CN108456894A - A kind of device of novel anode material and preparation method thereof, electrolytic ozone generation - Google Patents
A kind of device of novel anode material and preparation method thereof, electrolytic ozone generation Download PDFInfo
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- CN108456894A CN108456894A CN201810105074.XA CN201810105074A CN108456894A CN 108456894 A CN108456894 A CN 108456894A CN 201810105074 A CN201810105074 A CN 201810105074A CN 108456894 A CN108456894 A CN 108456894A
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000010405 anode material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 48
- 239000000725 suspension Substances 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 34
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001301 oxygen Substances 0.000 claims abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 31
- 239000010936 titanium Substances 0.000 claims description 31
- 229910052719 titanium Inorganic materials 0.000 claims description 31
- 229910001220 stainless steel Inorganic materials 0.000 claims description 21
- 239000010935 stainless steel Substances 0.000 claims description 21
- 239000010406 cathode material Substances 0.000 claims description 15
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 10
- 238000000197 pyrolysis Methods 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- -1 power supply Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 10
- 231100000614 poison Toxicity 0.000 abstract description 2
- 230000007096 poisonous effect Effects 0.000 abstract description 2
- 230000003252 repetitive effect Effects 0.000 abstract description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 31
- 238000005868 electrolysis reaction Methods 0.000 description 26
- 239000002351 wastewater Substances 0.000 description 21
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 18
- 230000000694 effects Effects 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 238000001514 detection method Methods 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- 239000010865 sewage Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 238000004448 titration Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- SXDBWCPKPHAZSM-UHFFFAOYSA-M bromate Inorganic materials [O-]Br(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-M 0.000 description 3
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- OQYYLGRLIXHSOB-UHFFFAOYSA-N ozone phenol Chemical compound [O-][O+]=O.OC1=CC=CC=C1 OQYYLGRLIXHSOB-UHFFFAOYSA-N 0.000 description 3
- 230000036647 reaction Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- 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
-
- 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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/322—Volatile compounds, e.g. benzene
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/78—Details relating to ozone treatment devices
- C02F2201/782—Ozone generators
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
Abstract
The present invention relates to novel anode material, the devices of preparation method, electrolytic ozone generation.Preparing anode material includes：By the SnC of 500~1500 parts by weight2O4It is added in reaction kettle, at least water of 150 parts by weight is added and stirs evenly；By the Sb of 5~8 parts by weight2O3It is added in reaction kettle, stirring and heating makes to be uniformly mixed, and obtains mixture；By the Ni (CH of 1~3 parts by weight3COO)2·4H2O is added in mixture, oxygen is passed through into reaction kettle, and heated, stirred, until material is in stopping heating after suspended state in reaction kettle, the material precipitation in reaction kettle takes upper layer suspension, obtain suspension containing Sn after precipitation is complete；Sn suspension will be contained coated on anode plate, be pyrolyzed at a temperature of 400~600 DEG C, and repetitive coatings pyrolytic process 7~9 times, form coating film；To coating film in 500~650 DEG C of 60~120min of sintering of temperature.The method that the present invention prepares anode material is simple, easy to operate, and when for producing ozone, no poisonous and harmful substance generates.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of novel anode material and preparation method thereof, Yi Ji electricity
Solution produces ozoniferous device.
Background technology
Ozone O3Be otherwise known as super oxygen, belongs to oxygen O2Allotrope.At normal temperatures, the half-life period of ozone be 15~
30min (minute), leads to the conventional storage difficulty of ozone and cost is higher.Meanwhile ozone is with extremely strong oxidisability and easily
Decomposability can be used as the uses such as purifying agent for polluted water, decolorising agent, disinfectant.Ozone sterilization disinfection speed is fast, effect is good, it is smelly
Oxygen reduction itself generates oxygen.Therefore, the use of ozone is widely recognized as, is universally acknowledged green disinfectant.
Currently, the production common method of ozone has corona method, electrolysis, ultraviolet method, nuclear radiation method.Wherein, corona method
Equipment investment it is higher, operating cost is high, and the ozone concentration produced is low；Ultraviolet method energy consumption is high, and the concentration for generating ozone is low,
It is not suitable for the production of a large amount of ozone；The investment of nuclear radiation method is big, dangerous, and frequency of use is very low.
It includes electrolysis air and electrolyzing pure water that electrolysis, which produces ozone mainly,.The process of electrolysis air production ozone will produce
NOxEqual noxious materials, required alternating voltage is higher, and electrolytic efficiency is low, and ozone enters water difficulty, and occupation area of equipment is big, using at
This is high；Electrolyzing pure water unit generate ozone efficiency highest, electrolytic process be using solid noble metal polymer as electrolyte,
In conjunction with cationic switch mode, ozone is obtained by way of low-voltage electrolysis, but in the technique, control system is more complicated,
Electrolytic efficiency is low, and ozone enters water difficulty, higher operating costs.
Therefore, the preparation and application of ozone are by the extensive concern of domestic and foreign scholars.
Invention content
In view of above-mentioned problems of the prior art, the present invention is intended to provide a kind of novel anode material and its preparation
Method, and the electrolyte including the anode material, the electrolyte can be prepared new by electrolytic ozone generation, in the present invention
The method of the anode material of type is easy, easily operated, and when using it for production ozone, efficiency is higher, saves the energy, and without toxic
Harmful substance generates.
The present invention proposes a kind of preparation method of novel anode material, and the anode material is by containing Sn suspension through heat
Solution, calcination process are attached on anode plate, are included the following steps：
A, the preparation of the suspension containing Sn：Prepare raw material：SnC2O4500~1500 parts by weight, Sb2O35~8 parts by weight, Ni
(CH3COO)2·4H2The parts by weight of O1~3；By SnC2O4It is added in reaction kettle, at least 150 weight is added into the reaction kettle
The water of part simultaneously stirs evenly；By Sb2O3Be added in the reaction kettle, stir and heat so that be uniformly mixed, mixed
Material；By Ni (CH3COO)2·4H2O is added in the mixture, and oxygen is then passed through into the reaction kettle, and heated,
Stirring, until for material in heating is stopped after suspended state, the material precipitation in the reaction kettle is to be precipitated complete in the reaction kettle
Quan Hou takes upper layer suspension to get to the suspension containing Sn；
B, pyrolysis processing：The suspension containing Sn is coated on the anode plate, is carried out at a temperature of 400~600 DEG C
Pyrolysis, and the coating-pyrolysis processing process 7~9 times is repeated, form coating film；
C, sintering processes：The coating film is sintered, the control of the temperature of the sintering processes process for 500~
650 DEG C, the sintering time control is 60~120min.
Further, the anode plate is by corrosion-resistant, heat safe made of metal is standby；Preferably, the anode plate is by titanium
Belong to and preparing.
As the preferred embodiment of the invention, deionized water is added into the reaction kettle.
As the preferred embodiment of the invention, the SnC2O4Take 550~900 parts by weight, the Sb2O3Take 5~8 weights
Measure part, the Ni (CH3COO)2·4H2O takes 1~3 parts by weight.
As the preferred embodiment of the invention, the flow for being passed through oxygen is 8~12L/min.
Further, the temperature for controlling the heating process is 50~60 DEG C, and the time of the heating is that 1~2h is (small
When).
The invention also provides a kind of novel anode material, the anode material is prepared by above-mentioned preparation method
's.
The invention also provides a kind of devices of electrolytic ozone generation, including anode material, cathode material, power supply, electrolysis
Liquid, the anode material are connect with the anode of the power supply by conducting wire, and the cathode of the cathode material and the power supply passes through
Conducting wire connects, and the anode material and the cathode material be placed in the electrolyte, and the anode material is above-mentioned new
The anode material of type.
As the preferred embodiment of the invention, the cathode material selects stainless steel plate.
Further, the power supply is DC power supply.
Novel anode material preparation method proposed by the present invention is easy, easily operated, without introducing complicated equipment.It should
When anode material is used for the device of electrolysis ozone, the generation of ozone, and the production without poisonous and harmful substance in the process can be effectively facilitated
It is raw.
The present invention proposes the device of electrolytic ozone generation, and catalyst film layer is formed on anode plate using suspension containing Sn,
Generation for promoting ozone.The electrolysis unit can be directly used for processing trade effluent, and energy conservation and environmental protection, treatment effeciency is high, equipment
Operation easily manipulation, it is at low cost.
Description of the drawings
Fig. 1 is the preparation method flow diagram of the suspension proposed by the present invention containing Sn.
Specific implementation mode
Below in conjunction with drawings and examples, the specific implementation mode of the present invention is described in more details, so as to energy
The advantages of enough more fully understanding the solution of the present invention and its various aspects.However, specific embodiments described below and reality
It applies example to be for illustrative purposes only, rather than limiting the invention.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
It shows the structure and/or processing step closely related with scheme according to the present invention, and is omitted little with relationship of the present invention
Other details.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that including a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
First, an object of the present invention is to propose a kind of preparation method of novel anode material.The anode of the present invention
Material is attached to after pyrolysis, calcination process on anode plate by containing Sn suspension, is specifically included the following steps：
(1) preparation of the suspension containing Sn
As shown in Figure 1, specifically comprising the following processes：
1. preparing raw material：SnC2O4500~1500 parts by weight, Sb2O35~8 parts by weight, Ni
(CH3COO)2·4H2The parts by weight of O1~3.
Suspension containing Sn prepared by the present invention includes mainly Sn elements, Sb elements, Ni elements, also, Sn elements, Sb first
Plain, Ni elements existence form is not limited to the three kinds of compounds taken in the preparation method of the present invention.In the other of the present invention
In some embodiments, Ni (CH3COO)2·4H2O can also select other positive bivalent compounds containing Ni；Sb2O3It can also select
With other positive trivalent iron compounds containing Sb；SnC2O4Other positive bivalent compounds containing Sn can also be selected.
Also, as the preferred embodiment of the invention, SnC2O4Weigh 550~900 parts by weight, Sb2O3Weigh 5~8 weights
Measure part, Ni (CH3COO)2·4H2O weighs 1~3 parts by weight.
2. by ready SnC2O4It is added in reaction kettle, at least water of 150 parts by weight and stirring is added into reaction kettle
Uniformly.Preferably, the amount that water is added is 150~450 parts by weight.Wherein, the time of stirring is preferably controlled to 3~5min.It is more excellent
Choosing, deionized water is added into reaction kettle.
3. by ready Sb2O3It is added in above-mentioned reaction kettle, continues 3~5min of stirring, and to the object in reaction kettle
Material carries out being slowly heated to temperature being 50~60 DEG C so that SnC2O4And Sb2O3It is uniformly mixed, obtains mixture.
4. ready Ni (CH are added into above-mentioned mixture3COO)2·4H2O, and continue to stir.Then, to reaction kettle
In be passed through oxygen, and heated, stir process, be heated to material in reaction kettle makes reaction in heating is stopped after suspended state
Material natural cooling in kettle, and staticly settling, it is to be precipitated completely after, take upper layer suspension to get to suspension containing Sn.
Wherein, suspension refers to solid particle dispersions in liquid, cannot be sunk quickly because of Brownian movement, at this time solid
The mixture of dispersed phase and liquid is known as suspension.
As the preferred embodiment of the invention, the flow that oxygen is passed through into reaction kettle is 8~12L/min.Reaction kettle
In be passed through oxygen after, the temperature that is heated is 50~60 DEG C, and reactor temperature is made to maintain 50~60 DEG C, is continued
It is passed through oxygen and stirs.Preferably, heating time control is 1~2h.
The time control of precipitation process is 6~8h, the material in reaction kettle can be made to precipitate complete.
Suspension containing Sn prepared by the present invention can save 30 days in the environment of 0~8 DEG C.
(2) pyrolysis processing process
The above-mentioned suspension containing Sn being prepared is coated on anode plate, pyrolysis temperature control is 400~600 DEG C, and
Repetitive coatings-pyrolysis processing process 7~9 times so that suspension containing Sn can fully cover on anode plate, form uniform apply
Overlay film.
(3) sintering processes process
The coating film that above-mentioned steps obtain is sintered so that firm, uniform catalyst is formed on anode plate
Film layer.Wherein, the sintering temperature control of this step is 500~650 DEG C, and sintering time control is 60~120min.
As the preferred embodiment of the present invention, anode plate is prepared by corrosion-resistant, heat safe conductive material, such as titanium
Category, graphite, platinum etc..It is furthermore preferred that anode plate selects titanium to prepare, cost of manufacture is lower, and performance is more superior.
The invention also provides a kind of device of electrolytic ozone generation, i.e. electrolysis unit, which can utilize catalysis electricity
Solution (Catalysis and Electrolysis) prepares ozone.Catalytic electrolysis method refers to, by adding in electrolysis unit
Add suitable catalyst, effectively facilitates the process of cell reaction progress.
The electrolysis unit of the present invention includes anode material, cathode material, power supply, electrolyte.Power supply is DC power supply.Its
In, the anode of anode material and power supply is connected by conducting wire, and the cathode of cathode material and power supply is connected by conducting wire, anode material
It is placed in electrolyte with cathode material.It is separated with insulating materials between anode material and cathode material.Also, the electrolysis unit
In anode material be prepared by above-mentioned preparation method.
Wherein, cathode material is prepared by corrosion resistant conductive material.Preferably, cathode material selects stainless steel plate.
In the electrolysis unit, various non-strong acid can be selected in electrolyte, the water body of non-highly basic is electrolysed.It is excellent as the present invention
The ozone that oxidation reaction electrolysis generates, energy occur after the electrolysis unit is passed through direct current, on anode material for the embodiment of choosing
Electrolyte water body is enough directly acted on, using the strong oxidizing property of ozone, realizes the removing polluted in water body.
After power supply is powered, the cation in water body shifts to cathode, absorbs electronics, and reduction occurs, and generates novel substance；
Anion in water body shifts to anode, and ejected electron occurs oxidation, also generates novel substance.
Specifically, due to containing a small amount of oxygen (O in water body2), electrolysis unit Anodic material of the invention is nearby sent out
The reduction reaction of generation is mainly near raw oxidation reaction and cathode material：
Anode reaction：
3H2O-6e-=O3+6H+
Cathode reaction：
3O2+6H++6e-=3H2O2
Total cell reaction：3O2+3H2O=O3+3H2O2
In this reaction process, the oxygen needed for cathode reaction comes from the oxygen constantly dissolved in water body.Cathode reaction institute
The H needed+Come from the H of sewage and anode reaction generation+.Under the catalysis of the suspension containing Sn prepared by the present invention, in electrolytic process
It not will produce pernicious gas.Also, hydrogen peroxide (the H that cell reaction generates2O2) it is used as a kind of Green Oxidant, easily it is decomposed into water
And oxygen, to environment and human body without any injury.
The ozone that anode material electrolysis generates can not only decompose a variety of virtues such as not degradable polychlorinated biphenyls, phenol, naphthalene
Hydrocarbon and unsaturated acyclic hydrocarbon, and the decolorizing effect of hydrophilic dye is become apparent from, it can be used for handling trade effluent.
Embodiment 1
Weigh 900g SnC2O4It is put into reaction kettle, 200g deionized waters is added and stir 3min, then add into reaction kettle
Enter 5gSb2O3, continue to stir 3min, then reaction kettle carried out being heated to temperature in the kettle being 50 DEG C, add 1gNi
(CH3COO)2·4H2O continues to stir.
It is passed through oxygen according to the flow of 10L/min into aforesaid reaction vessel, it is 50 DEG C that heating, which maintains reactor temperature, is held
Continuous logical oxygen simultaneously stirs.Stop heating reaction kettle after 1.5h, makes reaction kettle natural cooling, and precipitate 6h, after taking precipitation
Upper layer suspension obtains suspension containing Sn.
Above-mentioned suspension containing Sn is coated in titanium plate, and is pyrolyzed at 500 DEG C, the coating-pyrolytic process 8 is repeated
It is secondary, then the titanium plate for being attached with coating film is sintered, 80min is sintered at 600 DEG C, is formed in obtained titanium plate uniform
Catalyst film layer.
The above-mentioned titanium plate coated with catalyst film layer is as anode, and stainless steel plate is as cathode.Titanium plate is connected by conducting wire
Titanium plate and stainless steel plate are placed in pending phenol by the anode of power supply, stainless steel by the cathode of wire connecting power
In waste water, power supply is powered, and oxidation and reduction reaction nearby occur respectively for anode and cathode, realize the purification sewage treatment of waste water.
The treatment effect of the present embodiment is shown in Table 1.
1 embodiment of table, 1 electrolysis unit handles the effect of phenolic waste water
| Project | Ozone | Phenol before processing | Phenol after processing |
| Concentration (mg/L) | 3.5 | 10 | <0.1 |
Wherein, the detection method of ozone concentration is using chemical iodimetric titration.The detection method of phenol concentration using
Bromate method.
Embodiment 2
Weigh 1200gSnC2O4It is put into reaction kettle, 400g deionized waters is added and stir 3min, then add into reaction kettle
Enter 8gSb2O3, continue to stir 3min, then reaction kettle carried out being heated to temperature in the kettle being 50 DEG C, add 2gNi
(CH3COO)2·4H2O continues to stir.
It is passed through oxygen according to the flow of 8L/min into aforesaid reaction vessel, it is 50 DEG C that heating, which maintains reactor temperature, is held
Continuous logical oxygen simultaneously stirs.Stop heating reaction kettle after 1.5h, makes reaction kettle natural cooling, and precipitate 6h, after taking precipitation
Upper layer suspension obtains suspension containing Sn.
Above-mentioned suspension containing Sn is coated in titanium plate, and is pyrolyzed at 550 DEG C, the coating-pyrolytic process 8 is repeated
It is secondary, then the titanium plate for being attached with coating film is sintered, 80min is sintered at 650 DEG C, is formed in obtained titanium plate uniform
Catalyst film layer.
The above-mentioned titanium plate coated with catalyst film layer is as anode, and stainless steel plate is as cathode.Titanium plate is connected by conducting wire
Titanium plate and stainless steel plate are placed in pending phenol by the anode of power supply, stainless steel by the cathode of wire connecting power
In waste water, power supply is powered, and oxidation and reduction reaction nearby occur respectively for anode and cathode, realize the purification sewage treatment of waste water.
The treatment effect of the present embodiment is shown in Table 2.
2 embodiment of table, 2 electrolysis unit handles the effect of phenolic waste water
| Project | Ozone | Phenol before processing | Phenol after processing |
| Concentration (mg/L) | 4 | 8 | <0.1 |
Wherein, the detection method of ozone concentration is using chemical iodimetric titration.The detection method of phenol concentration using
Bromate method.
Embodiment 3
Weigh 550g SnC2O4It is put into reaction kettle, 160g deionized waters is added and stir 3min, then add into reaction kettle
Enter 5gSb2O3, continue to stir 3min, then reaction kettle carried out being heated to temperature in the kettle being 50 DEG C, add 3gNi
(CH3COO)2·4H2O continues to stir.
It is passed through oxygen according to the flow of 12L/min into aforesaid reaction vessel, it is 50 DEG C that heating, which maintains reactor temperature, is held
Continuous logical oxygen simultaneously stirs.Stop heating reaction kettle after 1.5h, makes reaction kettle natural cooling, and precipitate 6h, after taking precipitation
Upper layer suspension obtains suspension containing Sn.
Above-mentioned suspension containing Sn is coated in titanium plate, and is pyrolyzed at 500 DEG C, the coating-pyrolytic process 8 is repeated
It is secondary, then the titanium plate for being attached with coating film is sintered, 80min is sintered at 650 DEG C, is formed in obtained titanium plate uniform
Catalyst film layer.
The above-mentioned titanium plate coated with catalyst film layer is as anode, and stainless steel plate is as cathode.Titanium plate is connected by conducting wire
Titanium plate and stainless steel plate are placed in pending phenol by the anode of power supply, stainless steel by the cathode of wire connecting power
In waste water, power supply is powered, and oxidation and reduction reaction nearby occur respectively for anode and cathode, realize the purification sewage treatment of waste water.
The treatment effect of the present embodiment is shown in Table 3.
3 embodiment of table, 3 electrolysis unit handles the effect of phenolic waste water
| Project | Ozone | Phenol before processing | Phenol after processing |
| Concentration (mg/L) | 4.5 | 10 | 0 |
Wherein, the detection method of ozone concentration is using chemical iodimetric titration.The detection method of phenol concentration using
Bromate method.
Embodiment 4
Weigh 1500g SnC2O4It is put into reaction kettle, 450g deionized waters is added and stir 5min, then add into reaction kettle
Enter 5gSb2O3, continue to stir 3min, then reaction kettle carried out being heated to temperature in the kettle being 60 DEG C, add 1gNi
(CH3COO)2·4H2O continues to stir.
It is passed through oxygen according to the flow of 9L/min into aforesaid reaction vessel, it is 60 DEG C that heating, which maintains reactor temperature, is held
Continuous logical oxygen simultaneously stirs.Stop heating reaction kettle after 1h, make reaction kettle natural cooling, and precipitate 7h, takes upper after precipitation
Layer suspension, obtains suspension containing Sn.
Above-mentioned suspension containing Sn is coated on platinized platinum, and is pyrolyzed at 400 DEG C, the coating-pyrolytic process 9 is repeated
It is secondary, then the platinized platinum for being attached with coating film is sintered, 90min is sintered at 500 DEG C, forms uniform catalyst film layer.
The above-mentioned platinized platinum coated with catalyst film layer is as anode, and stainless steel plate is as cathode.Platinized platinum is connected by conducting wire
Platinized platinum and stainless steel plate are placed in by the cathode of wire connecting power and pending contain naphthalene by the anode of power supply, stainless steel
In waste water, power supply is powered, and oxidation and reduction reaction nearby occur respectively for anode and cathode, realize the purification sewage treatment of waste water.
The treatment effect of the present embodiment is shown in Table 4.
4 embodiment of table, 4 electrolysis unit handles the effect of the waste water containing naphthalene
| Project | Ozone | Naphthalene before processing | Naphthalene after processing |
| Concentration (mg/L) | 3.2 | 9.8 | <0.2 |
Wherein, the detection method of ozone concentration is using chemical iodimetric titration.The detection method of naphthalene concentration is using gas
Phase chromatography.
Embodiment 5
Weigh 500g SnC2O4It is put into reaction kettle, 150g deionized waters is added and stir 4min, then add into reaction kettle
Enter 6gSb2O3, continue to stir 3min, then reaction kettle carried out being heated to temperature in the kettle being 55 DEG C, add 1gNi
(CH3COO)2·4H2O continues to stir.
It is passed through oxygen according to the flow of 10L/min into aforesaid reaction vessel, it is 55 DEG C that heating, which maintains reactor temperature, is held
Continuous logical oxygen simultaneously stirs.Stop heating reaction kettle after 2h, make reaction kettle natural cooling, and precipitate 6h, takes upper after precipitation
Layer suspension, obtains suspension containing Sn.
Above-mentioned suspension containing Sn is coated in titanium plate, and is pyrolyzed at 450 DEG C, the coating-pyrolytic process 7 is repeated
It is secondary, then the titanium plate for being attached with coating film is sintered, 60min is sintered at 650 DEG C, is formed in obtained titanium plate uniform
Catalyst film layer.
The above-mentioned titanium plate coated with catalyst film layer is as anode, and stainless steel plate is as cathode.Titanium plate is connected by conducting wire
Titanium plate and stainless steel plate are placed in by the cathode of wire connecting power and pending contain naphthalene by the anode of power supply, stainless steel
In waste water, power supply is powered, and oxidation and reduction reaction nearby occur respectively for anode and cathode, realize the purification sewage treatment of waste water.
The treatment effect of the present embodiment is shown in Table 5.
5 embodiment of table, 5 electrolysis unit handles the effect of the waste water containing naphthalene
| Project | Ozone | Naphthalene before processing | Naphthalene after processing |
| Concentration (mg/L) | 4.2 | 9 | <0.1 |
Wherein, the detection method of ozone concentration is using chemical iodimetric titration.The detection method of naphthalene concentration is using gas
Phase chromatography.
Reference examples
Only using titanium plate as anode, stainless steel plate is as cathode.For titanium plate by the anode of wire connecting power, stainless steel is logical
The cathode of wire connecting power is crossed, and titanium plate and stainless steel plate are placed in pending waste water containing naphthalene or phenolic waste water, electricity
Source is powered, and electrolytic condition carries out the electrolysis processing of sewage with embodiment 1.
After testing, under the experimental condition, and it is not detected as ozone generation.The processing of waste water containing naphthalene and phenolic waste water is imitated
Fruit is as shown in table 6：
6 reference examples electrolysis unit of table handles the effect of waste water containing naphthalene or phenolic waste water
| Project | Naphthalene before processing | Naphthalene after processing | Phenol before processing | Phenol after processing |
| Concentration (mg/L) | 8.9 | 8.2 | 9.3 | 8.7 |
To sum up, the suspension containing Sn that prepared by the present invention can be good at promoting the generation of ozone in electrolytic process, for dirt
The purified treatment of water has the effect of very considerable, is advantageously implemented industrial applications.
Finally it should be noted that：Obviously, the above embodiment is merely an example for clearly illustrating the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the art, it can also do on the basis of the above description
Go out other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
The obvious changes or variations that Shen goes out are still in the protection scope of this invention.
Claims (10)
1. a kind of preparation method of novel anode material, which is characterized in that the anode material by contain Sn suspension through pyrolysis,
Calcination process is attached on anode plate, is included the following steps：
A, the preparation of the suspension containing Sn：Prepare raw material：SnC2O4500~1500 parts by weight, Sb2O35~8 parts by weight, Ni
(CH3COO)2·4H2The parts by weight of O1~3；By SnC2O4It is added in reaction kettle, at least 150 weight is added into the reaction kettle
The water of part simultaneously stirs evenly；By Sb2O3Be added in the reaction kettle, stir and heat so that be uniformly mixed, mixed
Material；By Ni (CH3COO)2·4H2O is added in the mixture, and oxygen is then passed through into the reaction kettle, and heated,
Stirring, until for material in heating is stopped after suspended state, the material precipitation in the reaction kettle is to be precipitated complete in the reaction kettle
Quan Hou takes upper layer suspension to get to the suspension containing Sn；
B, pyrolysis processing：The suspension containing Sn is coated on the anode plate, is pyrolyzed at a temperature of 400~600 DEG C,
And coating-pyrolysis processing the process 7~9 times is repeated, form coating film；
C, sintering processes：The coating film is sintered, the temperature control of the sintering processes process is 500~650
DEG C, the sintering time control is 60~120min.
2. the preparation method of anode material according to claim 1, which is characterized in that the anode plate is by corrosion-resistant, resistance to
The made of metal of high temperature is standby；Preferably, the anode plate is prepared by titanium.
3. the preparation method of anode material according to claim 1, which is characterized in that the SnC2O4Take 550~900 weights
Measure part, the Sb2O3Take 5~8 parts by weight, the Ni (CH3COO)2·4H2O takes 1~3 parts by weight.
4. the preparation method of anode material according to claim 1, which is characterized in that into the reaction kettle be added go from
Sub- water.
5. the preparation method of anode material according to claim 1, which is characterized in that the flow for being passed through oxygen is 8
~12L/min.
6. the preparation method of anode material according to claim 1, which is characterized in that control the temperature of the heating process
It it is 50~60 DEG C, the time of the heating is 1~2h.
7. a kind of novel anode material, which is characterized in that the anode material is by any preparations of claim 1-6
What method was prepared.
8. a kind of device of electrolytic ozone generation, including anode material, cathode material, power supply, electrolyte, the anode material with
The anode of the power supply is connected by conducting wire, and the cathode material is connect with the cathode of the power supply by conducting wire, the anode
Material and the cathode material are placed in the electrolyte, which is characterized in that the anode material is described in claim 7
Novel anode material.
9. the device of electrolytic ozone generation according to claim 8, which is characterized in that the cathode material selects stainless steel
Plate.
10. the device of electrolytic ozone generation according to claim 8, which is characterized in that the power supply is DC power supply.
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| PCT/CN2019/073092 WO2019149142A1 (en) | 2018-02-02 | 2019-01-25 | Novel anode material and preparation method therefor, and device for generating ozone by electrolysis |
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| WO2019149142A1 (en) * | 2018-02-02 | 2019-08-08 | 苏州庚泽新材料科技有限公司 | Novel anode material and preparation method therefor, and device for generating ozone by electrolysis |
| WO2019218935A1 (en) * | 2018-05-18 | 2019-11-21 | 苏州庚泽新材料科技有限公司 | Ozone generating electrode, method for preparing same, and electrolysis device having same |
| WO2019233247A1 (en) * | 2018-06-05 | 2019-12-12 | 苏州庚泽新材料科技有限公司 | Active material containing sn-sb-transition metal element, preparation method thereof, and ozone-generating electrode containing the active material |
| CN111389408A (en) * | 2020-04-17 | 2020-07-10 | 苏州庚泽新材料科技有限公司 | Catalyst, preparation method and application thereof |
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| CN111533368A (en) * | 2020-04-17 | 2020-08-14 | 苏州庚泽新材料科技有限公司 | Method for treating sewage |
| CN111547820A (en) * | 2020-04-17 | 2020-08-18 | 昆山恒久润机电安装工程有限公司 | Anode plate, preparation method thereof and composite oxidant generating unit |
| WO2021022762A1 (en) * | 2019-08-07 | 2021-02-11 | 深圳市耐菲尔医疗器械科技有限公司 | Anode, preparation method therefor and use thereof, ozone (superoxygen) generating system, and tooth rinser |
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