CN110451609A - A kind of sanitary wastewater/tap water Electro Sorb oxidation depth purification device - Google Patents
A kind of sanitary wastewater/tap water Electro Sorb oxidation depth purification device Download PDFInfo
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- CN110451609A CN110451609A CN201910636344.4A CN201910636344A CN110451609A CN 110451609 A CN110451609 A CN 110451609A CN 201910636344 A CN201910636344 A CN 201910636344A CN 110451609 A CN110451609 A CN 110451609A
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Classifications
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- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2001/46133—Electrodes characterised by the material
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- 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
- C02F2201/002—Construction details of the apparatus
- C02F2201/007—Modular design
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Abstract
The present invention provides a kind of sanitary wastewater/tap water Electro Sorb oxidation depth purification device, including three-level purification system (50)；It is connected to the three-level water purification collection system (51) and tail washings recovery system (52) of three-level purification system (50).The three-level purification system (50) includes three-level purification system shell, sanitary wastewater or tap water water inlet (1), coagulation unit, two stage treatment unit and three stage treatment unit, liquid separator (24), and the sanitary wastewater or tap water water inlet (1), coagulation unit, two stage treatment unit and three stage treatment unit, liquid separator (24) are from top to bottom arranged in three-level purification system shell；The three-level water purification collection system (51) includes 3 fluid reservoirs being set side by side, respectively flushing water fluid reservoir (32), clean water fluid reservoir (33), direct drinking fluid reservoir (34)；Tail washings recovery system (52) includes waste liquid fluid reservoir (35) and tail washings leakage fluid dram (25).System of the invention can be used using simple, multi-stage treatment units because of the comprehensive collocation of change of water quality, can disinfection by-products in deep purifying sanitary wastewater/tap water, the secondary use of sanitary wastewater can be achieved.
Description
Technical field
The invention belongs to purification of waste water fields, in particular to sanitary sewage and deep purification for tap water device.
Background technique
Sewage treatment is the water quality requirement for draining a certain water body to reach sewage or reusing, and is purified to it
Process.Sewage treatment is widely used in building, agricultural, traffic, the energy, petrochemical industry, environmental protection, urban landscape, medical treatment, food and drink etc.
Every field also comes into the daily life of common people more and more.For sanitary sewage, be mainly derived from kitchen cooking,
Shower, washing, lavatory flushing water etc., it is predominantly various essentially free of heavy metal and poisonous and harmful substance in sanitary sewage
The inorganic matter of form and the complex mixture of organic matter, including size solid particle, glue and solidifying the shape diffusion for floating and suspending
Object and pure solution.For tap water, sterilize most of using traditional cholorination.But chlorination method easily has with what is coexisted in water
The reactions such as machine object such as natural organic matter (NOMs) generate halogenated alkane, the disinfection by-products such as halogenated aryl hydrocarbon, such substance toxicity compared with
Greatly and there are carcinogenic, teratogenesis, mutagenesis risk, generate larger threat to human health.Tap water purifying is mainly used
The means such as filtering and porous material absorption remove the impurity such as silt, bacterium, heavy metal, chlorine residue, organic matter in water.Filtering is main
Using materials such as PP cotton, PP felt, carbon cloth, ceramic element and various hollow fiber ultrafiltration films；Absorption mainly using active carbon,
The porous materials such as ceramic particle.Electrochemical oxidation technology is as a kind of high-level oxidation technology, due to producing in electrochemical reaction process
Raw active intermediate matter (HClO, OH, Cl2、H2O2、O3) have the function of sterilization, and have and added without Xiang Shuizhong
Medicament, purification of water quality efficiency is higher, it is without secondary pollution, using the advantages that more convenient, easily controllable, in drinking water disinfection side
Face, especially some small-sized water supply projects or the occasion for being unfavorable for storing disinfectant show huge development potentiality.Currently, electric
Chemical oxidation techniques have obtained remarkable result in disinfection and sterilization field, but electrochemical disinfection technology is while killing microorganism,
Also some problems are showed.Wherein most distinct issues are to commonly use chloride (such as NaCl) conduct during electrochemical disinfection
Electrolyte can generate the high-valence states chlorine class inorganic byproduct such as chlorate, perchlorate in electrochemical process, or even will form pair
The harmful disinfection by-products of human body (DBPs).Sewage treatment divide according to degree for the treatment of can be divided into coagulation, two stage treatment and
Tertiary treatment.Coagulation is mainly the solid matter removed in sewage in suspended state, commonly uses physical method.After coagulation
Waste water BOD removal rate only has 20%, should not still discharge, and must also carry out two stage treatment.The main task of two stage treatment is significantly
The organic matter in sewage in colloid and dissolved state is removed, BOD removal rate is 80%~90%.Dirt generally Jing Guo two stage treatment
Water can reach discharge standard, commonly use activated sludge process and biological membrane processing method.The purpose of tertiary treatment is further to remove
Certain special polluter, such as fluorine removal, dephosphorization, belong to advanced treating, commonly use chemical method.Such as patent application
201811409432.2 disclose a kind of countryside sewage treatment equipment, by be provided with first order treatment box, second level treatment box,
Third level treatment box and plumbing for waste water can carry out multistep treatment, the grit placing box being arranged in plumbing for waste water to drinking water in rural China
With peat placing box, removal of impurities and taste removal processing can be carried out to drinking water in rural China, the first order treatment box of setting can be to agriculture
Village's domestic water carries out the heavy metal ion in flocculation material and colloid and water body in removing water body, the second level processing of setting
Case can live to the aerobic organic matter in the water body of drinking water in rural China and handle, and the third level treatment box of setting can be with
The substance for making water eutrophication in the water body of drinking water in rural China is absorbed, it can be with by the water body of multistep treatment
Discharged after reaching discharge standard, can with effective solution drinking water in rural China cannot be handled and random exhaust emission environment
The problem of.For the patent application, although being provided with tertiary treatment, it is only that continuous processing is carried out to sewage, reaches row
The standard put can not achieve the mode according to the purposes selection processing water of water after processing, in addition, even if carrying out tertiary treatment,
The standard of drinking water can not be reached.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of dresses that deep purifying can be realized to sanitary sewage/tap water
The secondary use, it can be achieved that sanitary wastewater is set, it can disinfection by-products in deep purifying tap water.
Based on the above technical problem,
Specifically, the technical scheme adopted by the invention is as follows:
A kind of sanitary wastewater/tap water Electro Sorb oxidation depth purification device, which is characterized in that including
Three-level purification system (50)；The three-level water purification collection system (51) and tail washings for being connected to three-level purification system (50) are returned
Receipts system (52) ().
Further,
The three-level purification system (50) includes three-level purification system shell, sanitary wastewater or tap water water inlet (1), one
Grade processing unit, two stage treatment unit and three stage treatment unit, liquid separator (24), the sanitary wastewater or tap water enter water
Mouth (1), coagulation unit, two stage treatment unit and three stage treatment unit, liquid separator (24) are from top to bottom arranged in three
In grade purification system shell；
The water only obtained by coagulation unit is level-one water, is collected in flushing water fluid reservoir (32), for gardens,
The flushing of flowers and plants lavatory etc.；Second level water is obtained by firsts and seconds processing unit, is collected in clean water fluid reservoir (33), water quality
Reach tap water requirement；Tertiary effluent is obtained by level-one, second level and three stage treatment unit, is collected in direct drinking fluid reservoir (34),
It can be used for direct drinking.
The coagulation unit includes rotor filter (3), coarse rack layer (4), magnetic nanometer adsorbent layer (5), thin
Grid layer (6), the rotor filter (3) are set to the lower section of sanitary wastewater or tap water water inlet (1), the coarse rack layer
(4), magnetic nanometer adsorbent layer (5), fine fack layer (6) are from top to bottom set in three-level purification system shell, meanwhile, it is described
Coarse rack layer (4), magnetic nanometer adsorbent layer (5), fine fack layer (6) are connected to the inner wall of three-level purification system shell respectively；
Before carrying out advanced treating, preliminary impurity elimination work is carried out to sanitary sewage by rotor filter, to visible solid
Grain object is removed.
The two stage treatment unit includes cathode one (8), nanoparticle microelectrode (11), metal mesh anode (12), cathode
Two (13)；
The cathode one (8), nanoparticle microelectrode (11), metal mesh anode (12), cathode two (13) are from top to bottom set
Be placed in three-level purification system shell, meanwhile, the cathode one (8), nanoparticle microelectrode (11), metal mesh anode (12),
Cathode two (13) is connected to the inner wall of three-level purification system (50) shell；The nanoparticle microelectrode (11) is uniformly distributed
Between cathode one (8), metal mesh anode (12), cathode two (13)；
The three stage treatment unit includes transition metal modification TiO2- MOFs film composite electrode (18).
Coagulation unit, two stage treatment unit and three stage treatment unit can be independently series-parallel using also can according to need
It uses.
Further,
At least one of the cathode one (8) and cathode two (13) are ferrite modification carbon fiber cloth electrode；
Cathode one (8), metal mesh anode (12), cathode two (13), TiO2Modification MOFs nanofiltration membrane electrode (18) connects respectively
It is connected to power supply (23), cathode one (8), metal mesh anode (12), cathode two (13), TiO2Modify MOFs nanofiltration membrane electrode (18) with
Multidirectional control switch (19), multidirectional control switch (20) multidirectional control switch (21) multidirectional control are respectively arranged between power supply (23)
System switch (22)；The multidirectional control switch (22) can be by motor switch Switching power positive and negative anodes, to nanoparticle microelectrode
(11), cathode one (8), cathode two (13) and transition metal modification TiO2-MOFs film composite electrode (18) carry out on-line cleaning, electricity
Source can be battery powered.
Further, the voltage range of the power supply (23) is 1-10V；
Further, the metal mesh anode (12) is platinum gauze electrode or stainless (steel) wire electrode.
Further, the mesh number of the metal mesh anode (12) is -120 mesh of 35 mesh.
Further,
The sanitary wastewater or tap water water inlet (1) are the controllable valve of bottle neck；Can be directly connected to running water tap or
Funnel is connected after disassembly and accesses sanitary wastewater, water body can be pressurized by compress cell.
Further, between the fine fack layer (6) and cathode one (8), multi-functional on-line monitoring device (7), institute are provided with
Multi-functional on-line monitoring device (7) is stated to be external on three-level purification system shell；
Further, it between the fine fack layer (6) and cathode one (8), is provided with exhaust valve (9), the exhaust valve (9)
It is arranged on three-level purification system (50) shell；
Further, the external device for absorbing tail gas of the exhaust valve (9) (10)；
Further, the transition metal modifies TiO2Below-MOFs film composite electrode (18), it is provided with miniature gas tank
(14), the miniature gas tank (14) is external on three-level purification system shell；The miniature gas tank (14) and three-level purification system
Shell is connected by pipeline, is additionally provided with gas flowmeter (15) and electricity between miniature gas tank (14) and three-level purification system shell
Magnet valve one (16)；
Further, the miniature gas tank (14) is miniature oxygen tank or ozone generator；
When carrying out Electro Sorb oxidation depth purified treatment, miniature gas tank (14) provides oxygen or ozone and carries out deeply to water body
Degree processing；The oxygen source occurred using air or high purity oxygen gas as ozone；Ozone or the oxygen gas-liquid after micro- aerator are filled
Divide after mixing and reaches ferrite modifying carbon fibers cloth electrochemical cathode with nano grade air bubbles.
When it is oxygen that miniature gas tank (14), which provide, when supply voltage 1-5V, two stage treatment unit forms several micro- electricity
Pole constitutes three dimensional particles electrode system, efficiently in situ to generate hydrogen peroxide；Transition metal contained by nanoparticle microelectrode (11) simultaneously
Ion can produce hydroxyl radical free radical, former to the contaminant trace species and disinfection by-products progress deep oxidation in waste water/tap water
It manages as follows:
O2+2H++2e-→H2O2,
Mn+H2O2→Mn+1+OH-+·OH
When it is ozone that miniature gas tank (14), which provide, when supply voltage 4-10V, nanoparticle is micro- in two stage treatment unit
Electrode (11) serves as catalyst, and catalysis ozone occurs chain reaction and generates hydroxyl radical free radical, dirty to the trace in waste water/tap water
It contaminates object and disinfection by-products carries out deep oxidation, principle is as follows:
O3+OH-→HO2 -+O2,
O2+2H++2e-→H2O2,
H2O2+2O3→·OH+3O2,
The inner bottom of three-level purification system shell is arranged in the liquid separator (24).Liquid separator is arranged
For, positioned at the bottom of purification system, it is only necessary to which when coagulation, the power switch of two tertiary treatment is closed, and needs one or two
When grade processing, the power switch of tertiary treatment is closed；When only needing tertiary treatment, the power switch of a two stage treatment is closed.
Further,
The three-level water purification collection system (51) includes 3 fluid reservoirs being set side by side, respectively flushing water liquid storage
Tank (32), clean water fluid reservoir (33), direct drinking fluid reservoir (34)；
Further, with solenoid valve, fluid flow between the three-level purification system (50) and water purification collection system (51)
Meter is connected with pipeline；
Further, the solenoid valve is set as 3, respectively solenoid valve one (26), solenoid valve two (27), solenoid valve three
(28)；
Further, the fluid flowmeter is set as 3, respectively fluid flowmeter one (29), fluid flowmeter two
(30), fluid flowmeter three (31)；
Further,
Tail washings recovery system (52) includes waste liquid fluid reservoir (35)；The three-level purification system (50) and tail washings leakage fluid dram
(25)；The tail washings leakage fluid dram (25) is set to the lower end of three-level purification system (50) shell, and the waste liquid fluid reservoir (35) is logical
Piping is connected on three-level purification system (50) shell.
The waste liquid that the tail washings recovery system (52) generates sanitary wastewater/tap water Electro Sorb oxidation depth purification device
It is recycled with cleaning solution, waste liquid rate is 5%-10%.
Magnetic nanometer adsorbent in magnetic nanometer adsorbent layer (5) can take out, with soaked in absolute ethyl alcohol 30-45min,
Drying continues to use；
Nanoparticle microelectrode (11) can carry out immersion 30-60min with dehydrated alcohol, carry out magnetic recovery with magnet, do
It is dry to continue to use；Other electrodes can be injected into anti-when 1-5mmol/L NaCl solution progress on-line cleaning, cleaning
Solution is answered, is opened respectively by multidirectional control switch (19), multidirectional control switch (20), multidirectional control switch (21), multidirectional control
After closing (22) progress anode and cathode exchange, electrolysis a period of time is carried out.
Further,
Magnetic nanometer adsorbent layer (5) and nanoparticle microelectrode (11) are magnetic carbon material in situ growth MOFs (gold
Belong to organic framework compounds (English name Metal organic Framework))；
Further,
The size of magnetic nanometer adsorbent layer (5) magnetic Nano material is 20-50nm；Specific surface area is 50-
300m2/g；Pore volume is 0.4-1.2cm3/g；Saturation magnetization is 15-35emu/g；It is adsorbable remove odors, chlorine residue, weight
Metal and the common organic matter of the overwhelming majority.
Further,
Nanoparticle microelectrode (11) the nanoparticle microelectrode size is 30-100nm, and specific surface area is 50-
200m2/g；Pore volume is 1.3-1.4cm3/g；Saturation magnetization is 5-15emu/g；
Further, the preparation method of the magnetic carbon material in situ growth MOFs includes the following steps:
1) preparation of magnetic carbon material:
1.1) magnetic Nano material is prepared into magnetic Nano material aqueous solution, magnetic Nano material is added in char-forming material
Ultrasound mixes in aqueous solution, obtains mixed solution one；
1.2) mixed solution that step 1.1) is prepared is in constant temperature blender with magnetic force in 40 DEG C -60 DEG C, revolving speed
Reaction obtains mixed solution two not less than for 24 hours under the conditions of 3rpm；
1.3) it is filtered, and washed by qualitative filter paper after being cooled to room temperature the mixed solution two obtained after step 1.2)
Wash filter cake until last time filtered fluid be in neutrality, obtain neutral sorbent；
1.4) neutral sorbent that step 1.3) is prepared is placed in 40 DEG C of -60 DEG C of Constant Temp. Ovens and dries not
Lower than 12h, it is then ground to powdery, obtains powdered absorbent；
1.5) powdered absorbent for obtaining step 1.4) is put into and is placed on N without spreading in lid silica crucible2As
In the electron tubes type electric furnaces for protecting gas air-flow, 600 DEG C and constant temperature 2h are warming up to 4-6 DEG C/min of heating rate, is ground after cooling,
Obtain magnetic carbon material；
Further, the step 1.1) magnetic Nano material is Zero-valent Iron, γ-Fe2O3Or the point that hydrothermal synthesis method is formed
Spar it is ferritic any one or a few；
Further, the step 1.1) char-forming material is that multi-walled carbon nanotube, graphene and biological carbon are a kind of or more
The combination of kind；
2) transition metal salt and organic ligand is taken to form growth in situ MOFs, growth in situ MOFs is adsorbed on the magnetic of step 1)
Property carbon material on obtain magnetic carbon material in situ growth MOFs；
3) the magnetic carbon nanometer in situ growth MOFs sieving obtained step 2), screens out the material having a size of 20-50nm,
As magnetic nanometer adsorbent layer；
The magnetic carbon nanometer in situ growth MOFs sieving that step 2) is obtained, screens out the material having a size of 20-50nm, i.e.,
For nanoparticle microelectrode；
Further,
Step 2): the magnetic carbon material that step 1) is prepared is uniform with ultrasonic disperse in ultrapure water, and transition is added
Metal salt simultaneously makes it completely dissolved, then organic ligand is added thereto, is transferred in autoclave and reacts after sealing stirring, instead
The solidliquid mixture in autoclave is taken out after answering, it is carried out at ultrapure water cleaning, sealing stirring and centrifugation
Reason obtains magnetic carbon material in situ growth MOFs to the solid washes of absolute alcohol after centrifugation after dry；
Further, the transition metal salt is Fe (NO3)3·9H2O、Al(NO3)3·9H2O、Cu(NO3)2·3H2O or
Co(NO3)2·6H2O any one or a few；
Further, the organic ligand is any one of trimesic acid and terephthalic acid (TPA).
Further, the transition metal modifies TiO2- MOFs film composite electrode (18) the preparation method comprises the following steps:
A) organic ligand solution the preparation of MOFs film: is passed through into electrochemical in-situ deposition method shape under three-electrode system
At MOFs film；
b)TiO2The preparation of-MOFs film: after the MOFs film that step 1) obtains is added in alcohol solvent, wait infiltrate sufficiently
Afterwards, butyl titanate (Ti (OBu) is slowly added dropwise4), ultrasound is then transferred in polytetrafluoroethylliner liner, is placed in stainless steel
Reaction kettle reacts, cooling, and washing is dried to obtain TiO2- MOFs film；
C) transition metal modifies TiO2The preparation of-MOFs film composite electrode: it is added what step b) was obtained in ultrapure water
TiO2After-MOFs film, after infiltrating sufficiently, it is added and contains Fe3+Solid chemical compound and MCl2Solid (M=V, Cr, Mn, Co, Ni,
Cu and Zn), ultrasound is then transferred in polytetrafluoroethylliner liner, is placed in stainless steel cauldron, reacts, and it is cooling, it washs, does
It is dry to obtain transition metal-modified TiO2-MOFs film composite electrode (18).
The transition metal modifies TiO2In-MOFs film composite electrode (18), TiO2, oxide, MOFs film (contain copper mesh) matter
Measure ratio are as follows: (4~15): (5~10): (75~91)." oxide " in aforementioned proportion is free of TiO2。
In aforementioned proportion, TiO2For TiO in step b)2TiO in-MOFs film2；
Oxide is step c) introducing, and oxide includes ferroso-ferric oxide, spinel oxide etc., is obtained by co-precipitation.
MOFs film (contain copper mesh) is the MOFs film being deposited on copper mesh that step 1) obtains, and when weight calculation amount calculates its copper mesh
Quality；
Further, the ferrite modification carbon fiber cloth electrode the preparation method comprises the following steps:
1) preparation of modified carbon fiber cloth: carrying out surface to carbon cloth with strong oxidizing solution or alkaline solution and be modified,
Drying is obtained by drying；
2) preparation of ferrite modification carbon cloth: step 1) is added when hydrothermal co-precipitation method prepares ferrite and obtains
Modified carbon fiber cloth, obtain ferrite modification carbon fiber cloth electrode.
Further,
Strong oxidizing solution described in step 1) are as follows: concentrated nitric acid, the concentrated sulfuric acid, chlorine, bromine, iodine oxyacid, Fenton reagent, mistake
Sulfate liquor, the one or more of potassium ferrate solution；
Alkaline solution described in step 1) is strong alkali solution,
Further, the strong alkali solution is KOH and/or NaOH；
Further, the preparation of step 1) modified carbon fiber cloth: carbon cloth is fully immersed in molten equipped with strong oxidizing property
In liquid, ultrasound is subsequently placed in isothermal reaction kettle and reacts, after surface residual debris impurity is washed with water, until pH, to neutrality, rear vacuum is dried
Case modified carbon fiber cloth obtained by drying；
Further；The mass volume ratio of the carbon cloth and strong oxidizing solution or alkaline solution is 1.0g:(100
~300mL)；
Further, in step 1), isothermal reaction kettle reaction temperature is 35-80 DEG C；
Further, in step 1), isothermal reaction kettle reaction temperature is 40-60 DEG C；
Further, in step 1), isothermal reaction kettle reaction temperature is 50 DEG C；
Further, in step 1), the reaction time is 12h~72h in isothermal reaction kettle；
Further, in step 1), the reaction time is for 24 hours~60h in isothermal reaction kettle；
Further, in step 1), the reaction time is 48h in isothermal reaction kettle；
Further, in step 1), with milli-Q water surface residual debris impurity；
Further, in step 1), vacuum drying oven temperature is 30-75 DEG C；
Further, in step 1), vacuum drying oven temperature is 35-50 DEG C；
Further, in step 1), vacuum drying oven temperature is 40 DEG C.
Further,
Chlorine in the step 1), bromine, iodine the concentration of oxyacid be 0.1-0.5mol/L,
Fenton reagent is 0.2-0.6mol/L Fe in the step 1)2+With the H of 30wt%2O2,
Persulfate solution concentration is 0.1-0.5mol/L in the step 1),
Potassium ferrate solution concentration is 0.1-0.5mol/L in the step 1),
Strong alkali solution is the KOH solution and/or 1-3mol/L NaOH solution of 1-3mol/L in the step 1).
Further, the step 2) are as follows:
2) preparation of ferrite modification carbon cloth: step 1) is added when hydrothermal co-precipitation method prepares ferrite and obtains
Modified carbon fiber cloth, ultrasonic mixing, constant temperature blender with magnetic force effect under react a period of time, will load later ferritic
Carbon cloth drying is put into the tube furnace under inert gas atmosphere protection, roasting a period of time, and taking-up is cooling to obtain iron oxygen
Body modification carbon fiber cloth electrode；
The ferrite of the step 2) is the single ferrite and/or spinel type ferrite of transition metal；
Further,
The step 2) are as follows:
2) it the preparation of ferrite modification carbon cloth: is added into ultrapure water and contains Fe3+Salt and M2+Salt, then
With magnetic stirrer so that it is uniformly mixed and is completely dissolved to obtain mixed solution, and polyethylene glycol is added thereto, or
Person's ammonium fluoride and urea composition continue to stir to obtain the final product, are placed on reaction in isothermal reaction kettle later, cool down, wash after completion of the reaction
Wash, be placed in thermostatic drying chamber and dry, be subsequently placed in electric tube furnace, be passed through inert gas as protection gas, roasting to get
Ferrite modification carbon cloth；In the above preparation method, the modified carbon fiber cloth is added in co-precipitation before being formed；
The one or more of described M=Fe, Mn, Ni, Cu, Co；
Further, the Fe3+Salt and M2+The molar concentration rate of salt is 1-4；Further, the Fe3+Salt and
M2+The molar concentration rate of salt is 2；
Further, the degree of isothermal reaction kettle temperature described in step 2) is 20-140 DEG C；Further, perseverance described in step 2)
Warm temperature of reaction kettle is 40-130 DEG C；
Further, the reaction time is 2-100h in isothermal reaction kettle described in step 2)；Further, institute in step 2)
Stating the reaction time in isothermal reaction kettle is 12-72h；
Further, maturing temperature described in step 2) is 300-400 DEG C；Further, temperature is roasted described in step 2)
Degree is 350 DEG C；
Further, in step 2), the heating rate of electric tube furnace is 2-10 DEG C/min；Further, in step 2), pipe
The heating rate of formula electric furnace is 5 DEG C/min；
Further, calcining time described in step 2) is 0.5-3 hours；Further, when being roasted described in step 2)
Between be 1 hour.
Further, the mass ratio of the ferrite in the step 2) and modified carbon fiber cloth material is 1:2~1:8.
The working principle of the invention is: passing through detection treatment sewage or tap water situation, such as TDS, BOD first
The purposes etc. of water, selects suitable processing unit to be handled after value, UV254 and processing.
Sanitary sewage to be processed or tap water are had by oneself pressure by compress cell or tap water first and enters water
Mouth (1), after rotor filter (3) remove visible particle object, using coarse rack layer (4), magnetic nanometer adsorbent layer
(5), fine fack layer (6) can obtain the flushing water for gardens, flowers and plants lavatory etc., then be stored with flushing water fluid reservoir (32).
After coagulation cell processing, it can be passed through oxygen, power supply (23) switch is opened simultaneously, 1-5V voltage is provided, is mentioned
For hydrogen peroxide and the hydroxyl radical free radical in situ of generating to flushing water progress secondary treatment, tap water requirement can reach；If being passed through ozone,
Power switch is opened simultaneously, 4-10V voltage is provided, ozone is provided and catalysis ozone generates hydroxyl radical free radical to through coagulation list
The flushing water that member processing obtains carries out secondary treatment, can reach tap water requirement, is then stored with clean water fluid reservoir (33).
After coagulation cell processing and two stage treatment unit, three stage treatment unit is entered, power supply is opened, most passes through afterwards
Cross transition metal modification TiO2Direct drinking can be obtained in-MOFs film composite electrode, is then stored with direct drinking fluid reservoir (34).
After purification device of the invention reaches service life, internal structure can be replaced, such as: coagulation unit
Rotor filter (3), coarse rack layer (4), magnetic nanometer adsorbent layer (5), fine fack layer (6), the yin of two stage treatment unit
Pole one (8), nanoparticle microelectrode (11), metal mesh anode (12), cathode two (13)；The transition metal of three stage treatment unit is repaired
Adorn TiO2- MOFs film composite electrode (18) etc..It can achieve the purpose utilized again.
Compared with prior art, the present invention having the following beneficial effects:
1) the device of the invention uses simple, gas effciency high (gas effciency is up to 90% or more), sewage treatment
It is high-efficient (tertiary treatment of basic waste water to be completed in 1 hour, if only needing level-one two stage treatment, or only need level-one three-level
When processing, need the time shorter, or even can be completed less than ten minutes), it can be according to water after sewage raw water type and processing
Purposes selects different purification devices, realizes in same reaction system to the advanced treating of heterogeneity sewage, significantly improves
Purifying water effect simultaneously reduces energy consumption, optimizes reaction unit structure, reduces the occupied area of reaction unit.
2) the device of the invention passes through the different advanced oxidation system reality of selection using the difference of the physico property of sewage
Existing single technique or the unapproachable water quality requirement of general technology, can also reduce cost of water treatment, have a vast market foreground.
3) the tail washings recovery system in the device of the invention is to sanitary wastewater/tap water Electro Sorb oxidation depth purification device
The waste liquid and cleaning solution of generation are recycled, and waste liquid rate is 5%-10%.
4) through the processed sewage of the device of the invention or tap water, can achieve following index: TDS, which can achieve, to be less than
10mg/L is even up to no better than 0 effect, and TDS removal rate is up to 98% or more or even 100%；UV254 (abs) can be with
It is less than 0.005, is even up to no better than 0 effect, UV254 (abs) removal rate is up to 98% or more or even 100%；
BOD5 can achieve less than 10mg/L, even up to 10mg/L, and removal rate is up to 99% or more.
5) the device of the invention, after 50 water process: TDS can achieve 0-10mg/L, and TDS removal rate is reachable
98% or more or even 100%；UV254 (abs) can achieve 0-0.005, and UV254 (abs) removal rate is up to 98% or more, very
To 100%；BOD5 can achieve 1-10mg/L, and removal rate is up to 99% or more.
6) the device of the invention, convenient for cleaning after use, after over cleaning, treatment effect can achieve device and use for the first time
90% or more, service life is up to 1000h or more.After reaching service life, internal purifying part is replaceable, and replaces letter
It is single, it is easily operated, it can achieve the purpose utilized again.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of purification device.
1- sanitary wastewater or tap water water inlet；2- booster；3- rotor filter；4- coarse rack layer；5- magnetic Nano
Adsorbent layer；6- fine fack layer；The multi-functional on-line monitoring device of 7-；8- cathode one；9- exhaust valve；10- device for absorbing tail gas；11-
Nanoparticle microelectrode；12- metal mesh anode；13- cathode two；The miniature oxygen tank of 14-；15- gas flowmeter；16- solenoid valve
One；17- bubble；18- transition metal modifies TiO2- MOFs film composite electrode；19- motor switch one；20- motor switch two；21-
Motor switch three；22- motor switch four；23- power supply；24- liquid separator；25- tail washings leakage fluid dram；26- solenoid valve；27- electricity
Magnet valve；28- solenoid valve；29- fluid flowmeter one；30- fluid flowmeter two；31- fluid flowmeter three；32- flushing water liquid storage
Tank；33- clean water fluid reservoir；34- direct drinking fluid reservoir；35- waste liquid fluid reservoir；50- three-level purification system；51- three-level water purification
Collection system；52- tail washings recovery system.
Specific embodiment
Below by specific embodiment, the present invention is further described, it is noted that for the ordinary skill of this field
For personnel, without departing from the principle of the present invention, several variations and modifications can also be made, these also should be regarded as belonging to
Protection scope of the present invention.
A kind of sanitary wastewater/tap water Electro Sorb oxidation depth purification device, including
Three-level purification system (50)；The three-level water purification collection system (51) and tail washings for being connected to three-level purification system (50) are returned
Receipts system (52).
The three-level purification system (50) includes three-level purification system shell, sanitary wastewater or tap water water inlet (1), one
Grade processing unit, two stage treatment unit and three stage treatment unit, liquid separator (24), the sanitary wastewater or tap water enter water
Mouth (1), coagulation unit, two stage treatment unit and three stage treatment unit, liquid separator (24) are from top to bottom arranged in three
In grade purification system shell；The coagulation unit includes rotor filter (3), coarse rack layer (4), magnetic nanometer adsorbent
Layer (5), fine fack layer (6), the rotor filter (3) is set to the lower section of sanitary wastewater or tap water water inlet (1), described
Coarse rack layer (4), magnetic nanometer adsorbent layer (5), fine fack layer (6) are from top to bottom set in three-level purification system shell,
Meanwhile the coarse rack layer (4), magnetic nanometer adsorbent layer (5), fine fack layer (6) are connected to three-level purification system shell respectively
Inner wall；Before carrying out advanced treating, preliminary impurity elimination work is carried out to sanitary sewage by rotor filter (3), to visible solid
Particulate matter is removed.The two stage treatment unit includes cathode one (8), nanoparticle microelectrode (11), metal mesh anode
(12), cathode two (13)；The cathode one (8), nanoparticle microelectrode (11), metal mesh anode (12), cathode two (13) by
It is set in three-level purification system shell under above, meanwhile, the cathode one (8), nanoparticle microelectrode (11), metal mesh sun
Pole (12), cathode two (13) are connected to the inner wall of three-level purification system shell；The nanoparticle microelectrode (11) is uniform
It is distributed in cathode one (8), metal mesh anode (12), between cathode two (13)；The three stage treatment unit includes that transition metal is repaired
Adorn TiO2- MOFs film composite electrode (18).
At least one of the cathode one (8) and cathode two (13) are ferrite modification carbon fiber cloth electrode；
In some embodiments, cathode one (8) is ferrite modification carbon fiber cloth electrode, and cathode two (13) is existing
Common cathode electrode in technology；
In further embodiments, cathode two (13) is ferrite modification carbon fiber cloth electrode, and cathode one (8) is existing
There is common cathode electrode in technology；
In some embodiments, cathode one (8) and cathode two (13) are ferrite modification carbon fiber cloth electrode；
Cathode one (8), metal mesh anode (12), cathode two (13), TiO2Modification MOFs nanofiltration membrane electrode (18) connects respectively
It is connected to power supply (23), cathode one (8), metal mesh anode (12), cathode two (13), TiO2Modify MOFs nanofiltration membrane electrode (18) with
Multidirectional control switch (19), multidirectional control switch (20) multidirectional control switch (21) multidirectional control are respectively arranged between power supply (23)
System switch (22)；
In some embodiments, the voltage range of the power supply (23) is 1-10V；
In some embodiments, the metal mesh anode (12) is platinum gauze electrode or stainless (steel) wire electrode.
In some embodiments, the mesh number of the metal mesh anode (12) is -120 mesh of 35 mesh.
In some embodiments, the sanitary wastewater or tap water water inlet (1) are the controllable valve of bottle neck；It can be directly connected to
Connection funnel accesses sanitary wastewater after running water tap or disassembly, can be pressurized by compress cell to water body.
In some embodiments, exhaust valve (9), the exhaust valve are provided between fine fack layer (6) and cathode one (8)
(9) it is arranged on three-level purification system (50) shell；
As optimal technical scheme, in some embodiments, the external device for absorbing tail gas of the exhaust valve (9) (10)；
As optimal technical scheme, wherein the transition metal modifies TiO2Below-MOFs film composite electrode (18), if
It is equipped with miniature gas tank (14), the miniature gas tank (14) is external on three-level purification system shell；The miniature gas tank (14) and
Three-level purification system shell is connected by pipeline, is additionally provided with gas stream between miniature gas tank (14) and three-level purification system shell
Meter (15) and solenoid valve one (16)；
Wherein, the miniature gas tank (14) is miniature oxygen tank or ozone generator；
When carrying out Electro Sorb oxidation depth purified treatment, miniature gas tank (14) provides oxygen or ozone and carries out deeply to water body
Degree processing；The oxygen source occurred using air or high purity oxygen gas as ozone；Ozone or the oxygen gas-liquid after micro- aerator are filled
Divide after mixing and reaches ferrite modifying carbon fibers cloth electrochemical cathode with nano grade air bubbles.
In some embodiments, miniature gas tank (14) provides oxygen, when supply voltage 1-5V, if two stage treatment unit is formed
Dry microelectrode constitutes three dimensional particles electrode system, efficiently in situ to generate hydrogen peroxide；Transition gold contained by nanoparticle microelectrode simultaneously
Belong to ion, can produce hydroxyl radical free radical, in waste water/tap water contaminant trace species and disinfection by-products carry out deep oxidation,
Principle is as follows:
O2+2H++2e-→H2O2,
Mn+H2O2→Mn+1+OH-+·OH
In some embodiments, miniature gas tank (14) provides ozone, when supply voltage 4-10V, receives in two stage treatment unit
Rice corpuscles microelectrode serves as catalyst, and catalysis ozone occurs chain reaction and generates hydroxyl radical free radical, to the trace in waste water/tap water
It measures pollutant and disinfection by-products carries out deep oxidation, principle is as follows:
O3+OH-→HO2 -+O2,
O2+2H++2e-→H2O2,
H2O2+2O3→·OH+3O2,
The inner bottom of the three-level purification system shell is additionally provided with liquid separator (24).
Wherein, the three-level water purification collection system (51) includes 3 fluid reservoirs being set side by side, respectively flushing water liquid storage
Tank (32), clean water fluid reservoir (33), direct drinking fluid reservoir (34)；
With solenoid valve, fluid flowmeter and pipeline company between the three-level purification system (50) and water purification collection system (51)
It connects；
The solenoid valve is set as 3, respectively solenoid valve one (26), solenoid valve two (27), solenoid valve three (28)；
The fluid flowmeter is set as 3, respectively fluid flowmeter one (29), fluid flowmeter two (30), liquid
Flowmeter three (31)；
Further,
Tail washings recovery system (52) includes waste liquid fluid reservoir (35) and tail washings leakage fluid dram (25)；The tail washings leakage fluid dram (25)
It is set to the lower end of three-level purification system (50) shell, the waste liquid fluid reservoir (35) is connected to three-level purification system by pipeline
(50) on shell.
The waste liquid that the tail washings recovery system (52) generates sanitary wastewater/tap water Electro Sorb oxidation depth purification device
It is recycled with cleaning solution, waste liquid rate is 5%-10%.
Magnetic nanometer adsorbent in magnetic nanometer adsorbent layer (5) can take out, with soaked in absolute ethyl alcohol 30-45min,
Drying continues to use；
Nanoparticle microelectrode (11) can carry out immersion 30-60min with dehydrated alcohol, carry out magnetic recovery with magnet, do
It is dry to continue to use；Other electrodes can be injected into anti-when 1-5mmol/L NaCl solution progress on-line cleaning, cleaning
Solution is answered, is opened respectively by multidirectional control switch (19), multidirectional control switch (20), multidirectional control switch (21), multidirectional control
After closing (22) progress anode and cathode exchange, electrolysis a period of time is carried out.
The water only obtained by coagulation unit is level-one water, is collected in flushing water fluid reservoir (32), for gardens,
The flushing of flowers and plants lavatory etc.；Second level water is obtained by firsts and seconds processing unit, is collected in clean water fluid reservoir (33), water quality
Reach tap water requirement；Tertiary effluent is obtained by level-one, second level and three stage treatment unit, is collected in direct drinking fluid reservoir (34),
It can be used for direct drinking.
Wherein, magnetic nanometer adsorbent layer (5) and nanoparticle microelectrode (11) are the growth of magnetic carbon material in situ
MOFs (metal organic framework compound (English name Metal organic Framework))；It is adsorbable to remove odors, is remaining
Chlorine, heavy metal and the common organic matter of the overwhelming majority.
Preferably, in some embodiments, the size of magnetic nanometer adsorbent layer (5) magnetic Nano material is
20-50nm；Specific surface area is 50-300m2/g；Pore volume is 0.4-1.2cm3/g；Saturation magnetization is 15-35emu/g；
Preferably, in some embodiments, nanoparticle microelectrode (11) the nanoparticle microelectrode size is 30-
100nm, specific surface area are 50-200m2/g；Pore volume is 1.3-1.4cm3/g；Saturation magnetization is 5-15emu/g；
The preparation method of the magnetic carbon material in situ growth MOFs includes the following steps:
1) preparation of magnetic carbon material:
1.1) magnetic Nano material is prepared into magnetic Nano material aqueous solution, magnetic Nano material is added in char-forming material
Ultrasound mixes in aqueous solution, obtains mixed solution one；
1.2) mixed solution that step 1.1) is prepared is in constant temperature blender with magnetic force in 40 DEG C -60 DEG C, revolving speed
Reaction obtains mixed solution two not less than for 24 hours under the conditions of 3rpm；
1.3) it is filtered, and washed by qualitative filter paper after being cooled to room temperature the mixed solution two obtained after step 1.2)
Wash filter cake until last time filtered fluid be in neutrality, obtain neutral sorbent；
1.4) neutral sorbent that step 1.3) is prepared is placed in 40 DEG C of -60 DEG C of Constant Temp. Ovens and dries not
Lower than 12h, it is then ground to powdery, obtains powdered absorbent；
1.5) powdered absorbent for obtaining step 1.4) is put into and is placed on N without spreading in lid silica crucible2As
In the electron tubes type electric furnaces for protecting gas air-flow, 600 DEG C and constant temperature 2h are warming up to 4-6 DEG C/min of heating rate, is ground after cooling,
Obtain magnetic carbon material；
Step 1.1) the magnetic Nano material is Zero-valent Iron, γ-Fe2O3Or the spinel ferrite that hydrothermal synthesis method is formed
The one or more of body；
Wherein, in some embodiments, the magnetic Nano material is Zero-valent Iron, γ-Fe2O3Or hydrothermal synthesis method is formed
Ferrospinel any one；
In some embodiments, the magnetic Nano material is Zero-valent Iron, γ-Fe2O3The combination of arbitrary proportion；
In some embodiments, the magnetic Nano material is the ferrospinel of Zero-valent Iron, hydrothermal synthesis method formation
The combination of arbitrary proportion；
In some embodiments, the magnetic Nano material is γ-Fe2O3, hydrothermal synthesis method formed ferrospinel
The combination of arbitrary proportion；
In some embodiments, the step 1.1) char-forming material is multi-walled carbon nanotube, graphene and biological carbon one
Kind or a variety of combinations；For example, in some embodiments, the step 1.1) char-forming material is multi-walled carbon nanotube, graphite
Any one of alkene and biological carbon, in further embodiments, rapid 1.1) the described char-forming material are multi-walled carbon nanotube, graphite
The combination of alkene or graphene, the combination of biological carbon or the combination of multi-walled carbon nanotube, biological carbon, in further embodiments,
Rapid 1.1) the described char-forming material is multi-walled carbon nanotube, the combination of graphene, the combination of biological carbon.In these embodiments, right
Without limitation in the two or the ratio of three.
2) transition metal salt and organic ligand is taken to form growth in situ MOFs, growth in situ MOFs is adsorbed on the magnetic of step 1)
Property carbon material on obtain magnetic carbon material in situ growth MOFs；
3) the magnetic carbon nanometer in situ growth MOFs sieving obtained step 2), screens out the material having a size of 20-50nm,
As magnetic nanometer adsorbent layer；
The magnetic carbon nanometer in situ growth MOFs sieving that step 2) is obtained, screens out the material having a size of 20-50nm, i.e.,
For nanoparticle microelectrode；
Preferably, step 2) are as follows: the magnetic carbon material that step 1) is prepared is in ultrapure water with ultrasound point
It dissipates uniformly, transition metal salt is added and makes it completely dissolved, then organic ligand is added thereto, be transferred to high pressure after sealing stirring
It reacts in reaction kettle, after reaction takes out the solidliquid mixture in autoclave, ultrapure water cleaning, sealing are carried out to it
Stirring and centrifugal treating obtain the growth of magnetic carbon material in situ to the solid washes of absolute alcohol after centrifugation after dry
MOFs；
In some embodiments, transition metal salt is Fe (NO3)3·9H2O、Al(NO3)3·9H2O、Cu(NO3)2·3H2O、
Co(NO3)2·6H2O any one or a few；
In some embodiments, the organic ligand is any one of trimesic acid and terephthalic acid (TPA).
The transition metal modifies TiO2- MOFs film composite electrode (18) the preparation method comprises the following steps:
A) organic ligand solution the preparation of MOFs film: is passed through into electrochemical in-situ deposition method shape under three-electrode system
At MOFs film；
b)TiO2The preparation of-MOFs film: after the MOFs film that step 1) obtains is added in alcohol solvent, wait infiltrate sufficiently
Afterwards, butyl titanate (Ti (OBu) is slowly added dropwise4), ultrasound is then transferred in polytetrafluoroethylliner liner, is placed in stainless steel
Reaction kettle reacts, cooling, and washing is dried to obtain TiO2- MOFs film；
C) transition metal modifies TiO2The preparation of-MOFs film composite electrode: it is added what step b) was obtained in ultrapure water
TiO2After-MOFs film, after infiltrating sufficiently, it is added and contains Fe3+Solid chemical compound and MCl2Solid (M=V, Cr, Mn, Co, Ni,
Cu and Zn), ultrasound is then transferred in polytetrafluoroethylliner liner, is placed in stainless steel cauldron, reacts, and it is cooling, it washs, does
It is dry to obtain transition metal-modified TiO2-MOFs film composite electrode (18).
The transition metal modifies TiO2In-MOFs film composite electrode (18), TiO2, oxide, MOFs film (contain copper mesh) matter
Measure ratio are as follows: (4~15): (5~10): (75~91)." oxide " in aforementioned proportion is free of TiO2。
In aforementioned proportion, TiO2For TiO in step b)2TiO in-MOFs film2；
Oxide is step c) introducing, and oxide includes ferroso-ferric oxide, spinel oxide etc., is obtained by co-precipitation.
The ferrite modification carbon fiber cloth electrode the preparation method comprises the following steps:
1) preparation of modified carbon fiber cloth: carrying out surface to carbon cloth with strong oxidizing solution or alkaline solution and be modified,
Drying is obtained by drying；
2) preparation of ferrite modification carbon cloth: step 1) is added when hydrothermal co-precipitation method prepares ferrite and obtains
Modified carbon fiber cloth, obtain ferrite modification carbon fiber cloth electrode.
In some embodiments, strong oxidizing solution described in step 1) are as follows: concentrated nitric acid, the concentrated sulfuric acid, chlorine, bromine, iodine contain
Oxygen acid, Fenton reagent, persulfate solution, the one or more of potassium ferrate solution；
Alkaline solution described in step 1) is strong alkali solution,
In some embodiments, the strong alkali solution is KOH and/or NaOH；
In some embodiments, the preparation of step 1) modified carbon fiber cloth: carbon cloth is fully immersed in equipped with strong oxygen
In the property changed solution, ultrasound is subsequently placed in isothermal reaction kettle and reacts, after surface residual debris impurity is washed with water, until pH is to neutrality, after
Vacuum drying oven modified carbon fiber cloth obtained by drying；
In some embodiments, the mass volume ratio of the carbon cloth and strong oxidizing solution or alkaline solution is
1.0g:(100~300mL)；
In some embodiments, in step 1), isothermal reaction kettle reaction temperature is 35-80 DEG C；
In some embodiments, in step 1), isothermal reaction kettle reaction temperature is 40-60 DEG C；
In some embodiments, in step 1), isothermal reaction kettle reaction temperature is 50 DEG C；
In some embodiments, in step 1), the reaction time is 12h~72h in isothermal reaction kettle；
In some embodiments, in step 1), the reaction time is for 24 hours~60h in isothermal reaction kettle；
In some embodiments, in step 1), the reaction time is 48h in isothermal reaction kettle；
In some embodiments, in step 1), with milli-Q water surface residual debris impurity；
In some embodiments, in step 1), vacuum drying oven temperature is 30-75 DEG C；
In some embodiments, in step 1), vacuum drying oven temperature is 35-50 DEG C；
In some embodiments, in step 1), vacuum drying oven temperature is 40 DEG C.
In some embodiments, chlorine in the step 1), bromine, iodine the concentration of oxyacid be 0.1-0.5mol/L,
Fenton reagent is 0.2-0.6mol/L Fe in the step 1)2+With the H of 30wt%2O2,
Persulfate solution concentration is 0.1-0.5mol/L in the step 1),
Potassium ferrate solution concentration is 0.1-0.5mol/L in the step 1),
Strong alkali solution is the KOH solution and/or 1-3mol/L NaOH solution of 1-3mol/L in the step 1).
The step 2) are as follows:
2) preparation of ferrite modification carbon cloth: step 1) is added when hydrothermal co-precipitation method prepares ferrite and obtains
Modified carbon fiber cloth, ultrasonic mixing, constant temperature blender with magnetic force effect under react a period of time, will load later ferritic
Carbon cloth drying is put into the tube furnace under inert gas atmosphere protection, roasting a period of time, and taking-up is cooling to obtain iron oxygen
Body modification carbon fiber cloth electrode；
The ferrite of the step 2) is the single ferrite and/or spinel type ferrite of transition metal；
In some embodiments, the step 2) are as follows:
2) it the preparation of ferrite modification carbon cloth: is added into ultrapure water and contains Fe3+Salt and M2+Salt, then
With magnetic stirrer so that it is uniformly mixed and is completely dissolved to obtain mixed solution, and polyethylene glycol is added thereto, or
Person's ammonium fluoride and urea composition continue to stir to obtain the final product, are placed on reaction in isothermal reaction kettle later, cool down, wash after completion of the reaction
Wash, be placed in thermostatic drying chamber and dry, be subsequently placed in electric tube furnace, be passed through inert gas as protection gas, roasting to get
Ferrite modification carbon cloth；In the above preparation method, the modified carbon fiber cloth is added in co-precipitation before being formed；
The one or more of described M=Fe, Mn, Ni, Cu, Co；
In some embodiments, the Fe3+Salt and M2+The molar concentration rate of salt is 1-4；Preferably, the Fe3+Salt
Class and M2+The molar concentration rate of salt is 2；
In some embodiments, the degree of isothermal reaction kettle temperature described in step 2) is 20-140 DEG C；Preferably, institute in step 2)
Stating isothermal reaction kettle temperature degree is 40-130 DEG C；
In some embodiments, the reaction time is 2-100h in isothermal reaction kettle described in step 2)；Preferably, step 2)
Described in isothermal reaction kettle the reaction time be 12-72h；
In some embodiments, maturing temperature described in step 2) is 300-400 DEG C；Preferably, it is roasted described in step 2)
Burning temperature is 350 DEG C；
In some embodiments, in step 2), the heating rate of electric tube furnace is 2-10 DEG C/min；Preferably, step 2)
In, the heating rate of electric tube furnace is 5 DEG C/min；
In some embodiments, calcining time described in step 2) is 0.5-3 hours；Further, described in step 2)
Calcining time is 1 hour.
In some embodiments, the mass ratio of the ferrite in the step 2) and modified carbon fiber cloth material be 1:2~
1:8。
In use, passing through detection treatment sewage or tap water situation, such as TDS, BOD value, COD value, UV254 first
With the purposes of water after processing etc., suitable processing unit is selected to be handled.
Sanitary sewage to be processed or tap water are had by oneself pressure by compress cell or tap water first and enters water
Mouth (1) (the controllable valve of bottle neck), after rotor filter (3) remove visible particle object, using coarse rack layer (4), magnetism
Nano adsorption oxidant layer (5), fine fack layer (6) can obtain then being stored up with flushing water for the flushing water of gardens, flowers and plants lavatory etc.
Flow container (32) storage.
After coagulation cell processing, it can be passed through oxygen, power supply (23) switch is opened simultaneously, 1-5V voltage is provided, is mentioned
For hydrogen peroxide and the hydroxyl radical free radical in situ of generating to flushing water progress secondary treatment, tap water requirement can reach；If being passed through ozone,
Power switch is opened simultaneously, 4-10V voltage is provided, ozone is provided and catalysis ozone generates hydroxyl radical free radical to through coagulation list
The flushing water that member processing obtains carries out secondary treatment, can reach tap water requirement, is then stored with clean water fluid reservoir (33).
After coagulation cell processing and two stage treatment unit, three stage treatment unit is entered, power supply is opened, most passes through afterwards
Cross transition metal modification TiO2Direct drinking can be obtained in-MOFs film composite electrode, is then stored with direct drinking fluid reservoir (34).
By taking following embodiment a as an example:
Sanitary wastewater is subjected to tertiary treatment, obtains direct drinking:
Sanitary sewage to be processed is had by oneself pressure by compress cell or tap water first and enters water inlet (1) (bottle neck
Controllable valve), after rotor filter (3) remove visible particle object, using coarse rack layer (4), magnetic nanometer adsorbent
Layer (5), fine fack layer (6), can obtain the flushing water for gardens, flowers and plants lavatory etc., then be deposited with flushing water fluid reservoir (32)
Storage.After coagulation cell processing, it is passed through oxygen, power supply (23) switch is opened simultaneously, 1-5V voltage is provided, production in situ is provided
Raw hydrogen peroxide and hydroxyl radical free radical carry out secondary treatment to flushing water；Then it is stored with clean water fluid reservoir (33).
After coagulation cell processing and two stage treatment unit, three stage treatment unit is entered, power supply is opened, most passes through afterwards
Cross transition metal modification TiO2Direct drinking can be obtained in-MOFs film composite electrode, is then stored with direct drinking fluid reservoir (34).
In this embodiment:
Device is connected with device for recovering tail gas, and metal mesh anode (12) is stainless (steel) wire electrode, and mesh number is 35-120 mesh.
Magnetic nanometer adsorbent layer (5) and nanoparticle microelectrode (11) are magnetic carbon material in situ growth MOFs；Institute
The size for stating magnetic nanometer adsorbent layer (5) magnetic Nano material is 20-50nm；Specific surface area is 50-300m2/g；Pore-body
Product is 0.4-1.2cm3/g；Saturation magnetization is 15-35emu/g；The micro- electricity of nanoparticle microelectrode (11) nanoparticle
Pole size is 30-100nm, and specific surface area is 50-200m2/g；Pore volume is 1.3-1.4cm3/g；Saturation magnetization is 5-
15emu/g。
The transition metal modifies TiO2In-MOFs film composite electrode (18), TiO2, oxide, MOFs film (contain copper mesh) matter
Measure ratio are as follows: 10:7:80.
The purification device of above-described embodiment is used for water process, as a result as follows:
The index parameter of 1 embodiment a water process of table
| Water index | Pending water | After coagulation | After two stage treatment | After tertiary treatment |
| TDS(mg/L) | >500 | 240 | 58 | 1 |
| UV254(abs) | >1 | 0.08 | 0.007 | 0.002 |
| BOD5(mg/L) | >100 | 22 | 12 | 1 |
Waste liquid is recycled, and waste liquid rate is 7%.
The sanitary wastewater of other embodiment/tap water Electro Sorb oxidation depth purification device is used for water process, is tied
Fruit is as follows:
The index parameter of 2 other embodiments water process of table
| Water index | Pending water | After coagulation | After two stage treatment | After tertiary treatment |
| TDS(mg/L) | >500 | 200-300 | 10-200 | 0-10 |
| UV254(abs) | >1 | 0.01-0.1 | 0.005-0.01 | 0-0.005 |
| BOD5(mg/L) | >100 | 15-35 | 10-15 | 1-10 |
Waste liquid is recycled, and waste liquid rate is 5%-10%.
The device of 100 water process will be used to clean, cleaning method are as follows:
Magnetic nanometer adsorbent in magnetic nanometer adsorbent layer (5) can take out, with soaked in absolute ethyl alcohol 30-45min,
Drying continues to use；
Nanoparticle microelectrode (11) can carry out immersion 30-60min with dehydrated alcohol, carry out magnetic recovery with magnet, do
It is dry to continue to use；Other electrodes can be injected into anti-when 1-5mmol/L NaCl solution progress on-line cleaning, cleaning
Solution is answered, is opened respectively by multidirectional control switch (19), multidirectional control switch (20), multidirectional control switch (21), multidirectional control
After closing (22) progress anode and cathode exchange, electrolysis a period of time is carried out.
After cleaning, water treatment efficiency can restore to 90% or more of first using effect.
It above are only the preferred embodiment of the invention, be not restricted to the present invention.Those skilled in the art is come
It says, other various forms of variations or variation can also be made on the basis of the above description.There is no need and unable to all
Embodiment illustrate.And the obvious changes or variations that thus scheme is extended out are still in protection of the invention
Within the scope of.
Claims (8)
1. a kind of sanitary wastewater/tap water Electro Sorb oxidation depth purification device, which is characterized in that including
Three-level purification system (50)；It is connected to three-level water purification collection system (51) and the tail washings recycling system of three-level purification system (50)
It unites (52).
2. sanitary wastewater according to claim 1/tap water Electro Sorb oxidation depth purification device, which is characterized in that
The three-level purification system (50) includes three-level purification system shell, at sanitary wastewater or tap water water inlet (1), level-one
Manage unit, two stage treatment unit and three stage treatment unit, liquid separator (24), the sanitary wastewater or tap water water inlet
(1), three-level is from top to bottom arranged in coagulation unit, two stage treatment unit and three stage treatment unit, liquid separator (24)
In purification system shell；
The coagulation unit includes rotor filter (3), coarse rack layer (4), magnetic nanometer adsorbent layer (5), fine fack
Layer (6), the rotor filter (3) are set to the lower section of sanitary wastewater or tap water water inlet (1), the coarse rack layer (4),
Magnetic nanometer adsorbent layer (5), fine fack layer (6) are from top to bottom set in three-level purification system shell, meanwhile, the thick lattice
Grid layer (4), magnetic nanometer adsorbent layer (5), fine fack layer (6) are connected to the inner wall of three-level purification system shell respectively；
The two stage treatment unit includes cathode one (8), nanoparticle microelectrode (11), metal mesh anode (12), cathode two
(13)；
The cathode one (8), metal mesh anode (12), cathode two (13) are from top to bottom set in three-level purification system shell,
Meanwhile the cathode one (8), metal mesh anode (12), cathode two (13) are connected to the inner wall of three-level purification system shell,
The nanoparticle microelectrode (11) is uniformly distributed in cathode one (8), metal mesh anode (12), between cathode two (13)；
The three stage treatment unit includes transition metal modification TiO2- MOFs film composite electrode (18).
3. sanitary wastewater according to claim 2/tap water Electro Sorb oxidation depth purification device, which is characterized in that
At least one of the cathode one (8) and cathode two (13) are ferrite modification carbon fiber cloth electrode；
Cathode one (8), metal mesh anode (12), cathode two (13), TiO2Modification MOFs nanofiltration membrane electrode (18) is connected to electricity
Source (23), cathode one (8), metal mesh anode (12), cathode two (13), TiO2Modify MOFs nanofiltration membrane electrode (18) and power supply
(23) the multidirectional control of multidirectional control switch (19), multidirectional control switch (20) multidirectional control switch (21) is respectively arranged between to open
It closes (22)；
Further, the voltage range of the power supply (23) is 1-10V；
Further, the metal mesh anode (12) is platinum gauze electrode or stainless (steel) wire electrode；
Further, the mesh number of the metal mesh anode (12) is 35-120 mesh.
4. sanitary wastewater according to claim 2/tap water Electro Sorb oxidation depth purification device, which is characterized in that
The sanitary wastewater or tap water water inlet (1) are the controllable valve of bottle neck；
Further, between the fine fack layer (6) and cathode one (8), it is provided with multi-functional on-line monitoring device (7), it is described more
Function on-line monitoring device (7) is external on three-level purification system shell；
Further, it is provided with exhaust valve (9) between the fine fack layer (6) and cathode one (8), exhaust valve (9) setting
On three-level purification system (50) shell；
Further, the external device for absorbing tail gas of the exhaust valve (9) (10)；
Further, the transition metal modifies TiO2Below-MOFs film composite electrode (18), it is provided with miniature gas tank (14), institute
Miniature gas tank (14) is stated to be external on three-level purification system shell；The miniature gas tank (14) and three-level purification system shell pass through
Pipeline connection, is additionally provided with gas flowmeter (15) and solenoid valve one between miniature gas tank (14) and three-level purification system shell
(16)；
Further, the miniature gas tank (14) is miniature oxygen tank or ozone generator；
Further, the inner bottom of three-level purification system shell is arranged in the liquid separator (24).
5. sanitary wastewater according to claim 1/tap water Electro Sorb oxidation depth purification device, which is characterized in that
The three-level water purification collection system (51) includes 3 fluid reservoirs being set side by side, respectively flushing water fluid reservoir (32), clear
Clean water fluid reservoir (33), direct drinking fluid reservoir (34)；
Further, between the three-level purification system (50) and water purification collection system (51) with solenoid valve, fluid flowmeter and
Pipeline connection；
Further, the solenoid valve is set as 3, respectively solenoid valve one (26), solenoid valve two (27), solenoid valve three
(28)；
Further, the fluid flowmeter is set as 3, respectively fluid flowmeter one (29), fluid flowmeter two (30),
Fluid flowmeter three (31)；
Further,
Tail washings recovery system (52) includes waste liquid fluid reservoir (35) and tail washings leakage fluid dram (25)；Tail washings leakage fluid dram (25) setting
In the lower end of three-level purification system (50) shell, the waste liquid fluid reservoir (35) is connected to three-level purification system (50) by pipeline
On shell.
6. sanitary wastewater according to claim 2/tap water Electro Sorb oxidation depth purification device, which is characterized in that
Magnetic nanometer adsorbent layer (5) and nanoparticle microelectrode (11) are magnetic carbon material in situ growth MOFs；
Further,
The size of magnetic nanometer adsorbent layer (5) magnetic Nano material is 20-50nm；Specific surface area is 50-300m2/g；Hole
Gap volume is 0.4-1.2cm3/g；Saturation magnetization is 15-35emu/g；
Further,
Nanoparticle microelectrode (11) the nanoparticle microelectrode size is 30-100nm, and specific surface area is 50-200m2/g；Hole
Gap volume is 1.3-1.4cm3/g；Saturation magnetization is 5-15emu/g；
Further, the preparation method of the magnetic carbon material in situ growth MOFs includes the following steps:
1) preparation of magnetic carbon material:
1.1) magnetic Nano material is prepared into magnetic Nano material aqueous solution, it is water-soluble that magnetic Nano material is added in char-forming material
Ultrasound mixes in liquid, obtains mixed solution one；
1.2) mixed solution that step 1.1) is prepared is in constant temperature blender with magnetic force in 40 DEG C -60 DEG C, revolving speed 3rpm item
Reaction obtains mixed solution two not less than for 24 hours under part；
1.3) it is filtered after being cooled to room temperature the mixed solution two obtained after step 1.2) by qualitative filter paper, and washs filter
Cake is in neutrality up to last time filtered fluid, obtains neutral sorbent；
1.4) neutral sorbent that step 1.3) is prepared is placed in 40 DEG C of -60 DEG C of Constant Temp. Ovens to dry and be not less than
Then 12h is ground to powdery, obtain powdered absorbent；
1.5) powdered absorbent for obtaining step 1.4) is put into and is placed on N without spreading in lid silica crucible2As protection gas
In the electron tubes type electric furnace of air-flow, 600 DEG C and constant temperature 2h are warming up to 4-6 DEG C/min of heating rate, is ground after cooling, obtains magnetic
Property carbon material；
Further, the step 1.1) magnetic Nano material is Zero-valent Iron, γ-Fe2O3, hydrothermal synthesis method formed spinelle
It is ferritic any one or a few；
Further, the step 1.1) char-forming material is that multi-walled carbon nanotube, graphene and biological carbon are one or more
Combination；
2) transition metal salt and organic ligand is taken to form growth in situ MOFs, growth in situ MOFs is adsorbed on the magnetic carbon of step 1)
Magnetic carbon material in situ growth MOFs is obtained on material；
3) the magnetic carbon nanometer in situ growth MOFs sieving obtained step 2), screens out the material having a size of 20-50nm, as
Magnetic nanometer adsorbent layer；
The magnetic carbon nanometer in situ growth MOFs sieving that step 2) is obtained, screens out the material having a size of 20-50nm, as receives
Rice corpuscles microelectrode；
Further,
Step 2): the magnetic carbon material that step 1) is prepared is uniform with ultrasonic disperse in ultrapure water, and transition metal is added
Salt simultaneously makes it completely dissolved, then organic ligand is added thereto, is transferred in autoclave and reacts after sealing stirring, reaction knot
The solidliquid mixture in autoclave is taken out after beam, ultrapure water cleaning, sealing stirring and centrifugal treating are carried out to it, it is right
Solid washes of absolute alcohol after centrifugation obtains magnetic carbon material in situ growth MOFs after dry；
Further, the transition metal salt is Fe (NO3)3·9H2O、Al(NO3)3·9H2O、Cu(NO3)2·3H2O、Co
(NO3)2·6H2O any one or a few；
Further, the organic ligand is any one of trimesic acid and terephthalic acid (TPA).
7. sanitary wastewater according to claim 2/tap water Electro Sorb oxidation depth purification device, which is characterized in that institute
State transition metal modification TiO2- MOFs film composite electrode (18) the preparation method comprises the following steps:
A) preparation of MOFs film: organic ligand solution is formed under three-electrode system by electrochemical in-situ deposition method
MOFs film；
b)TiO2The preparation of-MOFs film: after the MOFs film that step 1) obtains is added in alcohol solvent, after infiltrating sufficiently, delay
It is slow that butyl titanate (Ti (OBu) is added dropwise4), ultrasound is then transferred in polytetrafluoroethylliner liner, is placed in stainless steel reaction
Kettle reacts, cooling, and washing is dried to obtain TiO2- MOFs film；
C) transition metal modifies TiO2The preparation of-MOFs film composite electrode: the TiO that step b) is obtained is added in ultrapure water2-
After MOFs film, after infiltrating sufficiently, it is added and contains Fe3+Solid chemical compound and MCl2Solid (M=V, Cr, Mn, Co, Ni, Cu and
Zn), ultrasonic, it is then transferred in polytetrafluoroethylliner liner, is placed in stainless steel cauldron, react, cooling, washing, dry
TiO is modified to transition metal2- MOFs film composite electrode (18)；
The transition metal modifies TiO2In-MOFs film composite electrode (18), TiO2, oxide, MOFs film (contain copper mesh) mass ratio
Are as follows: (4~15): (5~10): (75~91).
8. sanitary wastewater according to claim 3/tap water Electro Sorb oxidation depth purification device, which is characterized in that institute
State ferrite modification carbon fiber cloth electrode the preparation method comprises the following steps:
1) preparation of modified carbon fiber cloth: carrying out surface to carbon cloth with strong oxidizing solution or alkaline solution and be modified, dry
It is obtained by drying；
2) preparation of ferrite modification carbon cloth: what addition step 1) obtained when hydrothermal co-precipitation method prepares ferrite changes
Property carbon cloth, obtains ferrite modification carbon fiber cloth electrode；
Further,
Strong oxidizing solution described in step 1) are as follows: concentrated nitric acid, the concentrated sulfuric acid, chlorine, bromine, iodine oxyacid, Fenton reagent, persulfuric acid
Salting liquid, the one or more of potassium ferrate solution；
Alkaline solution described in step 1) is strong alkali solution,
Further, the strong alkali solution is KOH and/or NaOH；
Further, the preparation of step 1) modified carbon fiber cloth: carbon cloth is fully immersed in equipped in strong oxidizing solution,
Ultrasound is subsequently placed in isothermal reaction kettle and reacts, after surface residual debris impurity is washed with water, until pH, to neutrality, rear vacuum drying oven dries
Dry modified carbon fiber cloth to obtain the final product；
Further；The mass volume ratio of the carbon cloth and strong oxidizing solution or alkaline solution be 1.0g:(100~
300mL)；
Further, in step 1), isothermal reaction kettle reaction temperature is 35-80 DEG C；
Further, in step 1), isothermal reaction kettle reaction temperature is 40-60 DEG C；
Further, in step 1), isothermal reaction kettle reaction temperature is 50 DEG C；
Further, in step 1), the reaction time is 12h~72h in isothermal reaction kettle；
Further, in step 1), the reaction time is for 24 hours~60h in isothermal reaction kettle；
Further, in step 1), the reaction time is 48h in isothermal reaction kettle；
Further, in step 1), with milli-Q water surface residual debris impurity；
Further, in step 1), vacuum drying oven temperature is 30-75 DEG C；
Further, in step 1), vacuum drying oven temperature is 35-50 DEG C；
Further, in step 1), vacuum drying oven temperature is 40 DEG C.
Further,
Chlorine in the step 1), bromine, iodine the concentration of oxyacid be 0.1-0.5mol/L,
Fenton reagent is 0.2-0.6mol/L Fe in the step 1)2+With the H of 30wt%2O2,
Persulfate solution concentration is 0.1-0.5mol/L in the step 1),
Potassium ferrate solution concentration is 0.1-0.5mol/L in the step 1),
Strong alkali solution is the KOH solution and/or 1-3mol/L NaOH solution of 1-3mol/L in the step 1).
Further, the step 2) are as follows:
2) preparation of ferrite modification carbon cloth: what addition step 1) obtained when hydrothermal co-precipitation method prepares ferrite changes
Property carbon cloth, ultrasonic mixing, constant temperature blender with magnetic force effect under react a period of time, ferritic carbon fiber will be loaded later
Wei Bu drying is put into the tube furnace under inert gas atmosphere is protected, roasting a period of time, and taking out cooling is to obtain ferrite to repair
Adorn modified carbon fiber cloth electrode；
The ferrite of the step 2) is the single ferrite and/or spinel type ferrite of transition metal；
Further,
The step 2) are as follows:
2) it the preparation of ferrite modification carbon cloth: is added into ultrapure water and contains Fe3+Salt and M2+Then salt uses magnetic force
Blender stirs so that it is uniformly mixed and is completely dissolved to obtain mixed solution, and polyethylene glycol is added thereto, or is fluorinated
Ammonium and urea composition continue to stir to obtain the final product, are placed on reaction in isothermal reaction kettle later, cool down after completion of the reaction, wash, after
It is placed in thermostatic drying chamber and dries, be subsequently placed in electric tube furnace, be passed through inert gas as protection gas, roast to get iron oxygen
Body modification carbon cloth；In the above preparation method, the modified carbon fiber cloth is added in co-precipitation before being formed；
The one or more of described M=Fe, Mn, Ni, Cu, Co；
Further, the Fe3+Salt and M2+The molar concentration rate of salt is 1-4；Further, the Fe3+Salt and M2+Salt
The molar concentration rate of class is 2；
Further, the degree of isothermal reaction kettle temperature described in step 2) is 20-140 DEG C；Further, constant temperature described in step 2) is anti-
Answering kettle temperature degree is 40-130 DEG C；
Further, the reaction time is 2-100h in isothermal reaction kettle described in step 2)；Further, perseverance described in step 2)
The reaction time is 12-72h in warm reaction kettle；
Further, maturing temperature described in step 2) is 300-400 DEG C；Further, maturing temperature described in step 2) is
350℃；
Further, in step 2), the heating rate of electric tube furnace is 2-10 DEG C/min；Further, in step 2), tubular type electricity
The heating rate of furnace is 5 DEG C/min；
Further, calcining time described in step 2) is 0.5-3 hours；Further, calcining time described in step 2) is 1
Hour.
Further, the mass ratio of the ferrite in the step 2) and modified carbon fiber cloth material is 1:2~1:8.
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| CN114033932A (en) * | 2021-11-09 | 2022-02-11 | 重庆化工职业学院 | Electrochemical gas monitoring device |
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