CN108425132B - A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate - Google Patents
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate Download PDFInfo
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- CN108425132B CN108425132B CN201810139367.XA CN201810139367A CN108425132B CN 108425132 B CN108425132 B CN 108425132B CN 201810139367 A CN201810139367 A CN 201810139367A CN 108425132 B CN108425132 B CN 108425132B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/13—Ozone
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
Abstract
The present invention uses frame board of the polytetrafluoroethylene (PTFE) as anode catalyst diaphragm plate, cost is relatively low, and polytetrafluoroethylene (PTFE) itself has corrosion resistant characteristic, its form for being configured to mesh plate, there is biggish contact area, and also assure due physical strength, so that the replacement and disassembly of anode diaphragm plate are more simple and convenient.Polytetrafluoroethylene (PTFE) mesh plate is into having crossed laser ablation and plasma polarization process, it is formd on polytetrafluoroethylene (PTFE) mesh plate convenient for accommodating and deposition of carbon nanotubes-brown lead oxide composite material ability, laser ablation can form pit on polytetrafluoroethylene (PTFE) mesh plate, laser treatment and plasma polarization process can also improve the activation energy of ptfe surface, make carbon nanotube-combination of the brown lead oxide composite material on polytetrafluoroethylene (PTFE) mesh plate more closely by molecule bonding force, and without the interference of extraneous other factors, so that catalytic action is more pure.
Description
Technical field
The present invention relates to electrolytic preparation Ozone Water technical field more particularly to a kind of ozone electrolytic cell anode catalyst diaphragm plates
Preparation method.
Background technique
Ozone is light blue gas, is a kind of extremely strong oxidant, by oxidation, inhibits the breeding and life of bacterium
It is long, and lead to the death of bacterium, it is a kind of strong fungicide again.Ozone can be dissolved in water, and the Ozone Water of certain ozone concentration is same
With extremely strong bactericidal effect.Ozone and ozone water energy are sterilized and are sterilized to food, drinking water, are disappeared to drinking water
When malicious, in addition to the bacterium in water can be killed, it is further purified outside the impurity in water, moreover it is possible to increase the oxygen content in water.Ozone and
All kinds of skin diseases that Ozone Water causes bacterium, bacterial inflammation, the diseases such as burn surfaces have certain curative effect.Ozone and
Ozone Water also has many advantages, such as without side-effects, non-toxic, without secondary pollution.Therefore, it is widely used in drinking water, food
The fields such as processing, health care, chemical industry, environmental protection.
The method for preparing ozone has corona method and electrolysis method, and electrolysis method is again can prepare high-concentrated ozone better than corona method.
Current electrolytic ozone generator, by electrolysis ozone generator, electrolysis ozone generator power supply, anode water tank, cathode water tank
Composition.
Solid polymer electrolyte water electrolysis technology originates from the research of General Electric Company earliest, is USA space
Plan exploitation low-temperature fuel cell was applied to the apparatus of oxygen supply aspect of spaceship and submarine later.Nowadays, solid polymerization
Object electrolyte technology be widely used hydrogen-oxygen fuel cell, Organic Electrochemical Synthesis,
The fields such as the preparation of sensor, ozone.From in the eighties of last century middle and later periods, solid polymer electrolyte technology is by more next
More using produces in ozoniferous research.In the structure of solid polymer electrolyte electrolytic ozone generation, solid polymer
For this solid electrolyte of amberplex instead of traditional liquid electrolyte, electrocatalytic particles are attached directly to solid polymer
On dielectric film two sides, solid polymer electrolyte composite membrane is formed, this structure of composite membrane can increase the contact of electrode reaction
Area greatly improves the mass transfer velocity of reactant, is conducive to the separation of reaction product, and reaction is combined together with separating, simplification
The structure of electrolysis unit.Currently, anode catalyst diaphragm can use the materials such as platinum, glass-like carbon, stannic oxide and brown lead oxide
Material, since the product ozone of ozone generator has very strong corrosivity, so must with containing platinum, antimony, tin organic solution at
The diaphragm plate is managed, its surface and inner passage is made to form the conductive lumarith of one layer of platiniferous, antimony, tin.Such ozone occurs
It is by poly- four when being film-made piece that the hardened structure of device anode film and its manufacture craft, which have the disadvantage that due to catalyst brown lead oxide particle,
What vinyl fluoride was bonded together, therefore the particle surface of the brown lead oxide just has polytetrafluoroethylene (PTFE), polytetrafluoroethylene (PTFE) is not urged
Change the function of reaction, it reduces effective contact area of brown lead oxide particle, so that reaction efficiency be made to decline, eventually leads to smelly
The generation rate of oxygen declines.Even if carefully having done upper corrosion protection processing, also it is difficult ensure totality channel by it is described containing platinum,
The anticorrosion layer of the conduction of antimony, tin tightly covers.And diaphragm plate corrosion protection processing quality be to influence ozone generator service life and efficiency
Deciding factor.
Disadvantage mentioned above is to improve the key limiting link of the efficiency and use cost of electrolysis type ozone generator, for smelly
The preparation of oxygen electrolytic cell anode catalyst diaphragm plate, general technical solution mainly has mull technique, ion-exchange, electrochemistry in the industry
Sedimentation etc., but these all do not get rid of the processes such as bonding, plating, pressed-powder anode catalyst granules, and existing preparation
Method can't guarantee that ozone generator anode construction has high working efficiency and working life.
By the research prior art, the preparation method of ideal ozone electrolytic cell anode catalyst diaphragm plate is not yet found, because
This, needs to develop a kind of new preparation method, makes ozone electrolytic cell anode catalyst diaphragm plate working efficiency with higher and work
Make the service life.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide a kind of ozone electrolytic cell anodes to urge
The preparation method of agent diaphragm plate, the present invention are used in combination using carbon nanotube and catalyst brown lead oxide, have high catalytic efficiency,
The advantages of long service life, while carbon nano tube compound material high conductivity, high-intensitive advantage can be preferably played, have
Wide application prospect.
In order to achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to 15-30mg/ml's
Carbon nano tube dispersion liquid；
(2) dissoluble lead salting liquid is prepared, soluble lead salt is dissolved in deionized water and is configured to saturation lead salt solution；
(3) alkaline solution is prepared, the concentration of alkaline solution is 15-20mg/ml；
(4) carbon nano tube dispersion liquid, alkaline solution and lead salt solution are added in reaction kettle and carry out hybrid reaction,
The volume ratio of the carbon nano tube dispersion liquid, alkaline solution and lead salt solution is 5-15:5-10:75-90；Water-bath keeps temperature
50-80 DEG C and continue stirring 24-48 hours；Mixed solution after taking out reaction carries out 50-100 DEG C of low temperature distillation in flask,
Until solvent removes, reactant is taken out, pickling for several times, washing is repeated, is finally rinsed with deionized water, until material washs
Liquid is in neutrality, and is entered back into baking oven drying, is obtained carbon nanotube-lead composite material；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 500-800 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 200-400nm, and the maximum power of laser generator is 10-20W, the repetition of laser generator
Frequency is 50-150KHz, and laser generator pulse width is 30-80ns, feed speed 8-15cm/min, laser generator energy
Metric density is 10-20J/cm2, a large amount of pits of two sides appearance of polytetrafluoroethylene (PTFE) mesh plate, the depth of the pit is 70-200
Micron, pit diameter are 80-160 microns, and the spacing between adjacent pit is 100-300 microns, polytetrafluoroethylene (PTFE) mesh plate
Porosity is 30%-65%；
(7) the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6) is polarised, obtains polarized poly- four
Vinyl fluoride mesh plate；
(8) carbon nanotube-lead composite material being prepared in step (4) is dispersed in deionized water again, through super
Sound stirs 24-48 hours, and carbon nanotube-lead composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-lead obtained in step (8)
In the saturation dispersion liquid of composite material, taken out after being kept for 3-10 minutes, at room temperature natural air drying, then repeatedly with deionized water
Washing, and low temperature drying is carried out, it obtains being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as ozone
Electrolytic cell anode catalyst diaphragm.
Preferably, reducing agent solution is also added into the hybrid reaction of step (4), the reducing agent is oxalic acid, described to go back
The concentration of former agent solution is 5-15mg/ml, and the dosage of the reducing agent solution is the 50-90% of the alkaline solution；
Preferably, carbon nanotube-lead composite material obtained in step (4) is carbon nanotube-brown lead oxide composite material.
Preferably, the soluble lead salt in the step (2) is the nitrate containing lead element, acetate, carbonate, salt
One or more of hydrochlorate, sulfate and complex salt；The alkaline solution is one kind or mixed of sodium hydroxide, potassium hydroxide
Close object.
Preferably, in the step (6) laser ablation processing be ultraviolet laser etching processing, be single laser pulse or
Multiple laser pulses act on same position progress；Polytetrafluoroethylene (PTFE) mesh plate after laser ablation is first molten in Nafion resin
It is impregnated 15-20 minutes in liquid, takes out natural cooling, the mixed solution for the isopropyl alcohol and water for being then 7:3 with mass ratio washs number
It is secondary, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 0.2-1mm.
Preferably, the polarization process in the step (7) is plasma polarization process, at low-temperature plasma polarization
Reason, power 3.5-5kw, scanning speed 400-600mm/min, plasma energy metric density are 1.5-3J/mm2。
Preferably, in the carbon nanotube-brown lead oxide composite material, the content of brown lead oxide is 70-85%, the carbon
Nanotube-brown lead oxide composite material partial size is 50-150 microns.
Compared with the prior art, the invention has the following beneficial effects:
(1), brown lead oxide catalyst growth is deposited on carbon nanotube using carbon nanotube as support construction by the present invention
Surface or carbon nanotube inside, since carbon nanotube has extraordinary orientating type and electric conductivity, so that entire anode is urged
Agent diaphragm plate electric conductivity with higher and current density, improve the working efficiency of electrolysis；Brown lead oxide is located in carbon nanotube,
Effective contact area of the brown lead oxide catalyst and reactive material is increased, catalytic efficiency can be improved, and then improve
Reaction efficiency and electrolysis production speed.Carbon nanotube mutual lapping on polytetrafluoroethylene (PTFE) mesh plate forms the close conductive mesh of matter
Network improves the electric conductivity and current density of entire anode catalyst diaphragm plate, and since the brown lead oxide as catalyst does not have
It is wrapped by or covers, Direct precipitation is on the carbon nanotubes, electric with being located in direct exposed or half exposed state
Cation-exchange membrane among solution electrode can be contacted directly, have relatively high contact area and catalytic efficiency, so that electric
The efficiency that solution prepares ozone significantly improves.
(2), the present invention uses frame board of the polytetrafluoroethylene (PTFE) as anode catalyst diaphragm plate, and cost is relatively low, and poly- four
Vinyl fluoride itself has corrosion resistant characteristic, is configured to the form of mesh plate, that is, has biggish contact area, but also protect
Due physical strength is demonstrate,proved, so that the replacement and disassembly of anode diaphragm plate are more simple and convenient.Polytetrafluoroethylene (PTFE) is to make originally
It is used to prepare catalyst diaphragm for binder, but the diaphragm that this mull technique is prepared can be by the titanium dioxide as catalyst
Lead is embedded therein, can reduce its contact with cation-exchange membrane, and then lead to the reduction of catalytic efficiency.The present invention is using poly-
Tetrafluoroethene is as framework material, not embedded catalyst particle, but these catalyst particle depositions are filled into framework material
Surface, and adherency appropriate is carried out by numerical value material identical with cation-exchange membrane, increases catalyst and cation
The contact area of exchange membrane, improves catalytic efficiency.
(3), polytetrafluoroethylene (PTFE) mesh plate of the invention is into laser ablation and plasma polarization process has been crossed, in polytetrafluoroethyl-ne
It is formd on alkene mesh plate convenient for accommodating and deposition of carbon nanotubes-brown lead oxide composite material ability, laser ablation can be
Form pit on polytetrafluoroethylene (PTFE) mesh plate, for accommodating carbon nanotube-brown lead oxide composite material, meanwhile, laser treatment and
Plasma polarization process can also improve the activation energy of ptfe surface, make carbon nanotube-dioxy by molecule bonding force
Change combination of the lead composite material on polytetrafluoroethylene (PTFE) mesh plate more closely, and without the interference of extraneous other factors, makes
It is more pure to obtain catalytic action.The present invention is first in Nafion resin solution in the polytetrafluoroethylene (PTFE) mesh plate after laser ablation
It impregnates, so that polytetrafluoroethylene (PTFE) web plate is online to be coated with one layer of very thin Nafion resin, this Nafion resin is also electrolysis
The main component of cation-exchange membrane used when Ozone Water is prepared, one layer of same substance is first set on anode catalyst diaphragm plate
Membrane material, anode catalyst can be promoted to contact with the closer of cation-exchange membrane, while making carbon nanotube-brown lead oxide
Composite material attaches more secured on polytetrafluoroethylene (PTFE) mesh plate, further increases catalytic efficiency.
(4), the present invention is using using chemical synthesis, directly beam system is on the carbon nanotubes for brown lead oxide, so that dioxy
Change lead in carbon nanotube combination and deposit it is more secured；The present invention uses twice dispersing redeposition technology, by carbon nanometer
Pipe-brown lead oxide composite material uniform deposition both ensure that the uniformity of deposition and noiseless on polytetrafluoroethylene (PTFE) mesh plate
Property, and make the combination of carbon nanotube-brown lead oxide composite material and polytetrafluoroethylene (PTFE) mesh plate that there is enough intensity, foot
To meet subsequent use demand.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.
Embodiment 1
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to the carbon of 15mg/ml
Nanotube dispersion liquid；
(2) lead acetate, ceruse mixed solution are prepared, soluble lead salt is dissolved in deionized water be configured to be saturated it is molten
Liquid；
(3) sodium hydroxide solution is prepared, the concentration of sodium hydroxide solution is 15mg/ml；
(4) carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution are added in reaction kettle and mix instead
It answers, the volume ratio of the carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution is 5:5:75；It joined reducing agent grass
Acid solution, the concentration of the oxalic acid solution are 5mg/ml, and dosage is the 50% of the sodium hydroxide solution, and water-bath keeps temperature 50
DEG C and continue stirring 24 hours；Mixed solution after taking out reaction carries out 50 DEG C of low temperature distillations in flask, until solvent is gone
It removes, takes out reactant, pickling for several times, washing is repeated, is finally rinsed with deionized water, until material cleaning solution is in neutrality,
Baking oven drying is entered back into, carbon nanotube-brown lead oxide composite material is obtained；Dioxy in carbon nanotube-brown lead oxide composite material
The content for changing lead is 70%, and carbon nanotube-brown lead oxide composite material partial size is 50 microns；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 500 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 200nm, and the maximum power of laser generator is 10, and the repetition rate of laser generator is
50KHz, laser generator pulse width are 30ns, and feed speed 8cm/min, laser generator energy density is 10J/cm2,
It is handled using single ultraviolet laser corrasion in same position；Polytetrafluoroethylene (PTFE) mesh plate after laser ablation first exists
It is impregnated 15 minutes in Nafion resin solution, takes out natural cooling, the mixing for the isopropyl alcohol and water for being then 7:3 with mass ratio is molten
Liquid washs for several times, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 0.2mm；The two of polytetrafluoroethylene (PTFE) mesh plate after etched processing
There are a large amount of pits in face, and the depth of the pit is 70 microns, and pit diameter is 80 microns, and the spacing between adjacent pit is
100 microns, the porosity of polytetrafluoroethylene (PTFE) mesh plate is 30%；
(7) plasma polarization process is carried out to the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6), using low temperature
Plasma polarization process, power 3.5kw, scanning speed 400mm/min, plasma energy metric density are 1.5J/mm2, obtain
Polarized polytetrafluoroethylene (PTFE) mesh plate；
(8) carbon nanotube being prepared in step (4)-brown lead oxide composite material is dispersed in deionized water again
In, through ultrasonic agitation 24 hours, carbon nanotube-brown lead oxide composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-two obtained in step (8)
In the saturation dispersion liquid for aoxidizing lead composite material, taken out after being kept for 3 minutes, natural air drying, then uses deionized water at room temperature
It washs repeatedly, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as
Ozone electrolytic cell anode catalyst diaphragm.
Embodiment 2
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to the carbon of 30mg/ml
Nanotube dispersion liquid；
(2) lead acetate, ceruse mixed solution are prepared, soluble lead salt is dissolved in deionized water be configured to be saturated it is molten
Liquid；
(3) sodium hydroxide solution is prepared, the concentration of sodium hydroxide solution is 20mg/ml；
(4) carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution are added in reaction kettle and mix instead
It answers, the volume ratio of the carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution is 15:10:90；It joined reduction
Agent oxalic acid solution, the concentration of the oxalic acid solution are 15mg/ml, and dosage is the 90% of the sodium hydroxide solution, and water-bath keeps temperature
80 DEG C of degree simultaneously continues stirring 48 hours；Mixed solution after taking out reaction carries out 100 DEG C of low temperature distillations in flask, until molten
Agent removal, takes out reactant, and pickling for several times, washing is repeated, is finally rinsed with deionized water, in material cleaning solution is in
Property, baking oven drying is entered back into, carbon nanotube-brown lead oxide composite material is obtained；Two in carbon nanotube-brown lead oxide composite material
The content of lead oxide is 85%, and carbon nanotube-brown lead oxide composite material partial size is 150 microns；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 800 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 400nm, and the maximum power of laser generator is 20W, and the repetition rate of laser generator is
150KHz, laser generator pulse width are 80ns, and feed speed 15cm/min, laser generator energy density is 20J/
cm2, handled using single ultraviolet laser corrasion in same position；Polytetrafluoroethylene (PTFE) mesh after laser ablation
Plate first impregnates 20 minutes in Nafion resin solution, takes out natural cooling, the isopropyl alcohol and water for being then 7:3 with mass ratio
Mixed solution washs for several times, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 1mm；Polytetrafluoroethylene (PTFE) mesh plate after etched processing
Two sides there are a large amount of pits, the depth of the pit is 200 microns, and pit diameter is 160 microns, between adjacent pit between
Away from being 300 microns, the porosity of polytetrafluoroethylene (PTFE) mesh plate is 65%；
(7) plasma polarization process is carried out to the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6), using low temperature
Plasma polarization process, power 5kw, scanning speed 600mm/min, plasma energy metric density are 3J/mm2, polarized
Polytetrafluoroethylene (PTFE) mesh plate；
(8) carbon nanotube being prepared in step (4)-brown lead oxide composite material is dispersed in deionized water again
In, through ultrasonic agitation 48 hours, carbon nanotube-brown lead oxide composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-two obtained in step (8)
In the saturation dispersion liquid for aoxidizing lead composite material, holding is taken out after ten minutes, and natural air drying, then uses deionized water at room temperature
It washs repeatedly, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as
Ozone electrolytic cell anode catalyst diaphragm.
Embodiment 3
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to the carbon of 20mg/ml
Nanotube dispersion liquid；
(2) lead acetate, ceruse mixed solution are prepared, soluble lead salt is dissolved in deionized water be configured to be saturated it is molten
Liquid；
(3) sodium hydroxide solution is prepared, the concentration of sodium hydroxide solution is 18mg/ml；
(4) carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution are added in reaction kettle and mix instead
It answers, the volume ratio of the carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution is 10:8:85；It joined reducing agent
Oxalic acid solution, the concentration of the oxalic acid solution are 8mg/ml, and dosage is the 75% of the sodium hydroxide solution, and water-bath keeps temperature
50-80 DEG C and continue stirring 36 hours；Mixed solution after taking out reaction carries out 80 DEG C of low temperature distillations in flask, until molten
Agent removal, takes out reactant, and pickling for several times, washing is repeated, is finally rinsed with deionized water, in material cleaning solution is in
Property, baking oven drying is entered back into, carbon nanotube-brown lead oxide composite material is obtained；Two in carbon nanotube-brown lead oxide composite material
The content of lead oxide is 80%, and carbon nanotube-brown lead oxide composite material partial size is 100 microns；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 750 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 300nm, and the maximum power of laser generator is 15W, and the repetition rate of laser generator is
100KHz, laser generator pulse width are 60ns, and feed speed 10cm/min, laser generator energy density is 15J/
cm2, handled using single ultraviolet laser corrasion in same position；Polytetrafluoroethylene (PTFE) mesh after laser ablation
Plate first impregnates 18 minutes in Nafion resin solution, takes out natural cooling, the isopropyl alcohol and water for being then 7:3 with mass ratio
Mixed solution washs for several times, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 0.5mm；Polytetrafluoroethylene (PTFE) mesh after etched processing
There are a large amount of pits in the two sides of plate, and the depth of the pit is 100 microns, and pit diameter is 120 microns, between adjacent pit
Spacing is 200 microns, and the porosity of polytetrafluoroethylene (PTFE) mesh plate is 50%；
(7) plasma polarization process is carried out to the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6), using low temperature
Plasma polarization process, power 4kw, scanning speed 500mm/min, plasma energy metric density are 2J/mm2, polarized
Polytetrafluoroethylene (PTFE) mesh plate；
(8) carbon nanotube being prepared in step (4)-brown lead oxide composite material is dispersed in deionized water again
In, through ultrasonic agitation 36 hours, carbon nanotube-brown lead oxide composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-two obtained in step (8)
In the saturation dispersion liquid for aoxidizing lead composite material, holding is taken out after five minutes, and natural air drying, then uses deionized water at room temperature
It washs repeatedly, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as
Ozone electrolytic cell anode catalyst diaphragm.
Embodiment 4
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to the carbon of 20mg/ml
Nanotube dispersion liquid；
(2) lead acetate, ceruse mixed solution are prepared, soluble lead salt is dissolved in deionized water be configured to be saturated it is molten
Liquid；
(3) sodium hydroxide solution is prepared, the concentration of sodium hydroxide solution is 16mg/ml；
(4) carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution are added in reaction kettle and mix instead
It answers, the volume ratio of the carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution is 12:7:80；It joined reducing agent
Oxalic acid solution, the concentration of the oxalic acid solution are 12mg/ml, and dosage is the 70% of the sodium hydroxide solution, and water-bath keeps temperature
60 DEG C and continue stirring 40 hours；Mixed solution after taking out reaction carries out 70 DEG C of low temperature distillations in flask, until solvent is gone
It removes, takes out reactant, pickling for several times, washing is repeated, is finally rinsed with deionized water, until material cleaning solution is in neutrality,
Baking oven drying is entered back into, carbon nanotube-brown lead oxide composite material is obtained；Dioxy in carbon nanotube-brown lead oxide composite material
The content for changing lead is 80%, and carbon nanotube-brown lead oxide composite material partial size is 120 microns；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 750 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 250nm, and the maximum power of laser generator is 18W, and the repetition rate of laser generator is
135KHz, laser generator pulse width are 75ns, and feed speed 12cm/min, laser generator energy density is 18J/
cm2, handled using single ultraviolet laser corrasion in same position；Polytetrafluoroethylene (PTFE) mesh after laser ablation
Plate first impregnates 17 minutes in Nafion resin solution, takes out natural cooling, the isopropyl alcohol and water for being then 7:3 with mass ratio
Mixed solution washs for several times, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 0.5mm；Polytetrafluoroethylene (PTFE) mesh after etched processing
There are a large amount of pits in the two sides of plate, and the depth of the pit is 140 microns, and pit diameter is 150 microns, between adjacent pit
Spacing is 250 microns, and the porosity of polytetrafluoroethylene (PTFE) mesh plate is 60%；
(7) plasma polarization process is carried out to the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6), using low temperature
Plasma polarization process, power 5kw, scanning speed 550mm/min, plasma energy metric density are 3J/mm2, polarized
Polytetrafluoroethylene (PTFE) mesh plate；
(8) carbon nanotube being prepared in step (4)-brown lead oxide composite material is dispersed in deionized water again
In, through ultrasonic agitation 40 hours, carbon nanotube-brown lead oxide composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-two obtained in step (8)
In the saturation dispersion liquid for aoxidizing lead composite material, taken out after being kept for 9 minutes, natural air drying, then uses deionized water at room temperature
It washs repeatedly, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as
Ozone electrolytic cell anode catalyst diaphragm.
Comparative example 1
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to the carbon of 20mg/ml
Nanotube dispersion liquid；
(2) lead acetate, ceruse mixed solution are prepared, soluble lead salt is dissolved in deionized water be configured to be saturated it is molten
Liquid；
(3) sodium hydroxide solution is prepared, the concentration of sodium hydroxide solution is 18mg/ml；
(4) carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution are added in reaction kettle and mix instead
It answers, the volume ratio of the carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution is 10:8:85；It joined reducing agent
Oxalic acid solution, the concentration of the oxalic acid solution are 8mg/ml, and dosage is the 75% of the sodium hydroxide solution, and water-bath keeps temperature
50-80 DEG C and continue stirring 36 hours；Mixed solution after taking out reaction carries out 80 DEG C of low temperature distillations in flask, until molten
Agent removal, takes out reactant, and pickling for several times, washing is repeated, is finally rinsed with deionized water, in material cleaning solution is in
Property, baking oven drying is entered back into, carbon nanotube-brown lead oxide composite material is obtained；Two in carbon nanotube-brown lead oxide composite material
The content of lead oxide is 80%, and carbon nanotube-brown lead oxide composite material partial size is 100 microns；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 750 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 100nm, and the maximum power of laser generator is 8W, and the repetition rate of laser generator is
40KHz, laser generator pulse width are 20ns, and feed speed 5cm/min, laser generator energy density is 5J/cm2,
It is handled using single ultraviolet laser corrasion in same position；Polytetrafluoroethylene (PTFE) mesh plate after laser ablation first exists
It is impregnated 10 minutes in Nafion resin solution, takes out natural cooling, the mixing for the isopropyl alcohol and water for being then 7:3 with mass ratio is molten
Liquid washs for several times, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 1mm；The two sides of polytetrafluoroethylene (PTFE) mesh plate after etched processing
There are a large amount of pits, the depth of the pit is 50 microns, and pit diameter is 60 microns, and the spacing between adjacent pit is 80 micro-
Rice, the porosity of polytetrafluoroethylene (PTFE) mesh plate are 20%；
(7) plasma polarization process is carried out to the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6), using low temperature
Plasma polarization process, power 2kw, scanning speed 300mm/min, plasma energy metric density are 1J/mm2, polarized
Polytetrafluoroethylene (PTFE) mesh plate；
(8) carbon nanotube being prepared in step (4)-brown lead oxide composite material is dispersed in deionized water again
In, through ultrasonic agitation 36 hours, carbon nanotube-brown lead oxide composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-two obtained in step (8)
In the saturation dispersion liquid for aoxidizing lead composite material, holding is taken out after five minutes, and natural air drying, then uses deionized water at room temperature
It washs repeatedly, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as
Ozone electrolytic cell anode catalyst diaphragm.
Comparative example 2
A kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, comprising the following steps:
(1) dispersion liquid for preparing carbon nanotube in deionized water by carbon nanotube dispersion is configured to the carbon of 20mg/ml
Nanotube dispersion liquid；
(2) lead acetate, ceruse mixed solution are prepared, soluble lead salt is dissolved in deionized water be configured to be saturated it is molten
Liquid；
(3) sodium hydroxide solution is prepared, the concentration of sodium hydroxide solution is 16mg/ml；
(4) carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution are added in reaction kettle and mix instead
It answers, the volume ratio of the carbon nano tube dispersion liquid, sodium hydroxide solution and lead salt solution is 12:7:80；It joined reducing agent
Oxalic acid solution, the concentration of the oxalic acid solution are 12mg/ml, and dosage is the 70% of the sodium hydroxide solution, and water-bath keeps temperature
60 DEG C and continue stirring 40 hours；Mixed solution after taking out reaction carries out 70 DEG C of low temperature distillations in flask, until solvent is gone
It removes, takes out reactant, pickling for several times, washing is repeated, is finally rinsed with deionized water, until material cleaning solution is in neutrality,
Baking oven drying is entered back into, carbon nanotube-brown lead oxide composite material is obtained；Dioxy in carbon nanotube-brown lead oxide composite material
The content for changing lead is 80%, and carbon nanotube-brown lead oxide composite material partial size is 120 microns；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 750 mesh；
(6) double-sided laser etching processing, the laser ablation are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Optical maser wavelength used by handling is 500nm, and the maximum power of laser generator is 30W, and the repetition rate of laser generator is
200KHz, laser generator pulse width are 90ns, and feed speed 20cm/min, laser generator energy density is 30J/
cm2, handled using multiple ultraviolet laser corrasions in same position；Polytetrafluoroethylene (PTFE) mesh after laser ablation
Plate first impregnates 17 minutes in Nafion resin solution, takes out natural cooling, the isopropyl alcohol and water for being then 7:3 with mass ratio
Mixed solution washs for several times, up to polytetrafluoroethylene (PTFE) mesh plate is with a thickness of 1mm；Polytetrafluoroethylene (PTFE) mesh plate after etched processing
Two sides there are a large amount of pits, the depth of the pit is 250 microns, and pit diameter is 180 microns, between adjacent pit between
Away from being 300 microns, the porosity of polytetrafluoroethylene (PTFE) mesh plate is 60%；
(7) plasma polarization process is carried out to the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6), using low temperature
Plasma polarization process, power 8kw, scanning speed 700mm/min, plasma energy metric density are 5J/mm2, polarized
Polytetrafluoroethylene (PTFE) mesh plate；
(8) carbon nanotube being prepared in step (4)-brown lead oxide composite material is dispersed in deionized water again
In, through ultrasonic agitation 40 hours, carbon nanotube-brown lead oxide composite material saturation dispersion liquid is prepared；
(9) polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-two obtained in step (8)
In the saturation dispersion liquid for aoxidizing lead composite material, taken out after being kept for 9 minutes, natural air drying, then uses deionized water at room temperature
It washs repeatedly, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as
Ozone electrolytic cell anode catalyst diaphragm.
Anode catalyst diaphragm plate prepared by above embodiments and comparative example is applied to smelly under the conditions of same process
The preparation of Ozone Water is carried out in Oxygen Generator, and blank comparative example is set, and traditional cementi legal system is used in the blank comparative example
Anode catalyst diaphragm plate made of standby carries out the electrolytic preparation of ozone；Timing detects the concentration of its Ozone Water, data such as 1 institute of table
Show.
Table 1: the ozone of each embodiment and comparative example prepares interpretation of result
By the data comparison of table 1 it can be found that by carbon nanotube by brown lead oxide carry out it is compound after can be preferable
The catalytic efficiency for improving brown lead oxide catalyst is sunk brown lead oxide catalyst growth using carbon nanotube as support construction
Product, since carbon nanotube has extraordinary orientating type and electric conductivity, makes inside the surface of carbon nanotube or carbon nanotube
Entire anode catalyst diaphragm plate electric conductivity with higher and current density are obtained, the working efficiency of electrolysis is improved；Brown lead oxide position
In in carbon nanotube, increasing effective contact area of the brown lead oxide catalyst and reactive material, catalysis effect can be improved
Rate, and then improve reaction efficiency and electrolysis production speed.
The process conditions of laser ablation also have an impact to the complete performance of catalytic efficiency, optical maser wavelength in laser ablation,
The maximum power of laser generator, the repetition rate of laser generator, laser generator pulse width, the feed speed of etching,
Laser generator energy density all can be to carbon nanotube-deposition of the brown lead oxide composite material on polytetrafluoroethylene (PTFE) mesh plate
It has a direct impact, excessively high or too low etch process parameters selection cannot make carbon nanotube-brown lead oxide composite material
The good combination on polytetrafluoroethylene (PTFE), and then its catalytic efficiency in cell reaction is influenced, therefore, it is necessary to suitable work is arranged
Skill parameter combination, and also there is apparent synergistic effect between these parameter combinations, inconvenient arbitrarily change.Of the invention poly- four
Vinyl fluoride mesh plate is formd on polytetrafluoroethylene (PTFE) mesh plate into laser ablation and plasma polarization process has been crossed convenient for accommodating
With deposition of carbon nanotubes-brown lead oxide composite material ability, laser ablation can form recessed on polytetrafluoroethylene (PTFE) mesh plate
Hole, for accommodating carbon nanotube-brown lead oxide composite material, meanwhile, laser treatment and plasma polarization process can also improve
The activation energy of ptfe surface makes carbon nanotube-brown lead oxide composite material in polytetrafluoroethylene (PTFE) by molecule bonding force
Combination on mesh plate more closely, and without the interference of extraneous other factors, so that catalytic action is more pure.
When by lead dioxide deposition growth on the carbon nanotubes, the reaction condition of deposition growing is also required to accurately set
It sets, inappropriate reaction condition and the cooperation of each content of material cannot reach preferable desired effect.Present invention setting is suitable
Reaction condition, using chemical synthesis, directly beam system is on the carbon nanotubes for brown lead oxide, so that brown lead oxide is received with carbon
Combination and deposition on mitron is more secured；The present invention uses twice dispersing redeposition technology, by carbon nanotube-brown lead oxide
Composite material uniform deposition not only ensure that the uniformity and non interference of deposition on polytetrafluoroethylene (PTFE) mesh plate, but also make carbon
The combination of nanotube-brown lead oxide composite material and polytetrafluoroethylene (PTFE) mesh plate has enough intensity, it is sufficient to meet subsequent
Use demand.Using polytetrafluoroethylene (PTFE) as the frame board of anode catalyst diaphragm plate, cost is relatively low, and polytetrafluoroethylene (PTFE) itself has
There is corrosion resistant characteristic, be configured to the form of mesh plate, that is, there is biggish contact area, and also assure due object
Intensity is managed, so that the replacement and disassembly of anode diaphragm plate are more simple and convenient.
Claims (5)
1. a kind of preparation method of ozone electrolytic cell anode catalyst diaphragm plate, which comprises the following steps:
(1) dispersion liquid for preparing carbon nanotube, in deionized water by carbon nanotube dispersion, the carbon for being configured to 15-30mg/ml is received
Mitron dispersion liquid；
(2) dissoluble lead salting liquid is prepared, soluble lead salt is dissolved in deionized water and is configured to saturation lead salt solution；
(3) alkaline solution is prepared, the concentration of alkaline solution is 15-20mg/ml；
(4) carbon nano tube dispersion liquid, alkaline solution and lead salt solution are added in reaction kettle and carry out hybrid reaction, it is described
The volume ratio of carbon nano tube dispersion liquid, alkaline solution and lead salt solution is 5-15:5-10:75-90；Water-bath keeps temperature 50-
80 DEG C and continue stirring 24-48 hours；Mixed solution after taking out reaction carries out 50-100 DEG C of low temperature distillation, directly in flask
It is removed to solvent, takes out reactant, pickling for several times, washing is repeated, is finally rinsed with deionized water, until material cleaning solution
It is in neutrality, enters back into baking oven drying, obtain carbon nanotube-lead composite material；It is molten that reducing agent is also added into the hybrid reaction
Liquid, the reducing agent are oxalic acid, and the concentration of the reducing agent solution is 5-15mg/ml, and the dosage of the reducing agent solution is institute
State the 50-90% of alkaline solution；
(5) prepare polytetrafluoroethylene (PTFE) mesh plate, the mesh specification on the polytetrafluoroethylene (PTFE) mesh plate is 500-800 mesh；
(6) double-sided laser etching processing, the laser ablation processing are carried out to polytetrafluoroethylene (PTFE) mesh plate obtained in step (5)
Used optical maser wavelength is 200-400nm, and the maximum power of laser generator is 10-20W, the repetition rate of laser generator
For 50-150KHz, laser generator pulse width is 30-80ns, feed speed 8-15cm/min, and laser generator energy is close
Degree is 10-20J/cm2, a large amount of pits of two sides appearance of polytetrafluoroethylene (PTFE) mesh plate, the depth of the pit is 70-200 microns,
Pit diameter is 80-160 microns, and the spacing between adjacent pit is 100-300 microns, the porosity of polytetrafluoroethylene (PTFE) mesh plate
For 30%-65%；
(7) the polytetrafluoroethylene (PTFE) mesh plate obtained after etching in step (6) is polarised, obtains polarized polytetrafluoroethyl-ne
Alkene mesh plate；The polarization process is plasma polarization process, and using low-temperature plasma polarization process, power 3.5-5kw is swept
Retouching speed is 400-600mm/min, and plasma energy metric density is 1.5-3J/mm2；
(8) carbon nanotube-lead composite material being prepared in step (4) is dispersed in deionized water, to stir through ultrasound again
It mixes 24-48 hours, carbon nanotube-lead composite material saturation dispersion liquid is prepared；
(9) that polytetrafluoroethylene (PTFE) mesh plate obtained in step (7) is immersed into carbon nanotube-lead obtained in step (8) is compound
In the saturation dispersion liquid of material, taken out after being kept for 3-10 minutes, natural air drying, is then washed with deionized water repeatedly at room temperature
It washs, and carries out low temperature drying, obtain being coated with carbon nanotube-lead composite material polytetrafluoroethylene (PTFE) mesh plate, as ozone electricity
Solve pond anode catalyst diaphragm.
2. the preparation method of ozone electrolytic cell anode catalyst diaphragm plate according to claim 1, which is characterized in that step
(4) carbon nanotube-lead composite material obtained in is carbon nanotube-brown lead oxide composite material.
3. the preparation method of ozone electrolytic cell anode catalyst diaphragm plate according to claim 2, which is characterized in that the step
Suddenly the soluble lead salt in (2) is the nitrate containing lead element, acetate, carbonate, hydrochloride, sulfate and complex salt
One or more of；The alkaline solution is sodium hydroxide, one kind of potassium hydroxide or mixture.
4. the preparation method of ozone electrolytic cell anode catalyst diaphragm plate according to claim 3, which is characterized in that the step
Suddenly the laser ablation processing in (6) is ultraviolet laser etching processing, is acted on together for single laser pulse or multiple laser pulses
One position carries out；Polytetrafluoroethylene (PTFE) mesh plate after laser ablation first impregnates 15-20 minutes in Nafion resin solution, takes
The mixed solution for the isopropyl alcohol and water that natural cooling out is then 7:3 with mass ratio washs for several times, until polytetrafluoroethylene (PTFE) mesh
Plate with a thickness of 0.2-1mm.
5. the preparation method of ozone electrolytic cell anode catalyst diaphragm plate according to claim 4, which is characterized in that the carbon
In nanotube-brown lead oxide composite material, the content of brown lead oxide is 70-85%, the carbon nanotube-brown lead oxide composite wood
The partial size of material is 50-150 microns.
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