CN102881384A - Method for preparing conductive high molecular material coated metal-based inert electrode material - Google Patents
Method for preparing conductive high molecular material coated metal-based inert electrode material Download PDFInfo
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- 229920001940 conductive polymer Polymers 0.000 claims description 52
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 14
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 14
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- 210000003097 mucus Anatomy 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 229920000767 polyaniline Polymers 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- 230000001680 brushing effect Effects 0.000 claims description 8
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- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000011133 lead Substances 0.000 claims description 3
- 229920000123 polythiophene Polymers 0.000 claims description 3
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- 241000216843 Ursus arctos horribilis Species 0.000 claims description 2
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- 238000005260 corrosion Methods 0.000 abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract description 2
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Abstract
The invention discloses a method for preparing a conductive high molecular material coated metal-based inert electrode material. The method comprises the following three steps: (1) preparing a metal framework substrate; (2) preparing a conductive high molecular coating material; and (3) coating the conductive high molecular coating material on the metal framework substrate. The prepared conductive high molecular material coated metal-based inert electrode material can obviously improve the electrocatalytic activity of a plate electrode and the corrosion resistance of a polar plate and is particularly suitable for a chloride system or a sulfate system containing high chloride ion content; and the composite material can be used for inert anodes, battery electrodes, sensor devices, capacitor electrodes and the like in the wet metallurgical extraction process of nonferrous metals, and the energy consumption can be obviously reduced in the electrodeposition process of the nonferrous metals.
Description
Technical field
The present invention relates to a kind of conducting polymer composite clad metal base inert electrode material preparation method, be mainly used in electrochemical process.
Background technology
Conducting polymer composite (polyaniline, polypyrrole, polythiophene) is with its good chemical stability and electrochemical reversibility, and good anti-corrosion of metal characteristic becomes one of the fastest functional material of present progress.Take conducting polymer composite as basic material, developing at present many new technologies, such as sensor element, electrode material, overall plastic anti-corrosion of metal technology, APollution prevention technology for ships, solar cell, electromangnetic spectrum, antistatic technology, electrochromism and stealth technology etc.But no matter be all to be powder by chemical oxidation or the conducting polymer composite of electrochemical oxidation gained, be difficult to processing and forming, and its conductance is mutually more far short of what is expected than also with metal.These shortcomings of conducting polymer composite have directly affected its scale and have used.Both ways conducting polymer composite various trials have been done around above problem people: at first be that conducting polymer is carried out chemical graft, so that prepared conducting polymer not only keeps high molecular conductivity, but also has solubility, be conducive to processing, but experimental results show that the raising of all solubilities is all to sacrifice conductivity as cost, this has changed the electric conductivity of conducting polymer composite so that the conductance of the conducting polymer composite of preparation all descends to some extent.In addition, the proposition such as Vincent and Armes exploitation water colloidal dispersion system is to solve the important method that is difficult to the processing and forming shortcoming.At present, people have developed polyaniline-coated inorganic nanoparticles (SiO for example
2, TiO
2, WC etc.) etc. material, the materials such as polyaniline-coated organic nanometer granule (such as PS, APS etc.).These have the material of polyaniline-coated can solve to a certain extent the processability of polyaniline.The conducting polymer composite of preparation has possessed the common property of conducting polymer and inorganic material like this, and still, the conductance of prepared composite material is still lower, the moulding material that machining gets or take coating or film as main.
Summary of the invention
The object of the present invention is to provide a kind of conducting polymer composite clad metal base inert electrode material preparation method, prepared composite material has higher conductance, and anticorrosion ability preferably is so that electrode material has preferably inertia and electric catalyticing characteristic.
The present invention is achieved through the following technical solutions:
A kind of conducting polymer composite clad metal base inert electrode material preparation method, step is as follows:
(1) preparation metallic framework substrate: use first deionized water drip washing 3～5 times, then soak 2～5min in acetone soln, taking out with temperature is 80 ℃～90 ℃ hot wash 1～3 time again, dries up with after the deionized water drip washing 1～3 time at last;
(2) preparation conducting polymer coating material:
1. will account for the conducting polymer composite of composite coating quality 30%～70%, dispersed with stirring seals ultrasonic dispersion 30min again in the organic solvent of capacity, obtain stable conducting polymer composite dispersion solution;
2. in mass ratio with polymethyl methacrylate (PMMA) and polyvinyl chloride (PVC)=(1～4): the mixture that (1～4) forms be dissolved in capacity with 1. go on foot selected phase with organic solvent in, the gross mass of described mixture accounts for 30%～70% of composite coating quality;
3. will 1. go on foot and the solution of 2. step preparation mixes, abundant dispersed with stirring, the organic solvent that at room temperature volatilizees obtains the conducting polymer composite coating mucus of thickness;
(3) at coated with conductive polymeric coating material in the metallic framework substrate: the conducting polymer composite coating mucus brushing of the thickness that step (2) is prepared is in the metallic framework substrate that step (1) is handled well, after coating is done for the first time, be coated with again the second layer, so circulate until the high polymer composite coating material that coats in the metallic framework substrate reaches till the thickness that needs; Perhaps
The metallic framework base material that step (1) is handled well is immersed in the conducting polymer composite coating mucus of the prepared thickness of step (2), then mention, after composite coating mucus is done, repeat again aforesaid operations, so circulate until the high polymer composite coating material that coats in the metallic framework substrate reaches till the thickness that needs.
As preferred version of the present invention, during described step (2) preparation conducting polymer coating material, also conducting polymer composite can be dispersed in the performed polymer of methyl methacrylate (MMA), again further polymerization under temperature action, obtaining can be for the conducting polymer composite coating liquid of brushing; Also can
Conductive high polymer monomer is added in aggregate in the liquid phase substance of polymethyl methacrylate (PMMA) and polyvinyl chloride (PVC) dissolving can be for the conducting polymer composite coating liquid of brushing.
Described conducting polymer composite is polyaniline, polypyrrole or polythiophene; Organic solvent is oxolane or chloroform.
Described metallic framework base material is: aluminium, magnesium alloy, stainless steel, titanium, lead or pb-ag alloy; The shape of metallic framework base material is: sheet material, netted or grizzly bar shape.
Reply metallic framework base material oil removing and activation processing in the described step (1).
Adopt layering to be coated with conducting polymer composite in the described step (3) and rinse in the metallic framework substrate, or employing is immersed in metallic framework the coating that realizes in the conducting polymer composite mucus metal base material several times.
As coating layer material, Metal Substrate prepares the composite inert electrode material as the skeleton of electrode material with conducting polymer composite in the present invention.So both solved the not difficult problem of easy-formation of conducting polymer composite, and because the introducing of metallic substrates, effectively solved the lower problem of conducting polymer composite conductance, conducting polymer composite preferably electric catalyticing characteristic and anti-corrosion of metal effect have preferably also been kept, so that prepared combination electrode material has preferably conductivity and inertia.Technical process of the present invention is simple, easily control.The conducting polymer clad metal base inert electrode composite material of the present invention's preparation can significantly improve the corrosion resistance of electro catalytic activity and the pole plate of battery lead plate, is particularly useful for the high sulfate system of chloride system or chloride ion-containing; This composite material can be used for inert anode, battery electrode, sensor component, electrode for capacitors in the non-ferrous metal hydrometallurgical extraction process etc., can significantly reduce the energy consumption of non-ferrous metal electrodeposition process.
Embodiment:
Embodiment one:
(1) step: pb-ag alloy test piece a slice of intercepting 0.5cm * 3cm * 4cm, use first respectively deionized water drip washing 3～5 times, then in acetone soln, soak 2～5min, take out test piece, be 80 ℃～90 ℃ hot wash 1～3 time again with temperature, then dry up with after the deionized water drip washing 1～3 time.
(2) step: take by weighing 1.5g polymethyl methacrylate (PMMA) and 0.5g polyvinyl chloride (PVC), add in the 40ml oxolane, and seal with preservative film, magnetic agitation is until dissolving (needing about 60min of time).
(3) step: 1.5g polyaniline (PNAI) is added under stirring in the 30ml oxolane, fully disperse.Solution with the preparation of (2) step mixes ultrasonic dispersion 30min again.Continue to make both fully mix dispersion (cumulative volume is 60ml approximately) about vigorous stirring 50min, continue stirring and make solvent evaporates, can suitably be heated to 45 ℃, accelerate volatilization.Until evaporate in the pasty state fluid of solution thickness, at this moment cumulative volume is about about 15ml.
(4) step: the pasty state viscous fluid of (3) step preparation is brushed on the pb-ag alloy base material, brushes at every turn and wait to do later on the lower one deck of again brushing, repeating to like this coating layer thickness is to get final product about 0.5cm.Leave standstill under the formed composite material room temperature and obtain prepared composite material about 40 hours.
The inert electrode material polymer compound layer that is prepared into is combined with substrate better, and the compound conductance of macromolecule is higher.
Embodiment two:
(1) step: aluminium test piece a slice of intercepting 0.5cm * 3cm * 4cm, use first respectively deionized water drip washing 3～5 times, then in acetone soln, soak 2～5min, take out test piece, be 80 ℃～90 ℃ hot wash 1～3 time again with temperature, then dry up with after the deionized water drip washing 1～3 time.
(2) step: take by weighing 2g polymethyl methacrylate (PMMA) and 1g polyvinyl chloride (PVC), minute several times add in the 80ml chloroform, and seal with preservative film, and magnetic agitation is until dissolving (needing about 140min of time).
(3) step: 2.5g polyaniline (PNAI) is added under stirring in the 30ml chloroform, fully disperse.Solution with the preparation of (2) step mixes ultrasonic dispersion 30min again.Continue to make both fully mix dispersion (cumulative volume is 80ml approximately) about vigorous stirring 50min, continue stirring and make solvent evaporates, can suitably be heated to 60 ℃, accelerate volatilization.Until evaporate in the pasty state fluid of solution thickness, at this moment cumulative volume is about about 20ml.
(4) step: the aluminium test piece of (1) step preparation is immersed in the rheid of (3) step preparation, (approximately 15min) slowly mentions after infiltrating fully, again test piece is infiltrated again after the polymer composite for the treatment of surface attachment solidifies and mention, get final product after the composite bed that so repeats to the test piece surface has 0.5cm.Leave standstill under the formed composite material room temperature and get prepared composite material about 40 hours.
The inert electrode material polymer compound layer that is prepared into is combined with substrate better, and the compound conductance of macromolecule is higher.
Embodiment three:
(1) step: titanium plate test piece a slice of intercepting 0.5cm * 3cm * 4cm, use first respectively deionized water drip washing 3～5 times, then in acetone soln, soak 2～5min, take out test piece, be 80 ℃～90 ℃ hot wash 1～3 time again with temperature, then dry up with after the deionized water drip washing 1～3 time.
(2) step: take by weighing 1.5g polymethyl methacrylate (PMMA) and 0.5g polyvinyl chloride (PVC), add in the 40ml oxolane, and seal with preservative film, magnetic agitation is until dissolving (approximately 60min).
(3) step: 1.5g polypyrrole (PPy) is added under stirring in the 30ml oxolane, fully disperse.Solution with the preparation of (2) step mixes ultrasonic dispersion 30min again.Continue to make both fully mix dispersion (cumulative volume is 60ml approximately) about vigorous stirring 50min, continue stirring and make solvent evaporates, can suitably be heated to 45 ℃, accelerate volatilization.Until evaporate in the pasty state fluid of solution thickness, at this moment cumulative volume is about about 15ml.
(4) step: the pasty state viscous fluid of (3) step preparation is brushed on the titanium plate substrate, brushes at every turn and wait to do later on the lower one deck of again brushing, repeating to like this coating layer thickness is to get final product about 0.5cm.Leave standstill under the formed composite material room temperature and obtain prepared composite material about 40 hours.
The inert electrode material polymer compound layer that is prepared into is combined with substrate better, and the compound conductance of macromolecule is higher.
Claims (6)
1. conducting polymer composite clad metal base inert electrode material preparation method is characterized in that step is as follows:
(1) preparation metallic framework substrate: use first deionized water drip washing 3～5 times, then soak 2～5min in acetone soln, taking out with temperature is 80 ℃～90 ℃ hot wash 1～3 time again, dries up with after the deionized water drip washing 1～3 time at last;
(2) preparation conducting polymer coating material:
1. will account for the conducting polymer composite of composite coating quality 30%～70%, dispersed with stirring seals ultrasonic dispersion 30min again in the organic solvent of capacity, obtain stable conducting polymer composite dispersion solution;
2. in mass ratio with polymethyl methacrylate (PMMA) and polyvinyl chloride (PVC)=(1～4): the mixture that (1～4) forms be dissolved in capacity with 1. go on foot selected phase with organic solvent in, the gross mass of described mixture accounts for 30%～70% of composite coating quality;
3. will 1. go on foot and the solution of 2. step preparation mixes, abundant dispersed with stirring, the organic solvent that at room temperature volatilizees obtains the conducting polymer composite coating mucus of thickness;
(3) at coated with conductive polymeric coating material in the metallic framework substrate: the conducting polymer composite coating mucus brushing of the thickness that step (2) is prepared is in the metallic framework substrate that step (1) is handled well, after coating is done for the first time, be coated with again the second layer, so circulate until the high polymer composite coating material that coats in the metallic framework substrate reaches till the thickness that needs; Perhaps
The metallic framework base material that step (1) is handled well is immersed in the conducting polymer composite coating mucus of the prepared thickness of step (2), then mention, after composite coating mucus is done, repeat again aforesaid operations, so circulate until the high polymer composite coating material that coats in the metallic framework substrate reaches till the thickness that needs.
2. described conducting polymer composite clad metal base inert electrode material preparation method according to claim 1, when it is characterized in that described step (2) preparation conducting polymer coating material, conducting polymer composite is dispersed in the performed polymer of methyl methacrylate (MMA), again further polymerization under temperature action, obtaining can be for the conducting polymer composite coating liquid of brushing; Also can
Conductive high polymer monomer is added in aggregate in the liquid phase substance of polymethyl methacrylate (PMMA) and polyvinyl chloride (PVC) dissolving can be for the conducting polymer composite coating liquid of brushing.
3. described conducting polymer composite clad metal base inert electrode material preparation method according to claim 1 is characterized in that described conducting polymer composite is polyaniline, polypyrrole or polythiophene; Organic solvent is oxolane or chloroform.
4. described conducting polymer composite clad metal base inert electrode material preparation method according to claim 1 is characterized in that described metallic framework base material is: aluminium, magnesium alloy, stainless steel, titanium, lead or pb-ag alloy; The shape of metallic framework base material is: sheet material, netted or grizzly bar shape.
5. described conducting polymer composite clad metal base inert electrode material preparation method according to claim 1 is characterized in that reply metallic framework base material oil removing and activation processing in the described step (1).
6. described conducting polymer composite clad metal base inert electrode material preparation method according to claim 1, it is characterized in that adopting layering to be coated with conducting polymer composite in the described step (3) rinses in the metallic framework substrate, or employing is immersed in metallic framework the coating that realizes in the conducting polymer composite mucus metal base material several times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876869A (en) * | 2019-01-26 | 2019-06-14 | 南开大学 | Titanium diboride surface cladding functional film material of core-shell structure and the preparation method and application thereof |
| CN110021732A (en) * | 2019-04-24 | 2019-07-16 | 扬州大学 | A kind of anti-corrosion method of carbon paper and metal junction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101764257A (en) * | 2009-11-20 | 2010-06-30 | 无锡欧力达新能源电力科技有限公司 | Rechargeable aluminium-sulfur battery and preparation method thereof |
| CN102505130A (en) * | 2011-12-01 | 2012-06-20 | 昆明理工大学 | Polyaniline-coated Al-based Pb-WC composite anode and preparation method thereof |
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2012
- 2012-09-24 CN CN201210357565.6A patent/CN102881384B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101764257A (en) * | 2009-11-20 | 2010-06-30 | 无锡欧力达新能源电力科技有限公司 | Rechargeable aluminium-sulfur battery and preparation method thereof |
| CN102505130A (en) * | 2011-12-01 | 2012-06-20 | 昆明理工大学 | Polyaniline-coated Al-based Pb-WC composite anode and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| S H DESHMUKH: "Electrical conductivity of polyaniline doped PVC–PMMA polymer blends", 《BULLETIN OF MATERIALS SCIENCE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109876869A (en) * | 2019-01-26 | 2019-06-14 | 南开大学 | Titanium diboride surface cladding functional film material of core-shell structure and the preparation method and application thereof |
| CN110021732A (en) * | 2019-04-24 | 2019-07-16 | 扬州大学 | A kind of anti-corrosion method of carbon paper and metal junction |
| CN110021732B (en) * | 2019-04-24 | 2022-02-11 | 扬州大学 | Corrosion prevention method for joint of carbon paper and metal |
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Denomination of invention: Preparation of metal based inert electrode materials coated with conductive polymer materials Effective date of registration: 20220526 Granted publication date: 20150701 Pledgee: Agricultural Bank of China Limited Kunming Xishan District sub branch Pledgor: KUNMING HENDERA SCIENCE AND TECHNOLOGY Co.,Ltd. Registration number: Y2022530000014 |
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