopropanol, institute
Solute is stated to be made up of ruthenium trichloride, chloro-iridic acid, butyl titanate and analysis oxygen killer；Metal in the active masking liquid of the internal layer from
Sub- concentration is 0.3-0.4mol/L, and solvent is 10 with stabilizer volume ratio:1.
Preferably, n-butanol, the mass ratio of isopropanol are 2 in the solvent:1.
Preferably, the stabilizer is concentrated hydrochloric acid.
Preferably, the analysis oxygen killer by antimony containing compounds, containing chromium compound, cerium-containing compound, cobalt compound, contain
Two or more composition in iron compound.
Preferably, in the active masking liquid of the internal layer, by metal ion molar percent, the gold in solution shared by ruthenium ion
Category ion ratio is 16-23mol%, and metal ion in solution ratio shared by iridium ion is 9-15mol%, solution shared by titanium ion
Middle metal ion ratio is 61-74mol%, and metal ion in solution ratio shared by analysis oxygen killer is 2-4mol%.
Preferably, in the active masking liquid of the internal layer, by metal ion molar percent, the gold in solution shared by ruthenium ion
Category ion ratio is 21mol%, and metal ion in solution ratio shared by iridium ion is 12mol%, GOLD FROM PLATING SOLUTION shared by titanium ion
Category ion ratio is 66mol%, and metal ion in solution ratio shared by analysis oxygen killer is 4mol%.
Preferably, the analysis oxygen killer is made up of antimony containing compounds, cerium-containing compound, iron containing compoundses, analyses oxygen inhibition
In agent, antimony ion, cerium ion, the mol ratio of iron ion are 23:9:8.
The present invention also provides a kind of preparation method of the active masking liquid of internal layer, comprises the following steps：
1) prepare solvent, solute and raw material needed for stabilizer, prepare solvent, solute respectively by proportioning standby；
2) solute is sequentially added in solvent, fully after dissolving, then stabilizer is poured into, be well mixed, you can.
The beneficial effects of the present invention are：
1st, the present invention provides a kind of internal layer active masking liquid, and internal layer activity masking liquid is main by solvent, solute and stabilizer structure
Into the active masking liquid of the internal layer is incorporated into hypochlorite generator's electrode, hypochlorite generator's electrode can be significantly improved
Oxygen evolution potential, analysis oxygen speed and service life；
2nd, the analysis oxygen killer in solute of the invention is by antimony containing compounds, containing chromium compound, cerium-containing compound, containing cobalt
Two or more composition in compound, iron containing compoundses；Electrode precipitation of oxygen in electrolytic process is primarily due to electricity
Contain substantial amounts of Lacking oxygen in the coating of pole in metal oxide lattice, the OH produced with electrolysis water-Ions binding generates oxygen, by
In Sb5+、Cr6+Valence state is than Ru in electrode coating4+、Ir4+Valence state is high, works as RuO2Lattice or IrO2Two Ru in lattice4+Or Ir4+
During substitution, in order to keep charge balance, a Lacking oxygen is eliminated, therefore, and the analysis oxygen ability of electrode dies down；By Ce3+/Ce4+、
Co2+/Co3+、Fe2+/Fe3+It is doped to Deng variable valency metal in electrode material, the precipitation of oxygen in electrolytic process can be reduced.Ce makees
It is exactly to store up oxygen function for one of most important performance of catalyst aid, this performance gains is in Ce3+/Ce4+This redox couple
Conversion process, the process can change with the Lacking oxygen of oxide crystal, and the change of the Lacking oxygen can adsorb electrolysis water generation
OH-In active oxygen, so as to limit the precipitation of oxygen；Therefore, electrode of the invention analysis oxygen killer can significantly improve secondary
The oxygen evolution potential of sodium chlorate electrode, reduction analysis oxygen speed, improve electrode life；
3rd, the preparation method of the active masking liquid of internal layer of the invention, the preparation method step is simple, easily operation, is easy to big rule
Mould industrialized production.
Brief description of the drawings
Fig. 1 is incorporated into the scanning electron microscopy structure of hypochlorite generator's electrode for the active masking liquid of internal layer of embodiment 1
Figure.
Embodiment
Below, with reference to embodiment, the present invention is described further：
A kind of active masking liquid of internal layer, including solvent, solute and stabilizer, the solvent is made up of n-butanol, isopropanol, molten
N-butanol, the mass ratio of isopropanol are 2 in agent:1, the solute is by ruthenium trichloride, chloro-iridic acid, butyl titanate and analysis oxygen inhibition
Agent is constituted, and analysis oxygen killer is by antimony containing compounds, containing in chromium compound, cerium-containing compound, cobalt compound, iron containing compoundses
Two or more composition, stabilizer is concentrated hydrochloric acid；Concentration of metal ions in the active masking liquid of the internal layer is 0.3-
0.4mol/L, solvent is 10 with stabilizer volume ratio:1.
Antimony containing compounds are more than one or both of Antimony pentachloride, antimony pentafluoride, sodium antimonate.
It is more than one or both of chromic nitrate, chromium sulfate, sodium chromate containing chromium compound.
Cerium-containing compound is more than one or both of cerium chloride, cerous nitrate, cerous sulfate, cerous carbonate.
Cobalt compound is more than one or both of cobalt nitrate, cobaltous sulfate, cobalt chloride, cobalt carbonate.
Iron containing compoundses are more than one or both of ferrous nitrate, ferrous sulfate, frerrous chloride.
In internal layer activity masking liquid, by metal ion molar percent, the metal ion ratio in solution shared by ruthenium ion
For 16-23mol%, metal ion in solution ratio shared by iridium ion is 9-15mol%, metal ion in solution shared by titanium ion
Ratio is 61-74mol%, and metal ion in solution ratio shared by analysis oxygen killer is 2-4mol%.
A kind of preparation method of the active masking liquid of internal layer, comprises the following steps：
1) prepare solvent, solute and raw material needed for stabilizer, prepare solvent, solute respectively by proportioning standby；
2) solute is sequentially added in solvent, fully after dissolving, then stabilizer is poured into, be well mixed, you can.
Embodiment 1
A kind of active masking liquid of internal layer, including solvent, solute and stabilizer, solvent is made up of n-butanol, isopropanol, in solvent
N-butanol, the mass ratio of isopropanol are 2:1, stabilizer is concentrated hydrochloric acid, solute by ruthenium trichloride, chloro-iridic acid, butyl titanate and
Oxygen killer composition is analysed, analysis oxygen killer is made up of Antimony pentachloride, cerous nitrate；Internal layer activity masking liquid in concentration of metal ions be
0.32mol/L, solvent is 10 with stabilizer volume ratio:1.
In internal layer activity masking liquid, by metal ion molar percent, the metal ion ratio in solution shared by ruthenium ion
For 17mol%, metal ion in solution ratio shared by iridium ion is 9mol%, and metal ion in solution ratio is shared by titanium ion
72mol%, metal ion in solution ratio shared by analysis oxygen killer is 3mol%, each ion molar content, and antimony ion is
2.5mol%, cerium ion is 0.5mol%.
Embodiment 2
A kind of active masking liquid of internal layer, including solvent, solute and stabilizer, solvent is made up of n-butanol, isopropanol, in solvent
N-butanol, the mass ratio of isopropanol are 2:1, stabilizer is concentrated hydrochloric acid, solute by ruthenium trichloride, chloro-iridic acid, butyl titanate and
Oxygen killer composition is analysed, analysis oxygen killer is made up of chromium sulfate, cobalt carbonate；Internal layer activity masking liquid in concentration of metal ions be
0.34mol/L, solvent is 10 with stabilizer volume ratio:1.
In internal layer activity masking liquid, by metal ion molar percent, the metal ion ratio in solution shared by ruthenium ion
For 19mol%, metal ion in solution ratio shared by iridium ion is 11mol%, metal ion in solution ratio shared by titanium ion
For 68mol%, metal ion in solution ratio shared by analysis oxygen killer is 3mol%, each ion molar content, antimony ion
For 2.2mol%, cobalt ions is 0.8mol%.
Embodiment 3
A kind of active masking liquid of internal layer, including solvent, solute and stabilizer, solvent is made up of n-butanol, isopropanol, in solvent
N-butanol, the mass ratio of isopropanol are 2:1, stabilizer is concentrated hydrochloric acid, solute by ruthenium trichloride, chloro-iridic acid, butyl titanate and
Oxygen killer composition is analysed, analysis oxygen killer is made up of sodium antimonate, chromium sulfate, cerium chloride；Metal ion in internal layer activity masking liquid
Concentration is 0.36mol/L, and solvent is 10 with stabilizer volume ratio:1.
In internal layer activity masking liquid, by metal ion molar percent, the metal ion ratio in solution shared by ruthenium ion
For 21mol%, metal ion in solution ratio shared by iridium ion is 12mol%, metal ion in solution ratio shared by titanium ion
For 66mol%, metal ion in solution ratio shared by analysis oxygen killer is 4mol%, each ion molar content, antimony ion
For 2.1mol%, chromium ion is 1.3mol%, and cerium ion is 0.6mol%.
Embodiment 4
A kind of active masking liquid of internal layer, including solvent, solute and stabilizer, the solvent is made up of n-butanol, isopropanol, molten
N-butanol, the mass ratio of isopropanol are 2 in agent:1, stabilizer is concentrated hydrochloric acid, and the solute is by ruthenium trichloride, chloro-iridic acid, metatitanic acid
Four butyl esters and analysis oxygen killer composition, analysis oxygen killer are made up of antimony pentafluoride, cerium chloride, ferrous sulfate；Internal layer activity masking liquid
In concentration of metal ions be 0.38mol/L, solvent and stabilizer volume ratio are 10:1.
In internal layer activity masking liquid, by metal ion molar percent, the metal ion ratio in solution shared by ruthenium ion
For 21mol%, metal ion in solution ratio shared by iridium ion is 12mol%, metal ion in solution ratio shared by titanium ion
For 66mol%, metal ion in solution ratio shared by analysis oxygen killer is 4mol%, each ion molar content, antimony ion
For 2.3mol%, cerium ion is 0.9mol%, and iron ion is 0.8mol%.
Experimental example：
The active masking liquid of embodiment 1-4 internal layer is incorporated into hypochlorite generator's electrode, sodium hypochlorite is tested
The oxygen evolution potential of device electrode, potential difference, the influence of reinforcing life.
Experimental procedure is as follows：
(1) use the titanium plate that Ti content 99.9%, thickness are 1mm as matrix, titanium plate sandblasting is polished and removes removing oxide layer
Afterwards, it is placed in the NaOH solution that concentration is 10% and shakes 30min, then titanium plate is carried out for 20% oxalic acid solution with concentration
2h is etched, is placed in after cleaning stand-by in ethanol solution；
(2) the active masking liquid of internal layer is prepared：With n-butanol：Isopropanol=2：1 mixed solution is as solvent, with tri-chlorination
Ruthenium, chloro-iridic acid, butyl titanate, analysis oxygen killer are solute, using concentrated hydrochloric acid as stabilizer, are configured to the active masking liquid of internal layer；
Wherein, the active masking liquid of internal layer that the active masking liquid of internal layer is embodiment 1-4；
(3) the active masking liquid of the internal layer of configuration is coated on the Titanium base by pretreatment, be put into 150 in thermostatic drying chamber
DEG C dry 15min after, be put into Muffle furnace in 450 DEG C of air atmospheres sinter 10min after take out be cooled to room temperature, repetitive coatings 20
It is secondary；Coated sample is finally sintered into 60min at 450 DEG C, room temperature is cooled to the furnace；
(4) test oxygen evolution potential, potential difference, reinforcing life.
Comparative example
In addition, for the performance of the active masking liquid of the internal layer for verifying the present invention, also setting up comparative example, comparative example step is as follows：
(1) use the titanium plate that Ti content 99.9%, thickness are 1mm as matrix, titanium plate sandblasting is polished and removes removing oxide layer
Afterwards, it is placed in the NaOH solution that concentration is 10% and shakes 30min, then titanium plate is carried out for 20% oxalic acid solution with concentration
2h is etched, is placed in after cleaning stand-by in ethanol solution；
(2) the active masking liquid of internal layer is prepared：With n-butanol：Isopropanol=2：1 mixed solution is as solvent, with tri-chlorination
Ruthenium, chloro-iridic acid, butyl titanate are solute, using concentrated hydrochloric acid as stabilizer, are configured to active coating solution；
(3) the active masking liquid of the internal layer of configuration is coated on the Titanium base by pretreatment, be put into 150 in thermostatic drying chamber
DEG C dry 15min after, be put into Muffle furnace in 450 DEG C of air atmospheres sinter 10min after take out be cooled to room temperature, repetitive coatings 20
It is secondary；Coated sample is finally sintered into 60min at 450 DEG C, room temperature is cooled to the furnace；
(4) test oxygen evolution potential, potential difference, reinforcing life.
Test result is as shown in table 1：
Each electrode measurement Contrast on effect of table 1
From table 1, comparative example is compared with embodiment 1-4, the oxygen evolution potential of the electrode of comparative example, potential difference, reinforcing longevity
Life is respectively less than embodiment 1-4 electrode, it can be seen that, the active masking liquid of internal layer of the invention is incorporated into hypochlorite generator's electrode
In, oxygen evolution potential, potential difference, the reinforcing life of hypochlorite generator can be remarkably promoted；In embodiment 1-4, embodiment 4 is
Optimum embodiment.
Reference picture 1, the scanning electron for the hypochlorite generator's electrode being incorporated into by the active masking liquid of the internal layer of embodiment 1 shows
Micro-structural figure can be seen that electrode coating even compact, and crackle is seldom, therefore the oxygen evolution activity point of coating is seldom, and oxygen
Cause electrode failure it is difficult to permeate into, so that electrode analyses oxygen rate reduction, electrode life extension.
For those skilled in the art, technical scheme that can be as described above and design, make other each
It is kind corresponding to change and deform, and all these change and deformation should all belong to the protection model of the claims in the present invention
Within enclosing.
Claims (8)
1. the active masking liquid of a kind of internal layer, it is characterised in that including solvent, solute and stabilizer, the solvent is by n-butanol, isopropyl
Alcohol is constituted, and the solute is made up of ruthenium trichloride, chloro-iridic acid, butyl titanate and analysis oxygen killer；The active masking liquid of the internal layer
In concentration of metal ions be 0.3-0.4mol/L, solvent and stabilizer volume ratio are 10:1.
2. the active masking liquid of internal layer according to claim 1, it is characterised in that the matter of n-butanol, isopropanol in the solvent
Amount is than being 2:1.
3. the active masking liquid of internal layer according to claim 1, it is characterised in that the stabilizer is concentrated hydrochloric acid.
4. the active masking liquid of internal layer according to claim 1, it is characterised in that the analysis oxygen killer by antimony containing compounds,
Containing two or more composition in chromium compound, cerium-containing compound, cobalt compound, iron containing compoundses.
5. the active masking liquid of internal layer according to claim 1, it is characterised in that in the active masking liquid of the internal layer, by metal from
Metal ion ratio in sub- molar percent, solution shared by ruthenium ion is 16-23mol%, GOLD FROM PLATING SOLUTION shared by iridium ion
Category ion ratio is 9-15mol%, and metal ion in solution ratio shared by titanium ion is 61-74mol%, is analysed shared by oxygen killer
Metal ion in solution ratio is 2-4mol%.
6. the active masking liquid of internal layer according to claim 1, it is characterised in that in the active masking liquid of the internal layer, by metal from
Metal ion ratio in sub- molar percent, solution shared by ruthenium ion is 21mol%, GOLD FROM PLATING SOLUTION shared by iridium ion belong to from
Sub- ratio is 12mol%, and metal ion in solution ratio shared by titanium ion is 66mol%, GOLD FROM PLATING SOLUTION shared by analysis oxygen killer
Category ion ratio is 4mol%.
7. the active masking liquid of internal layer according to claim 6, it is characterised in that the analysis oxygen killer by antimony containing compounds,
In cerium-containing compound, iron containing compoundses composition, analysis oxygen killer, antimony ion, cerium ion, the mol ratio of iron ion are 23:9:8.
8. a kind of preparation method of the active masking liquid of internal layer according to claim 1, it is characterised in that comprise the following steps：
1) prepare solvent, solute and raw material needed for stabilizer, prepare solvent, solute respectively by proportioning standby；
2) solute is sequentially added in solvent, fully after dissolving, then stabilizer is poured into, be well mixed, you can.
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Application publication date: 20170908 |