CN104370348A - Electrocatalytic oxidation coated electrode for treating oilfield wastewater and preparing method thereof - Google Patents
Electrocatalytic oxidation coated electrode for treating oilfield wastewater and preparing method thereof Download PDFInfo
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- CN104370348A CN104370348A CN201410540861.9A CN201410540861A CN104370348A CN 104370348 A CN104370348 A CN 104370348A CN 201410540861 A CN201410540861 A CN 201410540861A CN 104370348 A CN104370348 A CN 104370348A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/463—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrocoagulation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
- C02F2001/46138—Electrodes comprising a substrate and a coating
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses an electrocatalytic oxidation coated electrode for treating oilfield wastewater and a preparing method thereof, wherein the preparing method comprises the following steps: preparing a titanium-based polar plate; mixing arbitrary one or more of iridium trichloride (Cl3Ru), tantalum chloride (Cl5Ta), platinum chloride (Cl4Pt2) and iridium chloride (IrCl3H2O) with ethanol, and after mixing evenly, coating the surface of the titanium-based polar plate with a hair brush; coating the MnO2 surface layer; drying; and sintering at the high temperature to form the titanium-based coated electrode. The electrode having better structural strength can be obtained by the method, and the effective reaction area and the service life of an electrode material are improved. The electrode can effectively remove dispersed oil and emulsified oil in the oily wastewater, can overcome the disadvantage that a common electrode lose efficacy because of being easily polluted by oil stain, can be widely and effectively applied to the fields of oilfield wastewater treatment and reinjection and the like, has the advantages of good treatment effect, good oil pollution resistance performance, small electrode loss, simple preparation method and operation, and good reproducibility, and is suitable for large-scale production and popularization.
Description
Technical field
The invention belongs to technical field of electrochemistry, coating of metal oxides titanium-matrix electrode being specifically related to an oily water treatment and preparation method thereof.
Background technology
Along with petrochemical industry is fast-developing, numerous industries such as ti-based coating electrode arises at the historic moment, and is widely used in chemical industry, environmental protection, water electrolysis, water treatment, electrometallurgy, plating.Titanium has stable protect oxide layer as base material, so have good weather resistance and stability under saline electrolysis condition.Metal titanium can be random mechanical workout, titanium plate can be made, titanium rod, titanium silk, titanium net, titanium pipe, porous plate etc., are widely used.
Coating of metal oxides Ti electrode, demonstrates incomparable remarkable performance, very fast in many electrolytic industry acquisition widespread uses, brings very large benefit through national economy.Compared with traditional Graphite Electrodes, lead 2-base alloy electrode, Ti electrode has the following advantages: power consumption is little, long working life, the corrosion of metal anode chlorine-resistant and alkali; Overcome the problem of graphite anode and lead anode dissolving consumption; The short circuit problem after being out of shape can be avoided, thus can improve current efficiency; Ti electrode is lightweight, can reduce labor intensity; Shape makes easily, can manufacture by high precision int; Matrix can Reusability; Low overpotential characteristic, between electrode, the bubble of surface and electrode is easily got rid of, and effectively can reduce bath voltage.
The performance of investigation of titanium anode coated with metal oxide is become better and better, and kind is also on the increase, and mainly contains titanium base ruthenium system coated electrode, titanium base iridium system coated electrode, Ti supported manganese dioxide coated electrode and ti-supported lead dioxide electric coated electrode.
Oily(waste)water is the source of sewage that in petroleum industry, output is maximum, accounts for 90% of oilfield sewage total amount.A large amount of oilfield sewages is as not thorough in process, and direct discharge can cause serious water environment pollution and whose wasting of resources; Reinjection into reservoir then can cause the blocking on stratum, reduces the rate of permeation on stratum, thus causes the decline of output.In oilfield sewage, oil content exists in a variety of forms, is broadly divided into oil slick, dispersed oil, oil in water emulsion according to the size of oil droplet.Oil slick particle diameter > 100 μm, accounts for about 80% of oil-containing total amount; Dispersed oil particle diameter 10 ~ 100 μm, unstable, oil slick or oil in water emulsion can be converted into; Oil in water emulsion particle diameter 0.1 ~ 10 μm, this part oil accounts for about 10% of oil-containing total amount; Oil in water emulsion is small due to particle diameter, there is the protection of electrostatic double layer or emulsifying agent, form stable, and conventional water treatment means are difficult to be removed, and therefore must carry out break milk separation by electrocatalysis means.
Adopt electrode to carry out oily water treatment and early have research, but due to oil-contaminated water of oil field complicated component, adopt traditional electrode to be easily polluted by the oil, perishable, and easily because pole plate distortion causes the reasons such as short circuit, do not obtain applying energetically in oil-field water process field.Conventional titanium base ruthenium system coated electrode, titanium base iridium system coated electrode, Ti supported manganese dioxide coated electrode and ti-supported lead dioxide electric coated electrode is adopted to run into such-and-such problem: if Ti supported manganese dioxide coated electrode catalytic activity and corrosion resistance are all not as good as titanium base ruthenium system's coated electrode and titanium base iridium system coated electrode; Titanium base ruthenium system's coated electrode and titanium base iridium system coated electrode expensive, and in actual production, when anode separates out oxygen, ruthenium system coating can sharply be damaged; And titanium base iridium system coated electrode is low due to oxygen overpotential, avoid above problem, but other performance is unsatisfactory, electrode coating easily peels off; Ti-supported lead dioxide electric coated electrode is large due to electrodeposition distortion, enbrittles, processing difficulties, and yield rate is low, is not suitable for scale production; Not only the preparation method of coating of metal oxides Ti electrode has a great impact its actual serviceability.Therefore, exploitation is a kind of economic and practical, can extensively and effectively apply to the field such as disposing polluted water in oil, re-injection, treatment effect is good, and fuel sensitivity is good, corrosion resistance and good, export license is little, preparation method is simple to operate, has good reproducibility, is applicable to the large-scale ti-based coating electrode produced and promote and has very important significance in oil-field water treating processes.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of new ti-based coating electrode and preparation method thereof.While the excellent oily water treatment performance of guarantee, have oil resistant corrosion resistance concurrently, and realize preparation technology simple to operation simultaneously.
Process a catalytic oxidation coated electrode for oilfield sewage, it is successively by titanium base stage plate, iridous chloride (Cl
3ru), tantalum chloride (Cl
5ta), platinum chloride (Cl
4pt
2), iridium chloride (IrCl
3h
2the middle layer of any one or a few composition coating O), MnO
2the top layer composition of coating.
Process a preparation method for the catalytic oxidation coated electrode of oilfield sewage, comprise following steps:
A, prepare titanium base stage plate;
B, with iridous chloride (Cl
3ru), tantalum chloride (Cl
5ta), platinum chloride (Cl
4pt
2), iridium chloride (IrCl
3h
2o) any one or a few in mixes with ethanol, mixes rear hairbrush and is coated to titanium base polar board surface;
C, coating MnO
2top layer;
D, drying;
E, high temperature sintering form ti-based coating electrode.
Can add in Manganse Dioxide, cobalt oxide, nickel oxide, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, nickelous nitrate in described step B any one or a few.
Described step C mesexine adopts thermal decomposition method and electrodip process to hocket to prepare manganese bioxide coated.
Described thermal decomposition method is by manganous nitrate wiring solution-forming, is coated in after on Titanium base with hairbrush, at 100 DEG C ~ 120 DEG C temperature, carries out thermolysis.
Described electrodip process prepares manganese bioxide coated formula: 150 g/L MnSO
4, 50 g/L H
2sO
4.
Drying means in described step D is 100 degrees Celsius.
The temperature of the high temperature sintering in described step e is 500 degrees Celsius.
Process current density 0.50 A/dm in described electrodip process
2, time 10 ~ 30min.
In described electrodip process, battery lead plate thickness is 1.0 ~ 3.0 mm, and more excellent scope is 1.5 ~ 1.8mm.
The object of this invention is to provide a kind of catalytic oxidation coated electrode processing oilfield sewage and preparation method thereof, while ensureing excellent oil-containing water treatment effect, realize simple preparation technology.The present invention selects titanium-matrix electrode plate, and the preparation method of described oily water treatment electrode special comprises: preparation coating solution, and by specific noble-metal coated to substrate surface, dry the battery lead plate forming appointed thickness, high temperature sintering four part is formed; Beneficial effect of the present invention is: can be obtained the electrode with better structural strength by the inventive method, improves effective affecting acreage and the work-ing life of electrode materials.This electrode effectively can remove dispersed oil in oily(waste)water and oil in water emulsion, can overcome the shortcoming that ordinary electrode was easily lost efficacy by oil pollution.Can extensively and effectively apply to the field such as disposing polluted water in oil, re-injection, treatment effect is good, and fuel sensitivity is good, and export license is little, and preparation method is simple to operate, has good reproducibility, is applicable to large-scale production and popularization.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Do detailed introduction below in conjunction with concrete embodiment to the present invention: as shown in Figure 1: a kind of catalytic oxidation coated electrode processing oilfield sewage, it is successively by titanium base stage plate, iridous chloride (Cl
3ru), tantalum chloride (Cl
5ta), platinum chloride (Cl
4pt
2), iridium chloride (IrCl
3h
2the middle layer of any one or a few composition coating O), MnO
2the top layer composition of coating.
A kind of preparation method containing the special ti-based coating electrode of sewage disposal provided by the present invention, comprises two large key steps:
The first step: be coated with brush applied coating.
First, select TA1 or TA2 type titanium base material as pole plate raw material, titanium base stage board size is L × d=1500 × (700 ~ 1000) mm.For tabular or netted, mesh grille is rhombus, specification 2 × 1 mm, 3 × 6 mm, 3 × 2 mm, 4.5 × 12.5 mm, 5 × 10 mm, 6 × 10 mm, 5 × 12 mm etc.
Using the iridous chloride (Cl as middle layer
3ru), tantalum chloride (Cl
5ta), platinum chloride (Cl
4pt
2), iridium chloride (IrCl
3h
2o) any one or plurality of raw materials in are that solvent mixes according to a certain percentage with ethanol, mix rear hairbrush and be coated to titanium base polar board surface, simultaneously can add suitable additive, additive include but not limited in Manganse Dioxide, cobalt oxide, nickel oxide, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, nickelous nitrate any one or a few.
The mass ratio of above-described titanium base material in battery lead plate is 60% ~ 95%; The mass percent of coat in electrode material is 0% ~ 35%, and the mass percent of additive in electrode material is 0 ~ 13%.
Adopt mixing raw material to be coated with brush applied coating, not only compensate for the various defects in use of single coating, and well solve Cost Problems.
First on titanium base stage plate, apply above-mentioned middle layer with hairbrush, then apply MnO
2top layer.
The MnO that thermal decomposition method and electrodip process obtain
2coating respectively has superiority: the coating that thermal decomposition method obtains has higher catalytic activity, and the Coating Durability that electrodip process obtains is better.Therefore top layer adopts thermal decomposition method and electrodip process to hocket to prepare manganese bioxide coated.
By manganous nitrate wiring solution-forming, be coated in after on Titanium base with hairbrush, carry out thermolysis.
The reaction formula of thermolysis is:
Mn(NO
3)
2→ MnO
2+ 2NO
2↑
Electrodip process prepares manganese bioxide coated composition and engineering: 150 g/L MnSO
4, 50 g/L H
2sO
4, current density 0.50 A/dm
2, time 10 ~ 30min.
Galvanic deposit anodic reaction is:
Mn
2++2H
2O+2e → MnO
2+ 2H
2↑
Second step: high temperature sintering forms a kind of oily water treatment dress ti-based coating electrode.
After painting brush applied coating completes, by pole plate horizontal, 100 DEG C of oven drying at low temperatures, are placed on high temperature sintering in 500 DEG C of equipment.The battery lead plate thickness produced is 1.0 ~ 3.0 mm, and coat-thickness is 20 μm.
Embodiment 1
(1) TA1 is selected to be base material;
(2) with alcohol dilution, the molar fraction of Ru is 0.3%, La as the molar fraction of additive is 0.2% ~ 0.4%.One deck is applied as middle layer with hairbrush.
(3) adopting thermal decomposition method and electrodip process to hocket to prepare the manganese bioxide coated coat-thickness that obtains is 20 μm.
(4) by pole plate horizontal, 100 DEG C of oven drying at low temperatures, are placed on high temperature sintering in 500 DEG C of equipment, and obtain a kind of catalytic oxidation coated electrode processing oilfield sewage, electrode performance is splendid, and oil resistant pollution capacity is strong.
Embodiment 2
(1) TA2 is selected to be base material;
(2) with alcohol dilution, the molar fraction of Ir is the molar fraction of 33%, Ta is 10%.One deck is applied as middle layer with hairbrush.
(3) repeat the operation of embodiment 1, obtain a kind of catalytic oxidation coated electrode processing oilfield sewage, oil resistant pollution capacity is strong.
Embodiment 3
(1) TA1 is selected to be base material;
(2) with alcohol dilution, the molar fraction of Ru is the molar fraction of 20%, Ir is 11%, applies one deck as middle layer with hairbrush.
(3) repeat the operation of embodiment 1, obtain a kind of catalytic oxidation coated electrode processing oilfield sewage.
Embodiment 4
Oilfield sewage in the present embodiment, takes from Daqing oil field sewage works, and the ti-based coating electrode adopting embodiment 3 to prepare, carries out oily(waste)water experiment, Q=2m by a certain amount of water sample insert experiment device
3/ h runs 100d, and Inlet and outlet water water-quality guideline is as follows.
The present embodiment is not limited to the present invention, and every employing similarity method of the present invention and similar change thereof, all should list protection scope of the present invention in.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Term practical herein, does not get rid of the possibility using other term.These terms are used to be only used to describe and explain essence of the present invention more easily; The restriction that they are construed to any one additional is all contrary with spirit of the present invention.
Claims (10)
1. process a catalytic oxidation coated electrode for oilfield sewage, it is successively by titanium base stage plate, iridous chloride (Cl
3ru), tantalum chloride (Cl
5ta), platinum chloride (Cl
4pt
2), iridium chloride (IrCl
3h
2the middle layer of any one or a few composition coating O), MnO
2the top layer composition of coating.
2. the special ti-based coating electrode of oily water treatment according to claim 1, is characterized in that described coat-thickness is 20um; The thickness of described coated electrode is 1.0-3.0mm.
3. process a preparation method for the catalytic oxidation coated electrode of oilfield sewage, it is characterized in that comprising following steps:
Prepare titanium base stage plate;
With iridous chloride (Cl
3ru), tantalum chloride (Cl
5ta), platinum chloride (Cl
4pt
2), iridium chloride (IrCl
3h
2o) any one or a few in mixes with ethanol, mixes rear hairbrush and is coated to titanium base polar board surface;
Coating MnO
2top layer;
Dry;
High temperature sintering forms ti-based coating electrode.
4. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 3, it is characterized in that can adding in described step B in Manganse Dioxide, cobalt oxide, nickel oxide, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, nickelous nitrate any one or a few.
5. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 3, is characterized in that described step C mesexine adopts thermal decomposition method and electrodip process to hocket to prepare manganese bioxide coated.
6. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 5, is characterized in that described thermal decomposition method is by manganous nitrate wiring solution-forming, is coated in after on Titanium base, at 100 DEG C ~ 120 DEG C temperature, carries out thermolysis with hairbrush.
7. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 5, is characterized in that described electrodip process is prepared manganese bioxide coated formula and is: 150 g/L MnSO
4, 50 g/L H
2sO
4.
8. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 3, is characterized in that the drying means in described step D is 100 degrees Celsius.
9. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 3, is characterized in that the temperature of the high temperature sintering in described step e is 500 degrees Celsius.
10. the preparation method of the special ti-based coating electrode of oily water treatment according to claim 7, is characterized in that process current density 0.50 A/dm in described electrodip process
2, time 10 ~ 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410540861.9A CN104370348A (en) | 2014-10-14 | 2014-10-14 | Electrocatalytic oxidation coated electrode for treating oilfield wastewater and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410540861.9A CN104370348A (en) | 2014-10-14 | 2014-10-14 | Electrocatalytic oxidation coated electrode for treating oilfield wastewater and preparing method thereof |
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|---|---|
| CN104370348A true CN104370348A (en) | 2015-02-25 |
Family
ID=52549594
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|---|---|---|---|
| CN201410540861.9A Pending CN104370348A (en) | 2014-10-14 | 2014-10-14 | Electrocatalytic oxidation coated electrode for treating oilfield wastewater and preparing method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110316917A (en) * | 2019-07-01 | 2019-10-11 | 任丘市谛赛驷环保科技有限公司 | A kind of preparation method for the advanced oxidation system handling oily sludge |
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| CN101225526A (en) * | 2007-10-29 | 2008-07-23 | 北京科技大学 | Nanocrystalline manganese bioxide coated anode and method for making same |
| CN102229442A (en) * | 2011-04-20 | 2011-11-02 | 上海电力学院 | Method for treating printing and dyeing wastewater with rare earth cerium doped titanium-based manganese dioxide electrode |
| CN103539228A (en) * | 2013-10-30 | 2014-01-29 | 北京师范大学 | Multiphase electro-catalytic industrial wastewater treatment device for efficiently removing heterocyclic compounds |
| KR20140056544A (en) * | 2012-10-29 | 2014-05-12 | 한국에너지기술연구원 | Cathode catalyst for lithium-air battery, method of manufacturing the same, and lithium-air battery comprising the same |
-
2014
- 2014-10-14 CN CN201410540861.9A patent/CN104370348A/en active Pending
Patent Citations (4)
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| CN101225526A (en) * | 2007-10-29 | 2008-07-23 | 北京科技大学 | Nanocrystalline manganese bioxide coated anode and method for making same |
| CN102229442A (en) * | 2011-04-20 | 2011-11-02 | 上海电力学院 | Method for treating printing and dyeing wastewater with rare earth cerium doped titanium-based manganese dioxide electrode |
| KR20140056544A (en) * | 2012-10-29 | 2014-05-12 | 한국에너지기술연구원 | Cathode catalyst for lithium-air battery, method of manufacturing the same, and lithium-air battery comprising the same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110316917A (en) * | 2019-07-01 | 2019-10-11 | 任丘市谛赛驷环保科技有限公司 | A kind of preparation method for the advanced oxidation system handling oily sludge |
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Effective date of abandoning: 20180112 |