CN106086978A - A kind of preparation method of the loaded palladium catalyst electrode based on Graphene/polypyrrole modifying - Google Patents
A kind of preparation method of the loaded palladium catalyst electrode based on Graphene/polypyrrole modifying Download PDFInfo
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Abstract
The preparation method of a kind of loaded palladium catalyst electrode based on Graphene/polypyrrole modifying, belongs to technical field of electrochemical water treatment.The present invention is with titanium net as matrix, after electroxidation polymerization in its surface forms polypyrrole, is taken in isopropanol the uniform drop coating of graphene dispersing solution after dispersion on its surface, and as negative electrode after fully drying, platinized platinum is as anode, with palladium bichloride (PdCl2) solution is electrolyte, galvanostatic deposition prepares Pd/Graphene/PPy SDBS/Ti electrode.Compared with the Pd/PPy SDBS/Ti electrode without graphene modified of preparation under equal conditions, Pd/Graphene/PPy SDBS/Ti electrode has higher catalysis activity.
Description
Technical field
The invention belongs to technical field of electrochemical water treatment, relate to a kind of supported palladium based on Graphene/polypyrrole modifying
The preparation method of catalyst electrode, is mainly used in the electrochemical reduction dechlorination of chlorinatedorganic in water.
Background technology
Chlorinatedorganic produces material as one and intermediate product has extensively at aspects such as agricultural chemicals, dyestuff, organic syntheses
General application is simultaneously discharged in environment.But, major part chlorinatedorganic is all toxic and be considered to have " carcinogenic, teratogenesis,
Mutagenesis " effect, and be difficult to degrade, it is the persistence organic pollutant of a quasi-representative.Therefore, chlorinatedorganic in water is carried out
The research removed is very necessary.Electrochemical techniques are as a kind of environmentally-friendly technique, in environmental improvement particularly waste water
The removal aspect of bio-refractory organic matter has good application prospect.
One of key of electrochemical treatments chlorinatedorganic is electrode, and the quality of electrode material directly affects organic dirt
The degradation effect of dye thing.Palladium, because having good reactive hydrogen storage capacity thus promoting dechlorination reaction, becomes catalyst research
Emphasis.Material with carbon element has a wide range of applications in catalytic field, when material with carbon element is as catalyst carrier, and the structure of carbon carrier
The performance of catalyst is had a significant impact.Researchers find, your gold the both sides of graphene planes structure all can support
The high conductivity of genus particle, especially Graphene and huge specific surface area so that it is be particularly suitable as catalyst carrier.Cause
This, it is that disposal organo-chlorine pollutant is more high that the loaded palladium catalyst electrode of graphene modified carries out electro-catalysis reduction dechlorination
Effect, the method for low consumption.
The present invention modifies using Graphene and polypyrrole as intermediate layer, using palladium as catalyst, is devoted to prepare efficiently
Electro-catalysis reduction dechlorination electrode.
Content of the invention
It is an object of the invention to solve the problems of the prior art, provide a kind of prepare simplicity, catalysis activity strong with
Titanium net is the loaded palladium catalyst electrode (Pd/Graphene/PPy-SDBS/Ti) based on Graphene/polypyrrole modifying of matrix
Preparation method.
The preparation method of above-mentioned Pd/Graphene/PPy-SDBS/Ti electrode and process, comprise the following steps:
(1) titanium net is inserted successively in sodium carbonate liquor (preferred concentration 0.3mol/L) and embathe oil removing, at oxalic acid solution
Boiling removal oxide on surface in (preferred concentration 0.1mol/L), then being rinsed well by redistilled water, nitrogen dries up standby；
(2) take neopelex (SDBS) to join in sulfuric acid (preferred concentration 0.3mol/L) and be sufficiently stirred for, molten
Adding the pyrroles (Py) having distilled fully to dissolve as deposition liquid after solution, SDBS concentration is preferably 1g/L, and pyrrole concentrations is preferably
0.1mol/L；The titanium net handled well with step (1) is as anode, and with platinized platinum as negative electrode, galvanostatic deposition prepares PPy-SDBS/Ti electricity
Pole, constant current sinks galvanostatic deposition 5min under preferred 5mA electric current；
(3) Graphene is joined in isopropanol, Graphene mass concentration 0.02%～0.1% (preferably 0.04%) is super
Sound makes it fully dispersed, and then the isopropanol dispersion liquid of drop coating Graphene is to PPy-SDBS/Ti electrode surface, horizontal positioned, fills
Divide and dry, obtain Graphene/PPy-SDBS/Ti standby, wherein preferably every 8cm2The corresponding drop coating of PPy-SDBS/Ti electrode surface
The isopropanol dispersion liquid of 50-70 μ L Graphene；
(4) take in palladium bichloride powder addition hydrochloric acid and be completely dissolved, prepare palladium chloride solution standby, wherein preferably employ every 1g
The corresponding hydrochloric acid solution 100ml adding 3mol/L of palladium bichloride correspondence are diluted with water the palladium chloride solution obtaining 4g/L；
(5) the Graphene/PPy-SDBS/Ti electrode prepared with step (3) is as negative electrode, and platinized platinum is anode, with step (4)
The palladium chloride solution of preparation is electrolyte, and galvanostatic deposition current density is 1.875～4.375mA/cm2, sedimentation time is 35
～55min, galvanostatic deposition prepares Pd/Graphene/PPy-SDBS/Ti electrode.
Use the loaded palladium catalyst electrode based on Graphene/polypyrrole modifying prepared by the present invention as negative electrode, be used for
The electrochemical reduction dechlorination of chlorinatedorganic in water has excellent performance.
Compared with prior art, the method have the advantages that
1st, the present invention is with titanium net as matrix, utilizes the high stability such as its high-low temperature resistant, corrosion-resistant, the high intensity of resistance to strong acid special
For it, the stability of point, beneficially holding electrode, realizes that the electrochemical reduction dechlorination to chlorinatedorganic provides basis.
2nd, the present invention deposits polypyrrole at titanium net surface, not only increases the specific surface area of electrode, and is follow-up graphite
The attachment of alkene is fixing provides condition.
3rd, the present invention is using Graphene as modification, makes full use of the characteristic of its high-specific surface area, high conductivity and stability,
Improve the specific surface area of electrode, thus provide more attachment site for palladium catalyst, be conducive to strengthening the catalysis of electrode
Activity.
4th, the present invention disperses graphene in organic solvent (isopropanol), and beneficially Graphene is dispersed.Afterwards
Use drop-coating by graphene modified in electrode surface, simple to operate.
5th, the present invention uses the method for drop coating and electrochemical deposition to prepare Pd/Graphene/PPy-SDBS/Ti electrode, tool
There is higher catalysis activity.
Brief description
Fig. 1 is the scanning electron microscopic picture of PPy-SDBS/Ti.
Fig. 2 is the scanning electron microscopic picture of Graphene/PPy-SDBS/Ti electrode.
Fig. 3 is the scanning electron microscopic picture of Pd/Graphene/PPy-SDBS/Ti electrode, is as can be seen from the figure tied by sheet
Structure forms flower ball-shaped structure.
Fig. 4 is the Pd/PPy-of the Pd/Graphene/PPy-SDBS/Ti electrode of embodiment the 1st, embodiment 2 and comparative example
The cyclic voltammetry scan curve of SDBS/Ti electrode.
Detailed description of the invention
Example below and comparative example will the present invention is further illustrated in conjunction with accompanying drawing, but the present invention be not limited to
Lower embodiment.
Embodiment 1:
(1) sodium carbonate liquor titanium net of 2cm × 2cm being inserted successively 0.3mol/L embathes oil removing, at 0.1mol/L
Oxalic acid solution in boil holding 30min remove oxide on surface, then rinsed well by redistilled water, nitrogen dries up standby
With；
(2) take neopelex (SDBS) to join in the sulfuric acid of 0.3mol/L and be sufficiently stirred for, add after dissolving
The pyrroles (Py) having distilled fully is dissolved as deposition liquid, and SDBS concentration is 1g/L, and pyrrole concentrations is 0.1mol/L.With step
(1) the titanium net handled well is anode, with platinized platinum as negative electrode, and galvanostatic deposition 5min under 5mA electric current, preparation PPy-SDBS/Ti electricity
Pole.As seen from Figure 1, PPy film is defined at electrode surface；
(3) Graphene of different quality is joined in isopropanol, Graphene mass concentration 0.04%, ultrasonic make it abundant
Dispersion, then drop coating 60 μ L dispersion liquid is to PPy-SDBS/Ti electrode surface, horizontal positioned, fully dries, obtains Graphene/
PPy-SDBS/Ti is standby.From Figure 2 it can be seen that Graphene has been attached to electrode surface；
(4) the corresponding hydrochloric acid solution 100ml adding 3mol/L of every 1g palladium bichloride correspondence are diluted with water the chlorine obtaining 4g/L
Change palladium solution for standby；
(5) the Graphene/PPy-SDBS/Ti electrode prepared with step (3) is as negative electrode, and platinized platinum is anode, with step (4)
The palladium chloride solution of preparation is electrolyte, and galvanostatic deposition current density is 3.125mA/cm2, sedimentation time is 45min, permanent electricity
Stream deposition prepares Pd/Graphene/PPy-SDBS/Ti electrode.As seen from Figure 3, palladium has deposited to electrode surface；
(6) the Pd/Graphene/PPy-SDBS/Ti electrode obtaining with step (5) is as working electrode, Pt piece for electrode,
Hg/Hg2SO4For reference electrode, at the H of 0.5mol/L2SO4Being circulated voltammetric scan in solution, sweep speed is 50mV/
Min, sweep limits is-700mV～700mV.
Embodiment 2:
(1) sodium carbonate liquor titanium net of 2cm × 2cm being inserted successively 0.3mol/L embathes oil removing, at 0.1mol/L
Oxalic acid solution in boil holding 30min remove oxide on surface, then rinsed well by redistilled water, nitrogen dries up standby
With；
(2) take neopelex (SDBS) to join in the sulfuric acid of 0.3mol/L and be sufficiently stirred for, add after dissolving
The pyrroles (Py) having distilled fully is dissolved as deposition liquid, and SDBS concentration is 1g/L, and pyrrole concentrations is 0.1mol/L.With step
(1) the titanium net handled well is anode, with platinized platinum as negative electrode, and galvanostatic deposition 5min under 5mA electric current, preparation PPy-SDBS/Ti electricity
Pole；
(3) Graphene of different quality is joined in isopropanol, Graphene mass concentration 0.06%, ultrasonic make it abundant
Dispersion, then drop coating 60 μ L dispersion liquid is to PPy-SDBS/Ti electrode surface, horizontal positioned, fully dries, obtains Graphene/
PPy-SDBS/Ti is standby；
(4) the corresponding hydrochloric acid solution 100ml adding 3mol/L of every 1g palladium bichloride correspondence are diluted with water the chlorine obtaining 4g/L
Change palladium solution for standby；
(5) the Graphene/PPy-SDBS/Ti electrode prepared with step (3) is as negative electrode, and platinized platinum is anode, with step (4)
The palladium chloride solution of preparation is electrolyte, and galvanostatic deposition current density is 2.5mA/cm2, sedimentation time is 45min, constant current
Deposition prepares Pd/Graphene/PPy-SDBS/Ti electrode.
(6) the Pd/Graphene/PPy-SDBS/Ti electrode obtaining with step (5) is as working electrode, Pt piece for electrode,
Hg/Hg2SO4For reference electrode, at the H of 0.5mol/L2SO4Being circulated voltammetric scan in solution, sweep speed is 50mV/
Min, sweep limits is-700mV～700mV.
Comparative example:
(1) sodium carbonate liquor titanium net of 2cm × 2cm being inserted successively 0.3mol/L embathes oil removing, at 0.1mol/L
Oxalic acid solution in boil holding 30min remove oxide on surface, then rinsed well by redistilled water, nitrogen dries up standby
With；
(2) take neopelex (SDBS) to join in the sulfuric acid of 0.3mol/L and be sufficiently stirred for, add after dissolving
The pyrroles (Py) having distilled fully is dissolved as deposition liquid, and SDBS concentration is 1g/L, and pyrrole concentrations is 0.1mol/L.With step
(1) the titanium net handled well is anode, with platinized platinum as negative electrode, and galvanostatic deposition 5min under 5mA electric current, preparation PPy-SDBS/Ti electricity
Pole；
(3) the corresponding hydrochloric acid solution 100ml adding 3mol/L of every 1g palladium bichloride correspondence is used to be diluted with water and obtain 4g/L
Palladium chloride solution；
(4) the PPy-SDBS/Ti electrode prepared with step (3) is as negative electrode, and platinized platinum is anode, the chlorine prepared with step (4)
Changing palladium solution is electrolyte, and galvanostatic deposition current density is 3.125mA/cm2, sedimentation time is 45min, galvanostatic deposition system
Obtain Pd/PPy-SDBS/Ti electrode.
(5) the Pd/PPy-SDBS/Ti electrode obtaining with step (5) is as working electrode, and Pt piece is for electrode, Hg/Hg2SO4
For reference electrode, at the H of 0.5mol/L2SO4Being circulated voltammetric scan in solution, sweep speed is 50mV/min, sweep limits
For-700mV～700mV.From fig. 4, it can be seen that embodiment 1 all has higher peak point current with embodiment 2 compared with comparative example, electricity
Polarity can be higher.
Claims (7)
1. the preparation method based on the loaded palladium catalyst electrode of Graphene/polypyrrole modifying, it is characterised in that include with
Lower step:
(1) insert titanium net in sodium carbonate liquor successively and embathe oil removing, in oxalic acid solution, boil removal oxide on surface, then
Being rinsed well by redistilled water, nitrogen dries up standby；
(2) take neopelex (SDBS) to join in sulfuric acid and be sufficiently stirred for, after dissolving, add the pyrroles having distilled
(Py) fully dissolving as deposition liquid, the titanium net handled well with step (1) is as anode, with platinized platinum as negative electrode, and galvanostatic deposition system
Standby PPy-SDBS/Ti electrode；
(3) Graphene is joined in isopropanol, Graphene (Graphene) mass concentration 0.02%～0.1%, ultrasonic make it
Fully dispersed, then the isopropanol dispersion liquid of drop coating Graphene is to PPy-SDBS/Ti electrode surface, horizontal positioned, fully dries,
Obtain Graphene/PPy-SDBS/Ti standby；
(4) take in palladium bichloride powder addition hydrochloric acid and be completely dissolved, prepare palladium chloride solution standby；
(5) the Graphene/PPy-SDBS/Ti electrode prepared with step (3) is as negative electrode, and platinized platinum is anode, prepares with step (4)
Palladium chloride solution be electrolyte, galvanostatic deposition current density is 1.875～4.375mA/cm2, sedimentation time is 35～
55min, galvanostatic deposition prepares Pd/Graphene/PPy-SDBS/Ti electrode.
2. the preparation side according to a kind of loaded palladium catalyst electrode based on Graphene/polypyrrole modifying described in claim 1
Method, it is characterised in that step (2) sulfuric acid concentration 0.3mol/L, SDBS concentration is 1g/L, and pyrrole concentrations is 0.1mol/L；Permanent electricity
Stream sinks for galvanostatic deposition 5min under 5mA electric current.
3. the preparation side according to a kind of loaded palladium catalyst electrode based on Graphene/polypyrrole modifying described in claim 1
Method, it is characterised in that step (3) Graphene mass concentration is 0.04%.
4. the preparation side according to a kind of loaded palladium catalyst electrode based on Graphene/polypyrrole modifying described in claim 1
Method, it is characterised in that the every 8cm of step (3)2The isopropanol of the corresponding drop coating 50-70 μ l Graphene of PPy-SDBS/Ti electrode surface divides
Dissipate liquid.
5. the preparation side according to a kind of loaded palladium catalyst electrode based on Graphene/polypyrrole modifying described in claim 1
Method, it is characterised in that prepared by step (4) palladium chloride solution: use the corresponding hydrochloric acid solution adding 3mol/L of every 1g palladium bichloride
100ml correspondence are diluted with water the palladium chloride solution obtaining 4g/L.
6. according to the loaded palladium catalyst electrode based on Graphene/polypyrrole modifying described in any one of claim 1-5.
7. according to a kind of loaded palladium catalyst electrode based on Graphene/polypyrrole modifying described in claim 1 in water
The application of the electrochemical reduction dechlorination of chlorinatedorganic.
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| CN107475761A (en) * | 2017-08-22 | 2017-12-15 | 哈尔滨工程大学 | The electropolymerization liquid and electropolymerization method of the sodium dodecyl benzene sulfonate-doped film of poly pyrrole of Mg alloy surface |
| CN108262071A (en) * | 2018-01-25 | 2018-07-10 | 河南科技大学 | The preparation method of the three-dimensional porous polypyrrole modifying Ti electrode of catalyst carrier |
| CN108262071B (en) * | 2018-01-25 | 2021-01-29 | 河南科技大学 | Preparation method of three-dimensional porous polypyrrole modified titanium electrode for catalyst carrier |
| CN112981497A (en) * | 2021-02-05 | 2021-06-18 | 浙江大学 | Preparation method and application of porous MXene hydrogel based on electrocoagulation process |
| CN113077919A (en) * | 2021-03-25 | 2021-07-06 | 徐州医科大学 | Metal Pd-loaded graphene/polypyrrole composite material and preparation method and application thereof |
| CN113981490A (en) * | 2021-11-05 | 2022-01-28 | 浙江师范大学行知学院 | Composite material containing palladium metal organic framework compound modified foam nickel and preparation method and application thereof |
| CN113981490B (en) * | 2021-11-05 | 2022-11-15 | 浙江师范大学行知学院 | Composite material of palladium-containing metal organic framework compound modified foam nickel and preparation method and application thereof |
| CN117230483A (en) * | 2023-11-13 | 2023-12-15 | 河南工学院 | Palladium-modified polyaniline/carbon nanotube composite electrode material, and preparation method and application thereof |
| CN117230483B (en) * | 2023-11-13 | 2024-02-06 | 河南工学院 | Palladium-modified polyaniline/carbon nanotube composite electrode material, and preparation method and application thereof |
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