CN108793342A - A kind of preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in water - Google Patents
A kind of preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in water Download PDFInfo
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- CN108793342A CN108793342A CN201810716965.9A CN201810716965A CN108793342A CN 108793342 A CN108793342 A CN 108793342A CN 201810716965 A CN201810716965 A CN 201810716965A CN 108793342 A CN108793342 A CN 108793342A
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- cobalt
- titanium
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- water
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Classifications
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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
- C02F1/46—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
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
-
- 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
- C02F2001/46142—Catalytic 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
Abstract
The invention belongs to water-treatment technology fields, it is related to a kind of preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in water, first the soluble precursor compound of cobalt, the soluble precursor compound of titanium and polyvinylpyrrolidone are dissolved in alcoholic solvent and catalyst precursor coating liquid are made, this coating liquid is coated in titanium plate, then obtains nano Co by drying, after thermal sintering successively3O4/TiO2Combination electrode.Advantage for present invention is：(1) compared with conventional precious metal catalyst (such as palladium, platinum), the price of cobalt be its more than one percent.(2) by adding butyl titanate, so that catalyst is generated solid solution at high temperature with titanium oxide, the combination of catalyst and titanium substrate is not only advantageous to, while also improving the stability of catalyst, to improve the service life of electrode.(3) by adding PVP, keep the dispersibility of catalyst more preferable, generate more active sites, to improve the efficiency that electrode restores nitrate anion.
Description
Technical field
The invention belongs to water-treatment technology fields, are related to a kind of titanium-matrix electrode coated with nano metal composite particles, tool
Body is related to a kind of preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in water.
Background technology
With greatly developing for industrial economy, a large amount of nutriment flows into receiving water body, leads to body eutrophication, shadow
Ring aquatile growth and breeding, cause it is huge ecology and economic loss, wherein nitrogen class be cause body eutrophication and
One of an important factor for pollution.Nitrate concentration in drinking water is excessively high, can induce some water bodys and generate some nitrosamines
Carcinogen causes newborn to be susceptible to suffer from methemoglobinemia (also known as " indigo plant answers syndrome ").And after nitrate enters human body
Generation nitrite can be decomposed, and nitrite is a kind of extremely toxic substance.In consideration of it, " Chinese water quality standard for drinking water "
(GB5749-2006) it provides, the greatest contamination object concentration of NO3-N and NO2-N ion is respectively 10.0mg/L and 0.1mg/
L。
Go water removal in the most common technology of nitrate include：(a) physico-chemical process, including ion exchange, absorption, electrodialysis and
It is reverse osmosis；(b) bioanalysis and (c) chemical method, such as active metal and catalytic hydrogenation.However, in physical and chemical process, nitrate
It can only be transferred to from water phase in resin or adsorbent, this needs is subsequently further processed.In chemical process, extraction and nanometer iron metal
The pH value of water is highly dependent on aluminum reduction process, this is severely limited in purifying water process.In bioprocess, by
In stringent pH value, the requirement of additional Organic Compounds and dissolved oxygen conditions, denitrification process is difficult to control, while also being needed
Post processor is wanted to remove by-product, such as biomass, organic matter, the muddy harmful bacteria secretion in drinking water.Past two
Over 10 years, the electrochemistry denitrogenation method of nitrate reductase reaction is furtherd investigate, because this technology can be not additional
Reducing agent H2In the case of use, and do not have biological risks.But the denitrification rates of this process are usually very low.
In order to improve nitrate reduction rate, researcher usually mutually ties electrochemical process and catalytic reduction process
It closes.They modify cathode surface by fixed noble metal catalyst, either use solid noble metal as electrode or will be electric
Catalytic activity ion is added in reaction solution etc. to develop electro-catalysis denitrification system.But since the height of noble metal is rare
And the costliness of price so that the practical application of noble metal catalyst receives serious limitation.
Invention content
According to the above-mentioned deficiencies of the prior art, the present invention provides the nanometer that a kind of low cost, activity be high, chemical property is stablized
The preparation method of combination electrode.
The technical scheme is that：A kind of preparation side for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in water
Method, it is characterised in that：First by the soluble precursor compound of cobalt, the soluble precursor compound of titanium and polyvinylpyrrolidine
Ketone (PVP), which is dissolved in alcoholic solvent, is made catalyst precursor coating liquid, this coating liquid is coated in titanium plate, then is passed through successively
Nano Co is obtained after drying, thermal sintering3O4/TiO2Combination electrode.
In the present invention, using the soluble precursor compound of cobalt as catalyst raw material, the soluble precursor compound of titanium
It is nanoparticie dispersion agents as stabilizer, PVP, three is dissolved according to a certain percentage, is mixed in alcoholic solvent.It is solidifying with colloidal sol
Glue method prepares nano Co for principle3O4/TiO2Combination electrode.Sol-gal process is a kind of wet-chemical preparing nanometer grade powder
Method is to be configured to metal organic or inorganic compound with the chemical reagent of liquid or metal alkoxide predecessor, predecessor are dissolved in
Uniform solution is formed in solvent, solute generates hydrolysis or alcoholysis reaction with solvent, generates the stable and sol body without precipitation
It is to be changed into gel after placement a period of time or after being dried colloidal sol, a large amount of liquid phase substance is usually contained in gel,
It needs to eventually form the nanometer grade powder of respective substance using heat treatment using extraction or evaporated liquid medium.
Wherein, preferred embodiment is as follows：
The soluble precursor compound of the cobalt is nitrate, acetate, the chlorate of cobalt, and cobalt is dense in coating liquid
Degree is 0.5mol/L~5mol/L.
The soluble precursor compound of the titanium is butyl titanate, titanium chloride or titanium sulfate, with coating liquid
Volume ratio is 1：5~50.Wherein, butyl titanate is most preferably added, when adding butyl titanate, it is also necessary to water and salt be added
Acid, for preventing tetrabutyl titanate hydrolysis.
The molecular weight that the polyvinylpyrrolidone is selected is 50,000~1,300,000, solid-to-liquid ratio 1:2~20.
The alcoholic solvent is ethyl alcohol or ethylene glycol.
For the titanium plate using preceding by pre-processing, the pretreatment includes with sand paper polishing, sulfuric acid corrosion, deionization
Water is spare after being cleaned by ultrasonic.
The coating liquid is coated in titanium plate 2-10 times, and every time by drying after coating, drying temperature is 80~100
℃。
The thermal sintering temperature is 400~600 DEG C, and the thermal sintering time is 30min~6h.
Prepared by the present invention obtains nano Co3O4/TiO2Combination electrode is used for the principle of nitrate anion in reductive water：Electrification
Learn denitrification process in nitrate anion reduction reaction substantially, as shown in formula (1,2).When containing chlorion in water body, in sun
The oxidisability chlorine that pole reaction generates can convert the ammonium ion of generation to nitrogen (formula (3,4)), to finally realize water body
The removing of middle total nitrogen.
2NO3 -+6H2O+10e-→N2+12OH- (1)
NO3 -+7H2O+8e-→NH4 ++10OH- (2)
Cl-+H2O-2e-→2H++ClO- (3)
3ClO-+2NH4 +→3H2O+3Cl-+N2+2H+ (4)
Cobalt, titanium and PVP mixed solutions coated in titanium-matrix electrode surface after aerobic high-temperature calcination, can mainly with
The form payload of the solid solution of cobaltosic oxide and titanium dioxide is conducive to extend the service life of electrode on Ti electrode.
There is high dispersive effect to be conducive to catalysed particulate and exist with the nanotopography disperseed, carried to be played to catalytic performance by wherein PVP
Rise effect.
Advantage for present invention is：(1) compared with conventional precious metal catalyst (such as palladium, platinum), the price of cobalt
Only its more than one percent.(2) by addition butyl titanate, catalyst is made to generate solid solution at high temperature with titanium oxide,
It is not only advantageous to the combination of catalyst and titanium substrate, while also improving the stability of catalyst, to improve making for electrode
With the service life, electrode does not occur obviously to inactivate using 1000~1800min.(3) by adding PVP, make the dispersibility of catalyst more
It is good, more active sites are generated, to improve the efficiency that electrode restores nitrate anion.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, to the technology in the embodiment of the present invention
Scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1：
It is spare after titanium sheet sand paper polishing, sulfuric acid corrosion, deionized water are cleaned by ultrasonic.
It is uniform to measure 6mL ethyl alcohol, 1mL butyl titanates, 1mL water, 1mL mixed in hydrochloric acid, weighs 8.73g cobalt nitrates and 2g
PVP is dissolved in wherein, and strong stirring makes cobalt nitrate be uniformly dispersed, and it is coating liquid to make a concentration of 3mol/L of cobalt, this solution.It will
Brush soaks in coating liquid, sweeps away brushing repeatedly in processed titanium plate, is then dried at a temperature of 100 DEG C, one time one
Face.This process was repeated ten times, and then in 600 DEG C of temperature lower calcinations 3 hours, heating rate is 5 DEG C of per minute, natural coolings, i.e.,
It must remove the electrode of nitrate in water removal.
Using this electrode as the nitrate in cathodic reduction water, nitrate anion initial concentration is 50mg/L, chlorine ion concentration
For 1000mg/L, initial pH is in neutral range without adjustment, after reaction carries out 90min, nitrate anion removal rate up to 90% with
On, and the generation that can't detect ammonium ion in whole process is reacted, product almost 100% is nitrogen.And electrode life
It is strengthened.
Embodiment 2：
Titanium sheet pre-processes and electrode preparation method such as example 1, except that the ingredient of coating liquid, coating liquid matches in this example
System is as follows：It is uniform to measure 6mL ethyl alcohol, 1mL butyl titanates, 1mL water, 1mL mixed in hydrochloric acid, weighs 7.14g cobalt chlorides and 2g
PVP is dissolved in wherein, and strong stirring makes cobalt chloride be uniformly dispersed, and it is coating liquid to make a concentration of 3mol/L of cobalt, this solution.It applies
It covers with calcination operation as described for example 1.
Using this electrode as the nitrate in cathodic reduction water, nitrate anion initial concentration is 50mg/L, chlorine ion concentration
For 1000mg/L, initial pH is in neutral range without adjustment, after reaction carries out 90min, nitrate anion removal rate up to 90% with
On, and the generation that can't detect ammonium ion in whole process is reacted, product almost 100% is nitrogen.And electrode life
It is strengthened.
Embodiment 3：
Titanium sheet pre-processes and electrode preparation method such as example 1, except that the ingredient of coating liquid, coating liquid matches in this example
System is as follows：It is uniform to measure 6mL ethyl alcohol, 1mL butyl titanates, 1mL water, 1mL mixed in hydrochloric acid, weighs 5.82g cobalt nitrates and 2g
PVP is dissolved in wherein, and strong stirring makes cobalt nitrate be uniformly dispersed, and it is coating liquid to make a concentration of 2mol/L of cobalt, this solution.It applies
Cover it is similar to example 1 with calcination operation, unlike coating number be four times, calcination temperature be 400 degree.
Using this electrode as the nitrate in cathodic reduction water, nitrate anion initial concentration is 50mg/L, chlorine ion concentration
For 1000mg/L, initial pH is in neutral range, after reaction carries out 120min, nitrate anion removal rate is up to 90% without adjustment
More than, and the generation that can't detect ammonium ion in whole process is reacted, product almost 100% is nitrogen.
Embodiment 4：
Titanium sheet pre-processes and electrode preparation method such as example 1, except that the ingredient of coating liquid, coating liquid matches in this example
System is as follows：It is uniform to measure 6mL ethyl alcohol, 1mL butyl titanates, 1mL water, 1mL mixed in hydrochloric acid, weighs 7.14g cobalt nitrates and 1g
PVP is dissolved in wherein, and strong stirring makes cobalt nitrate be uniformly dispersed, and it is coating liquid to make a concentration of 3mol/L of cobalt, this solution.It applies
It covers same as Example 1 with calcination operation.
Using this electrode as the nitrate in cathodic reduction water, nitrate anion initial concentration is 50mg/L, chlorine ion concentration
For 1000mg/L, initial pH is in neutral range, after reaction carries out 120min, nitrate anion removal rate is up to 90% without adjustment
More than, and the generation that can't detect ammonium ion in whole process is reacted, product almost 100% is nitrogen.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case of can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (7)
1. a kind of preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in water, it is characterised in that：First by cobalt
Soluble precursor compound, the soluble precursor compound of titanium and polyvinylpyrrolidone are dissolved in be made in alcoholic solvent and urge
This coating liquid is coated in titanium plate by agent presoma coating liquid, then obtains nanometer by drying, after thermal sintering successively
Co3O4/TiO2Combination electrode.
2. the preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in a kind of water according to claim 1,
It is characterized in that：The soluble precursor compound of the cobalt is nitrate, acetate, the chlorate of cobalt, cobalt in coating liquid
A concentration of 0.5mol/L~5mol/L.
3. the preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in a kind of water according to claim 1,
It is characterized in that：The soluble precursor compound of the titanium is butyl titanate, titanium chloride or titanium sulfate, with coating liquid
Volume ratio be 1：5~50.
4. the preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in a kind of water according to claim 1,
It is characterized in that：The molecular weight that the polyvinylpyrrolidone is selected is 50,000~1,300,000, solid-to-liquid ratio 1:2~20.
5. the preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in a kind of water according to claim 1,
It is characterized in that：The alcoholic solvent is ethyl alcohol or ethylene glycol.
6. the preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in a kind of water according to claim 1,
It is characterized in that：The coating liquid is coated in titanium plate 2-10 time, every time by drying after coating, drying temperature for 80~
100℃。
7. the preparation method for the high dispersive cobalt titanium composite Nano electrode that nitrate nitrogen restores in a kind of water according to claim 1,
It is characterized in that：The thermal sintering temperature is 400~600 DEG C, and the thermal sintering time is 30min~6h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110304734A (en) * | 2019-06-17 | 2019-10-08 | 大连理工大学 | A kind of cultivation tail water New Method for Processing for strengthening removal of inorganic nitrogen using bacterium algae-catalysis electrode |
| CN110787799A (en) * | 2019-08-16 | 2020-02-14 | 浙江工业大学 | Preparation method of foamed copper oxide/TNTs photoelectric composite material |
| CN111807474A (en) * | 2019-04-10 | 2020-10-23 | 青岛理工大学 | Preparation method of phosphorus-doped cobalt nanowire array for nitrate-nitrogen reduction in water |
| CN112723493A (en) * | 2021-01-18 | 2021-04-30 | 华侨大学 | Cobaltosic oxide/magnesium oxide-titanium composite electrode, preparation method and application thereof, and treatment method of ammonia nitrogen-containing wastewater |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807474A (en) * | 2019-04-10 | 2020-10-23 | 青岛理工大学 | Preparation method of phosphorus-doped cobalt nanowire array for nitrate-nitrogen reduction in water |
| CN110304734A (en) * | 2019-06-17 | 2019-10-08 | 大连理工大学 | A kind of cultivation tail water New Method for Processing for strengthening removal of inorganic nitrogen using bacterium algae-catalysis electrode |
| CN110304734B (en) * | 2019-06-17 | 2021-05-11 | 大连理工大学 | Novel cultivation tail water treatment method for enhancing inorganic nitrogen removal by utilizing bacteria and algae-catalytic electrode |
| CN110787799A (en) * | 2019-08-16 | 2020-02-14 | 浙江工业大学 | Preparation method of foamed copper oxide/TNTs photoelectric composite material |
| CN110787799B (en) * | 2019-08-16 | 2022-08-23 | 浙江工业大学 | Preparation method of foamed copper oxide/TNTs photoelectric composite material |
| CN112723493A (en) * | 2021-01-18 | 2021-04-30 | 华侨大学 | Cobaltosic oxide/magnesium oxide-titanium composite electrode, preparation method and application thereof, and treatment method of ammonia nitrogen-containing wastewater |
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Application publication date: 20181113 |