CN102864465B - A kind of preparation method of high reactivity Ti/Pr2O3-PbO2 modified electrode - Google Patents

A kind of preparation method of high reactivity Ti/Pr2O3-PbO2 modified electrode Download PDF

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CN102864465B
CN102864465B CN201210355057.4A CN201210355057A CN102864465B CN 102864465 B CN102864465 B CN 102864465B CN 201210355057 A CN201210355057 A CN 201210355057A CN 102864465 B CN102864465 B CN 102864465B
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rare earth
electrode
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praseodymium
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CN102864465A (en
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王凤武
徐迈
李书东
方文彦
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Huainan Normal University
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Abstract

The present invention relates to one and prepare rare earth oxide-praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti base nanometer PbO of modification 2the preparation method of modified electrode material, one of involved key issue prepares rare earth praseodymium sesquioxide (Pr 2o 3) the lead electrode material of modification.The present invention adopts electrodip process, selects rare earth oxide-praseodymium sesquioxide modification Ti/PbO 2metal oxide electrode, is first preparing titanium base PbO 2during electrode, in alkaline electro plating solution, first by high current density, afterwards by low current density, first obtain transition layer α-PbO 2layer, subsequently in acid electroplating liquid, the α-PbO plated 2layer plates again the β-PbO with catalytic activity 2, finally at the dilute nitric acid solution containing rare earth praseodymium nitrate, adopt cyclic voltammetric electrochemical plating to Ti/PbO 2electrode carries out modification, obtains praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti/PbO of doping vario-property 2-Pr 2o 3modified electrode material.

Description

A kind of preparation method of high reactivity Ti/Pr2O3-PbO2 modified electrode
Technical field
The invention belongs to electrode materials preparation field, relate to one and prepare rare earth oxide-praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti base nanometer PbO of modification 2the preparation method of modified electrode material.
Background technology
In recent years, the Organic electro-synthesis technique being called as green synthesis techniques is novel and effective chemical synthesis process as one, is day by day subject to people's attention.Compared with traditional organic synthesis method, Organic electro-synthesis, by this most clean reagent of electronics, avoids the use of other reductive agent or oxygenant, and can operate at normal temperatures and pressures, environmental friendliness; By regulating voltage and electric current (density) to control the carrying out reacted, the Automated condtrol of whole process can also be convenient to.
Organic Electrochemical Synthesis technology utilizes electrochemical principle to realize matter and energy to transform, and the surface reaction characteristic between electrode and ionogen affects the core of electrochemical reaction performance and essential place.Therefore, for organic electrochemistry reaction process, have the electrode research and development of efficient electric catalytic performance, the electrolytical synthesis of excellent property and electrode and electrolytical matching optimization be model electrochemical react research and develop in extremely important key issue.Electroorganic synthesis is realized by clean electrochemical techniques, the performance of electrode materials is its industrialized key factor of restriction, not only directly affect selectivity and the speed of reaction of reaction, and the energy consumption of influence process, decide technology and the economy of whole Organic electro-synthesis process.
Lead dioxide electrode has the satisfactory electrical conductivity of metalloid, have in water solution system good electrocatalysis characteristic, overpotential for oxygen evolution high, by big current and good corrosion resistance, in electrochemical industry, obtain application as insoluble anode very early.At first, do not have matrix in lead dioxide electrode, there is mechanical workout difficulty, yield rate is low, fragile, manufacturing time length and high in cost of production problem.In order to improve the performance of lead dioxide electrode, people use that corrosion resistance is strong, thermal expansivity and the close metal titanium of plumbic oxide as matrix, utilize electro-deposition techniques to prepare ti-supported lead dioxide electric pole Ti/PbO thereon 2this electrode not only quality is light, and not easily produces the deposition layer stripping problem caused because of temperature variation.Titanium owing to having stronger erosion resistance, its thermal expansivity and PbO 2close, so not easily produce the deposition layer peeling that causes because of temperature variation so by widely as PbO 2the matrix of electrode.Experts and scholars both domestic and external are to this has been large quantifier elimination, and this work is just in the ascendant constantly deeply to be developed.
Current PbO 2although the research of electrode oneself obtain some progress, but many places are in laboratory study or small-scale application stage, need to improve in stability, electro catalytic activity etc., Problems existing is in particular in the following aspects: surfactivity layer is combined the firm not β-PbO as source/drain with substrate 2be a kind of porous material, and internal stress being comparatively large, easily there is crack in coating, and in electrode use procedure, electrolytic solution may expand and is seeped into substrate surface and causes active coating to come off.
PbO 2dissolving PbO 2electrode uses rear surface to there will be thickly dotted hole, and corner angle disappear, and is that caused by PbO2 dissolves, this not only can cause the decline of electrode electrocatalysis characteristic and stability, also likely causes Lead contamination.
In order to improve the stability of lead dioxide electrode, electroconductibility and erosion resistance, researchist develops the novel lead dioxide electrode be made up of Titanium base, bottom, middle layer and upper layer.Bottom can silver-plated, pb-ag alloy, or coating palladous oxide, tin-antimony oxide etc.; Middle layer is the α-PbO that there is not distortion 2coating; Upper layer is β-PbO 2.α-PbO 2layer plays the transitional function that buffering merges, and prevents β-PbO 2peeling off of layer.
Titanium base PbO 2while electrode has good electroconductibility and degradation capability, also there are some problems, i.e. the crystal boundary gap of coating, the O produced during electrolysis 2the TiO of poorly conductive is formed through the crystal boundary gap titanium oxide matrix of coating 2cause matrix passivation, worsen electrode performance.
In order to overcome this passivation phenomenon, have developed on titanium base, first cover layer of metal or the metal oxide preparation method as bottom or middle layer.The metal used or metal oxide comprise the oxide compound of the oxide compound of Pt and Pd, Au and Al, Ag alloy and Sn, Sb, in early days main on Titanium base compound platinum metals and coating platinum group metal oxide make the bottom of electrode, thus avoid the anti-TiO in Gaoyang 2formation.
Preparation method and application's condition of research and exploitation electrode materials, makes electrode have specific composition, structure, thus has satisfactory stability, longer work-ing life and good electro catalytic activity and reaction preference is the problem merited attention.Develop the anode material that uses in sulfuric acid medium, deep fundamental research is carried out on the factor affecting anode material preparation process, structure and use properties and seems and be even more important.Adopt rare earth oxide (Pr 2o 3) improve Ti base PbO 2the catalytic performance of electrode and chemical property fundamentally solve current Ti/PbO 2the problems such as the electrode inactivation that metal oxide electrode exists, electrocatalysis characteristic difference are the most promising research directions.
Summary of the invention
The present invention relates to one and prepare rare earth oxide-praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti base nanometer PbO of modification 2the preparation method of modified electrode material, one of involved key issue prepares rare earth praseodymium sesquioxide (Pr 2o 3) modification lead electrode material.The present invention adopts electrodip process, selects rare earth oxide-praseodymium sesquioxide modification Ti/PbO 2metal oxide electrode, is first preparing titanium base PbO 2during electrode, in alkaline electro plating solution, first by high current density, afterwards by low current density, first obtain transition layer α-PbO 2, subsequently in acid electroplating liquid, the α-PbO plated 2layer plates again the β-PbO with catalytic activity 2, finally at the dilute nitric acid solution containing rare earth praseodymium nitrate, adopt cyclic voltammetric electrochemical plating to Ti/PbO 2electrode carries out modification, obtains praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti/PbO of doping vario-property 2-Pr 2o 3modified electrode material.
Convenient and swift method prepares rare earth oxide-praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti base nanometer PbO of modification 2modified electrode material takes following technical scheme to realize:
(1) first by Ti matrix use 250 orders, 600 orders and 1000 order sand papering polishings respectively, make it to present argenteous metalluster.The object of polishing makes Rough Metal Surface smooth, smooth.Then rinse well with distilled water, dehydrated alcohol, then use hydrofluoric acid clean.Rinse with acetone deoiling, dehydrated alcohol subsequently, the greasy dirt of removing Ti matrix surface.
(2) in alkaline electro plating solution, first by high current density, afterwards by low current density, transition layer α-PbO is first obtained 2.Alkaline electro plating solution forms: 0.1 ~ 0.4molL -1pbO+2.5molL -1naOH, the electrode after above-mentioned steps process is placed in the saturated solution that PbO is dissolved in NaOH solution, and temperature is 35 ~ 40 DEG C, and current density is 0.3 ~ 0.5Adm -2, electroplating time 60 ~ 120min, process can do negative electrode with pure stereotype for this reason.
(3) in acid electroplating liquid, the α-PbO plated 2layer plates again the 3-PbO with catalytic activity 2.Acid electroplating liquid forms: 0.2molL -1hNO 3, 0.02 ~ 0.04molL -1naF, 0.65mol/l lead nitrate, current density is 5 ~ 6Adm -2lower plating 1 ~ 2h.
(4) at the solution containing rare earth praseodymium nitrate, adopt cyclic voltammetric electrochemical plating to Ti/PbO 2electrode carries out modification, obtains praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti/PbO of doping vario-property 2-Pr 2o 3modified electrode material
Wherein: described in alkaline electro plating solution, first by high current density, afterwards by low current density, first obtain transition layer α-PbO2 layer, bath voltage is 1 ~ 2V.
Described Ti is in acid electroplating liquid, and the α-PbO2 layer plated plates the β-PbO2 with catalytic activity again, and bath voltage is 2 ~ 3V.
Described at the solution containing rare earth praseodymium nitrate, praseodymium nitrate content is praseodymium nitrate 0.2 ~ 0.5mol/l.
Described Ti metal adopts the pure titanium metal (purity is 99.5%) of TA1 type.
Described ethanol is dehydrated alcohol and removes the treating processes of minor amount of water through 4A molecular sieve.
Described cyclic voltammetry sweep limit is 0 ~ 2V, and scanning speed is 0.02 ~ 0.1Vs-1, the scanning number of turns 40 ~ 80.
Embodiment
Embodiment 1
1, first the Ti matrix of 2cm × 2cm × 5mm is used respectively 250 orders, 600 orders and 1000 order sand papering polishings, make it to present argenteous metalluster.Then clean with distilled water flushing, then use hydrofluoric acid clean, carry out the ultrasonic irrigation of 20min subsequently with acetone, dehydrated alcohol, the greasy dirt of removing Ti matrix surface.
2, cleaned titanium sheet is put into electrolyzer as anode, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, at 0.1molL -1pbO+2.5molL -1the alkaline electro plating solution of NaOH, voltage 1V, temperature is 35 DEG C, electroplating time 60min, first at Ti metallic surface plating transition layer α-PbO 2.
3, the Ti/ α-PbO will plated 2be placed on 0.2molL -1hNO 3+ 0.02molL -1in NaF+0.65mol/l lead nitrate acid electroplating liquid, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, is plating α-PbO 2surface plate the β-PbO that one deck has catalytic activity again 2, bath voltage is 2V, plating 2h.
4, by Ti/ β-PbO obtained for the 3rd step 2be placed on the solution of 0.2mol/l praseodymium nitrate, adopt cyclic voltammetry sweep limit to be 0 ~ 2V, scanning speed is 0.02Vs -1carry out rare-earth-doped modification to electrode, scanning 40 circle, namely obtains Ti/Pr 2o 3-PbO 2.
Embodiment 2
1, first the Ti matrix of 2cm × 2cm × 5mm is used respectively 250 orders, 600 orders and 1000 order sand papering polishings, make it to present argenteous metalluster.Then clean with distilled water flushing, then use hydrofluoric acid clean, carry out the ultrasonic irrigation of 20min subsequently with acetone, dehydrated alcohol, the greasy dirt of removing Ti matrix surface.
2, cleaned titanium sheet is put into electrolyzer as anode, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, at 0.2molL -1pbO+2.5molL -1the alkaline electro plating solution of NaOH, voltage 2V, temperature is 35 DEG C, electroplating time 90min, first at Ti metallic surface plating transition layer α-PbO 2.
3, the Ti/ α-PbO will plated 2be placed on 0.2molL -1hNO 3+ 0.03molL -1in NaF+0.65mol/l lead nitrate acid electroplating liquid, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, the α-PbO plated 2surface plate the β-PbO that one deck has catalytic activity again 2.Bath voltage is 3V, plating 2h.
4, by Ti/ β-PbO obtained for the 3rd step 2be placed on the solution of 0.2mol/l praseodymium nitrate, adopt cyclic voltammetry sweep limit to be 0 ~ 2V, scanning speed is 0.04Vs -1carry out rare-earth-doped modification to electrode, scanning 40 circle, namely obtains Ti/Pr 2o 3-PbO 2.
Embodiment 3
1, first by 250 orders, 600 orders and the 1000 order sand papering polishings respectively of the Ti matrix of 2cm × 2cm × 5mm, make it to present argenteous metalluster.Then clean with distilled water flushing, then use hydrofluoric acid clean, carry out the ultrasonic irrigation of 20min subsequently with acetone, dehydrated alcohol, the greasy dirt of removing Ti matrix surface.
2, cleaned titanium sheet is put into electrolyzer as anode, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, at 0.3molL -1pbO+2.5molL -1the alkaline electro plating solution of NaOH, voltage 2V, temperature is 35 DEG C, electroplating time 120min, first at Ti metallic surface plating transition layer α-PbO 2.
3, the Ti/ α-PbO will plated 2be placed on 0.2molL -1hNO 3+ 0.04molL -1in NaF+0.65mol/l acid electroplating liquid, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, the α-PbO plated 2surface plate the β-PbO that one deck has catalytic activity again 2.Bath voltage is 3V, plating 1.5h.
4, by Ti/3-PbO obtained for the 3rd step 2be placed on the solution of 0.3mol/l praseodymium nitrate, adopt cyclic voltammetry sweep limit to be 0 ~ 2V, scanning speed is 0.06Vs -1carry out rare-earth-doped modification to electrode, scanning 40 circle, namely obtains Ti/Pr 2o 3-PbO 2.
Embodiment 4
1, first by 250 orders, 600 orders and the 1000 order sand papering polishings respectively of the Ti matrix of 2cm × 2cm × 5mm, make it to present argenteous metalluster.Then clean with distilled water flushing, then use hydrofluoric acid clean, carry out the ultrasonic irrigation of 20min subsequently with acetone, dehydrated alcohol, the greasy dirt of removing Ti matrix surface.
2, cleaned titanium sheet is put into electrolyzer as anode, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, at 0.4molL -1pbO+2.5molL -1the alkaline electro plating solution of NaOH, voltage 2V, temperature is 40 DEG C, electroplating time 120min, first at Ti metallic surface plating transition layer α-PbO 2.
3, the Ti/ α-PbO will plated 2be placed on 0.2molL -1hNO 3+ 0.04molL -1in NaF+0.65mol/l lead nitrate acid electroplating liquid, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, is plating α-PbO 2surface plate the β-PbO that one deck has catalytic activity again 2.Bath voltage is 3V, plating 1.5h.
4, by Ti/ β-PbO obtained for the 3rd step 2be placed on the solution of 0.4mol/l praseodymium nitrate, adopt cyclic voltammetry sweep limit to be 0 ~ 2V, scanning speed is 0.08Vs -1carry out rare-earth-doped modification to electrode, scanning 80 circle, namely obtains Ti/Pr 2o 3-PbO 2.
Embodiment 5
1, first the Ti matrix of 2cm × 2cm × 5mm is used respectively 250 orders, 600 orders and 1000 order sand papering polishings, make it to present argenteous metalluster.Then clean with distilled water flushing, then use hydrofluoric acid clean, carry out the ultrasonic irrigation of 20min subsequently with acetone, dehydrated alcohol, the greasy dirt of removing Ti matrix surface.
2, cleaned titanium sheet is put into electrolyzer as anode, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, at 0.4molL -1pbO+2.5molL -1the alkaline electro plating solution of NaOH, voltage 1.5V, temperature is 40 DEG C, electroplating time 90min, first at Ti metallic surface plating transition layer α-PbO 2.
3, the Ti/ α-PbO will plated 2be placed on 0.2molL -1hNO 3+ 0.04molL -1in NaF+0.65mol/l lead nitrate acid electroplating liquid, the pure stereotype of 4cm × 4cm × 5mm does negative electrode, is plating α-PbO 2surface plate the β-PbO that one deck has catalytic activity again 2.Bath voltage is 2.5V, plating 2h.
4, by Ti/ β-PbO obtained for the 3rd step 2be placed on the solution of 0.5mol/l praseodymium nitrate, adopt cyclic voltammetry sweep limit to be 0 ~ 2V, scanning speed is 0.1Vs -1carry out rare upper doping vario-property to electrode, scanning 60 circle, namely obtains Ti/Pr 2o 3-PbO 2.

Claims (6)

1. prepare rare earth oxide-praseodymium sesquioxide (Pr for one kind 2o 3) the high catalytic activity Ti base nanometer PbO of modification 2the preparation method of modified electrode material, is characterized in that:
(1) by Ti matrix with after sand papering polishing, use distilled water, dehydrated alcohol, hydrofluoric acid clean successively, acetone deoiling, dehydrated alcohol rinse, to remove the greasy dirt of Ti matrix surface;
(2) the Ti matrix handled well is put into alkaline electro plating solution, be equipped with cathode material, α-PbO on its plated surface 2layer, wherein alkaline electro plating solution is by 0.1 ~ 0.4 molL -1pbO and 2.5 molL -1naOH composition;
(3) α-PbO will plated again 2the Ti matrix of layer is placed in acid electroplating liquid, then plates the β-PbO with catalytic activity 2layer, wherein acid electroplating liquid is by 0.2 molL -1hNO 3, 0.02 ~ 0.04 molL -1naF and 0.65 molL -1pb (NO 3) 2composition;
(4) finally put into the solution containing rare earth praseodymium nitrate, adopt cyclic voltammetric electrochemical plating to Ti/PbO 2electrode carries out modification, and cyclic voltammetry sweep limit is 0 ~ 2V, and scanning speed is 0.05 ~ 0.1 Vs -1, obtain praseodymium sesquioxide (Pr 2o 3) the high catalytic activity Ti/PbO of doping vario-property 2-Pr 2o 3modified electrode material.
2., in the method for claim 1, sand paper adopts 250 orders, 600 orders and 1000 orders.
3., in the method for claim 1, in step (2), during plating, temperature is 35 ~ 40 DEG C, and current density is 0.3 ~ 0.5 Adm -2, electroplating time 60 ~ 120min; Cathode material is pure stereotype.
4., in the method for claim 1, the current density in step (3) during plating is 5 ~ 6 Adm -2, electroplating time is 60 ~ 120min.
5., in the method for claim 1, the solution content of rare earth praseodymium nitrate is praseodymium nitrate 0.2 ~ 0.5 molL -1.
6. in the method for claim 1, the cyclic voltammetry scanning scanning number of turns 40 ~ 80.
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CN103132076B (en) * 2013-02-07 2015-10-07 浙江工业大学 Ti-supported lead dioxide electric pole of a kind of lanthanum, gadolinium codoped and its preparation method and application
CN103205780B (en) * 2013-04-15 2017-04-26 昆明理工恒达科技有限公司 Grate type titanium-based PbO2 electrode for nonferrous metal electrodeposition and preparation method of grate type titanium-based PbO2 electrode
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