CN110438527A - The preparation method of the transient metal doped anode containing ruthenium coating - Google Patents
The preparation method of the transient metal doped anode containing ruthenium coating Download PDFInfo
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- CN110438527A CN110438527A CN201910717772.XA CN201910717772A CN110438527A CN 110438527 A CN110438527 A CN 110438527A CN 201910717772 A CN201910717772 A CN 201910717772A CN 110438527 A CN110438527 A CN 110438527A
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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
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
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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
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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
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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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
- C25B11/093—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 at least one noble metal or noble metal oxide and at least one non-noble metal oxide
Abstract
The present invention provides a kind of preparation methods of transient metal doped catalysis electrode containing ruthenium coating, belong to technical field of chlor-alkali industry.The present invention contains RuO by heating preparation first2The masking liquid of nano particle is then respectively adding Cr (NO3)3、Mn(NO3)2Two kinds of common transition salting liquids, and mixing masking liquid even application is finally calcined in Muffle furnace high temperature in the titanium sheet substrate after polishing, ultrasound, etching, can respectively obtain two kinds of ruthenium chromium, ruthenium manganese anodes containing ruthenium coating.By transition metal dopant to RuO2The adjusting of electronic structure and chemical state, change in coating catalytic activity, obtained ruthenium chromium and ruthenium the manganese anode containing ruthenium coating with high analysis chlorine catalytic activity.
Description
Technical field
The invention belongs to technical field of chlor-alkali industry, more specifically, it relates to which a kind of transient metal doped applies containing ruthenium
The preparation method of layer anode.
Background technique
Chlorine industry is very important one of chemical industry, and product sodium hydroxide, chlorine, hydrogen can not only be applied
In chemical industry itself, light industry, metallurgy, petro chemical industry etc. can also be widely used in.It is passed in electrolytic bath for chlorine-alkali industry
The anode material of system is platinum, graphite and metal, but platinum is expensive, graphite and metal poor corrosion resistance；It compares
In these traditional anode materials, coated titanium electrode receives the concern of scholar with high stability, high catalytic activity.Industry at present
On be widely used that in titanium plate coating ruthenium titanium oxide, but that there are still analysis chlorine oxygen evolution potential differences is small, produces chlorine low efficiency
Disadvantage.Therefore, how reducing analysis chlorine reaction overpotential, improving current efficiency is the matter of utmost importance for needing to solve.
In order to improve the catalytic activity of anode material, current research can be divided mainly into the following aspects: apply in ruthenium titanium
Doping other elements form binary or ternary mixed oxide in layer；Middle layer is added and changes electrode structure；Substrate is carried out
Correlation modification etc..102268688 A of Chinese invention patent CN discloses " the ruthenium palladium cobalt coated titanium electrode of tin-antimony interlayer ",
Although the electrode has preferable stability, analysis chlorine oxygen evolution potential difference is small, produces chlorine low efficiency.Chinese invention patent CN
103014752 A disclose a kind of " TiO2The preparation method of nano-tube array load catalyst containing ruthenium coating ", this method is in titanium
On piece is prepared for TiO2Nano-tube array, although high specific surface area increases the analysis chlorine activity of catalyst, the analysis of electrode
Chlorine activity and oxygen evolution activity be while increased, thus its to analyse the variation of chlorine current efficiency little.
Summary of the invention
It is existing to overcome the purpose of the present invention is a kind of open preparation method of the transient metal doped anode containing ruthenium coating
Drawbacks described above existing for technology.
The preparation method of the transient metal doped anode containing ruthenium coating of one kind of the present invention, method and step include:
(1) substrate pretreated
Titanium sheet is successively carried out to thick (500 mesh), thin (2000 mesh) sand paper polishing, to remove the oxidation film of titanium plate surface, and
Successively 10min is ultrasonically treated in acetone, ethyl alcohol, deionized water；The oxalic acid etching solution that mass fraction is 10% is prepared, it will be ultrasonic
After titanium sheet that treated etches 2h in 90 DEG C of etching solution, the titanium sheet substrate with uneven surface can be finally obtained；
(2) preparation of the anode containing ruthenium coating
Masking liquid is coated to step (1) treated on anode substrate surface, metal oxide deposition is 0.25~
0.75mg/cm2；
It will be coated with the anode substrate of anodic coating liquid, dry 15~30min at 100~120 DEG C, then 300~400
DEG C sintering 20~40min, cooled to room temperature；
To guarantee that active coating even application to the surface of basis material, is brushed using above-mentioned step is repeated multiple times
It applies, dry, thermal oxide, brushing amount is 0.02mL/cm each time2, until mother liquor is finished；
Last time is sintered 2~3h at a temperature of 300~400 DEG C after applying and obtains anode containing ruthenium coating；
Preferably, above-mentioned steps 2~10 times repeatedly；
The anodic coating liquid, solvent are water, the component including following mole:
RuO20.02~0.03mol/L
0.001~0.003mol/L of doped metal salt
The doped metal salt is the nitrate of chromium, manganese；
Containing RuO2The preparation of nano particle masking liquid:
In RuCl3The NaOH solution that mass concentration is 20~30% is added in aqueous solution, 80~100 DEG C, preferably 90 DEG C anti-
10~30min, preferably 20min are answered, can be prepared by containing RuO2The masking liquid of nano particle；
RuCl3In aqueous solution, RuCl3Content be 0.01~1mol/L, preferably 0.03~0.05mol/L；
RuCl3The volume ratio of aqueous solution and the NaOH solution are as follows:
RuCl3Aqueous solution: NaOH solution=10~20:1, preferably 15:1；
Contain RuO for what doping metals salting liquid addition step (1) obtained2In the masking liquid of nano particle, it can be obtained described
Anodic coating liquid；
In the doping metals salting liquid, the content of doped metal salt is 0.01~1mol/L, preferably 0.03~
0.05mol/L；
Doping metals salting liquid with contain RuO2The volume ratio of the masking liquid of nano particle are as follows:
Doping metals salting liquid: contain RuO2Masking liquid=1:10~20 of nano particle, preferably 1:15；
The present invention disadvantage high for the chlorine evolution potential of existing coated electrode, provides a kind of method of containing transition metal
For improving traditional catalysis electrode containing ruthenium coating, prepared it is several have excellent performance it is transient metal doped containing ruthenium coating electricity
Pole effectively reduces the analysis chlorine overpotential of electrode.
It is prepared first containing RuO2The solution of nano particle, then Cr (NO is added thereto respectively3)3、Mn(NO3)2Two kinds are not
Same transition metal salt solution, and masking liquid even application will be mixed on titanium-base, metal oxygen is then formed by thermal oxidation method
Compound is simultaneously doped to containing in ruthenium coating, the analysis chlorine catalytic activity of last test coated electrode.The transition metal wherein adulterated can be with
The formation of bonding structure between ruthenium and oxygen is interfered, RuO is adjusted2Electronic structure and chemical state, thus promoted in coating
Catalytic activity.
The present invention mainly has the advantage that
(1) by a kind of simple method by transient metal doped to containing in ruthenium coating, the presence of transition metal can have
Effect ground changes RuO2The electronic structure of coating reduces analysis chlorine and reacts overpotential, improves catalytic activity.
(2) by two kinds of common transient metal doped and its catalytic performance detections, metal-doped to others have
Directive function is significant.The method of the present invention is simple and easy, safe operation, is mixed using two kinds of transition metal prepared by the present invention
Miscellaneous catalysis electrode containing ruthenium coating can efficiently reduce analysis chlorine reaction overpotential, improve current density, can be used as chlorine industry
Analysis chlorine anode.
Detailed description of the invention
Fig. 1 is that the ruthenium chrome coating electrode of different metal oxides deposition analyses the linear volt-ampere curve of chlorine reaction.Wherein, positive
Pole liquid is the NaCl aqueous solution of saturation, and catholyte is the NaOH aqueous solution of 5mol/L, cathode chamber and E.I.Du Pont Company, anode chamber
N2010 cation-exchange membrane separates.Coated anode obtained is working electrode, and Pt and saturated calomel electrode are respectively as to electrode
And reference electrode, test temperature are 25 DEG C, scanning speed 20mV/s.It is 0.25mg/ that I, which is metal oxide deposition, in Fig. 1
cm2Ruthenium chrome coating anode；It is 0.50mg/cm that II, which is metal oxide deposition, in Fig. 12Ruthenium chrome coating anode；III in Fig. 1
It is 0.75mg/cm for metal oxide deposition2Ruthenium chrome coating anode.
Fig. 2 is that the linear volt-ampere by the analysis chlorine reaction of catalysis electrode containing ruthenium coating of different transient metal doped front and backs is bent
Line.A is without transient metal doped anode containing ruthenium coating in Fig. 2；B is ruthenium chrome coating anode in Fig. 2；C is ruthenium manganese coating in Fig. 2
Anode.
Fig. 3 is that current density reaches 10mA/cm2When the corresponding chlorine evolution potential comparison diagram of each catalysis electrode.A is nothing in Fig. 3
Transient metal doped anode containing ruthenium coating；B is ruthenium chrome coating anode in Fig. 3；C is ruthenium manganese coated anode in Fig. 3.
Specific embodiment
Embodiment 1
(1) substrate pretreated
Titanium sheet is successively carried out to thick (500 mesh), thin (2000 mesh) sand paper polishing, to remove the oxidation film of titanium plate surface, and
Successively 10min is ultrasonically treated in acetone, ethyl alcohol, deionized water；The oxalic acid etching solution that mass fraction is 10% is prepared, it will be ultrasonic
After titanium sheet that treated etches 2h in 90 DEG C of etching solution, the titanium sheet substrate with uneven surface can be finally obtained；
(2) preparation of the anode containing ruthenium coating
Masking liquid is coated to step (1) treated on anode substrate surface, metal oxide deposition is 0.50mg/
cm2；
It will be coated with the anode substrate of anodic coating liquid, 30min is dried at 100 DEG C, then 300 DEG C of sintering 40min, from
So it is cooled to room temperature；
To guarantee active coating even application to the surface of basis material, brushed for 7 times repeatedly using above-mentioned step,
Dry, thermal oxide, brushing amount is 0.02mL/cm each time2, until mother liquor is finished；
Last time is sintered 3h at a temperature of 300 DEG C after applying and obtains anode containing ruthenium coating；
The anodic coating liquid, solvent are water, the component including following mole:
RuO2 0.028mol/L
Containing RuO2The preparation of nanoparticle coating liquid:
In 3mL RuCl30.2mL NaOH solution (25wt%) is added in (0.03mol/L) aqueous solution, in 90 DEG C of oil bath
20min is reacted in middle heating.Acquired solution is cooled to room temperature in ice bath immediately, can be prepared by 3.2mL containing RuO2Nanometer
The anodic coating liquid of particle.
(3) catalytic performance test
Using three-electrode system, anolyte is the NaCl aqueous solution of saturation, and catholyte is the NaOH aqueous solution of 5mol/L, yin
Pole room and anode chamber are separated with the N2010 cation-exchange membrane of E.I.Du Pont Company, and anode containing ruthenium coating obtained is working electrode, Pt
With saturated calomel electrode respectively as to electrode and reference electrode, test temperature is 25 DEG C, scanning speed 20mV/s.As a result see
Fig. 2A.
Embodiment 2
(1) with the step (1) in embodiment 1
(2) preparation of ruthenium chrome coating anode
Masking liquid is coated to step (1) treated on anode substrate surface, metal oxide deposition is 0.50mg/
cm2；
It will be coated with the anode substrate of anodic coating liquid, 30min is dried at 100 DEG C, then 300 DEG C of sintering 40min, from
So it is cooled to room temperature；
To guarantee active coating even application to the surface of basis material, brushed for 7 times repeatedly using above-mentioned step,
Dry, thermal oxide, brushing amount is 0.02mL/cm each time2, until mother liquor is finished；
Last time is sintered 3h at a temperature of 300 DEG C after applying and obtains anode containing ruthenium coating；
The anodic coating liquid, solvent are water, the component including following mole:
RuO2 0.026mol/L
Doped metal salt 0.002mol/L
[1]RuO2The preparation of nano particle masking liquid:
In 3mL RuCl30.2mL NaOH solution (25wt%) is added in (0.03mol/L) aqueous solution, in 90 DEG C of oil bath
20min is reacted in middle heating.Acquired solution is cooled to room temperature in ice bath immediately, can be prepared by 3.2mL containing RuO2Nanometer
The masking liquid of particle.
[2] contain RuO for what 0.2ml doping metals salting liquid addition step (1) obtained2In the masking liquid of nano particle
Obtain the anodic coating liquid；The doped metal salt is the nitrate of chromium.
In the doping metals salting liquid, the content of doped metal salt is 0.03mol/L；
Doping metals salting liquid with contain RuO2The volume ratio of the masking liquid of nano particle are as follows:
Doping metals salting liquid: contain RuO2Masking liquid=1:15 of nano particle；
(3) with the step (3) in embodiment 1, as a result see Fig. 2 B.
Embodiment 3
(1) with the step (1) in embodiment 1
(2) preparation of ruthenium manganese coated anode
Masking liquid is coated to step (1) treated on anode substrate surface, metal oxide deposition is 0.50mg/
cm2；
It will be coated with the anode substrate of anodic coating liquid, 30min is dried at 100 DEG C, then 300 DEG C of sintering 40min, from
So it is cooled to room temperature；
To guarantee active coating even application to the surface of basis material, brushed for 7 times repeatedly using above-mentioned step,
Dry, thermal oxide, brushing amount is 0.02mL/cm each time2, until mother liquor is finished；
It is finally sintered 3h at a temperature of 300 DEG C and obtains ruthenium manganese coated anode；
The anodic coating liquid, solvent are water, the component including following mole:
RuO2 0.026mol/L
Doped metal salt 0.002mol/L
[1]RuO2The preparation of nano particle masking liquid:
In 3mL RuCl30.2mL NaOH solution (25wt%) is added in (0.03mol/L) aqueous solution, in 90 DEG C of oil bath
20min is reacted in middle heating.Acquired solution is cooled to room temperature in ice bath immediately, can be prepared by 3.2mL containing RuO2Nanometer
The masking liquid of particle.
[2] contain RuO for what 0.2ml doping metals salting liquid addition step (1) obtained2In the masking liquid of nano particle
Obtain the anodic coating liquid；The doped metal salt is the nitrate of manganese.
In the doping metals salting liquid, the content of doped metal salt is 0.03mol/L；
Doping metals salting liquid with contain RuO2The volume ratio of the masking liquid of nano particle are as follows:
Doping metals salting liquid: contain RuO2Masking liquid=1:15 of nano particle；
(3) with the step (3) in embodiment 1, as a result see Fig. 2 C.
Experimental result of the invention: from fig. 1, it can be seen that when the painting liquid measure applied on electrode is too low, coating is too thin so that analysis
Chlorine catalytic activity is lower, and apply liquid measure it is excessively high when the too thick activity that can also reduce electrode of coating, wherein metal oxide deposition
For 0.50mg/cm2Ruthenium chrome coating anode analysis chlorine activity highest.Figure it is seen that the doping of chromium, manganese can be effectively
Analysis chlorine catalytic activity is promoted, the current potential comparison in Fig. 3 then can more clearly obtain this conclusion.
Claims (8)
1. the preparation method of the transient metal doped anode containing ruthenium coating, which comprises the steps of:
(1) substrate pretreated:
Obtain the titanium sheet substrate with uneven surface；
(2) preparation of the anode containing ruthenium coating:
Anode masking liquid is coated to step (1) treated on anode substrate surface, it is dry, then it is sintered and cooled；
The anodic coating liquid, solvent are water, the component including following mole:
RuO20.02~0.03mol/L
0.001~0.003mol/L of doped metal salt.
2. the method according to claim 1, wherein anode masking liquid is coated at step (1) in step (2)
On anode substrate surface after reason, metal oxide deposition is 0.25~0.75mg/cm2。
3. according to the method described in claim 2, it is characterized in that, the anode base of anodic coating liquid will be coated in step (2)
Body dries 15~30min, then 300~400 DEG C of 20~40min of sintering, cooled to room temperature at 100~120 DEG C.
4. according to the method described in claim 3, it is characterized in that, in step (2), using the above-mentioned repeated multiple times progress of step
It brushes, dry, thermal oxide, brushing amount is 0.02mL/cm each time2, until mother liquor is finished；
Last time is sintered 2~3h at a temperature of 300~400 DEG C after applying and obtains anode containing ruthenium coating.
5. according to the method described in claim 4, it is characterized in that, above-mentioned steps 2~10 times repeatedly.
6. the method according to claim 1, wherein the doped metal salt is the nitrate of chromium or manganese.
7. the method according to claim 1, wherein the preparation method of the anodic coating liquid, including it is as follows
Step:
Containing RuO2The preparation of nano particle masking liquid:
In RuCl3The NaOH solution that mass concentration is 20~30% is added in aqueous solution, 80~100 DEG C, reacts 10~30min, i.e.,
It can be made containing RuO2The masking liquid of nano particle；
RuCl3In aqueous solution, RuCl3Content be 0.01~1mol/L；
RuCl3The volume ratio of aqueous solution and the NaOH solution are as follows:
RuCl3Aqueous solution: NaOH solution=10~20:1；
Contain RuO for what doping metals salting liquid addition step (1) obtained2In the masking liquid of nano particle, the anode can be obtained
Coating solution.
8. the method according to the description of claim 7 is characterized in that in the doping metals salting liquid, doped metal salt
Content is 0.01~1mol/L；Doping metals salting liquid with contain RuO2The volume ratio of the masking liquid of nano particle are as follows: doped metal salt
Solution: contain RuO2Masking liquid=1:10~20 of nano particle.
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| CN110714193A (en) * | 2019-11-28 | 2020-01-21 | 江苏理工学院 | Preparation method of ternary metal oxide coating on surface of aluminum alloy piston |
| CN114180682A (en) * | 2021-12-13 | 2022-03-15 | 中国科学院生态环境研究中心 | Alkali metal-RuO2-TiO2Coated titanium electrode and preparation method thereof |
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Application publication date: 20191112 |