CN103343378B - The preparation method of the high stability catalysis electrode that a kind of carbon nano tube-doped Nafion membrane is modified and application - Google Patents
The preparation method of the high stability catalysis electrode that a kind of carbon nano tube-doped Nafion membrane is modified and application Download PDFInfo
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Abstract
The preparation method of the high stability catalysis electrode that a kind of carbon nano tube-doped Nafion membrane is modified and application, belong to catalysis electrode technical field.The MWCNTs processed is scattered in the alcoholic solution of the Nafion that mass fraction is 0.05～0.15%, ultrasonic disperse, obtains uniform MWCNTs-Nafion suspension, take this uniform suspension and be coated in titanium on the net, naturally dry, obtain MWCNTs-Nafion/Ti；Again with MWCNTs-Nafion/Ti for negative electrode, platinized platinum is anode, with PdCl2Solution is electrolyte, and electro-deposition prepares carbon nano tube-doped Nafion membrane and modifies load Pd catalysis electrode, PdCl in electrolyte2Concentration is 5～10mmol/L, and initial pH is 0.2～0.4, and depositing current density is 5.0～7.5mA/cm2, sedimentation time is 50～70min.Electrode stability height prepared by the present invention significantly improves, and catalysis activity is high, cost is low, have certain application prospect.
Description
Technical field
The preparation method that the present invention relates to a kind of combination electrode, particularly relates to a kind of preparation method with carbon nano tube modified high stability load electrode, for the chlorinatedorganic electrochemical reduction dechlorination in water, belongs to catalysis electrode technical field.
Background technology
Chloro organic cpd, owing to its difficult degradation, majority have " three cause " effect, hazardness is great.On " blacklist " that international environmental protection tissue is announced; what rank the first is halides and the material that can form halides in the environment; owing to it is of a great variety; it is again important industrial chemicals, intermediate and organic solvent; thus it is widely used in the industries such as chemical industry, medicine, pesticide, process hides, tap water has detected chlorinatedorganic.Therefore, what up-to-date Chinese water standard was focused on very much is emphasized.In recent years, in water chlorinatedorganic minimizing technology research receive much concern.The method of every removal chlorinatedorganics such as Integrated comparative burning method, biological degradation method, absorption method, alkali metal reduction and electrochemical techniques.Electro-catalysis reduction dechlorination, as a kind of eco-friendly technology, it is believed that be the technology having application prospect most.It is by electrochemical reaction, the hydrogenation-dechlorination reaction in catalytic cathode, it is achieved remove chlorinatedorganic from sewage, and one of key technology of electrochemical reduction dechlorination is in that electrode.
Palladium (Pd) is because having the reactive hydrogen storage capability of excellence and higher overpotential of hydrogen evolution, it is possible to ensures reactive hydrogen and the abundant reaction of chloro organic point, and becomes the emphasis of catalyst research.The electrocatalytic hydrogenation dechlorination electrode reported in recent years, it is roughly divided into two classes: a class is based on the Pd electrode that the good material with carbon element of adsorptivity is carrier, such as, Pd/ NACF (Pd/ACF) electrode and Pd/ carbon felt electrode etc., the adsorptivity good due to material with carbon element and electric conductivity, thus there is co-catalysis effect, improve the catalysis activity of overall electrode, but, it is limited to the instability of substrate, and can not use continuously；The another kind of carrier being based on high stability, such as, Pd/ glass carbon (Pd/GC) electrode and Pd/ titanium (Pd/Ti) electrode, this kind of electrode improves the stability of substrate, but owing to directly depositing Pd in substrate, catalyst and carrier pull-out capacity are poor, easy to fall off, and catalysis activity is general, it is impossible to promote.
Summary of the invention
It is an object of the invention to solve the problems of the prior art, it is provided that the preparation method of the composite catalyzing electrode (Pd/MWCNTs-Nafion/Ti electrode) that the carbon nano tube-doped Nafion membrane of a kind of high stability and catalysis activity is modified.
The preparation method of Pd/MWCNTs-Nafion/Ti composite electro catalytic electrode provided by the present invention, comprises the following steps:
(1) by Palladous chloride. (PdCl2) powder is dissolved in hydrochloric acid, obtains the PdCl of 5～10mmol/L with deionized water dilution2Solution, adding HCl adjustment electrolyte pH is 0.2～0.4, add a certain amount of surfactant cetyl trimethylammonium bromide (CTAB), dodecyl sodium sulfate (SLS) or cetyl benzenesulfonic acid sodium (SDBS), obtain the CTAB of 0.05～0.10mmol/L, or 0.5～1.0mmol/LSLS, or the SDBS of 0.5～1.0mmol/L；
(2) after titanium net being embathed oil removing in sodium carbonate liquor, boiling with deoxygenation compound in oxalic acid solution, redistilled water cleans up, and nitrogen dries up standby；
(3) take multi-walled carbon nano-tubes (MWCNTs) and be immersed in concentrated nitric acid, 50～60 DEG C of ultrasonic 4h in ultrasound wave, filter, wash with secondary redistilled water, until filtrate is neutral, dry；
(4) take the MWCNTs processed that step (3) obtains and be scattered in the alcoholic solution of the Nafion that mass fraction is 0.05～0.15%, ultrasonic disperse 30min, obtain uniform MWCNTs-Nafion suspension (concentration of optimization treated MWCNTs is 1g/L), stand for standby use；
(5) taking the suspension that step (4) obtains, the Ti that uniform drop coating processed in step (2) is online, and room temperature is dried, and obtains MWCNTs-Nafion/Ti；
(6) with step (5) prepare MWCNTs-Nafion/Ti electrode for negative electrode, platinized platinum is anode, with PdCl prepared by step (1)2Solution is electrolyte, and electro-deposition prepares composite catalyzing electrode (Pd/MWCNTs-Nafion/Ti electrode), and depositing current density is 5.0～7.5mA/cm2, sedimentation time is 50～70min.
With the Pd/MWCNTs-Nafion/Ti electrode of above-mentioned preparation for catalytic cathode, for the chlorinatedorganic electrochemical reduction dechlorination in water, carry out dechlorination test with 2,4,6-trichlorophenols (2,4,6-TCP) for target contaminant, it is shown that high catalytic activity and high stability.
Compared with prior art, the method have the advantages that
(1) present invention adopts the alcoholic solution of Nafion, stablized, scattered MWCNTs-Nafion suspension, having fast filming characteristic owing to Nafion solution possesses, thus obtaining stable MWCNTs-Nafion/Ti modified membrane, the stability for combination electrode provides material base；
(2) present invention is with MWCNTs-Nafion for middle decorative layer, owing to MWCNTs is proton conductor, Nafion is electronic conductor, can change Pd depositional configuration on MWCNTs-Nafion film in electro-deposition, increase the degree of exposure of high activity Pd crystal face, and then increase the catalysis activity of electrode.
(3) present invention adopts the method for electrochemical deposition to prepare Pd/MWCNTs-Nafion/Ti electrode, and the stability in the large of electrode is high, and the catalysis activity of electrode is high, provides possibility for its further genralrlization.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of MWCNTs-Nafion/Ti modified membrane in embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of Pd/MWCNTs-Nafion/Ti combination electrode in embodiment 1.
Fig. 3 is the cyclic voltammetry curve of electrode 1, electrode 2, electrode 3 prepared by embodiment 1,2,3.
Fig. 4 is the dechlorination effect figure of 2,4,6-TCP on electrode 1 in embodiment 4.
Fig. 5 is that in embodiment 5, on electrode 1,2,4,6-TCP repeats dechlorination effect figure.
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Detailed description of the invention
Embodiment 1
(1) PdCl is weighed2Powder is dissolved in HCl, adds deionized water, is configured to the PdCl of 7mmol/L2Solution, adding HCl adjustment pH is 0.2；
(2), after Ti net being embathed 20min oil removing in the sodium carbonate liquor of 0.3mol/L, the oxalic acid solution of 0.1mol/L boils 30min(deoxygenation compound), redistilled water cleans up, and nitrogen dries up standby；
(3) take the MWCNTs of 0.5g in the concentrated nitric acid (mass fraction: 68%) of 50mL, in ultrasound wave ultrasonic 4h(50 DEG C), filter, with the washing of secondary redistilled water, until filtrate be neutral, dry under infrared lamp；
(4) MWCNTs processed taking 10mg step (3) is scattered in the alcoholic solution of the Nafion that 10mL mass fraction is 0.1%, ultrasonic disperse 30min, and obtaining concentration is the uniform MWCNTs-Nafion suspension of 1g/L, stand for standby use；
(5) taking the suspension that 0.1mL step (4) obtains, uniform drop coating is on the Ti net (2cm × 2cm) processed, and room temperature is dried, and obtains MWCNTs-Nafion/Ti；Its stereoscan photograph is shown in that Fig. 1, MWCNTs-Nafion anchor on Ti, and MWCNTs good dispersion；
(6) the MWCNTs-Nafion/Ti electrode obtained with step (5) is for negative electrode, and platinized platinum is anode, takes the PdCl of 50mL step 1) preparation2Solution, adds the surfactant CATB of 0.09mmol/L, with 6.25A/cm2Electric current, deposits 70min, prepares Pd/MWCNTs-Nafion/Ti combination electrode, rinses well, and 65 DEG C are dried overnight.Its scanning electron microscope is according to seeing Fig. 2, it can be seen that electrode surface has two kinds of pattern Pd crystal grains, and this morphosis is conducive to hydrogenation-dechlorination to react, i.e. catalysis activity is high；
By Pd/MWCNTs-Nafion/Ti electrode, it is placed in 0.5mol/LH2SO4In solution, with platinized platinum for electrode, with Hg/Hg2SO4Electrode is that reference electrode is circulated voltammetric scan.Electric potential scanning ranges for-800mV～800mV, and scanning speed is 50mV/s.Gained cyclic voltammetry curve is shown in a in Fig. 3, hydrogen adsorption peak occurs at about-650mV, and peak point current is-219.6mA.
Embodiment 2
(1) PdCl is taken2Powder is dissolved in HCl, adds deionized water, is configured to the PdCl of 5mmol/L2Solution, adding HCl adjustment pH is 0.3；
(2), after Ti net being embathed 20min oil removing in the sodium carbonate liquor of 0.3mol/L, the oxalic acid solution of 0.1mol/L boils 30min(deoxygenation compound), redistilled water cleans up, and nitrogen dries up standby；
(3) take the MWCNTs of 0.5g in the concentrated nitric acid (mass fraction: 68%) of 50mL, in ultrasound wave ultrasonic 3.5h(55 DEG C), filter, with the washing of secondary redistilled water, until filtrate be neutral, dry under infrared lamp；
(4) MWCNTs processed taking 10mg step (3) is scattered in the alcoholic solution of the Nafion that 10mL mass fraction is 0.05%, ultrasonic disperse 30min, and obtaining concentration is the uniform MWCNTs-Nafion suspension of 1g/L, stand for standby use；
(5) taking the suspension that 0.15mL step (4) obtains, uniform drop coating is on the Ti net (2cm × 2cm) processed, and room temperature is dried, and obtains MWCNTs-Nafion/Ti；
(6) the MWCNTs-Nafion/Ti electrode obtained with step 5) is for negative electrode, and platinized platinum is anode, takes the PdCl that 50mL step (1) is prepared2Solution, adds the surfactant SLS of 0.5mmol/L, with 5A/cm2Electric current, deposits 60min, and constant current prepares Pd/MWCNTs-Nafion/Ti combination electrode, rinses well, and 65 DEG C are dried overnight；
By Pd/MWCNTs-Nafion/Ti electrode, it is placed in 0.5mol/LH2SO4In solution, with platinized platinum for electrode, with Hg/Hg2SO4Electrode is that reference electrode is circulated voltammetric scan.Electric potential scanning ranges for-800mV～800mV, and scanning speed is 50mV/s.Gained cyclic voltammetry curve is shown in the b in Fig. 3, hydrogen adsorption peak occurs at about-650mV, and peak point current is-212.1mA.
Embodiment 3
(1) PdCl is weighed2Powder is dissolved in HCl, adds deionized water, is configured to the PdCl of 10mmol/L2Solution, adding HCl adjustment pH is 0.2；
(2), after Ti net being embathed 20min oil removing in the sodium carbonate liquor of 0.3mol/L, the oxalic acid solution of 0.1mol/L boils 30min(deoxygenation compound), redistilled water cleans up, and nitrogen dries up standby；
(3) take the MWCNTs of 0.5g in the concentrated nitric acid of 50mL, in ultrasound wave ultrasonic 4.5h(50 DEG C), filter, with the washing of secondary redistilled water, until filtrate be neutral, dry under infrared lamp；
(4) MWCNTs processed taking 10mg step (3) is scattered in the alcoholic solution of the Nafion that 10mL mass fraction is 0.15%, ultrasonic disperse 30min, and obtaining concentration is the uniform MWCNTs-Nafion suspension of 1g/L, stand for standby use；
(5) taking the suspension that 0.10mL step (4) obtains, uniform drop coating is on the Ti net (2cm × 2cm) processed, and room temperature is dried, and obtains MWCNTs-Nafion/Ti；
(6) the MWCNTs-Nafion/Ti electrode obtained with step (5) is for negative electrode, and platinized platinum is anode, takes the PdCl that 50mL step (1) is prepared2Solution, adds the surfactant SDBS of 0.5mmol/L, with 6.25A/cm2Electric current, deposits 70min, and constant current prepares Pd/MWCNTs-Nafion/Ti combination electrode, rinses well, and 65 DEG C are dried overnight；
By Pd/MWCNTs-Nafion/Ti electrode, it is placed in 0.5mol/LH2SO4In solution, with platinized platinum for electrode, with Hg/Hg2SO4Electrode is that reference electrode is circulated voltammetric scan.Electric potential scanning ranges for-800mV～800mV, and scanning speed is 50mV/s.Gained cyclic voltammetry curve is shown in the c in Fig. 3, hydrogen adsorption peak occurs at about-650mV, and peak point current is-229.3mA.
Embodiment 4
With the electrode 1 of embodiment 1 preparation for work negative electrode, Pt sheet is anode, with the 2,4 of 0.5mmol/L, 6-TCP is target contaminant, carries out electro-catalysis dechlorination test, and reactor is H type dual chamber electrolyzer, cylindrical single chamber volume 30mL, centre cation exchange membrane separates, and die opening is 8cm；
Dechlorination condition: supporting electrolyte is 0.05mol/L sodium sulfate, initial pH is 2.3, anode chamber's 0.05mmol/L aqueous sulfuric acid；Catholyte stirs with speed 400rpm, with the thorough dechlorination (see figure 4) of 6mA electric current, constant current dechlorination 80min, 2,4,6-TCP and intermediate product thereof.
Embodiment 5
With the electrode 1 of embodiment 1 preparation for work negative electrode, according to the dechlorination condition of embodiment 4, continuously performing a batch dechlorination experiment, namely same electrode is reused, and experimental result is shown in Fig. 5.After repeating 8 times, dechlorination efficiency remains in that 100%.
Above-described embodiment shows, Pd/MWCNTs-Nafion/Ti combination electrode prepared by the present invention, has higher electro-catalysis reduction dechlorination activity and stability, and photocatalyst crystals pattern has no report, hydrogen absorption peak, higher than the electro-catalysis dechlorination electrode of prior art, has and better applies potential.
Claims (4)
1. the preparation method of the high stability catalysis electrode of a carbon nano tube-doped Nafion membrane modification, it is characterised in that comprise the following steps:
(1) by Palladous chloride. (PdCl2) powder is dissolved in hydrochloric acid, obtains the PdCl of 5～10mmol/L with deionized water dilution2Solution, adding HCl adjustment electrolyte pH is 0.2～0.4, add a certain amount of surfactant cetyl trimethylammonium bromide (CTAB), dodecyl sodium sulfate (SLS) or cetyl benzenesulfonic acid sodium (SDBS), obtain the CTAB of 0.05～0.10mmol/L, or 0.5～1.0mmol/LSLS, or the SDBS of 0.5～1.0mmol/L；
(2) after titanium net being embathed oil removing in sodium carbonate liquor, boiling with deoxygenation compound in oxalic acid solution, redistilled water cleans up, and nitrogen dries up standby；
(3) take multi-walled carbon nano-tubes (MWCNTs) and be immersed in concentrated nitric acid, 50～60 DEG C of ultrasonic 4h in ultrasound wave, filter, wash with secondary redistilled water, until filtrate is neutral, dry；
(4) take the MWCNTs processed that step (3) obtains and be scattered in the alcoholic solution of the Nafion that mass fraction is 0.05～0.15%, ultrasonic disperse 30min, obtain uniform MWCNTs-Nafion suspension, stand for standby use；
(5) taking the suspension that step (4) obtains, the Ti that uniform drop coating processed in step (2) is online, and room temperature is dried, and obtains MWCNTs-Nafion/Ti；
(6) with step (5) prepare MWCNTs-Nafion/Ti electrode for negative electrode, platinized platinum is anode, with PdCl prepared by step (1)2Solution is electrolyte, and electro-deposition prepares Pd/MWCNTs-Nafion/Ti electrode, and depositing current density is 5.0～7.5mA/cm2, sedimentation time is 50～70min.
2. in accordance with the method for claim 1, it is characterised in that the concentration of MWCNTs optimization treated in step (4) is 1g/L.
3. the catalysis electrode that the carbon nano tube-doped Nafion membrane prepared according to the method for claim 1 or 2 is modified.
4. the catalysis electrode that the carbon nano tube-doped Nafion membrane prepared according to the method for claim 1 or 2 is modified is catalytic cathode, for the chlorinatedorganic electrochemical reduction dechlorination in water.
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| CN105606674A (en) * | 2015-12-22 | 2016-05-25 | 张利琴 | Modified gold electrode and preparation method thereof |
| CN105905993A (en) * | 2016-06-14 | 2016-08-31 | 北京工业大学 | Method for preparing supported palladium catalyst electrode on basis of graphene-doped Nafion film modification |
| CN116371446A (en) * | 2023-04-19 | 2023-07-04 | 中国科学院生态环境研究中心 | Iron-nitrogen compound-carbon nano tube composite material, preparation method and application |
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