CN1962471A - Method for electrolyzing organic waste water using iridium tantalum stannum oxide coating titanium electrode - Google Patents
Method for electrolyzing organic waste water using iridium tantalum stannum oxide coating titanium electrode Download PDFInfo
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- CN1962471A CN1962471A CN 200610144146 CN200610144146A CN1962471A CN 1962471 A CN1962471 A CN 1962471A CN 200610144146 CN200610144146 CN 200610144146 CN 200610144146 A CN200610144146 A CN 200610144146A CN 1962471 A CN1962471 A CN 1962471A
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Abstract
The invention discloses an organic waste water disposing method through coating electrode electrolytic disposal of iridium tantalum tin oxide in the electrochemical and environmental chemical technique domain, which is characterized by the following: adding additive in the electrolytic procedure; adopting DC or pulse current with DC density at 1000-2000A .m-2 and electrode board gap at 0.3-1.0cm; possessing saw pulse current with peak current density at 1200-3000A .m-2 and pulse period at 0.5-2.0ms; setting the on-off rate at 1: 3-3: 1 with auxiliary DC component at 0-1000A .m-2 and electrode board gap at 0.5-1.5cm.
Description
Technical field
The invention belongs to electrochemistry and environmental chemistry technical field, be particularly related to a kind of employing nanocrystalline iridium tantalum stannum oxide coating titanium electrode, add the organic additive of synergistic oxidation, galvanic current or pulsed current electrolysis mode, efficient electrolysis is handled the method for organic waste water.
Background technology
It is the treatment process that redox, decomposition, coagulating sedimentation combine that electrolysis treatment is handled organic waste water.Because its non-secondary pollution, quick, simple has obtained extensive studies in recent years.In the electrolysis treatment waste water electrode materials select for use very importantly, select the improper electrolytic efficiency that can make to reduce, treatment effect does not reach requirement, power consumption increases.The method of currently used electrolyzing organic waste water can be divided into two classes according to the anode that adopts: the dissolving anode that 1) adopts solubility, mainly be iron or aluminium, add iron filings therein, wadding is coagulated in electrolysis, and the oxidizing substance that produces when working in coordination with electrolysis is handled waste water.What number of patent application CN 98811458.5, CN 99113796.5, CN 94103287.6 and CN 93111832.8 and patent No. WO9735808 were adopted is exactly this kind method.Its difference is different with treatment unit of arranging of electrode.Number of patent application CN 02111901.5 is on this basis, the zeolite that adds 0%～10% cats product modification of copper and iron gross weight according to the different situations of waste water, like this than stronger with the ability of electrolysis treatment difficult degradation pollutent in internal electrolysis of iron or the iron charcoal, decolorizing effect is more remarkable, and the pH scope that is suitable for is bigger.This type of electrolytic process can treatment of wastes with processes of wastes against one another, consumes energy not, and biggest advantage is that processing costs is low.Its shortcoming is that speed of response is slow and influenced by pH very big, and reaction column easily stops up, and high-concentration waste water is handled difficulty, and the reactor turndown ratio is relatively poor.2) adopt insoluble anode, by the strong oxide group (as HO) that electrolysis produces, the organism in the oxidized waste water reaches the effect of handling waste water.It is that matrix is coated with PbO that number of patent application CN 03133317.6 adopts with the titanium
2Or SeO
2The electrode of coating is made anode, and 30～120 minutes Refinery Wastewater of electrolysis are respond well.Titanium base PbO
2Electrode pair phenol has degradation property preferably, but has the dissolved problem, and its toxicity can produce secondary pollution.For titanium base ruthenium-iridium-tantalum coated electrode, pole plate is spaced apart 3～10mm, and control current density is 2450～6440Am
-2, the electrolysis residence time is 30～120min.Current density is bigger, and electrolysis time is longer, and institute's consumes energy is more, and is unreasonable economically.(method of electrocogulative treatment of industrial waste water and device, application number 98811458.5 publication numbers 1279651, have the electrocatalysis flocculence sewage treatment equipment of pole plate guarantor apart from device, application number 99113796.5 publication numbers 1278515, the method of wastewater treatment that relates to electrolysis-oxidation style, application number 94103287.6 publication numbers 1107443, nitro-diazophenol wasted water treatment process, application number 93111832.8 publication numbers 1095692, AN ELECTRO-FLOCCULATION PROCESS, patent No. WO9735808, the method for the treatment of used water difficult to degradate by catalytic internal electrolysis of iron, application number 02111901.5 publication number 1382649, electro-catalytic oxidation technology is handled the method for low chemical oxygen demand waste water, application number 03133317.6 publication number 1458075)
This also is the major cause of present strong oxidizing property electrode not seen widespread use.Existing problem mainly is two problems: the one, handle the problem of waste water time, i.e. and how the efficient of electrocatalysis method improves; Another is problem electrode life, and promptly how the stability of electrode improves.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts nanocrystalline iridium tantalum stannum oxide coating titanium electrode electrolyzing organic waste water, when reducing energy consumption, improve, satisfy the actual needs of industrial electrolyzing organic waste water the treatment of organic matters of organic effect.
The present invention adopts the nanocrystalline iridium tantalum stannum oxide coating titanium electrode with higher electrocatalysis characteristic and high stability, electrolyzing organic waste water, and when electrolysis, add additive, electric current adopts galvanic current or pulsed current during electrolysis; Galvanic current density 1000～2000Am
-2, polar plate spacing 0.3～1.0cm; Sawtooth pulse electric current, peak current density are 1200～3000Am
-2, the recurrence interval is 0.5～2.0ms, and break make ratio is 1: 3～3: 1, and the additional straight flow component is 0～1000Am
-2, polar plate spacing 0.5～1.5cm.
Electrode of the present invention is an iridium tantalum stannum oxide coating titanium electrode, comprises nanocrystalline iridium tantalum stannum oxide coating titanium electrode IrO
2-Ta
2O
5-SnO
2/ Ti and with IrO
2-Ta
2O
5-SnO
2/ Ti is as the titanium electrode SnO of bottom, surface applied tin-oxide
2/ IrO
2-Ta
2O
5-SnO
2/ Ti, IrO
2-Ta
2O
5-SnO
2/ Ti electrode coating grain-size is between 5～40nm.
Additive of the present invention is NaCl, NaCl concentration 0.1～6%.
IrO of the present invention
2-Ta
2O
5-SnO
2/ Ti adopts the thermal decomposition method preparation, and technology is: masking liquid preparation H
2IrCl
6And TaCl
5Propyl carbinol and Virahol mixed solution, propyl carbinol and Virahol volume ratio 1～3, wherein the atomic ratio of Ir and Ta is 7: 6, total metal concentration of Ir+Ta is 0.1～0.5mol/L; Pure titanium plate, after the pickling etching is brushed masking liquid on pure titanium plate two sides through alkali Rising-of-water oil removing, be hung on the hanger, place baking oven to dry 10～20min down for 90～150 ℃, 300～450 ℃ of sintering 10～20min in retort furnace decompose metal-salt and generate oxide coating again; Take out the back air cooling to room temperature, repeat above step, make nanocrystalline iridium tantalum stannum oxide coating titanium electrode IrO until applying 5～10 layers
2-Ta
2O
5-SnO
2/ Ti, grain-size is between 5～40nm.
SnO of the present invention
2/ IrO
2-Ta
2O
5-SnO
2/ Ti adopts the thermal decomposition method preparation, and technology is: make IrO
2-Ta
2O
5-SnO
2/ Ti is as bottom, and thermal decomposition method applies SnO thereon
2Layer, coating liquid is that the atomic percent of Sn is propyl carbinol and the Virahol mixed solution of 0.1～0.4g/L, propyl carbinol and Virahol volume ratio 1～3 apply 3～8 times; Place retort furnace 300～550 ℃ sintering temperature 1～3 hour at last, obtain SnO
2/ IrO
2-Ta
2O
5-SnO
2/ Ti electrode.
Electrolysis treatment contains in the organic organic waste water process, and there are two kinds of mechanism in organic anodic oxidation: the one, and complete oxidation, decomposition, its final product is CO
2, this approach is generally at SnO
2, PbO
2Take place on the oxide anode surface; The 2nd, optionally oxidation, this process often occurs in IrO
2, RuO
2The isoreactivity electrode surface, the intermediate product ((Ch.Comninellis that organic reactant generally only can oxidized generation has certain stability, Electrocatalysis in the electrochemical conversion/combussion of organicpollutants for waste water treatment.electrochemical Acta, 1994,39 (11-12): 1857-1862).This mainly is owing to oxygen mechanism difference is analysed on two type oxide surfaces in the aqueous solution, think that the oxygen evolution reaction mechanism of electrode surface can be divided into two big classes: the one, suboxide oxidation transformation before analysing oxygen is the oxide compound of high valence state, high oxide and then be decomposed into former suboxide and emit oxygen simultaneously, Ir, Ru oxide compound promptly belong to this type of, and oxygen evolution potential is lower; Another kind of oxide compound such as SnO
2, PbO
2Deng, the absorption by the OH free radical is separated out oxygen, and its oxygen evolution potential approaches OH-/HO
2-The standard equilibrium potential (1.77V vs SHE) that galvanic couple is right, oxygen evolution potential is higher.And critical effect is just played in the organic oxidative degradation of OH radical pair of strong oxidizing property.Here it is adopts this type of electrode, reason that can fine processing organic waste water.Especially the adding of Sn, electrode overpotential for oxygen evolution height, organism intermediate product formation speed is low, be difficult to gather, and more strengthened the ability of electrocatalysis degrading waste water.
So the present invention adds additive NaCl in waste water, when electrolysis, produce the ClO of strong oxidizing property
-Ion can the common oxide treatment organic waste water in synergetic electrode surface.In addition, the adding of NaCl can reduce the bath voltage of electrode, reduces the consumption of electric energy.The NaCl concentration that adds concerns as shown in Figure 1 with processing back organic waste water chemical oxygen demand (COD) (COD).
Electric current adopts galvanic current or pulsed current during electrolysis of the present invention.
Each parameter that the present invention is adopted under dc state comprises electrode materials, current density, NaCl concentration, battery lead plate spacing and electrolysis time.Show that according to a large amount of tests for different waste water, selected parameter is distinguishing.In concrete enforcement, illustrated.
The parameter that the present invention is adopted under the pulse electrolysis state comprises selection, peak current density, recurrence interval, break make ratio, the additional straight flow component of waveform.When dc electrolysis,, thereby cause concentration polarization inevitably because active oxygen leaves the organism in the continuous oxidized organic wastewater of anode.And during pulse electrolysis, when current lead-through, can not be reduced by organism fully near the anodic active oxygen; When electric current turn-offed, the active oxygen around the anode continued and the organism effect.Like this, periodic repetition pulse electric current continuously is applied to oxidation of organic compounds as far as possible fully, and is unlikely to the physical adsorption active oxygen and the chemisorption active oxygen can generate oxygen and enter air.Like this, not only save electric energy but also improved the processing efficiency of organic waste water.
Description of drawings
The present invention has carried out the electrolysis treatment test to different organic waste water.Below by example treatment process is further specified.
Accompanying drawing is 1NaCl concentration and processing back COD relation.SnO
2-IrO
2-Ta
2O
5COD is with the variation that adds NaCl concentration during/Ti electrolysis organic waste water.(experiment condition: negative electrode is 9cm
2The titanium plate, annode area 2 * 2.5cm
2, anodic current density is 1600Am
-2, polar plate spacing 0.6cm.)
The relation of 2 dc electrolysis Refinery Wastewater treatment times of accompanying drawing and COD.SnO
2/ IrO
2-Ta
2COD is with the variation that adds NaCl concentration during O/Ti electrolysis refinery water.(experiment condition: negative electrode is 9cm
2The titanium plate, annode area 2 * 2.5cm
2, anodic current density is 1600Am
-2, NaCl concentration, 5% polar plate spacing 0.5cm.)
Accompanying drawing 3 dc electrolysis are handled the relation of ethene wastewater treatment time and COD.SnO
2-IrO
2-Ta
2O
5COD curve over time when/Ti electrolysis handle to add the ethene waste water of 0.1%NaCl.(experiment condition: negative electrode is 9cm
2The titanium plate, annode area 2 * 2.5cm
2, current density 1600Am
-2, polar plate spacing 10mm.)
Embodiment
Embodiment 2 dc electrolysis are handled actual production ethene waste water.Initial COD value is 50mg/L.Electricity consumption is SnO very
2-IrO
2-Ta
2O
5/ Ti, NaCl concentration 0.1%, current density 1600Am
-2, annode area 5cm
-2, polar plate spacing 1cm.The NaCl concentration content that adds is very low, and after the electrolysis 1 minute, the clearance of COD value reaches 90.8%.Water quality standard meets the requirement of boiler cycling use of water.The electric energy that 1 ton of this kind ethene of calculating electrolysis waste water is consumed is 2.0 degree.The relation of treatment time and COD such as accompanying drawing 3.
The synthetic hexylene glycol waste water of ethene waste water, comprehensive wastewater and ethene of certain petro-chemical corporation is handled in embodiment 3 pulse electrolysis.The employing electrode is SnO
2-IrO
2-Ta
2O
5/ Ti, annode area 4cm
-2, polar plate spacing 1cm.Adopt zigzag wave, peak current density is 2500Am
-2, the recurrence interval is 1ms, break make ratio is that 1: 1 and additional straight flow component are 0.Every detected result shows, water reuse standard during the solid matter (SS) of organic waste water and turbidity have substantially met before the electrolysis, but COD in the waste water and colourity also are difficult to remove fully.Adopt the pulsed current electrolysis to handle organic waste water, the COD of organic waste water, colourity, solid matter (SS) can both effectively be removed after the electrolysis.Water reuse standard (COD is lower than 20mg/L), especially comprehensive wastewater COD can reduce to below the 10mg/L during wherein the COD of organic waste water can reach substantially, the standard of water reuse during ethene and ethylene glycol waste water also can meet substantially; And colourity also is lower than middle water reuse standard (colourity is lower than 10); Though the solid matter of organic waste water has reached standard (SS is lower than 30mg/L) before the electrolysis, the SS of organic waste water further reduces after the electrolysis.The current consumption average out to 2.5kWhm of every cubic metre of water of electrolysis treatment
-3Water parameter result is as shown in table 1 before and after electrolytic working conditions and the electrolysis.
Organic waste water parameter synopsis before and after table 1 pulse electrolysis
| The waste water title | Ethene waste water | Comprehensive wastewater | Ethylene glycol waste water | |
| Former water parameter | COD/mg·dm -3 | 72.83 | 71.50 | 62.28 |
| Specific conductivity/μ Scm -1 | 15890 | 15970 | 13860 | |
| Colourity | 8 | 18 | 11 | |
| SS/mg·L -1 | 4 | 3 | 1 | |
| Working conditions | Bath voltage/V | 5.95 | 5.81 | 6.70 |
| Current consumption/kWhm -3 | 2.48 | 2.42 | 2.79 | |
| Electrolysis time/ |
10 | 10 | 15 | |
| The water outlet parameter | COD/mg·dm -3 | 17.72 | 8.89 | 21.31 |
| Specific conductivity/μ Scm -1 | 15920 | 16340 | 14050 | |
| Colourity | ＜5 | ＜5 | ＜5 | |
| SS/mg·L -1 | ＜1 | ＜1 | ＜1 | |
Claims (5)
1. method that adopts the iridium tantalum stannum oxide coating titanium electrode electrolyzing organic waste water, it is characterized in that, employing has the nanocrystalline iridium tantalum stannum oxide coating titanium electrode of higher electrocatalysis characteristic and high stability, electrolyzing organic waste water, and add additive when electrolysis, electric current adopts galvanic current or pulsed current during electrolysis; Galvanic current density 1000～2000Am
-2, polar plate spacing 0.3～1.0cm; Sawtooth pulse electric current, peak current density are 1200～3000Am
-2, the recurrence interval is 0.5～2.0ms, and break make ratio is 1: 3～3: 1, and the additional straight flow component is 0～1000Am
-2, polar plate spacing 0.5～1.5cm.
2. in accordance with the method for claim 1, it is characterized in that described electrode is an iridium tantalum stannum oxide coating titanium electrode, comprise nanocrystalline iridium tantalum stannum oxide coating titanium electrode IrO
2-Ta
2O
5-SnO
2/ Ti and with IrO
2-Ta
2O
5-SnO
2/ Ti is as the titanium electrode SnO of bottom, surface applied tin-oxide
2/ IrO
2-Ta
2O
5-SnO
2/ Ti, IrO
2-Ta
2O
5-SnO
2/ Ti electrode coating grain-size is between 5～40nm.
3. in accordance with the method for claim 1, it is characterized in that described additive is NaCl, NaCl concentration 0.1～6%.
4, in accordance with the method for claim 2, IrO
2-Ta
2O
5-SnO
2/ Ti adopts the thermal decomposition method preparation, and technology is: masking liquid preparation H
2IrCl
6And TaCl
5Propyl carbinol and Virahol mixed solution, propyl carbinol and Virahol volume ratio 1～3, wherein the atomic ratio of Ir and Ta is 7: 6, total metal concentration of Ir+Ta is 0.1～0.5mol/L; Pure titanium plate, after the pickling etching is brushed masking liquid on pure titanium plate two sides through alkali Rising-of-water oil removing, be hung on the hanger, place baking oven to dry 10～20min down for 90～150 ℃, 300～450 ℃ of sintering 10～20min in retort furnace decompose metal-salt and generate oxide coating again; Take out the back air cooling to room temperature, repeat above step, make nanocrystalline iridium tantalum stannum oxide coating titanium electrode IrO until applying 5～10 layers
2-Ta
2O
5-SnO
2/ Ti, grain-size is between 5～40nm.
5, according to claim 2 or 4 described methods, SnO
2/ IrO
2-Ta
2O
5-SnO
2/ Ti adopts the thermal decomposition method preparation, and technology is: make IrO
2-Ta
2O
5-SnO
2/ Ti is as bottom, and thermal decomposition method applies SnO thereon
2Layer, coating liquid is that the atomic percent of Sn is propyl carbinol and the Virahol mixed solution of 0.1～0.4g/L, propyl carbinol and Virahol volume ratio 1～3 apply 3～8 times; Place retort furnace 300～550 ℃ sintering temperature 1～3 hour at last, obtain SnO
2/ IrO
2-Ta
2O
5-SnO
2/ Ti electrode.
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| CN101830542A (en) * | 2010-04-27 | 2010-09-15 | 华南师范大学 | Method for electrolyzing orange G by adopting cerium-doped tin antimony oxide coated titanium electrode |
| CN102168283A (en) * | 2011-04-08 | 2011-08-31 | 江苏美特林科特殊合金有限公司 | Electrode coating and preparation method thereof |
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| CN106365265A (en) * | 2016-11-21 | 2017-02-01 | 北京益清源环保科技有限公司 | Modified zeolite particle electrode with function of removing phenol through electrocatalysis and preparation method |
| CN108217851A (en) * | 2018-01-09 | 2018-06-29 | 北京大学 | A kind of method using iridium dioxide electrode electro-catalysis processing TNT waste water |
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| CN101830542A (en) * | 2010-04-27 | 2010-09-15 | 华南师范大学 | Method for electrolyzing orange G by adopting cerium-doped tin antimony oxide coated titanium electrode |
| CN102168283A (en) * | 2011-04-08 | 2011-08-31 | 江苏美特林科特殊合金有限公司 | Electrode coating and preparation method thereof |
| CN102168283B (en) * | 2011-04-08 | 2014-01-15 | 江苏美特林科特殊合金有限公司 | Electrode coating and preparation method thereof |
| CN104030407A (en) * | 2014-06-05 | 2014-09-10 | 盐城工学院 | Electrochemical pretreatment method of metalaxyl pesticide wastewater |
| CN106365265A (en) * | 2016-11-21 | 2017-02-01 | 北京益清源环保科技有限公司 | Modified zeolite particle electrode with function of removing phenol through electrocatalysis and preparation method |
| CN108217851A (en) * | 2018-01-09 | 2018-06-29 | 北京大学 | A kind of method using iridium dioxide electrode electro-catalysis processing TNT waste water |
| CN109706513A (en) * | 2019-03-12 | 2019-05-03 | 江阴安诺电极有限公司 | The preparation method of coated anode plate |
| CN109763021A (en) * | 2019-03-27 | 2019-05-17 | 贵州省过程工业技术研究中心 | A kind of low Ag metal composite anode materials preparation method |
| CN112795974A (en) * | 2020-12-25 | 2021-05-14 | 西安泰金工业电化学技术有限公司 | Preparation method of titanium anode for PCB electroplating |
| CN114892247A (en) * | 2022-05-26 | 2022-08-12 | 山东聚力焊接材料有限公司 | Welding wire copper plating device, electrode plate manufacturing method and welding wire copper plating method |
| CN114892247B (en) * | 2022-05-26 | 2024-02-09 | 山东聚力焊接材料有限公司 | Welding wire copper plating device, electrode plate manufacturing method and welding wire copper plating method |
| CN114950089A (en) * | 2022-06-11 | 2022-08-30 | 华中科技大学 | Electrochemical degradation method for chlorine-containing volatile/semi-volatile organic compound |
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