CN104759272B - A kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator and its production method of anode and anode - Google Patents
A kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator and its production method of anode and anode Download PDFInfo
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- CN104759272B CN104759272B CN201410747989.2A CN201410747989A CN104759272B CN 104759272 B CN104759272 B CN 104759272B CN 201410747989 A CN201410747989 A CN 201410747989A CN 104759272 B CN104759272 B CN 104759272B
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Abstract
The membrane electrode and its production method of anode and anode of a kind of membrane electrode low-voltage electrolysis formula ozone generator are related to the membrane electrode of electrolysis ozone generator.The present invention is high using electro catalytic activity, corrosion resistance is high, non-secondary pollution boron-doped diamond is as anode catalyst, further, boron-doped diamond is deposited directly in POROUS TITANIUM PLATE using vapour deposition process, and is hot pressed into the anode construction for integrating POROUS TITANIUM PLATE, anode catalyst and proton exchange polymer membrane with proton exchange polymer membrane.Compared with prior art, not only preparation process is simple for the anode construction, it is easy to assembly, be conducive to produce in batches, and the Boron-doped diamond for being deposited on POROUS TITANIUM PLATE surface has porous structure, effectively improves permeable, permeability, phenomena such as avoiding that the decline of catalyst performance, slot pressure and temperature is caused to increase since water-permeable and air permeable is unsmooth, membrane electrode service life is improved, ensures that membrane electrode electrolysis ozone generator can be run steadily in the long term.
Description
Technical field
The present invention relates to electrolysis type ozone generator technical fields, and in particular to the membrane electrode of electrolysis ozone generator.
Background technology
Ozone is a kind of extremely strong oxidant, the energy with strong sterilizing effect and oxidative degradation organic pollution
The advantages that power, and the product after reacting is the oxygen beneficial to human body, without side-effects, non-toxic, non-secondary pollution, in waste water
The application in the fields such as advanced oxidation processing, drinking water deep purification, environmental protection, food processing, medical treatment and nursing, preserving fruit and vegetable utilizing becomes
It obtains more and more extensive.
The method that ozone is produced in existing market at present is broadly divided into corona discharge method, UV radiation and solid polymer
Film (PEM membrane) electrode low tension solution.Wherein, it is smelly to be prepared by a kind of novel electrochemical method for PEM membrane electrode low tension solution
Oxygen, compared with corona discharge method and UV radiation, this method, which has, prepares concentration of ozone gas height, not nitrogen-containing oxide etc.
Carcinogen, manufacturing cost are low, membrane electrode service life is long, equipment is installed and safeguarded the advantages that simple, become a kind of most city
The ozone preparation method of field competitiveness.
PEM membrane electrode is the core component of low-voltage electrolysis formula ozone generator.Typical case's PEM membrane electrode assembly includes more at present
Hole titanium plate, anode catalyst, cathod catalyst and solid polymer proton exchange membrane etc..Wherein, anode catalyst and anode knot
Structure (being made of POROUS TITANIUM PLATE, anode catalyst and proton exchange polymer membrane) plays a key effect to generator performance.
Electrochemistry formated ozone technology require anode catalyst material to ozone be precipitated have good electro catalytic activity and
Corrosion resistance.Graphite, vitreous carbon, Pt metal are to have used anode material in the research of early stage electrochemistry formated ozone technology
Material, but due to Pt metal electrode price too expensive；The shortcomings of being easy to be corroded and consume during graphite and vitreous carbon use,
Low-voltage electrolysis formula ozone generator product generally use electro catalytic activity on existing market is high, corrosion resistance is good, price
Anode catalyst of the brown lead oxide material as membrane electrode inexpensively.
Anode construction is also an important factor for influencing electrochemistry formated ozone efficiency.It is sent out in current electrochemistry formated ozone
In raw device system, be by anode material after batch mixing film-making through be hot-pressed onto in solid polymer proton exchange membrane formed catalyst with
Membrane electrode assembly, then pass through machinery pressure with POROUS TITANIUM PLATE (POROUS TITANIUM PLATE plays the role of water conservancy diversion, conduction and support catalyst)
It is tight to constitute anode construction.With tradition detaches be electrode compared with, this membrane electrode integrated technology have equipment it is simple, it is small,
Current efficiency height, low power consumption and other advantages.
Although the used anode catalyst of PEM membrane electrode and anode construction of above-mentioned low-voltage electrolysis formula ozone generator exist
It is had many advantages in electrochemistry formated ozone performance, but there is also can not be ignored：On the one hand, brown lead oxide is as sun
No matter electrode catalyst closes from the preparation link, brown lead oxide diaphragm process of brown lead oxide raw material or in electrochemistry
During ozone, actually can not all toxic Pb ions be avoided to cause secondary pollution to environment；On the other hand, at present using sun
The relatively cumbersome complexity of pole structure preparation process, it is not easy to ensure product quality, and in the process of running, catalyst is easy stifled
POROUS TITANIUM PLATE is filled in, causes water, gas circulation unsmooth, superpressure increases, and reduces membrane electrode service life.The shortcomings that these two aspects, all will
It can hinder business promotion and the practical application of PEM membrane electrode low-voltage electrolysis ozone generator product.
Invention content
The purpose of the present invention is to provide a kind of anode catalysts of membrane electrode low-voltage electrolysis formula ozone generator.
The present invention also aims to provide a kind of anode construction of membrane electrode low-voltage electrolysis formula ozone generator.
The present invention also aims to provide a kind of anode fabrication method of membrane electrode low-voltage electrolysis formula ozone generator.
The present invention also aims to provide a kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator.
Following technical scheme may be used to realize in the present invention to achieve the above object：
A kind of anode catalyst of membrane electrode low-voltage electrolysis formula ozone generator, which is characterized in that use boron doping Buddha's warrior attendant
Anode catalyst of the stone material as low-voltage electrolysis ozone generator membrane electrode.Boron-doped diamond not only has very strong
Mechanical strength, chemical inertness, thermal stability and corrosion resistance, while there is broader electrochemical window, it can further increase
Yield of ozone, and no matter be also mounted on ozone generator and run from the preparation of its raw material, boron carbon does not have environment
Toxicity will not generate secondary pollution to environment.Therefore, boron-doped diamond belongs to environmental type anode catalyst.
A kind of anode construction of membrane electrode low-voltage electrolysis formula ozone generator, including a proton exchange polymer membrane, it is special
Sign is that being compressed on the proton exchange polymer membrane has the POROUS TITANIUM PLATE that a deposition has anode catalyst, constitutes the film electricity
The anode construction of pole low-voltage electrolysis formula ozone generator.
The anode catalyst, which is characterized in that be deposited directly in POROUS TITANIUM PLATE using boron-doped diamond material, institute
It states boron-doped diamond material and deposits the boron-doped diamond Catalytic Layer to be formed with porous structure.
The POROUS TITANIUM PLATE is equipped with a plurality of holes, it is preferable that the porosity of POROUS TITANIUM PLATE is preferably 30-45%, aperture
Preferably 15-48 μm.Further preferred average grain diameter is 25 μm, and size is 30mm × 30mm square sheet POROUS TITANIUM PLATEs.Institute
Boron-doped diamond material is stated to be deposited in the hole of the lower surface of the POROUS TITANIUM PLATE and the lower part of the POROUS TITANIUM PLATE.
A kind of anode fabrication method of membrane electrode low-voltage electrolysis formula ozone generator, which is characterized in that pass through chemical gaseous phase
Anode catalyst is deposited directly in POROUS TITANIUM PLATE by sedimentation, then constitutes collection POROUS TITANIUM with proton exchange polymer membrane hot pressing
The membrane electrode anode construction that plate, anode catalyst and proton exchange polymer membrane are integrated, the anode catalyst are mixed using boron
Miscellaneous diamond.The structure is completely free of existing prepare and is milled involved by ozone generator membrane electrode anode construction, bonds, roll
The complex techniques processes such as piece and hot pressing, manufacture craft is simple, easy to assembly, is conducive to produce in batches.Moreover, because titanium plate is more
Pore structure deposits Boron-doped diamond on its surface and porous structure, the anode catalyst film of this porous structure is also presented
Permeable, permeability can be effectively improved, avoids leading to the decline of catalyst performance, slot pressure and temperature liter since water-permeable and air permeable is unsmooth
Phenomena such as high, improves membrane electrode service life, ensures that membrane electrode electrolysis ozone generator can be run steadily in the long term.
A kind of anode fabrication method of membrane electrode low-voltage electrolysis formula ozone generator is as follows：
Step 1 carries out pre-treatment to POROUS TITANIUM PLATE：Use potassium hydroxide, tertiary sodium phosphate and ethylenediamine tetra-acetic acid water-soluble first
Liquid, which impregnates, carries out oil removing degreasing, with aqueous sulfuric acid carries out acid etch after deionized water is rinsed with remove POROUS TITANIUM PLATE surface with
The oxidation film of its apparent gap, to build roughening, active matrix surface.
Before step 1, first POROUS TITANIUM PLATE can also be cut into and meet existing low-voltage electrolysis formula ozone generator membrane electrode
Anode construction require size.The POROUS TITANIUM PLATE porosity ranges of selection require to be 30-45%, and aperture is 15-48 μm.
Step 2 is ground the POROUS TITANIUM PLATE by step 1 processing with bortz powder, then molten in acetone successively
Then ultrasonic cleaning in liquid and deionized water solution is put into nitrogen drying in Dewar bottle for use.The step is subsequently to change
The advantageous nucleation point of vapor diamond deposition offer is provided, there is the diamond nucleation density for increasing POROUS TITANIUM PLATE surface and improve and sink
Product film quality effect.Bortz powder grain size is preferably smaller than 5 μm.
Step 3 is deposited using heated filament auxiliary chemical vapor deposition method by the processed POROUS TITANIUM PLATE surface of step 2
One layer of uniform anode catalyst, the anode catalyst use boron-doped diamond material.Reactant gas source be methane, hydrogen and
Borine.Wherein, methane is carbon source, and borine is boron source, carrier of the hydrogen as methane and borine air source.Implementing to be vapor-deposited
Cheng Zhong controls the incorporation of boron in diamond thin by the atomic ratio (B/C) of boron and carbon in change air source, heavy by controlling
The product time regulates and controls Catalytic Layer film thickness.
POROUS TITANIUM PLATE is covered with the side of boron-doped diamond material using hot press and polymer proton is handed over by step 4
It changes film hot pressing compression to be combined together, anode construction is made.
In step 4, by proton exchange polymer membrane be covered with Boron-doped diamond POROUS TITANIUM PLATE machinery heat
Before pressure, it is also necessary to which using sand paper, roughening treatment is carried out to its surface, to improve Boron-doped diamond and film layer combination effect.
A kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator, is made of an anode construction and a cathode construction；
The anode construction includes a proton exchange polymer membrane, and being compressed on the proton exchange polymer membrane has a deposition
The POROUS TITANIUM PLATE for having anode catalyst constitutes a kind of anode construction of membrane electrode low-voltage electrolysis formula ozone generator.The anode
It includes a pallium-on-carbon cathod catalyst diaphragm that catalyst, which uses boron-doped diamond material, the cathode construction,.
Description of the drawings
Fig. 1 is a kind of structural schematic diagram of the membrane electrode of the present invention；
Fig. 2 is that the electrolysis type ozone generator of anode construction using the present invention and the electrolysis type ozone of the prior art occur
With the time cycle of operation is extended, (daily run time 24 hours is single with hour to yield of ozone (mg/h) to device in the process of running
Position, h) variation diagram.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Conjunction is specifically illustrating that the present invention is further explained.
Referring to Fig.1, the present invention is high using electro catalytic activity, corrosion resistance is high, non-secondary pollution boron-doped diamond conduct
Boron-doped diamond is further deposited directly in POROUS TITANIUM PLATE, and and polymer by anode catalyst using vapour deposition process
Proton exchange membrane is hot pressed into the anode construction for integrating POROUS TITANIUM PLATE, anode catalyst and proton exchange polymer membrane.With it is existing
There is technology to compare, not only preparation process is simple for the anode construction, easy to assembly, is conducive to produce in batches, and is deposited on porous
The Boron-doped diamond on titanium plate surface has porous structure, effectively improves permeable, permeability, avoids due to water-permeable and air permeable
Phenomena such as unsmooth decline for leading to catalyst performance, slot pressure and temperature increase, improves membrane electrode service life, ensures membrane electrode electricity
Solution ozone generator can be run steadily in the long term.
Specific embodiment is as follows：
It is research matrix to choose the POROUS TITANIUM PLATE that average grain diameter is 25 μm, and it is 30mm × 30mm square that it, which cuts into size,
Shape piece.
Above-mentioned POROUS TITANIUM PLATE base material is put into the aqueous solution being made of potassium hydroxide, tertiary sodium phosphate and ethylenediamine tetra-acetic acid,
Impregnated at 50-60 DEG C 5 minutes removal surface grease, and using 20% aqueous sulfuric acid at 50-60 DEG C to POROUS TITANIUM PLATE into
Row acid etch, which obtains surface for 5-8 minutes, has the fresh matrix surface of certain roughness.
Above-mentioned POROUS TITANIUM PLATE sill surface is ground, uses grain size for 2.5 μm of diamond paste
It is ground 2-5 minutes on polished machine, speed of grinding plate 300r/h.Successively in acetone soln and ultrasound in going from aqueous solution after grinding
Cleaning 5-10 minutes is used in combination nitrogen drying to be put into Dewar bottle for use.
It is thin in above-mentioned POROUS TITANIUM PLATE substrate surface deposition boron-doped diamond using heated filament auxiliary chemical vapor deposition method
Film.In chemical vapor deposition processes, it is 1 to be strict with methane and hydrogen volume ratio：99 and borine and hydrogen volume ratio be 2：
98, and atomic ratio (B/C) volume ratio for controlling boron and carbon in the present embodiment is 2.5%.Reaction temperature is 800 DEG C, reative cell
Pressure 5kPa, sedimentation time are 6 hours.Obtained Boron-doped diamond average thickness is 6 μm.Through the above steps, it makes
It being deposited directly to sun of the porous type Boron-doped diamond as low-voltage electrolysis formula ozone generator in POROUS TITANIUM PLATE for a kind of
Electrode catalyst.
Above-mentioned POROUS TITANIUM PLATE Boron-doped diamond side is covered with using hot press to exchange with polymer proton
Film hot pressing, hot pressing temperature are 80-100 DEG C, and hot pressing time is 5-10 minutes.To ensure Boron-doped diamond and polymeric material
Proton exchange fully bonds, and before hot pressing, is carried out to proton exchange polymer membrane surface using 1500 or No. 2000 sand paper
Roughening treatment, and a small amount of Nafion solution is coated to the Boron-doped diamond surface on POROUS TITANIUM PLATE surface using nozzle.It is logical
Above-mentioned steps are crossed, are prepared a kind of using Boron-doped diamond as the anode construction of the novel membrane electrode of anode catalyst.
Above-mentioned novel boron-doped diamond membrane electrode anode construction is assembled into pallium-on-carbon cathod catalyst diaphragm
Complete membrane electrode, as shown in Figure 1.A kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator, by an anode construction and
One cathode construction is constituted；Anode construction includes a proton exchange polymer membrane 1, and being compressed on proton exchange polymer membrane 1 has one to sink
Product has the POROUS TITANIUM PLATE 3 of anode catalyst 2, anode catalyst 2 to use boron-doped diamond material；Anode catalyst layer has porous
Structure, cathode construction include a pallium-on-carbon cathod catalyst diaphragm 4.POROUS TITANIUM PLATE 3 is equipped with a plurality of holes, boron doping Buddha's warrior attendant
Stone material is deposited in the hole of the lower surface of POROUS TITANIUM PLATE and the lower part of POROUS TITANIUM PLATE；The porosity of POROUS TITANIUM PLATE is 30-
45%, aperture is 15-48 μm.
This membrane electrode is installed in ozone generator, constant-current supply trial operation is applied to, and tests this possess newly
The membrane electrode ozone generator gas generation property of type boron-doped diamond anode construction, and under same service condition with it is existing by
The membrane electrode ozone generator performance that brown lead oxide constitutes anode construction is compared.Gas generation property comparison result is as follows：
Figure it is seen that the ozone generator gas generation property of the utility model is substantially better than the ozone hair of the prior art
The gas generation property of raw device.Within 3 trial operation periods half a month by a definite date, the yield of ozone presentation of the ozone generator of the prior art declines
Subtract trend, as the cycle of operation extends, 300-400mg/h is decayed to from initial stage higher 600-700mg/h, and the utility model
The yield of ozone of ozone generator decays within the entire trial operation period that performance is not significant, and remains essentially in 700-
Within the scope of 800mg/h.This result not only illustrates that the membrane electrode anode catalyst of the utility model can further increase ozone production
Amount, but also illustrate that the utility model constructed with porous type membrane electrode anode construction with good structural stability,
So that ozone generator can also keep relative stability aerogenesis yield efficiency in long-play.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (2)
1. a kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator, is made of an anode construction and a cathode construction；
The anode construction includes a proton exchange polymer membrane, which is characterized in that is compressed on the proton exchange polymer membrane
There is a deposition to have the POROUS TITANIUM PLATE of anode catalyst, constitutes the anode construction；
Anode catalyst using boron-doped diamond material as low-voltage electrolysis ozone generator membrane electrode；
It is deposited directly in POROUS TITANIUM PLATE using boron-doped diamond material, the boron-doped diamond material deposits the boron to be formed
Doped diamond Catalytic Layer has porous structure；
Anode catalyst is deposited directly in POROUS TITANIUM PLATE by chemical vapour deposition technique, then hot with proton exchange polymer membrane
Pressure constitutes the membrane electrode anode construction for integrating POROUS TITANIUM PLATE, anode catalyst and proton exchange polymer membrane；
The cathode construction includes a pallium-on-carbon cathod catalyst diaphragm；By membrane electrode anode construction, with pallium-on-carbon cathode catalysis
Agent diaphragm is assembled into complete membrane electrode；
The POROUS TITANIUM PLATE is equipped with a plurality of holes, and the boron-doped diamond material is deposited on the following table of the POROUS TITANIUM PLATE
In the hole of face and the lower part of the POROUS TITANIUM PLATE；
It is research matrix to choose the POROUS TITANIUM PLATE that average pore size is 25 μm, and it is 30mm × 30mm squares to be cut into size
Piece,
Above-mentioned POROUS TITANIUM PLATE base material is put into the aqueous solution being made of potassium hydroxide, tertiary sodium phosphate and ethylenediamine tetra-acetic acid, in 50-
5 minutes removal surface greases are impregnated at 60 DEG C, and harsh to POROUS TITANIUM PLATE progress at 50-60 DEG C using 20% aqueous sulfuric acid
Erosion, which obtains surface for 5-8 minutes, has the fresh matrix surface of certain roughness,
Above-mentioned POROUS TITANIUM PLATE sill surface is ground, grain size is used to be ground for 2.5 μm of diamond paste
It is ground 2-5 minutes on throwing machine, speed of grinding plate 300r/h is cleaned by ultrasonic 5- in acetone soln and deionized water successively after grinding
10 minutes, it is used in combination nitrogen drying to be put into Dewar bottle for use,
Boron-doped diamond is deposited in above-mentioned POROUS TITANIUM PLATE substrate surface using heated filament auxiliary chemical vapor deposition method,
In chemical vapor deposition processes, it is 1 to be strict with methane and hydrogen volume ratio：99 and borine and hydrogen volume ratio be 2：98, and
The atomic ratio for controlling boron and carbon is 2.5%, and reaction temperature is 800 DEG C, chamber pressure 5kPa, and sedimentation time is 6 hours, is obtained
It is 6 μm to obtain Boron-doped diamond average thickness, and through the above steps, preparation one kind is deposited directly to porous in POROUS TITANIUM PLATE
Anode catalyst of the type Boron-doped diamond as low-voltage electrolysis formula ozone generator；
Above-mentioned POROUS TITANIUM PLATE is covered with by Boron-doped diamond side and proton exchange polymer membrane heat using hot press
Pressure, hot pressing temperature are 80-100 DEG C, and hot pressing time is 5-10 minutes, to ensure that Boron-doped diamond is handed over polymer proton
It changes film fully to bond, before hot pressing, proton exchange polymer membrane surface is roughened using 1500 or No. 2000 sand paper
Processing, and a small amount of Nafion solution is coated to the Boron-doped diamond surface on POROUS TITANIUM PLATE surface using nozzle, by upper
Step is stated, is prepared a kind of using Boron-doped diamond as the anode construction of the membrane electrode of anode catalyst；
The yield of ozone of ozone generator is maintained within the scope of 700-800mg/h.
2. a kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator according to claim 1, which is characterized in that institute
The porosity for stating POROUS TITANIUM PLATE is 30-45%.
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Families Citing this family (9)
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| CN108396307A (en) * | 2018-01-18 | 2018-08-14 | 昆明理工大学 | A kind of preparation method of the diamond thin with strong film base adhesion strength |
| CN108411331B (en) * | 2018-02-11 | 2020-02-18 | 中氧科技（广州）有限公司 | Membrane electrode assembly of low-voltage electrolysis ozone generator and preparation method thereof |
| CN108611655B (en) * | 2018-03-18 | 2020-11-06 | 广州市德百顺电气科技有限公司 | Electrode unit and electrode composed of same |
| AU2019243601B2 (en) * | 2018-03-29 | 2023-03-23 | NorthStar Medical Radioisotopes LLC | Systems and methods for ozone water generator |
| CN109112571B (en) * | 2018-08-16 | 2019-10-01 | 浙江工业大学 | One kind loading boron, the catalyst and its preparation method and application of N doping diamond based on oxidation platinum alloy |
| CN110508311A (en) * | 2019-08-30 | 2019-11-29 | 浙江工业大学 | A kind of porous boron doped carbon supported platinum nano beaded catalyst and its preparation method and application based on electrostatic spinning technique |
| CN110724930B (en) * | 2019-11-06 | 2021-11-09 | 杭州超然金刚石有限公司 | Preparation method of diamond film |
| CN115433955B (en) * | 2022-10-13 | 2023-06-13 | 杭州热威洁净技术有限公司 | Three-electrode low-voltage electrolytic ozone generating device |
| CN117418247B (en) * | 2023-12-18 | 2024-03-15 | 中国科学院生态环境研究中心 | Ozone generating device and method for electrochemical coupling oxygen dissociation |
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Effective date of registration: 20190124 Address after: 201415 No. 1299 Juting Road, Zhuanghang Town, Fengxian District, Shanghai Patentee after: Shanghai Vm Electric Power Technology Co., Ltd. Address before: Room 101, 549 Sanmin Road, Zhuangxing Town, Fengxian District, Shanghai Patentee before: Shanghai Wei Aimu Environmental Protection Technology Co., Ltd |
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