CN105712428A - Antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode and preparation method thereof - Google Patents
Antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode and a preparation method thereof.The antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode consists of a titanium dioxide nanotube array substrate, an antimony-doped tin oxide intermediate layer and an antimony-doped tin oxide compound carbon nanotube active layer.A titanium-based titanium dioxide nanotube array is firstly prepared by adopting an anodic oxidation method to serve as a substrate material, the antimony-doped tin oxide intermediate layer is prepared by adopting a sol-gel method, and finally the carbon nanotube compounded antimony /tin oxide active layer is prepared by adopting a pulse electrodeposition method, and the antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode is obtained.By utilizing the high specific surface area of carbon nanotubes and introducing an antimony/tin dioxide composite material, the electric catalysis efficiency of the electrode is greatly improved, so that the electrode has the synergic effect of electric catalysis-adsorption.In addition, tin-antimony and antimony-tin intermediate layer doped in the carbon nanotubes form a eutectoid, the service life of the electrode is prolonged, and the electrode has a great application value in the field of electrochemical catalysis.
Description
Technical field
The invention belongs to electro catalytic electrode technical field, be specifically related to a kind of antimony-doped stannic oxide-CNT composite adsorption
Property electrode and preparation method thereof.
Background technology
Organic wastewater with difficult degradation thereby brings serious environmental pollution, traditional water treatment technology can not by its from water environment thoroughly
Remove.Electrochemical oxidation process, with its high efficiency, eco-friendly feature, attracts wide attention.Electrochemical oxidation process master
To be not required to additionally add reductant-oxidant with electronics as reagent, it is to avoid other interpolation medicament and the secondary pollution that causes are asked
Topic, reaction condition is gentle, simple to operate, is a kind of energy-conservation green technology.Electrochemical reaction occurs at plate table
Face, it is anode material that the characteristic of anode has been largely fixed organic degradation efficiency, electrode material and electrode pattern
The emphasis of preparation research.
In recent years, CNT attracts wide attention because of its high intensity, remarkable electric conductivity and chemical stability.Many walls
CNT is mainly made up of the coaxial pipe of several layers to tens of layers the carbon atom of hexagonal arrangement, has metallic conduction
Property, it is highly suitable to be applied for electro-catalysis field.The CNT of acidified modification forms CNT fragment, and at it
Surface introduces a series of oxy radical such as hydroxyl, carboxyl, improves CNT dispersibility in aqueous and stability.
Document 1 (Preparation of Ti/SnO2-Sb electrodes modified by carbon nanotube for anodic
oxidation of dye wastewater and combination with nanofiltration,Electrochimica Acta 2014,
117,192-201.) by the most carbon nano tube-doped enter in stannum antimony electrodeposit liquid, use the method for pulse electrodeposition by stannum antimony
Deposit on titanio, prepare carbon nano tube modified stannum antimony electrode, effectively enhance electrode to organic oxidative degradation
Ability, but this electrode life is short.Therefore, exploitation titanio stannic oxide electrode, extends its service life and improves further
Its treatment effect to organic wastewater with difficult degradation thereby, tool is of great significance.
Summary of the invention
For the deficiency that in prior art, stannic oxide electrode electro-catalysis efficiency is low, electrode life is short, the invention provides one
Kind of electro-catalysis efficiency is high, have electro-catalysis-absorbing synergic effect, the antimony-doped stannic oxide-CNT of length electrode life is multiple
Close adsorptivity electrode.
The technical scheme is that a kind of antimony-doped stannic oxide-CNT composite adsorption electrode, by titanium dioxide
Nano-tube array matrix, antimony-doped stannic oxide intermediate layer and antimony-doped stannic oxide composite carbon nanometer tube active layer composition.
The present invention also provides for the preparation method of above-mentioned antimony-doped stannic oxide-CNT composite adsorption electrode, and one mixes antimony
The preparation method of tin dioxide-carbon nanotube composite adsorption electrode, specifically comprises the following steps that
Step 1, titanium plate surface polished smooth, clean up, after suitable acid etching as anode, rustless steel as negative electrode,
Isobarically Control, containing 0.07～0.08mol/L Fluohydric acid., 0.095～0.105mol/L electrolyte and 0.95～1.05mol/L
The electrolyte Anodic Oxidation 60～70min of concentrated sulphuric acid, then rinses well titanium plate, prepares titanium in 450～500 DEG C of roastings
Based titanium dioxide nanotube matrix；
Step 2, by titanium-based titanium dioxide nanotube matrix in citric acid, organic solvent, Tin tetrachloride pentahydrate and trichlorine
The mol ratio changing antimony is 120～150:25～45:7～carries out dipping brushing in the mixed solution of 10:1, is dried afterwards, weight
The step that multiple dipping is brushed and is dried, finally prepares in 450～500 DEG C of roastings and has the electrode in antimony-doped stannic oxide intermediate layer；
Step 3, is modified CNT in the mixed solution of the concentrated nitric acid that volume ratio is 1:3～5 and concentrated sulphuric acid,
Then 1.5～2.5mol/L the Butter of antimony. aqueous solution of stannum dichloride aqueous solution, 0.5～1.5mol/L, 2～3mol/L nitre
Acid silver aqueous solution and concentrated nitric acid mixed solution in be modified, wherein stannum dichloride aqueous solution, Butter of antimony. aqueous solution,
The volume ratio of silver nitrate aqueous solution and concentrated nitric acid is 0.8～1.2:0.3～0.7:3～8:20～30, with water eccentric cleaning in
The electrode in antimony-doped stannic oxide intermediate layer step 2 prepared after property is as anode, carbon nano tube suspension after modification
In carry out electro-deposition, electro-deposition voltage is 20V, and electrodeposition time is 10～15min, and cathode and anode spacing is 1～1.5cm,
Dried under atmosphere of inert gases, the 550～600 DEG C of prepared antimony-doped stannic oxide of calcining-CNT composite adsorption electricity
Pole.
Preferably, in step 1, described electrolyte is sodium fluoride or potassium fluoride.
Preferably, in step 1, the heating rate of roasting is 1～2 DEG C/min, roasting time 3～5h.
Preferably, in step 2, the heating rate of roasting is 1～2 DEG C/min, and roasting time is 1～2h.
Preferably, in step 2, described organic solvent is ethylene glycol or isopropanol.
Preferably, in step 3, calcination time is 3～5h.
Further, the present invention provides above-mentioned antimony-doped stannic oxide-CNT composite adsorption electrode at electrocatalytic oxidation
Application in hardly degraded organic substance.
Compared with prior art, its remarkable advantage is the present invention:
The antimony-doped stannic oxide of the present invention-CNT composite adsorption electrode have Nano tube array of titanium dioxide matrix,
Antimony-doped stannic oxide intermediate layer and antimony-doped stannic oxide composite carbon nanometer tube active layer.CNT active layer makes electrode to having
Machine thing has an absorbability, and in stannum antimony intermediate layer and CNT, the stannum antimony of doping has oxidation to the Organic substance of absorption
Degradation, makes electrode have electro-catalysis-absorbing synergic effect, thus effectively enhances the electro-catalysis efficiency of electrode；With
Time CNT in stannum antimony and the stannum antimony intermediate layer of doping form eutectic, improve electrode life, can be widely applied to
The electrocatalytic oxidation of persistent organic pollutants.
Accompanying drawing explanation
Fig. 1 is Nano tube array of titanium dioxide (a), electrode (b) containing antimony-doped stannic oxide intermediate layer and embodiment 1
The FESEM figure of middle gained antimony-doped stannic oxide-CNT composite adsorption electrode (c).
Fig. 2 is Nano tube array of titanium dioxide (a), electrode (b) containing antimony-doped stannic oxide intermediate layer and embodiment 1
The contact angle figure of middle gained antimony-doped stannic oxide-CNT composite adsorption electrode (c).
Fig. 3 is multi-walled carbon nano-tubes (a), gained in electrode (b) containing antimony-doped stannic oxide intermediate layer and embodiment 1
The XRD figure of antimony-doped stannic oxide-CNT composite adsorption electrode (c).
Fig. 4 is the cyclic voltammetry curve figure of embodiment 1 gained antimony-doped stannic oxide-CNT composite adsorption electrode.
Fig. 5 is embodiment 1 gained antimony-doped stannic oxide-CNT composite adsorption electrode and tradition antimony-doped stannic oxide
The clearance figure that electrode degrading phenol changed with the response time.
Fig. 6 is embodiment 1 gained antimony-doped stannic oxide-CNT composite adsorption electrode and tradition antimony-doped stannic oxide
The mineralising current efficiency figure that electrode degrading phenol changes with electrode access times.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.
Embodiment 1
Titanium plate is cut into size 1.0cm × 3.0cm, with sand papering titanium surface until flat smooth；Ultrasonic cleaning removes
Surface and oil contaminant；Then in 18% hydrochloric acid solution, heat 20min remove oxide layer；Finally it is placed in deionized water standby.
Using the titanium plate handled well as anode, an equal amount of corrosion resistant plate is negative electrode, and controlling plate immerses electrolyte 2cm, plate
Spacing 1.0cm, quickly stirs with magnetic stirring apparatus simultaneously, and electrolyte is 0.07mol/L Fluohydric acid., 0.095mol/L fluorine
Changing potassium and 0.95mol/L sulfur aqueous acid, controlling operation voltage is 20V, takes out, spend after anodic oxidation 70min
Ion rinses, and is warming up to 500 DEG C with the speed of 1 DEG C/min after drying in Muffle furnace, and roasting 3h naturally cools to room
Temperature i.e. prepares Nano tube array of titanium dioxide matrix.
By titanium-based titanium dioxide nanotube matrix in the mixing of citric acid, ethylene glycol, Tin tetrachloride pentahydrate and Butter of antimony.
Solution carries out dipping brush, be dried, repeat this step.Citric acid, ethylene glycol, Tin tetrachloride pentahydrate and tri-chlorination
The mol ratio of antimony is 120:25:7:1.450 DEG C of roastings prepare the electrode with antimony-doped stannic oxide intermediate layer, and heating rate is
1 DEG C/min, roasting time is 1h.
CNT is first modified in the concentrated nitric acid that volume ratio is 1:3 and concentrated sulphuric acid and mixed solution.Then exist
The mixed solution of 1.5mol/L stannum dichloride, 0.5mol/L Butter of antimony., 2mol/L silver nitrate aqueous solution and concentrated nitric acid enters
Row modification, the volume ratio of stannum dichloride, Butter of antimony., silver nitrate aqueous solution and concentrated nitric acid is 0.8:0.3:3:20, with water from
The heart cleans to neutral.Again the electrode with antimony-doped stannic oxide intermediate layer is hanged as anode, CNT after modification
Carrying out electro-deposition in supernatant liquid, electro-deposition voltage is 20V, and electrodeposition time is 10min, and cathode and anode spacing is 1cm.Dry
After dry, under atmosphere of inert gases, roasting calcining heat is 550 DEG C, and calcination time is 3h, prepares novel antimony-doped stannic oxide
-CNT composite adsorption electrode.
Fig. 1 is Nano tube array of titanium dioxide (a), electrode (b) containing antimony-doped stannic oxide intermediate layer and embodiment 1
The FESEM figure of middle gained antimony-doped stannic oxide-CNT composite adsorption electrode (c).In figure, Titanium base is height
Orderly nano-tube array, stannum antimony interlayer surfaces is fine and close, CNT active layer and stannum antimony intermediate layer strong bonded.
Fig. 2 is Nano tube array of titanium dioxide (a), electrode (b) containing antimony-doped stannic oxide intermediate layer and embodiment 1
The contact angle figure of middle gained antimony-doped stannic oxide-CNT composite adsorption electrode (c).It can be seen that due to carbon
The existence of nanotube active layer, the hydrophobicity of electrode increases, and beneficially Organic substance is in the absorption on its surface, but electrode surface
Still in hydrophilic, do not affect the electrolysis effectiveness of electrode.
Fig. 3 is multi-walled carbon nano-tubes (a), gained in electrode (b) containing antimony-doped stannic oxide intermediate layer and embodiment 1
The XRD figure of antimony-doped stannic oxide-CNT composite adsorption electrode (c).Figure can analyze SnO2Crystal
Structure is tetragonal structure, only detects a small amount of titanium peak, SnO is described2Coating preferably covers Titanium base.Carbon nanometer
Pipe 002 peak position overlaps with stannum 110, so the peak of CNT not detected in combination electrode.
Fig. 4 is the cyclic voltammetry curve figure of gained antimony-doped stannic oxide in embodiment 1-CNT composite adsorption electrode,
In figure, the cyclic voltammetry curve of combination electrode has obvious oxidoreduction peak.
Embodiment 2
Titanium plate is cut into size 1.0cm × 3.0cm, with sand papering titanium surface until flat smooth；Ultrasonic cleaning removes
Surface and oil contaminant；Then in 18% hydrochloric acid solution, heat 20min remove oxide layer；Finally it is placed in deionized water standby.
Using the titanium plate handled well as anode, an equal amount of corrosion resistant plate is negative electrode, and controlling plate immerses electrolyte 2cm, plate
Spacing 1.0cm, quickly stirs with magnetic stirring apparatus simultaneously, and electrolyte is 0.08mol/L Fluohydric acid., 0.105mol/L fluorine
Changing sodium and 1.05mol/L sulfur aqueous acid, controlling operation voltage is 20V, takes out, spend after anodic oxidation 60min
Ion rinses, and is warming up to 450 DEG C with the speed of 2 DEG C/min after drying in Muffle furnace, and roasting 5h naturally cools to room
I.e. prepare Nano tube array of titanium dioxide matrix.
By titanium-based titanium dioxide nanotube matrix in the mixing of citric acid, ethylene glycol, Tin tetrachloride pentahydrate and Butter of antimony.
Solution carries out dipping brush, be dried, repeat this step.Citric acid, isopropanol, Tin tetrachloride pentahydrate and tri-chlorination
The mol ratio of antimony is 150:45:10:1.500 DEG C of roastings prepare the electrode with antimony-doped stannic oxide intermediate layer, heating rate
Being 2 DEG C/min, roasting time is 1h.
CNT is first modified in the concentrated nitric acid that volume ratio is 1:5 and concentrated sulphuric acid and mixed solution.Then exist
The mixed solution of 2.5mol/L stannum dichloride, 1.5mol/L Butter of antimony., 3mol/L silver nitrate aqueous solution and concentrated nitric acid enters
Row modification, the volume ratio of stannum dichloride, Butter of antimony., silver nitrate aqueous solution and concentrated nitric acid is 1.2:0.7:8:30, with water from
The heart cleans to neutral.Again the electrode with antimony-doped stannic oxide intermediate layer is hanged as anode, CNT after modification
Carrying out electro-deposition in supernatant liquid, electro-deposition voltage is 20V, and electrodeposition time is 10min, and cathode and anode spacing is 1cm.Dry
After dry, under atmosphere of inert gases, roasting calcining heat is 600 DEG C, and calcination time is 5h, prepares novel antimony-doped stannic oxide
-CNT composite adsorption electrode.
Embodiment 3
Antimony-doped stannic oxide-CNT composite adsorption the electrode of preparation in comparing embodiment 1
(Ti-NTs/SnO2-Sb/CNTs) and according to the titanio stannic oxide electrode prepared of electrodeposition process of document 1 report
(TiO2/SnO2-Sb) the Electrocatalysis Degradation effect of Pyrogentisinic Acid (Phenol).
Compound concentration is each 100mL of BA simulated wastewater of 100mg/L, each addition 0.1M Na2SO4As electrolyte,
Respectively by Ti-NTs/SnO2-Sb/CNTs and TiO2/SnO2-Sb electrode is as anode, and rustless steel, as negative electrode, controls electricity
Current density 30mA/cm2, compare the electrocatalytic oxidation property of two kinds of electrode Pyrogentisinic Acids.
Fig. 5 is the Ti-NTs/SnO of the present invention2-Sb/CNTs electrode and TiO2/SnO2When-Sb electrode degrading phenol is with reaction
Between change clearance figure.It can be seen that after electrolysis 3h, Ti-NTs/SnO2-Sb/CNTs electrode and TiO2/SnO2-Sb
The clearance of electrode Pyrogentisinic Acid is respectively 83.2% and 65.7%, and the Ti-NTs/SnO of preparation is described2-Sb/CNTs electrode has
There is higher electrocatalytic oxidation property.
Embodiment 4
Antimony-doped stannic oxide-CNT composite adsorption electrode (the Ti-NTs/SnO of preparation in embodiment 12-Sb/CNTs)
And TiO2/SnO2The adsorption effect of-Sb electrode Pyrogentisinic Acid.
Compound concentration is each 100mL of BA simulated wastewater of 100mg/L, and Pyrogentisinic Acid adsorbs 3h under agitation,
5 adsorption tests are repeated under similarity condition.
Fig. 6 is the present embodiment Ti-NTs/SnO2-Sb/CNTs electrode and TiO2/SnO2-Sb electrode degrading phenol makes with electrode
Adsorption of Phenol spirogram with number of times change.Ti-NTs/SnO in figure2-Sb/CNTs electrode Pyrogentisinic Acid in the case of no power have
The adsorbance of 42.3%, and along with the increase of access times, the adsorbance of electrode Pyrogentisinic Acid slowly reduces, but does not has
In traditional stannum antimony electrode of CNT active layer and document 1, the carbon nano tube modified stannum antimony electrode of report does not possess absorption
Effect.
Claims (8)
1. antimony-doped stannic oxide-CNT composite adsorption electrode, it is characterised in that described mixes antimony titanium dioxide
Tin-carbon nanometer tube composite adsorption electrode is by Nano tube array of titanium dioxide matrix, antimony-doped stannic oxide intermediate layer and mixes antimony
Tin ash composite carbon nanometer tube active layer forms.
The preparation side of a kind of antimony-doped stannic oxide the most according to claim 1-CNT composite adsorption electrode
Method, it is characterised in that specifically comprise the following steps that
Step 1, titanium plate surface polished smooth, clean up, after suitable acid etching as anode, rustless steel as negative electrode,
Isobarically Control, containing 0.07～0.08mol/L Fluohydric acid., 0.095～0.105mol/L electrolyte and 0.95～1.05mol/L
The electrolyte Anodic Oxidation 60～70min of concentrated sulphuric acid, then rinses well titanium plate, prepares titanium in 450～500 DEG C of roastings
Based titanium dioxide nanotube matrix；
Step 2, by titanium-based titanium dioxide nanotube matrix in citric acid, organic solvent, Tin tetrachloride pentahydrate and trichlorine
The mol ratio changing antimony is 120～150:25～45:7～carries out dipping brushing in the mixed solution of 10:1, is dried afterwards, weight
The step that multiple dipping is brushed and is dried, finally prepares in 450～500 DEG C of roastings and has the electrode in antimony-doped stannic oxide intermediate layer；
Step 3, is modified CNT in the mixed solution of the concentrated nitric acid that volume ratio is 1:3～5 and concentrated sulphuric acid,
Then 1.5～2.5mol/L the Butter of antimony. aqueous solution of stannum dichloride aqueous solution, 0.5～1.5mol/L, 2～3mol/L nitre
Acid silver aqueous solution and concentrated nitric acid mixed solution in be modified, wherein stannum dichloride aqueous solution, Butter of antimony. aqueous solution,
The volume ratio of silver nitrate aqueous solution and concentrated nitric acid is 0.8～1.2:0.3～0.7:3～8:20～30, with water eccentric cleaning in
The electrode in antimony-doped stannic oxide intermediate layer step 2 prepared after property is as anode, carbon nano tube suspension after modification
In carry out electro-deposition, electro-deposition voltage is 20V, and electrodeposition time is 10～15min, and cathode and anode spacing is 1～1.5cm,
Dried under atmosphere of inert gases, the 550～600 DEG C of prepared antimony-doped stannic oxide of calcining-CNT composite adsorption electricity
Pole.
The preparation side of a kind of antimony-doped stannic oxide the most according to claim 2-CNT composite adsorption electrode
Method, it is characterised in that in step 1, described electrolyte is sodium fluoride or potassium fluoride.
The preparation side of a kind of antimony-doped stannic oxide the most according to claim 2-CNT composite adsorption electrode
Method, it is characterised in that in step 1, the heating rate of roasting is 1～2 DEG C/min, roasting time 3～5h.
The preparation side of a kind of antimony-doped stannic oxide the most according to claim 2-CNT composite adsorption electrode
Method, it is characterised in that in step 2, the heating rate of roasting is 1～2 DEG C/min, and roasting time is 1～2h.
The preparation side of a kind of antimony-doped stannic oxide the most according to claim 2-CNT composite adsorption electrode
Method, it is characterised in that in step 2, described organic solvent is ethylene glycol or isopropanol.
The preparation side of a kind of antimony-doped stannic oxide the most according to claim 2-CNT composite adsorption electrode
Method, it is characterised in that calcination time is 3～5h.
A kind of antimony-doped stannic oxide-CNT composite adsorption electrode the most according to claim 1 and 2 is urged at electricity
Change the application in oxidation hardly degraded organic substance.
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| CN114772685A (en) * | 2022-04-26 | 2022-07-22 | 南京理工大学 | Electrochemical device applied to oily wastewater treatment and treatment method thereof |
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