CN101914782A - Metallic oxide anode suitable for Fenton system and preparation method thereof - Google Patents
Metallic oxide anode suitable for Fenton system and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a metallic oxide anode suitable for a Fenton system. In the invention, titanium is used as a matrix; a coating containing ruthenium and other components M is coated on the surface of the matrix, and other components M are one or more than one of iridium, titanium or stannum. The preparation method of the metallic oxide anode comprises the following steps of: pretreating a titanium plate to remove an oxidation film and surface greasy dirt, and then placing the titanium plate in 10wt% of oxalate solution for slight-boiling etching so as to make the surface formed into a rugged pitted surface; forming coating liquid by using a metal chloride and an organic solvent which is n-butyl alcohol or isopropanol; spreading the coating liquid onto the surface of the titanium plate, drying and then placing the titanium plate into a muffle furnace for oxidizing for 10min at 450-550 DEG C; taking out an electrode and cooling, and then removing loose matter from the surface; repeating the coating 10-15 times in such a way; and finally, calcining a sample at the temperature of 450-550 DEG C to convert the chloride into a corresponding oxide. The invention has simple preparation method; the prepared metallic oxide anode can obtain higher organic matter removing efficiency when being used for the Fenton system to treat waste water which is difficult to degrade, such as garbage leachate and the like.
Description
Technical field
The present invention relates to a kind of anode electrode that is applicable to Fenton system and preparation method thereof, belong to field of waste water treatment.
Background technology
The Fenton method has special advantages when handling Persistent organic pollutants, be a kind of very promising wastewater processing technology.This technology can be removed the hardly degraded organic substance that traditional wastewater processing technology can't be removed by the efficient oxidation, its essence is H
2O
2At Fe
2+Katalysis generate down hydroxyl radical free radical (OH) with high reaction activity, OH can make its degraded with most of organism effects.
The Fenton method is the method that electrochemistry and Fenton oxidation are combined, and has reaction conditions gentleness, organic matter degradation efficient height and the high advantage of salinity, and Fenton method degradation of organic substances has obtained numerous scholars' extensive concern at present.The essence of Fenton method is the Fe that produces with electrochemical process
2+And H
2O
2Lasting source as Fenton reagent.
Electrode materials is the effectively key of degradable organic pollutant of Fenton method.Because the Fenton reaction needed is to carry out under 3～5 the strong oxidizing property condition at pH, characteristics such as not corrosion, erosion resistance are strong so anode material must possess, good stability, anode material also must have higher oxygen evolution reaction overpotential to avoid the electrode side reaction simultaneously.With regard to anode material; ti-based coating electrode (being called for short DSA) is regarded as one of most important invention in the 20 discipline electrochemical field, has been widely used in aspects such as chlorine industry, oxymuriate production, marine anti-pollution, galvanic protection, sewage disposal, electrodialysis, fuel cell and organism synthesize.The DSA electrode is cheap, and erosion resistance is strong, can work in the electrolyte solution of many highly corrosive media or particular requirement; In addition, the electrochemical catalysis activity of DSA electrode mainly comes from oxide coating, and the chemical constitution of regulation and control oxide coating just can realize the different catalysis characteristicses of DSA electrode.Above speciality allows the DSA electrode be applicable to that as anode Fenton system becomes possibility, therefore has important and practical meanings with DSA as the metal oxide anode in the matrix exploitation Fenton system.At present, the preparation method of ti-based coating electrode mainly contains: thermal decomposition method, magnetron sputtering method, sol-gel method and electro-deposition method etc., thermal decomposition method are compared with other preparation methods has advantages such as preparation is easy, cheap, particularly the life-span is long.A kind of processing method for the treatment of carbolic acid waste water by electrochemical oxidation (patent No.: ZL 200610096628.1) adopts thermal decomposition method to prepare the Ti-base Sn-Sb metal oxide electrode; A kind of nanocrystalline iridium series oxide coating electrode preparation method (CN1995464A) adopts thermal decomposition method to prepare a kind of IrO
2-Ta
2O
5-MO
2The coated titanium base electrode.
Summary of the invention
Problem to be solved by this invention provides active high metal oxide anode of Fenton system and preparation method thereof that is applicable to.
The metal oxide anode of Fenton system that is applicable to provided by the present invention is: be matrix with the titanium, at matrix surface oxide coating is arranged, this oxide coating is made of ruthenium and other constituent elements M, M is one or more in iridium, titanium or the tin, and wherein the molar percentage of component ruthenium is 10～70%; The content of oxide coating is 1.05～1.35mg/cm
2
The above-mentioned preparation method of the metal oxide anode of Fenton system that is applicable to is:
Oxide film and surface and oil contaminant are removed in the pre-treatment of titanium plate, placed the little etching of boiling of 10wt% oxalic acid solution then, make the surface form rough pitted skin layer; The muriate of ruthenium and M is dissolved in organic solvent formation masking liquid; Masking liquid is applied to titanium plate surface, after the drying, puts it into temperature again and be oxidation in 450～550 ℃ the retort furnace; The surface porosity thing is removed in the cooling of taking-up electrode; So repeat to apply 10～15 times; At last sample is calcined down at 450～550 ℃, made muriate be converted into corresponding oxide compound.
Can be in the described preprocessing process with titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring, the titanium plate is immersed in the NaOH saturated solution boils 30min again.
When described oxalic acid solution concentration was high, the etched time was short; When concentration was hanged down, the time can proper extension.Take all factors into consideration, be chosen as 10wt%.
Described organic solvent can be propyl carbinol or Virahol.
In the oxidising process of titanium plate in retort furnace, play preliminary oxidation, the time can be 10min.
Should guarantee in the coating procedure that it is 1.05～1.35mg/cm that oxide coating generates rear oxidation thing content
2For realizing this purpose, the coating standard can be: 0.01～0.025ml/cm
2
Also add a little hydrochloric acid in the described masking liquid, its objective is to prevent hydrolysis.
The present invention compares the beneficial effect that is had with prior art:
The electrochemical catalysis activity of ti-based coating electrode (being called for short DSA) mainly comes from oxide coating, the chemical constitution of regulation and control oxide coating just can realize the different catalysis characteristicses of DSA electrode, therefore be widely used in Industrial Wastewater Treatment, as coking chemical waste water, petrochemical wastewater and dyeing waste water etc.DSA is introduced Fenton technology, not only brought into play the electric catalyticing characteristic of DSA itself, and in Fenton technology, have synergistic effect between electrochemical process and the traditional Fenton technology.Preparation method of the present invention is simple, and price is cheaper, can obtain higher organic matter removal efficient when the battery lead plate of preparation is applied to waste water such as Fenton system treating refuse percolate.
Embodiment
Describe content of the present invention in detail below by embodiment.Applied for one piece about Fenton system patent (ZL02147755.8 before the inventor, a kind of wastewater treatment method and equipment), with the preparation the titanium-based metal oxide electrode as anode, be applied to carry out the wastewater treatment experiment in the system that this patent describes, with percolate as typical used water difficult to degradate.
Embodiment one:
Preparation RuO
2-IrO
2/ Ti anode:
1, substrate pretreated
With titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring; The titanium plate is immersed in the NaOH saturated solution boils 30min, remove surface and oil contaminant, use washed with de-ionized water; The titanium plate is little etching 2h that boils in 10% oxalic acid solution; Use washed with de-ionized water, air-dry, put into dehydrated alcohol and preserve standby.
2, the preparation of masking liquid
Take by weighing quantitative RuCl respectively
33H
2O, IrCl3H
2O mixes with the propyl carbinol and the 2ml concentrated hydrochloric acid of certain volume, obtains masking liquid, is coated with the fluid component mole percent level and is: Ru: Ir=70%: 30%.
3, brushing and moulding
Masking liquid is applied to titanium plate surface with spread pen, and the coating standard is: 0.01ml/cm
2Then electrode is put into the electric heating constant temperature baking oven, at 100 ℃ of dry 10min; Putting it into and mixing up temperature in advance is oxidation 10min in 550 ℃ the retort furnace; Take out and brush away the surface porosity thing with hairbrush after electrode fully cools off; Repeat above-mentioned steps, so repeat to apply 10～15 times; At last sample is calcined 1h down at 550 ℃.It is 1.05mg/cm that anode is made rear oxidation thing content
2
RuO with preparation
2-IrO
2/ Ti electrode is as anode, in the Fenton system that patent (ZL02147755.8) is described, carry out wastewater treatment, as typical used water difficult to degradate, its water quality characteristic is: chemical oxygen demand cod 3424mg/L, NH with the actual percolate of Wuhan City's refuse landfill
4 +-N 2450mg/L, total nitrogen TN 2796mg/L, pH 8.5, Cl
-2728mg/L, biochemical oxygen demand (BOD) BOD on the 5th
5365mg/L.
Operational condition is as follows: percolate 1L, and reacting initial pH is 3, and polar plate spacing is 2cm, and electric current is 2A, and hydrogen peroxide and ferrous ion add continuously, and the hydrogen peroxide dosage is 220mmol/L, and the ferrous ion dosage is 18mmol/L.Behind the reaction 1h, COD removes efficient can reach 75.1%.
Embodiment two:
Preparation RuO
2-IrO
2/ Ti anode:
1, substrate pretreated
With titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring; The titanium plate is immersed in the NaOH saturated solution boils 30min, remove surface and oil contaminant, use washed with de-ionized water; The titanium plate is little etching 2h that boils in 10% oxalic acid solution; Use washed with de-ionized water, air-dry, put into dehydrated alcohol and preserve standby.
2, the preparation of masking liquid
Take by weighing quantitative RuCl respectively
33H
2O, IrCl3H
2O mixes with the Virahol and the 2ml concentrated hydrochloric acid of certain volume, obtains masking liquid, and being coated with the fluid component mole percent level is Ru: Ir=50%: 50%.
3, brushing and moulding
Masking liquid is applied to titanium plate surface with spread pen, and the coating standard is: 0.02ml/cm
2Then electrode is put into the electric heating constant temperature baking oven, at 100 ℃ of dry 10min; Putting it into and mixing up temperature in advance is oxidation 10min in 500 ℃ the retort furnace; Take out and brush away the surface porosity thing with hairbrush after electrode fully cools off; Repeat above-mentioned steps, so repeat to apply 10～15 times; At last sample is calcined 1h down at 500 ℃.It is 1.2mg/cm that anode is made rear oxidation thing content
2
RuO with preparation
2-IrO
2/ Ti electrode is as anode, carries out wastewater treatment in the Fenton system that patent (ZL02147755.8) is described, and as typical used water difficult to degradate, its water quality characteristic is with embodiment one with the actual percolate of Wuhan City's refuse landfill.
Operational condition is as follows: percolate 1L, and reacting initial pH is 3, and polar plate spacing is 2cm, and electric current is 2A, and hydrogen peroxide and ferrous ion add continuously, and the hydrogen peroxide dosage is 220mmol/L, and the ferrous ion dosage is 12mmol/L.Behind the reaction 1h, COD removes efficient can reach 72.9%.
Embodiment three:
Preparation RuO
2-IrO
2-TiO
2/ Ti anode:
1, substrate pretreated
With titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring; The titanium plate is immersed in the NaOH saturated solution boils 30min, remove surface and oil contaminant, use washed with de-ionized water; The titanium plate is little etching 2h that boils in 10% oxalic acid solution; Use washed with de-ionized water, air-dry, put into dehydrated alcohol and preserve standby.
2, the preparation of masking liquid
Take by weighing quantitative RuCl respectively
33H
2O, IrCl3H
2O, TiCl
3Mix with the propyl carbinol and the 2ml concentrated hydrochloric acid of certain volume, obtain masking liquid, be coated with the fluid component mole percent level and be: Ru: Ir: Ti=10%: 10%: 80%.
3, brushing and moulding
Masking liquid is applied to titanium plate surface with spread pen, and the coating standard is: 0.025ml/cm
2Then electrode is put into the electric heating constant temperature baking oven, at 100 ℃ of dry 10min; Putting it into and mixing up temperature in advance is oxidation 10min in 500 ℃ the retort furnace; Take out and brush away the surface porosity thing with hairbrush after electrode fully cools off; Repeat above-mentioned steps, so repeat to apply 10～15 times; At last sample is calcined 1h down at 500 ℃.It is 1.35mg/cm that anode is made rear oxidation thing content
2
RuO with preparation
2-IrO
2-TiO
2/ Ti electrode is as anode, in the Fenton system that patent (ZL02147755.8) is described, carry out wastewater treatment, as typical used water difficult to degradate, its water quality characteristic is: chemical oxygen demand cod 5260mg/L, NH with the actual percolate of Wuhan City's refuse landfill
4 +-N 680mg/L, pH 6.84, Cl
-3000mg/L, BOD
5(biochemical oxygen demand (BOD) on the 5th) 2000mg/L.Percolate is earlier through biochemical treatment, and COD can drop to about 1000mg/L.
Operational condition is as follows: percolate bio-chemical effluent 1L, and reacting initial pH is 3, and polar plate spacing is 2cm, and electric current is 2A, and hydrogen peroxide and ferrous ion add continuously, and the hydrogen peroxide dosage is 57mmol/L, and the ferrous ion dosage is 9.5mmol/L.Behind the reaction 1h, COD removes efficient can reach 76.2%.
Embodiment four:
Preparation RuO
2-IrO
2-TiO
2/ Ti anode:
1, substrate pretreated
With titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring; The titanium plate is immersed in the NaOH saturated solution boils 30min, remove surface and oil contaminant, use washed with de-ionized water; The titanium plate is little etching 2h that boils in 10% oxalic acid solution; Use washed with de-ionized water, air-dry, put into dehydrated alcohol and preserve standby.
2, the preparation of masking liquid
Take by weighing quantitative RuCl respectively
33H
2O, IrCl3H
2O, TiCl
3Mix with the Virahol and the 2ml concentrated hydrochloric acid of certain volume, obtain masking liquid, be coated with the fluid component mole percent level and be: Ru: Ir: Ti=10%: 20%: 70%.
3, brushing and moulding
Masking liquid is applied to titanium plate surface with spread pen, and the coating standard is: 0.01ml/cm
2Then electrode is put into the electric heating constant temperature baking oven, at 100 ℃ of dry 10min; Putting it into and mixing up temperature in advance is oxidation 10min in 450 ℃ the retort furnace; Take out and brush away the surface porosity thing with hairbrush after electrode fully cools off; Repeat above-mentioned steps, so repeat to apply 10～15 times; At last sample is calcined 1h down at 450 ℃.It is 1.1mg/cm that anode is made rear oxidation thing content
2
RuO with preparation
2-IrO
2-TiO
2/ Ti electrode is as anode, carries out wastewater treatment in the Fenton system that patent (ZL02147755.8) is described, and as typical used water difficult to degradate, its water quality characteristic is with embodiment three with the actual percolate of Wuhan City's refuse landfill.
Operational condition is as follows: percolate bio-chemical effluent 1L, and reacting initial pH is 3, and polar plate spacing is 2cm, and electric current is 2A, and hydrogen peroxide and ferrous ion add continuously, and the hydrogen peroxide dosage is 56mmol/L, and the ferrous ion dosage is 9.3mmol/L.Behind the reaction 1h, COD removes efficient can reach 75.3%.
Embodiment five:
Preparation RuO
2-IrO
2-TiO
2-SnO
2/ Ti anode:
1, substrate pretreated
With titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring; The titanium plate is immersed in the NaOH saturated solution boils 30min, remove surface and oil contaminant, use washed with de-ionized water; The titanium plate is little etching 2h that boils in 10% oxalic acid solution; Use washed with de-ionized water, air-dry, put into dehydrated alcohol and preserve standby.
2, the preparation of masking liquid
Take by weighing quantitative RuCl respectively
33H
2O, IrCl3H
2O, TiCl
3, SnCl
4Mix with the propyl carbinol and the 2ml concentrated hydrochloric acid of certain volume, obtain masking liquid, being coated with the fluid component mole percent level is Ru: Ir: Ti: Sn=30%: 10%: 55%: 5%.
3, brushing and moulding
Masking liquid is applied to titanium plate surface with spread pen, and the coating standard is: 0.02ml/cm
2Then electrode is put into the electric heating constant temperature baking oven, at 100 ℃ of dry 10min; Putting it into and mixing up temperature in advance is oxidation 10min in 450 ℃ the retort furnace; Take out and brush away the surface porosity thing with hairbrush after electrode fully cools off; Repeat above-mentioned steps, so repeat to apply 10～15 times; At last sample is calcined 1h down at 450 ℃.It is 1.25mg/cm that anode is made rear oxidation thing content
2
RuO with preparation
2-IrO
2-TiO
2-SnO
2/ Ti electrode is as anode, in the Fenton system that patent (ZL02147755.8) is described, carry out wastewater treatment, as typical used water difficult to degradate, its water quality characteristic is: chemical oxygen demand cod 2720mg/L, NH with the actual percolate of Wuhan City's refuse landfill
4 +-N 2850mg/L, pH 8.03, Cl
-2900mg/L.
Operational condition is as follows: adopt operate continuously, the electrochemical reactor useful volume is 1L, reacting initial pH is 3, polar plate spacing is 2cm, electric current is 4A, percolate hydraulic detention time HRT 40min, and hydrogen peroxide and ferrous ion add continuously, the hydrogen peroxide dosage is 170mmol/L, and the ferrous ion dosage is 19mmol/L.Behind the reaction 2h, COD removes efficient can reach 60.0%.
Embodiment six:
Preparation RuO
2-IrO
2-TiO
2-SnO
2/ Ti anode:
1, substrate pretreated
With titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring; The titanium plate is immersed in the NaOH saturated solution boils 30min, remove surface and oil contaminant, use washed with de-ionized water; The titanium plate is little etching 2h that boils in 10% oxalic acid solution; Use washed with de-ionized water, air-dry, put into dehydrated alcohol and preserve standby.
2, the preparation of masking liquid
Take by weighing quantitative RuCl respectively
33H
2O, IrCl3H
2O, TiCl
3, SnCl
4Mix with the Virahol and the 2ml concentrated hydrochloric acid of certain volume, obtain masking liquid, being coated with the fluid component mole percent level is Ru: Ir: Ti: Sn=30%: 10%: 59%: 1%.
3, brushing and moulding
Masking liquid is applied to titanium plate surface with spread pen, and the coating standard is: 0.025ml/cm
2Then electrode is put into the electric heating constant temperature baking oven, at 100 ℃ of dry 10min; Putting it into and mixing up temperature in advance is oxidation 10min in 550 ℃ the retort furnace; Take out and brush away the surface porosity thing with hairbrush after electrode fully cools off; Repeat above-mentioned steps, so repeat to apply 10～15 times; At last sample is calcined 1h down at 550 ℃.It is 1.30mg/cm that anode is made rear oxidation thing content
2
RuO with preparation
2-IrO
2-TiO
2-SnO
2/ Ti electrode is as anode, carries out wastewater treatment in the Fenton system that patent (ZL02147755.8) is described, and as typical used water difficult to degradate, its water quality characteristic is with embodiment five with the actual percolate of Wuhan City's refuse landfill.
Operational condition is as follows: adopt operate continuously, the electrochemical reactor useful volume is 1L, reacting initial pH is 3, polar plate spacing is 2cm, electric current is 4A, percolate hydraulic detention time HRT 40min, and hydrogen peroxide and ferrous ion add continuously, the hydrogen peroxide dosage is 170mmol/L, and the ferrous ion dosage is 19mmol/L.Behind the reaction 2h, COD removes efficient can reach 55.2%.
Claims (8)
1. metal oxide anode that is applicable to Fenton system, it is characterized in that: with the titanium is matrix, at matrix surface oxide coating is arranged, and this oxide coating is made of ruthenium and other constituent elements M, M is one or more in iridium, titanium or the tin, and wherein the molar percentage of component ruthenium is 10～70%; The content of oxide coating is 1.05～1.35mg/cm
2
2. the described preparation method who is applicable to the metal oxide anode of Fenton system of claim 1, it is characterized in that: oxide film and surface and oil contaminant are removed in the pre-treatment of titanium plate, place the little etching of boiling of oxalic acid solution then, make the surface form rough pitted skin layer; Metal chloride and organic solvent are formed masking liquid; Masking liquid is applied to titanium plate surface, after the drying, puts it into temperature again and be oxidation in 450～550 ℃ the retort furnace; The surface porosity thing is removed in the cooling of taking-up electrode; So repeat to apply 10～15 times; At last sample is calcined down at 450～550 ℃, made muriate be converted into corresponding oxide compound.
3. preparation method according to claim 2 is characterized in that: in the preprocessing process with titanium plate surface successively with file, 60 orders, 300 order sand paperings to metalluster occurring, the titanium plate is immersed in the NaOH saturated solution boils 30min again.
4. according to claim 2 or 3 described preparation methods, it is characterized in that: described oxalic acid solution concentration is 10wt%.
5. according to claim 2 or 3 described preparation methods, it is characterized in that: organic solvent is propyl carbinol or Virahol.
6. according to claim 2 or 3 described preparation methods, it is characterized in that: in the oxidising process of titanium plate in retort furnace, the time is 10min.
7. according to claim 2 or 3 described preparation methods, it is characterized in that: the coating standard is 0.01～0.025ml/cm in the coating procedure
2
8. according to claim 2 or 3 described preparation methods, it is characterized in that: also add a little hydrochloric acid in the described masking liquid.
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| CN114538571A (en) * | 2022-03-09 | 2022-05-27 | 四川塔菲尔环境科技有限公司 | Praseodymium and niobium modified Ti/RuO2Dimensionally stable anode, preparation method and application |
| CN114560536A (en) * | 2022-03-09 | 2022-05-31 | 四川塔菲尔环境科技有限公司 | Terbium rhenium modified Ti/RuO2Dimensionally stable anode, preparation method and application |
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