CN109402666A - A kind of heavy metal containing wastewater treatment titanium-based composite anode preparation method - Google Patents
A kind of heavy metal containing wastewater treatment titanium-based composite anode preparation method Download PDFInfo
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- CN109402666A CN109402666A CN201811606375.7A CN201811606375A CN109402666A CN 109402666 A CN109402666 A CN 109402666A CN 201811606375 A CN201811606375 A CN 201811606375A CN 109402666 A CN109402666 A CN 109402666A
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- 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
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- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
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- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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- 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
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Abstract
The invention discloses a kind of preparation methods of titanium-based composite anode, belong to heavy metal containing wastewater treatment field.Obtained anode is made of Titanium base, silicon dioxide intermediate layer and iridium cerium niobium ternary active oxide coating.With traditional IrO2Anode is compared, SiO2The addition of middle layer increases the active surface area of Oxygen anodic evolution reaction.Nb2O5Addition refined oxide-coated surface crystal grain, keep coating more compact, anode stability improve.CeO2Play pore-foaming agent, CeO is added2Keep oxide dispersion in coating more uniform, the raising of anode electro catalytic activity.Anode produced by the present invention has good analysis oxygen performance and service life, is the preferable selection of heavy metal containing wastewater treatment field anode material.
Description
Technical field
The present invention relates to a kind of heavy metal containing wastewater treatment field more particularly to a kind of preparation methods of titanium-based composite anode.
Background technique
In recent years, economical to increase rapidly, it promotes the fields such as medicine, pesticide, Chemical Manufacture and flourishes, an a large amount of huge sum of moneys
Belong to waste water to generate therewith, if heavy metal wastewater thereby fail to handle it is up to standard drain into water body, in soil, will seriously pollute environment, endanger
Evil human health.Electrocatalytic oxidation method, which handles heavy metal wastewater thereby, to be had thoroughly efficiently, and advantage without secondary pollution, this promotes more
More scholars are dedicated to the research using electro-catalytic oxidation technology processing heavy metal wastewater thereby, and electrode is to influence electrocatalytic oxidation effect
Central factor.
Dimensional stability metal oxide anode because of its good electrocatalysis characteristic and high stability, low consumption rate and
Long-life, and it is light-weight, be easily processed into required shape, with high cost performance and wide spectrum adaptability, be widely used
In the fields such as chlorine industry, sea water desalination, wastewater treatment, electro synthesis, anodic oxidation.
There are still some problems in the application for traditional titanium-based iridium system binary coated anode, and such as: noble metal is expensive, causes
Keep electrode preparation cost excessively high；Matrix titanium is oxidizable, so that coating adhesion strength is weakened and is fallen off, electrode is caused to inactivate.It is applied in iridium system
Nd is adulterated in layer, the inertia constituent element such as Si, Ce is made multicomponent composite oxide coating, activating oxide stability can be improved, subtract
Few noble metal dosage, saves electrode preparation cost, improves electrode catalyst efficiency, it is made to be more suitable for processing heavy metal wastewater thereby.
Summary of the invention
The preparation method that the object of the present invention is to provide a kind of suitable for handling the titanium-based composite anode of heavy metal wastewater thereby, should
Preparation method device is simple, and gained Oxygen anodic evolution function admirable, long service life and current efficiency are relatively high, can significantly drop
Low power consumption.
To achieve the above object, the technical scheme adopted by the invention is that:
A kind of preparation method suitable for handling the titanium-based composite anode of heavy metal wastewater thereby, which comprises
Step 1, pre-processing titanium substrate specifically include cutting, sand paper polishing, alkali cleaning oil removing, oxalic acid etching, ultrasonic cleaning and baking oven
Drying；
The dehydrated alcohol and KNO that 1:1 is mixed by volume is added in ethyl orthosilicate by step 23Mixed solution in, be added matter
The HCl solution that amount score is 10% adjusts under the conditions of pH value of solution is 3,25 DEG C and hydrolyzes 5 hours obtained SiO2Precursor solution；
Step 3 uses Ti plate for working electrode, and Ag/AgCl electrode is reference electrode, and graphite electrode is to constitute three electrodes to electrode
Middle layer is made in system, electro-deposition 200s；
Step 4, by dehydrated alcohol, 1:1 mixes to obtain solvent by volume with isopropanol, and chloro-iridic acid, cerous nitrate and nitric acid niobium are dissolved in
Coating solution is obtained in gained solvent.
Gained coating solution is evenly applied to interlayer surfaces by step 5, and drying, calcining are obtained with SiO2For centre
Layer, iridium cerium niobium ternary compound oxides are the composite anode of active coating.
It in the step 1, is polished using 200-300 mesh sand paper, the titanium-base after polishing is placed in mass fraction
For 20% sodium hydroxide solution and slightly boiled 1 hour progress alkaline degreasing in the acetone solution that 1:1 is mixed by volume.
Iridium in coating solution, cerium, three metal ion species of niobium total concentration be 0.2mol/L.
In the step 5, active coating is applied to 10 layers, and drying temperature is 80-100 DEG C, and drying time is 10-15 points
Clock；Calcination temperature is 425-475 DEG C, and calcination time is 10-15 minutes, and burning the time eventually is 1-2 hours.
Preparation method process provided by the invention is relatively easy it can be seen from above-mentioned technical proposal, gained Oxygen anodic evolution
Function admirable, long service life and current efficiency are relatively high, and power consumption can be greatly lowered.
To achieve the above object, the technical scheme adopted by the invention is that:
A kind of preparation method suitable for handling the titanium-based composite anode of heavy metal wastewater thereby, which comprises
Step 1, pre-processing titanium substrate specifically include cutting, sand paper polishing, alkali cleaning oil removing, oxalic acid etching, ultrasonic cleaning and baking oven
Drying；
The dehydrated alcohol and KNO that 1:1 is mixed by volume is added in ethyl orthosilicate by step 23Mixed solution in, be added matter
The HCl solution that amount score is 10% adjusts under the conditions of pH value of solution is 3,25 DEG C and hydrolyzes 5 hours obtained SiO2Precursor solution；
Step 3 uses Ti plate for working electrode, and Ag/AgCl electrode is reference electrode, and graphite electrode is to constitute three electrodes to electrode
Middle layer is made in system, electro-deposition 200s；
Step 4, by dehydrated alcohol, 1:1 mixes to obtain solvent by volume with isopropanol, and chloro-iridic acid, cerous nitrate and nitric acid niobium are dissolved in
Coating solution is obtained in gained solvent；
Gained coating solution is evenly applied to interlayer surfaces by step 5, and drying, calcining are obtained with SiO2For middle layer, iridium
Cerium niobium ternary compound oxides are the composite anode of active coating.
It in the step 1, is polished using 200-300 mesh sand paper, the titanium-base after polishing is placed in mass fraction
For 20% sodium hydroxide solution and slightly boiled 1 hour progress alkaline degreasing in the acetone solution that 1:1 is mixed by volume.
Iridium in coating solution, cerium, three metal ion species of niobium total concentration be 0.2mol/L.
In the step 5, active coating is applied to 10 layers, and drying temperature is 80-100 DEG C, and drying time is 10-15 points
Clock；Calcination temperature is 425-475 DEG C, and calcination time is 10-15 minutes, and burning the time eventually is 1-2 hours.
Preparation method process provided by the invention is relatively easy it can be seen from above-mentioned technical proposal, gained Oxygen anodic evolution
Function admirable, long service life and current efficiency are relatively high, and power consumption can be greatly lowered.
Detailed description of the invention
Fig. 1 is Ti/e-SiO of the present invention2/IrO2-CeO2-Nd2O5The preparation flow figure of titanium-based composite anode.
Specific embodiment
Embodiment one:
It will be cut into 5cm*5cm with a thickness of the titanium plate of 1mm first, is then polishing to the silvery white non-ferrous metal light of presentation with 200 mesh sand paper
Pool.By 20% sodium hydroxide solution of mass fraction, 1:1 is mixed by volume with acetone soln, and ultrasound makes it be uniformly dispersed in 10 minutes,
Titanium-base after polishing is placed in one, oil removing 1 hour under the conditions of 60 DEG C, it is 10% grass that titanium plate, which is then placed in mass fraction, again
It in acid solution, is etched 2 hours under the conditions of 90 DEG C, after ten minutes with deionized water ultrasonic cleaning, is placed in baking oven and dries for use.
5mL ethyl orthosilicate is added to 100mL 1:1 is mixed by volume dehydrated alcohol and KNO3Mixed solution
In, the HCl solution that addition mass fraction is 10% adjusts under the conditions of pH value of solution is 3,25 DEG C and hydrolyzes 5 hours obtained SiO2Presoma
Solution.
Use Ti plate for working electrode, Ag/AgCl electrode is reference electrode, and graphite electrode is to constitute three electrode bodies to electrode
Middle layer is made in system, electro-deposition 200s.
The chloro-iridic acid of certain mass, cerous nitrate and nitric acid niobium is miscible.
By dehydrated alcohol, 1:1 mixes to obtain solvent by volume with isopropanol, will be miscible after chloro-iridic acid, cerous nitrate and nitric acid
Niobium, which is dissolved in solvent, obtains coating solution.Chloro-iridic acid in coating solution, nitric acid niobium total mol concentration be 0.19mol/L, nitre
The molar concentration of sour cerium is 0.01 mol/L.
Gained coating solution is evenly applied to interlayer surfaces with banister brush, is placed in 80 DEG C of drying 10min in baking oven, and
425 DEG C of calcining 10min in Muffle furnace are placed on, taking-up is placed in air cooling 10min.It, will after repeating the above steps 10 times
Electrode is placed in Muffle furnace, and 1 hour is calcined under the conditions of 425 DEG C to get to SiO2For middle layer, the oxidation of iridium cerium niobium tri compound
Object is the titanium-based composite anode of active coating.
Use 2cm*2cm platinized platinum for electrode, self-made electrode is working electrode, calomel electrode is that reference electrode constitutes three electricity
Polar body system tests the oxygen evolution potential of anode, is lower than 1.3V derived from Oxygen anodic evolution current potential processed.It is 2A/cm in current density2Under the conditions of,
Use self-made electrode for anode, stainless steel electrode is that cathode constitutes two electrode systems, molten in the sulfuric acid that molar concentration is 1mol/L
Service life of the test gained anode in strong acid system, show that the made true service life of titanium-based composite anode is higher than 3 in liquid
Year.
Embodiment two:
It will be cut into 5cm*5cm with a thickness of the titanium plate of 1mm first, is then polishing to the silvery white non-ferrous metal light of presentation with 200 mesh sand paper
Pool.By 20% sodium hydroxide solution of mass fraction, 1:1 is mixed by volume with acetone soln, and ultrasound makes it be uniformly dispersed in 10 minutes,
Titanium-base after polishing is placed in one, oil removing 1 hour under the conditions of 60 DEG C, it is 10% grass that titanium plate, which is then placed in mass fraction, again
It in acid solution, is etched 2 hours under the conditions of 90 DEG C, after ten minutes with deionized water ultrasonic cleaning, is placed in baking oven and dries for use.
5mL ethyl orthosilicate is added to 100mL 1:1 is mixed by volume dehydrated alcohol and KNO3Mixed solution
In, the HCl solution that addition mass fraction is 10% adjusts under the conditions of pH value of solution is 3,25 DEG C and hydrolyzes 5 hours obtained SiO2Presoma
Solution.
Use Ti plate for working electrode, Ag/AgCl electrode is reference electrode, and graphite electrode is to constitute three electrode bodies to electrode
Middle layer is made in system, electro-deposition 200s.
The chloro-iridic acid of certain mass, cerous nitrate and nitric acid niobium is miscible.
By dehydrated alcohol, 1:1 mixes to obtain solvent by volume with isopropanol, will be miscible after chloro-iridic acid, cerous nitrate and nitric acid
Niobium, which is dissolved in solvent, obtains coating solution.Chloro-iridic acid in coating solution, nitric acid niobium total mol concentration be 0.18mol/L, nitre
The molar concentration of sour cerium is 0.02 mol/L.
Gained coating solution is evenly applied to interlayer surfaces with banister brush, is placed in 90 DEG C of drying 10min in baking oven, and
450 DEG C of calcining 10min in Muffle furnace are placed on, taking-up is placed in air cooling 10min.It, will after repeating the above steps 10 times
Electrode is placed in Muffle furnace, and 1 hour is calcined under the conditions of 450 DEG C to get to SiO2For middle layer, the oxidation of iridium cerium niobium tri compound
Object is the titanium-based composite anode of active coating.
Use 2cm*2cm platinized platinum for electrode, self-made electrode is working electrode, calomel electrode is that reference electrode constitutes three electricity
Polar body system tests the oxygen evolution potential of anode, is lower than 1.3V derived from Oxygen anodic evolution current potential processed.It is 2A/cm in current density2Under the conditions of,
Use self-made electrode for anode, stainless steel electrode is that cathode constitutes two electrode systems, molten in the sulfuric acid that molar concentration is 1mol/L
Service life of the test gained anode in strong acid system, show that the made true service life of titanium-based composite anode is higher than 3 in liquid
Year.
Embodiment three:
It will be cut into 5cm*5cm with a thickness of the titanium plate of 1mm first, is then polishing to the silvery white non-ferrous metal light of presentation with 200 mesh sand paper
Pool.By 20% sodium hydroxide solution of mass fraction, 1:1 is mixed by volume with acetone soln, and ultrasound makes it be uniformly dispersed in 10 minutes,
Titanium-base after polishing is placed in one, oil removing 1 hour under the conditions of 60 DEG C, it is 10% grass that titanium plate, which is then placed in mass fraction, again
It in acid solution, is etched 2 hours under the conditions of 90 DEG C, after ten minutes with deionized water ultrasonic cleaning, is placed in baking oven and dries for use.
5mL ethyl orthosilicate is added to 100mL 1:1 is mixed by volume dehydrated alcohol and KNO3Mixed solution
In, the HCl solution that addition mass fraction is 10% adjusts under the conditions of pH value of solution is 3,25 DEG C and hydrolyzes 5 hours obtained SiO2Presoma
Solution.
Use Ti plate for working electrode, Ag/AgCl electrode is reference electrode, and graphite electrode is to constitute three electrode bodies to electrode
Middle layer is made in system, electro-deposition 200s.
The chloro-iridic acid of certain mass, cerous nitrate and nitric acid niobium is miscible.
By dehydrated alcohol, 1:1 mixes to obtain solvent by volume with isopropanol, will be miscible after chloro-iridic acid, cerous nitrate and nitric acid
Niobium, which is dissolved in solvent, obtains coating solution.Chloro-iridic acid in coating solution, nitric acid niobium total mol concentration be 0.16mol/L, nitre
The molar concentration of sour cerium is 0.04 mol/L.
Gained coating solution is evenly applied to interlayer surfaces with banister brush, is placed in 100 DEG C of drying 15min in baking oven,
And 475 DEG C of calcining 15min in Muffle furnace are placed on, taking-up is placed in air cooling 10min.After repeating the above steps 10 times,
Electrode is placed in Muffle furnace, 1 hour is calcined under the conditions of 475 DEG C to get to SiO2For middle layer, iridium cerium niobium tri compound oxygen
Compound is the titanium-based composite anode of active coating.
Use 2cm*2cm platinized platinum for electrode, self-made electrode is working electrode, calomel electrode is that reference electrode constitutes three electricity
Polar body system tests the oxygen evolution potential of anode, is lower than 1.3V derived from Oxygen anodic evolution current potential processed.It is 2A/cm in current density2Under the conditions of,
Use self-made electrode for anode, stainless steel electrode is that cathode constitutes two electrode systems, molten in the sulfuric acid that molar concentration is 1mol/L
Service life of the test gained anode in strong acid system, show that the made true service life of titanium-based composite anode is higher than 3 in liquid
Year.
Claims (3)
1. a kind of heavy metal containing wastewater treatment preparation method of titanium-based composite anode, which is characterized in that the described method includes:
Step 1, pre-processing titanium substrate specifically include cutting, sand paper polishing, alkali cleaning oil removing, oxalic acid etching, ultrasonic cleaning and baking oven
Drying；
The dehydrated alcohol and KNO that 1:1 is mixed by volume is added in ethyl orthosilicate by step 23Mixed solution in, be added quality
The HCl solution that score is 10% adjusts under the conditions of pH value of solution is 3,25 DEG C and hydrolyzes 5 hours obtained SiO2Precursor solution；
Step 3 uses Ti plate for working electrode, and Ag/AgCl electrode is reference electrode, and graphite electrode is to constitute three electrodes to electrode
Middle layer is made in system, electro-deposition 200s；
Step 4, by dehydrated alcohol, 1:1 mixes to obtain solvent by volume with isopropanol, and chloro-iridic acid, cerous nitrate and nitric acid niobium are dissolved in
Coating solution is obtained in gained solvent；
Gained coating solution is evenly applied to interlayer surfaces by step 5, and drying, calcining are obtained with SiO2For middle layer, iridium
Cerium niobium ternary compound oxides are the titanium-based composite anode of active coating.
2. the preparation method of titanium-based composite anode according to claim 1, which is characterized in that during described in step 1, adopt
It is polished with 200-300 mesh sand paper, the titanium-base after polishing is placed in the sodium hydroxide solution and acetone that mass fraction is 20%
Slightly boiled 1 hour progress alkaline degreasing in the solution of 1:1 mixing by volume.
3. the preparation method of titanium-based composite anode according to claim 1, which is characterized in that iridium, cerium, niobium in coating solution
The total concentration of three metal ion species is 0.2mol/L；
The preparation method of titanium-based composite anode according to claim 1, which is characterized in that active coating described in step 5 is
10 layers, drying temperature is 80-100 DEG C, and drying time is 10-15 minutes；Calcination temperature is 425-475 DEG C, calcination time 10-
15 minutes, burning the time eventually was 1-2 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642339A (en) * | 2019-09-19 | 2020-01-03 | 武汉大学 | Porous Ti/IrO2-Nb2O5-Bi2O3Preparation method and application of electrode |
| CN115650376A (en) * | 2022-11-21 | 2023-01-31 | 天津环科环境咨询有限公司 | DSA electrode based on phenolic resin assistance and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908237A (en) * | 2006-07-20 | 2007-02-07 | 福州大学 | Titanium anode coated with iridium possessing high cerium content and high oxygen separated activity |
| CN102677092A (en) * | 2012-05-30 | 2012-09-19 | 浙江大学 | Preparation method of titanium anode |
-
2018
- 2018-12-27 CN CN201811606375.7A patent/CN109402666A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908237A (en) * | 2006-07-20 | 2007-02-07 | 福州大学 | Titanium anode coated with iridium possessing high cerium content and high oxygen separated activity |
| CN102677092A (en) * | 2012-05-30 | 2012-09-19 | 浙江大学 | Preparation method of titanium anode |
Non-Patent Citations (2)
| Title |
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| A.J. TEREZO等: "Fractional factorial design applied to investigate properties of Ti:IrO2-Nb2O5 electrodes", 《ELECTROCHIMICA ACTA》 * |
| CARLOS H. M. FERNANDES等: "ELECTROCHEMICAL TREATMENT OF WASTEWATER FROM BIODIESEL PRODUCTION USING A DSA KIND ELECTRODE:Ti/IrO2-Nb2O5", 《QUIM. NOVA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642339A (en) * | 2019-09-19 | 2020-01-03 | 武汉大学 | Porous Ti/IrO2-Nb2O5-Bi2O3Preparation method and application of electrode |
| CN115650376A (en) * | 2022-11-21 | 2023-01-31 | 天津环科环境咨询有限公司 | DSA electrode based on phenolic resin assistance and preparation method and application thereof |
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