CN109824123A - A kind of SnO2- NiO oxide coating electrode and its preparation method and application - Google Patents
A kind of SnO2- NiO oxide coating electrode and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of SnO2- NiO oxide coating electrode and preparation method thereof and degradation methyl orange solution application, the electrode is respectively by stannous chloride, nickel chloride is dissolved in dehydrated alcohol, then the stannous chloride that will be obtained, the solution of nickel chloride mixes by a certain percentage, certain proportion is measured every time to be coated on Titanium base, and the SnO of optimal components is obtained using thermal decomposition method2- NiO oxide coating electrode, SnO of the invention2- NiO oxide coating electrode significantly can remove methyl orange solution in neutral conditions, have a good application prospect in electrolytic industry.
Description
Technical field
The invention belongs to functional electric catalysis electrode technical fields, and in particular to a kind of SnO2- NiO oxide coating electrode
And its preparation method and application.
Background technique
China's water resource there is currently main problem be that shortage of water resources and water pollution are serious.The dyestuff discharged at present is useless
Water high organic content, biochemical is poor, COD high, and BOD/COD is low, and coloration is high, and complicated component is toxic, direct emission this
Class waste water will cause serious environmental pollution, and being effectively treated and recycling to such waste water can alleviate China's water resource
The pressure of shortage, methyl orange are a kind of common acid indicators, are largely present in waste water from dyestuff and a kind of more difficult to degrade
Azo colored compound, the absorption peak at 460 nm is the suction generated by methyl orange-N==N-azo colour developing group
There is good linear corresponding relations between receipts peak and solution concentration, so selecting model of the methyl orange as Electrocatalysis Degradation
Compound.Electro-catalytic oxidation technology is the main means of the processing of organic wastewater, because it can be H organic matter permineralization2O
And CO2It waits small-molecule substances and receives significant attention.
" core " of electro-catalytic oxidation technology is electrode material, and influence electrochemistry waste water treatment process it is main because
Element.The pairs of electrode performance of element group of electrode can produce a very large impact, and different acid-base property is often presented in the industrial wastewater of discharge,
Being also required to corresponding electro catalytic electrode could effectively degrade to it.Therefore the property of the electrode of research heterogeneity proportion
Can, to the catalytic effect of the organic solution of different pH values, the maximum electro-catalysis effect of electrode can be played.SnO2/ Ti electricity
Pole is a kind of higher electrode of overpotential for oxygen evolution, and current efficiency is higher, with SnO2DSA electrode based on coating, to difficult in waste water
The organic pollutant of biochemical degradation has a higher degradation efficiency, at the same electrodes in base metal can be greatly lowered industrial application at
This, and then receive significant attention.
Summary of the invention
The purpose of the present invention is to provide a kind of SnO2- NiO oxide coating electrode is applied to containing neutral and acid
Electrolyte methyl orange degradation, can to organic matter complete decomposition, to achieve the above object, the present invention adopts the following technical scheme:
A kind of SnO2The preparation method of-NiO oxide coating electrode the following steps are included:
(1) stannous chloride and nickel chloride for weighing certain mass, are dissolved in dehydrated alcohol respectively, carry out by a certain percentage
Mixing, sonic oscillation are allowed to be uniformly dissolved, and obtain the mixed solution of stannous chloride and nickel chloride；
(2) mixed solution of the stannous chloride of resulting different mol ratio and nickel chloride is put into chamber type electric resistance furnace drying, centainly
Grinding is taken out after time, places into drying, repeatedly grinding drying, is taken out behind several days, gained powder sample need to be superfine, in Germany
The resistance to suitable temperature range of synchronous solving setting of speeding is tested, and is obtained sample transition temperature, is determined annealing temperature；
(3) step (1) is obtained into mixed solution, is painted on Titanium base using certain carrying capacity single side is drawn with pipettor gun, often
Through infrared illumination curing after secondary coating, chamber type electric resistance furnace thermal oxide is placed into, brushed-dried repeatedly-thermal oxide is until reach
Suitable load, it is last it is annealed, come out of the stove air-cooled, obtain the Ti/Ni of heterogeneityxSn1-xO2 (0≤x≤1) electrode；
Further, stannous chloride and nickel chloride molar ratio are (4 ~ 10): (1 ~ 6) in the mixed solution that step (1) obtains.
Further, 2 ~ 8h is divided into step (2) between drying-milling time, synchronous solving setting temperature range is
300~1000℃。
Further, coating carrying capacity in step (3) every time is 1 ~ 30 μ L, is brushed 2 ~ 15 times altogether, oxidate temperature 300-
700 DEG C, curing time is 1 ~ 20min, and thermal oxidation time is 1 ~ 30min, and annealing degenerate temperature is 300 ~ 700 DEG C.
SnO is made in above-mentioned preparation method2- NiO oxide coating electrode is applied to degradation methyl orange solution, specific steps
Are as follows: by methyl orange respectively with Na2SO4Powder and concentrated sulfuric acid mixing, and be added in 1L deionized water, it is uniformly mixing to obtain neutral item
The methyl orange solution of part and acid condition is put it into respectively in the water-bath with certain temperature, then by SnO2- NiO oxidation
Object coated electrode is placed under three-electrode system, using timing voltage method, with a constant current to methyl orange solution on potentiostat
Degradation certain time takes a sample every several minutes, carries out ultra-violet and visible spectrophotometer test.
Above-mentioned methyl orange and Na2SO4Quality be respectively 0 ~ 50mg and 10 ~ 30g, H2SO4Volume be 10 ~ 30mL, water-bath
Pot temperature is 20 ~ 50 DEG C, and potentiostat electric current is 0.1 ~ 2A, and degradation time is 0.5 ~ 6h, sample interval 30min.
Remarkable advantage of the invention is:
(1) present invention is prepared for a kind of SnO using thermal decomposition method2- NiO oxide coating electrode, enhances coating and Titanium base
Between binding force, slow down the wear rate of electrode coating；Interface resistance is reduced, the catalytic performance of electrode can be improved.
(2) present invention is prepared for a kind of novel SnO2- NiO oxide coating electrode is replaced expensive using base metal elements
Metallic element, raw materials used cheap, process stabilizing, catalytic activity has also obtained a degree of raising, has reached practical
Change and industrialized condition.
(3) present invention has studied SnO2Electro-catalysis of-NiO the oxide coating electrode in neutral and acidic methylene orange solution
Effect finds SnO2- NiO oxide coating electrode can make the methyl orange solution fully degraded of neutrallty condition, under acid condition
SnO2- NiO oxide coating electrode electrode coating causes catalytic effect to decline due to falling off, SnO2- NiO oxide coating
Electrode is applicable in neutral solution, can be with SnO2- NiO oxide coating electrode the service life is extended, and the work of electro catalytic electrode is reduced
Industry chemical conversion is originally.
Detailed description of the invention
Fig. 1 is the XRD diagram of embodiment 1-4 counter electrode；
Fig. 2 is removal rate curve of the embodiment 1-4 counter electrode in neutral (a) and acid (b) condition Methyl Orange；
The small ultraviolet absorptivity figure of the electrode of Fig. 3 embodiment 3 methyl orange degradation product under the conditions of neutral (a) and acid (b)；
Fig. 4 is the polarization curve of embodiment 1-4 counter electrode.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
(1) by stannous chloride, nickel chloride is separately added into dehydrated alcohol dissolution, and 9:1 is allowed to be sufficiently mixed in molar ratio, then single side
It is painted on Titanium base, it is 1.5mg that tin element, which coats carrying capacity, every time through infrared illumination curing 10 minutes after coating；
(2) by gained stannous chloride, the mixed solution of nickel chloride is put into chamber type electric resistance furnace drying, takes out grinding after 2 ~ 8h, then put
Enter drying, repeatedly grinding drying, taken out behind several days, gained powder sample need to be superfine, sets in the resistance to synchronous solving of speeding of Germany
Setting maximum temperature is to be tested at 700 DEG C, obtains sample transition temperature, determines the annealing temperature of sample；
(3) electrode prepared is placed on 500 DEG C of thermal oxide 10min in chamber type electric resistance furnace, come out and cooled down.Brushing-drying-repeatedly
Thermal oxide comes out of the stove air-cooled until masking liquid is used up finally in 500 DEG C of 2 h of annealing, obtains the Ti/Ni of heterogeneity0.1Sn0.9O2Electricity
Pole；
(4) methyl orange of 20mg and the Na of 14.2g are weighed2SO4Powder measures the concentrated sulfuric acid of 27.2ml, be separately added into 1L go from
It in sub- water, stirs evenly, configuration is obtained into methyl orange solution and is put into the water-bath with 45 DEG C, the electrode obtained is placed in three electrodes
Under system, using chronoamperometry, with 0.5A electric current respectively to 2 kinds of one timings of methyl orange mixed solution degradation on potentiostat
Between, a sample is taken every several minutes, carries out ultra-violet and visible spectrophotometer test respectively.
Embodiment 2
(1) by stannous chloride, nickel chloride is separately added into dehydrated alcohol dissolution, and 8:2 is allowed to be sufficiently mixed in molar ratio, then single side
It is painted on Titanium base, it is 1.5mg that tin element, which coats carrying capacity, every time through infrared illumination curing 10 minutes after coating；
(2) by gained stannous chloride, the mixed solution of nickel chloride is put into chamber type electric resistance furnace drying, takes out grinding after 2 ~ 8h, then put
Enter drying, repeatedly grinding drying, taken out behind several days, gained powder sample need to be superfine, sets in the resistance to synchronous solving of speeding of Germany
Setting maximum temperature is to be tested at 700 DEG C, obtains sample transition temperature, determines the annealing temperature of sample；
(3) electrode prepared is placed on 500 DEG C of thermal oxide 10min in chamber type electric resistance furnace, come out and cooled down.Brushing-drying-repeatedly
Thermal oxide comes out of the stove air-cooled until masking liquid is used up finally in 500 DEG C of 2 h of annealing, obtains the Ti/Ni of heterogeneity0.2Sn0.8O2Electricity
Pole；
(4) methyl orange of 20mg and the Na of 14.2g are weighed2SO4Powder measures the concentrated sulfuric acid of 27.2ml, be separately added into 1L go from
It in sub- water, stirs evenly, configuration is obtained into methyl orange solution and is put into the water-bath with 45 DEG C, the electrode obtained is placed in three electrodes
Under system, using chronoamperometry, degraded certain times to 2 kinds of methyl orange solutions respectively on potentiostat with 0.5A electric current,
A sample is taken every several minutes, carries out ultra-violet and visible spectrophotometer test respectively.
Embodiment 3
(1) by stannous chloride, nickel chloride is separately added into dehydrated alcohol dissolution, and 7:3 is allowed to be sufficiently mixed in molar ratio, then single side
It is painted on Titanium base, it is 1.5mg that tin element, which coats carrying capacity, every time through infrared illumination curing 10 minutes after coating；
(2) by gained stannous chloride, the mixed solution of nickel chloride is put into chamber type electric resistance furnace drying, takes out grinding after 2 ~ 8h, then put
Enter drying, repeatedly grinding drying, taken out behind several days, gained powder sample need to be superfine, sets in the resistance to synchronous solving of speeding of Germany
Setting maximum temperature is to be tested at 700 DEG C, obtains sample transition temperature, determines the annealing temperature of sample；
(3) electrode prepared is placed on 500 DEG C of thermal oxide 10min in chamber type electric resistance furnace, come out and cooled down.Brushing-drying-repeatedly
Thermal oxide comes out of the stove air-cooled until masking liquid is used up finally in 500 DEG C of 2 h of annealing, obtains the Ti/Ni of heterogeneity0.3Sn0.7O2Electricity
Pole；
(4) methyl orange of 20mg and the Na of 14.2g are weighed2SO4Powder measures the concentrated sulfuric acid of 27.2ml, be separately added into 1L go from
It in sub- water, stirs evenly, configuration is obtained into methyl orange solution and is put into the water-bath with 45 DEG C, the electrode obtained is placed in three electrodes
Under system, using chronoamperometry, degraded certain times to 2 kinds of methyl orange solutions respectively on potentiostat with 0.5A electric current,
A sample is taken every several minutes, carries out ultra-violet and visible spectrophotometer test respectively.
Embodiment 4
(1) by stannous chloride, nickel chloride is separately added into dehydrated alcohol dissolution, and 6:4 is allowed to be sufficiently mixed in molar ratio, then single side
It is painted on Titanium base, it is 1.5mg that tin element, which coats carrying capacity, every time through infrared illumination curing 10 minutes after coating；
(2) by gained stannous chloride, the mixed solution of nickel chloride is put into chamber type electric resistance furnace drying, takes out grinding after 2 ~ 8h, then put
Enter drying, repeatedly grinding drying, taken out behind several days, gained powder sample need to be superfine, sets in the resistance to synchronous solving of speeding of Germany
Setting maximum temperature is to be tested at 700 DEG C, obtains sample transition temperature, determines the annealing temperature of sample；
(3) electrode prepared is placed on 500 DEG C of thermal oxide 10min in chamber type electric resistance furnace, come out and cooled down.Brushing-drying-repeatedly
Thermal oxide comes out of the stove air-cooled until masking liquid is used up finally in 500 DEG C of annealing 2h, obtains the Ti/Ni of heterogeneity0.4Sn0.6O2Electricity
Pole；
(4) methyl orange of 20mg and the Na of 14.2g are weighed2SO4Powder measures the concentrated sulfuric acid of 27.2ml, be separately added into 1L go from
It in sub- water, stirs evenly, configuration is obtained into methyl orange solution and is respectively put into the water-bath with 45 DEG C, the electrode obtained is placed in three
Under electrode system, using chronoamperometry, with 0.5A electric current respectively to 2 kinds of one timings of methyl orange solution degradation on potentiostat
Between, a sample is taken every several minutes, carries out ultra-violet and visible spectrophotometer test respectively.
Fig. 1 is embodiment 1-4 stannous chloride, the XRD spectrum of the electrode of nickel chloride different proportion preparation.26.5 ° and 33.8 °
Diffraction maximum correspond to SnO2Crystal face, 43.2 ° of diffraction maximum corresponds to the crystal face of NiO, it is seen that when Ni content is lower
When, only there is SnO2Diffraction maximum, when Sn:Ni atomic molar ratio reaches 7:3, the diffraction maximum of NiO just starts to occur, Sn:
When Ni atomic molar ratio is 7:3, electrode electro-catalysis effect is preferable.
Fig. 2 is removal rate curve of the counter electrode in neutral (a) and acid (b) condition Methyl Orange.It is seen that
The removal rate of methyl orange reduces afterwards as the increase of Ni content first increases, and Sn, Ni atomic molar ratio are 7:3 removal rate highest, system
Standby SnO2- NiO oxide coating electrode can be up to 82% to the methyl orange removal rate under the conditions of neutrality, and electrode is to acidity
Under the conditions of methyl orange degradation rate highest only up to 64%.
Fig. 3 is the small ultraviolet light absorption of electrode methyl orange degradation product under the conditions of neutral (a) and acid (b) of embodiment 3
Degree figure, absorption peak of the curve methyl orange at 462 position nm existing characteristics absorption peaks, 462 nm be by methyl orange-N==
The absorption peak that N-azo colour developing group generates.As can be seen from Figure, the absorbance of methyl orange subtracts with the increase of degradation time
It is small.By the degradation of 3h, the absorbance of methyl orange is high in the dulling luminosity ratio neutral solution of methyl orange in acid solution, explanation
SnO2- NiO oxide coating electrode can make the methyl orange solution fully degraded of neutrallty condition.
Fig. 4 is embodiment 1-4 stannous chloride, the polarization of electrode curve graph of nickel chloride different proportion preparation.It can from figure
Find out, electrode is in Na2SO4Oxygen evolution reaction occurs when current potential is greater than 1.5 V in solution, electric current starts to increase rapidly, when Sn:Ni original
Sub- molar ratio is the electrode oxygen evolution potential highest of 7:3, when degrading using constant current, has best electro-catalysis effect.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (6)
1. a kind of SnO2The preparation method of-NiO oxide coating electrode, it is characterised in that: the following steps are included:
(1) stannous chloride and nickel chloride for weighing certain mass, are dissolved in dehydrated alcohol respectively, carry out by a certain percentage
Mixing, sonic oscillation are allowed to be uniformly dissolved, and obtain the mixed solution of stannous chloride and nickel chloride；
(2) step (1) is obtained into mixed solution, is painted on Titanium base using certain carrying capacity single side is drawn with pipettor gun, often
Through infrared illumination curing after secondary coating, chamber type electric resistance furnace thermal oxide is placed into, brushed-dried repeatedly-thermal oxide is until reach
Suitable load, it is last it is annealed, come out of the stove air-cooled, obtain the Ti/Ni of heterogeneityxSn1-xO2Electrode, 0≤x≤1.
2. SnO according to claim 12The preparation method of-NiO oxide coating electrode, it is characterised in that: step (1) is mixed
The molar ratio for closing Chlorine in Solution stannous and nickel chloride is (4 ~ 10): (1 ~ 6).
3. SnO according to claim 12The preparation method of-NiO oxide coating electrode, it is characterised in that: every in step (3)
Secondary coating carrying capacity is 1 ~ 30 μ L, is brushed 2 ~ 15 times altogether, and oxidate temperature is 300 ~ 700 DEG C, and curing time is 1 ~ 20min, hot oxygen
The change time is 1 ~ 30min, and annealing time is 1 ~ 5h, and degenerate temperature is 300 ~ 700 DEG C.
4. SnO made from a kind of preparation method according to any one of claims 1-42- NiO oxide coating electrode.
5. a kind of SnO as claimed in claim 52Application of-NiO the oxide coating electrode in degradation methyl orange, feature exist
In: with Na2SO4Solution is electrolyte, and the Electrocatalysis Degradation of methyl orange is carried out using the electrode.
6. SnO according to claim 52Application of-NiO the oxide coating electrode in degradation methyl orange, feature exist
In: the Na2SO4The concentration of solution is 10 ~ 30g/L, and degradation temperature is 20 ~ 50 DEG C, and electric current used is 0.1 ~ 2A, degradation time
For 0.5 ~ 6h.
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Cited By (1)
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| CN111871420A (en) * | 2020-08-03 | 2020-11-03 | 重庆工业职业技术学院 | Preparation method and application of titanium-based stannic oxide-supported fluorite nickel oxide electrocatalyst |
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