CN1303000C - Method and apparatus for treating waste water by microwave photocatalysis - Google Patents
Method and apparatus for treating waste water by microwave photocatalysis Download PDFInfo
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- CN1303000C CN1303000C CNB2004100659797A CN200410065979A CN1303000C CN 1303000 C CN1303000 C CN 1303000C CN B2004100659797 A CNB2004100659797 A CN B2004100659797A CN 200410065979 A CN200410065979 A CN 200410065979A CN 1303000 C CN1303000 C CN 1303000C
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Abstract
The present invention discloses a method and a device used for treating waste water by microwave photocatalysis. Primary treatment of trash extraction by a grid, settling and pH regulation of the waste water to be treated are carried out, and then the waste water enters a device used for treating waste water by microwave photocatalysis, and the microwave photocatalysis is carried out. The device comprises a microwave reaction furnace, a waste water reaction chamber and an electrode-free lamp, wherein the waste water reaction chamber is placed in the chamber of the microwave reaction furnace, an annular fixer is erected on convex posts on inner wall of the waste water reaction chamber, the electrode-free lamp is inserted into a small hole of the annular fixer, a quartz stirrer is arranged in the waste water reaction chamber, and the centre shaft of the quartz stirrer is connected with an outer rotating electric machine through openings at the upper part of the waste water reaction chamber and at the upper part of the microwave reaction furnace. The present invention can prolong the service life of the electrode-free lamp, and can enhance the efficiency of photocatalytic degradation, the device has the advantages of simplicity, small occupation area and little energy consumption; a microwave function and a photocatalytic oxidation technology of ultraviolet-visible light and catalysts are synthesized, the removal rate of waste water whose organic substance concentration is smaller than 100 mg/l can reach over 90%.
Description
One, technical field
The present invention relates to the method and the device of wastewater treatment, particularly, is the ultraviolet-visible light that utilizes microwave, microwave-excitation electrodeless lamp to produce, a kind of method and apparatus of loaded with nano catalyst treatment waste water.
Two, background technology
Current, the pollutant kind and the quantity that enter in environment, the particularly water body are more and more, the threat human existence that poisonous and harmful, three causes, the organic pollutant of difficult degradation is serious.At present, the method for the chemistry of various decontaminations, physics, biology is a lot, and these methods require to have demonstrated respectively advantage separately at dissimilar pollutents and pollution control.Yet all in all, traditional treatment technology some can only make pollutent shift, and produces serious secondary pollution; Some bad adaptability, often powerless when Pollutant levels are too high or too low; And various new pollution processing and control methods, though for the removal of organic pollutant provides some original technology, as liquid-liquid extraction method, macroporous adsorbent resin method, membrane separation process, supersonic method etc., but industry such as China's papermaking at present, printing and dyeing, pharmacy, petrochemical industry and place where the garage is piled up still have a large amount of poisonous organic wastewaters to discharge, and lack efficiently, treatment process completely.
Current, microwave technology is subjected to people's generally attention.Microwave is the hertzian wave of frequency 300MHz～3006Hz.Microwave action is very special in the mode of material.At first, microwave is to the direct effect on the material molecule level, causes " the pole-changing effect " of material molecule by microwave field, makes heating (heat effect) more rapidly; Simultaneously, increased the probability of collision between reactant molecule greatly, made reactive behavior increase (non-thermal effect).Secondly, microwave action has selectivity.During microwave heating, the very fast intensification of polar material, apolar substance does not then absorb or sees through microwave.Microwave has been widely used in environmental science, successfully be used for the sterilization of clearing up of environmental sample and tap water etc. as microwave, the technology of utilizing microwave and external ultraviolet lamp photodegradation organic pollutant is also arranged, wherein, UV-light is a kind of to the highly effective energy of organic matter degradation, because ultraviolet ray has higher energy, most of chemical bond is ruptured, or combine with catalyzer, produce active substance, thereby change organic pollutant into carbonic acid gas and water, reach the purpose of decontamination.But the energy consumption of these methods is big, and the equipment complexity simultaneously, when the degraded target contaminant, may be brought new pollution again into.
In recent years, there is the scholar to utilize the microwave-excitation electrodeless lamp to produce UV-light and handles waste water, as " microwave-electrodeless ultraviolet light catalysis oxidation method for treating water " (publication number CN 1482072A), electrodeless ultraviolet lamp be applied to waste water from dyestuff degraded (Meng Xiangzhou etc. the research of electrodeless ultraviolet light degrading activity brilliant blue KN-R dye solution. Wuhan University Of Science and Engineering's journal, 2003,16 (5): 32～36), after the 40mg/L Reactive Brilliant Blue KN-R is handled 110min, percent of decolourization is 73%, and TOC removes 34%.The advantage of this method is that the electrodeless lamp that can produce UV-light does not need extra power supply that energy is provided, and, simple, the easy row of the device of microwave and ultraviolet cooperating effect.But this electrodeless lamp glimpses when being subjected to microwave-excitation, and luminous efficiency is not high, and light intensity is less, and the degraded required time is longer; And the temperature after electrodeless lamp is stimulated can reach 700～1400K, and as not lowering the temperature timely and effectively, the spectral line that is excited will broaden because of self-priming, and shortens the life-span of electrodeless lamp.
Three, summary of the invention
1, goal of the invention
The invention provides a kind of method and apparatus for the treatment of waste water by microwave photocatalysis, utilize microwave, microwave-excitation electrodeless lamp to produce the organic pollutant in ultraviolet-visible light, the loaded with nano catalyzer photochemical catalytic oxidation waste water, provide effective method and apparatus for the difficult degradation poisonous organic wastewater purifies.
2, technical scheme
The present invention proposes the method and apparatus for the treatment of waste water by microwave photocatalysis.The method for the treatment of waste water by microwave photocatalysis comprises the grid removal of impurities, staticly settles, pH regulator, and waste water carries out microwave and photo catalysis through the laggard device of going into the microwave light treating wastewater through catalysis of connected of above-mentioned preliminary treatment.
The pH value of waste water will be controlled between 2～10, and is off-limits, needs to carry out pH regulator with soda acid.Acid-alkali accommodation pH value of solution scope is 2～10.The microwave and photo catalysis of waste water is handled and is carried out in the device for the treatment of waste water by microwave photocatalysis, goes out on water (flow) direction is taked down or the enterprising mode that goes out down; The residence time of waste water in the microwave and photo catalysis reactor is 20～40 minutes, and the temperature of waste water solution remains on below 100 ℃, and pressure is normal pressure: the nanocatalyst of microwave and photo catalysis is semiconductor material TiO
2, ZnO, CdS, or the composite catalyst of oxide compound such as semiconductor material doped with Cu, Fe, Ag, Cd, Zn, Mn, Co, Ni, the mass percent of blended metal oxide is 0.1%～5.0%, and sol-gel method, chemical Vapor deposition process and solution left standstill method etc. are adopted in the preparation of nanocatalyst.
The method for the treatment of waste water by microwave photocatalysis, its principle of work is: the microwave-excitation electrodeless lamp produces ultraviolet-visible light, generates the OH or the OOH of noble potential behind irradiation nanocatalyst film surface, and the oxidation organic pollutant; Perhaps excite the ultraviolet-visible light of generation directly organism to be carried out photodegradation, realize the purification of waste water.
The device of above-mentioned treating waste water by microwave photocatalysis, comprise microwave reaction stove, waste water reaction chamber and electrodeless lamp, lay the waste water reaction chamber in the microwave reaction furnace chamber, set up annular fixer on the projection of waste water reaction chamber interior walls, electrodeless lamp inserts in the aperture of annular fixer, quartzy agitator places the waste water reaction chamber, and the opening on top, beam warp waste water reaction chamber and microwave reaction stove top links to each other with the outer buttons rotating motor in the quartzy agitator.
The device of the treating waste water by microwave photocatalysis that the present invention proposes, microwave reaction stove two side is built-in with wave guide and 5～20 magnetrons, and the power of each magnetron is 0.5～2.0kW, and microwave reaction stove inwall adopts stainless material or material nickeliferous, aluminium; Waste water reaction chamber container adopts materials such as tetrafluoroethylene, polystyrene, pottery for seeing through the material of microwave, and container upper cover is removable vent cover; The waste water reaction chamber interior walls is raised with 3～9 projections, places annular fixer on the projection, in order to fixing electrodeless lamp; The annular fixer adopts the quartz material that does not absorb UV-light, and 4～8 sizeable apertures are arranged on the annular fixer; Quartzy agitator be-coaxial multipage quartz plate, loaded with nano catalyzer on the quartz plate, and quartzy agitator not only has stirring action, also has support of the catalyst and can see through the function of UV-light, raising light utilization efficiency; The microwave non-electrode lamp is the right cylinder or the rectangular parallelepiped of quartzy hollow, and the end circular diameter of electrodeless lamp is consistent with the hole diameter on the belt fixer, and it highly is not less than 2/3 of waste water reaction chamber height; After the manufacture craft of electrodeless lamp is draws air to 2.5～5.0kPa, charge into 0.5～2.0kPa argon gas or helium, and drip 1～5 of mercury metal, finally sealed; The water-in of waste water reaction chamber links to each other with the tetrafluoroethylene water pipe with water outlet; The opening part on microwave reaction furnace side face and top all is wrapped with the aluminium cover.
Beneficial effect
The present invention compared with prior art, the microwave non-electrode lamp is dipped in the waste water solution, its surface temperature is remained at below 100 ℃ (boiling points of water), can prolong electrodeless lamp work-ing life, and the ultraviolet-visible light that electrodeless lamp produces directly acts on organic waste water, can improve photocatalytic degradation efficient; This device is simple, and floor space is few, and reaction pressure is a normal pressure, less energy consumption; Combine the photocatalysis oxidation technique of microwave action and ultraviolet-visible light, catalyzer, the organic pollutant of can the catalyzed degradation poisonous and harmful, being difficult to degrade with ordinary method, particularly phenols, dyestuff, hormone, agricultural chemicals etc., to the waste water of organic concentration less than 100mg/L, clearance reaches more than 90%.
Four, description of drawings
Fig. 1 is the inventive method schematic flow sheet.
Fig. 2 is apparatus of the present invention sectional views.
Fig. 3 is quartzy agitator structure synoptic diagram.
Fig. 4 is annular fixer vertical view.
Five, embodiment
Below further specify by example.
Preparation 50mg/L m-nitrophenol aqueous solution simulation phenolic wastewater, need not the grid removal of impurities, leave standstill back regulator solution pH3～7, phenolic wastewater enters the waste water reaction chamber [11] of 25L with the flow velocity of 1.5L/min through under meter [4] and pump [5], the waste water of speed control in making waste water reaction chamber [11] stopped 15～20 minutes, and water (flow) direction is the enterprising mode that goes out down.Microwave power 1000W after 4 electrodeless lamps [17] that are arranged in microwave field are subjected to microwave-excitation, produces ultraviolet-visible light, utilizes sol-gel method to load on Ti0 on the quartzy agitator [13]
2Nanocatalyst is subjected to the ultraviolet-visible rayed, and simultaneously, with the speed rotation of 30r/m, at this moment, phenolic wastewater solution is subjected to microwave, ultraviolet-visible light and TiO to quartzy agitator [13] simultaneously under motor [12] drives
2The effect of nanocatalyst.The steam that produces in the waste water reaction chamber [11] is discharged by upper opening, is dipped in electrodeless lamp [17] temperature in the waste water less than 100 ℃.The m-nitrophenol concentration of discharging through wastewater outlet [19] is less than 5mg/L, and TOC reduces 76%.
Preparation 50mg/L rhodamine-B aqueous solution dye wastewater, regulating the pH value is 3～7, leave standstill after under meter [4] and pump [5] enter the waste water reaction chamber [11] of 25L with the flow velocity of 1L/min, the waste water of speed control in making reaction chamber stopped 25～30 minutes, and water (flow) direction is the enterprising mode that goes out down.Microwave power 1500W is placed in after 6 electrodeless lamps [17] in the reaction chamber are subjected to microwave-excitation, produces ultraviolet-visible light, and quartzy agitator [13] is gone up load Mn/TiO
2Catalyzer, doping 0.5%, quartzy agitator externally motor [12] drive rotates with the speed of 20r/min down.Temperature in the waste water reaction chamber is less than 100 ℃, normal pressure.The concentration of rhodamine-B is less than 10mg/L in the waste water that wastewater outlet is discharged, and TOC reduces 70%.The waste water of discharging is handled [8] again through refluxing, and all the other steps are the same, and water outlet remains rhodamine-B after testing less than 1mg/L, and residue TOC is reduced to 5% of starting point concentration.
The simulation of the preparation 40mg/L dihydroxyphenyl propane aqueous solution contains environmental hormone waste water, regulate pH3～7, leave standstill after under meter [4] and pump [5] enter the waste water reaction chamber [11] of 25L with the flow velocity of 1L/min, the waste water of speed control in making reaction chamber stopped 25～30 minutes, and water (flow) direction is the enterprising mode that goes out down.Microwave power 1500W is placed in after 6 electrodeless lamps [17] are subjected to microwave-excitation in the reaction chamber, produces ultraviolet-visible light, and quartzy agitator [13] is gone up the Ni/TiO of load
2Catalyzer (doping 0.5%) is subjected to the irradiation of ultraviolet-visible light, and simultaneously, quartzy agitator externally motor [12] drive rotates with the speed of 20r/min down.Temperature in the waste water reaction chamber is less than 100 ℃, normal pressure.The concentration of dihydroxyphenyl propane is about 10mg/L in the waste water that wastewater outlet is discharged, and TOC reduces 50%.The waste water of discharging is handled [8] again through refluxing, and all the other steps are the same, and water outlet remains dihydroxyphenyl propane 2mg/L after testing, and residue TOC is 8% of a starting point concentration.
Embodiment 4
Preparation 30mg/L G-30027 aqueous solution simulation agricultural chemicals waste water, need not to filter, regulate pH 3～7, leave standstill after under meter [4] and pump [5] enter the waste water reaction chamber [11] of 25L with the flow velocity of 1L/min, the residence time of waste water in reaction chamber is 25～30 minutes, and water (flow) direction is the enterprising mode that goes out down.Microwave power 1500W has been placed in after 6 electrodeless lamps [17] are subjected to microwave-excitation in the reaction chamber, produces ultraviolet-visible light, and quartzy agitator [13] is gone up the Co/TiO of load
2Catalyzer (doping 1.0%) is subjected to the irradiation of ultraviolet-visible light, and simultaneously, externally motor [12] drive is down with the speed rotation of 20r/m for quartzy agitator, and at this moment, waste water containing pesticide solution is subjected to microwave, ultraviolet-visible light and Co/TiO simultaneously
2The effect of catalyzer.Temperature in the waste water reaction chamber is less than 100 ℃, normal pressure.The concentration of G-30027 is less than 5mg/L in the waste water that wastewater outlet is discharged, and TOC reduces 60%.The waste water of discharging is handled [8] again through refluxing, and all the other methods are the same, water outlet after testing, no G-30027 residue, remaining TOC is 5% of starting point concentration.
Certain laboratory composite waste, major ingredient is phenol, para-chlorophenol, m-nitrophenol, tropeolin-D, rhodamine-B, dihydroxyphenyl propane, nonyl phenol, G-30027, thiophos, TOC is 82mg/L before handling, through the grid removal of impurities, after leaving standstill, regulate pH3～7, the stillness of night enters the waste water reaction chamber [11] of 25L with the flow velocity of 1L/min through under meter [4] and pump [5], waste water stopped in reaction chamber 25～30 minutes, and water (flow) direction is the enterprising mode that goes out down.Microwave power 3000W inserts 8 electrodeless lamps [17] on the fixer that goes in ring, and quartzy agitator [13] is gone up loaded Cu/TiO
2Catalyzer, doping 1.0%, simultaneously, quartzy agitator speed with 20r/m under motor [12] drives is rotated.Temperature in the waste water reaction chamber is less than 100 ℃, normal pressure.Through the waste water that wastewater outlet is discharged, TOC reduces 65%.The waste water of discharging is handled [8] once again through refluxing, and residue TOC is 6% of initial soln TOC.
Certain paper mill effluent, pH=13 before handling, TOC is greater than 100mg/L, through grid removal of impurities [1], staticly settle [2], clear water diluting soln TOC to 70mg/L, pH regulator [3] regulator solution pH value is 3～7, enter the waste water reaction chamber [11] of 25L in the device for the treatment of waste water by microwave photocatalysis with the flow velocity of 1L/min through under meter [4] and pump [5], waste water stopped in reaction chamber 25～30 minutes, and water (flow) direction is the enterprising mode that goes out down.Microwave power 3000W inserts 8 electrodeless lamps [17] on the fixer that goes in ring, and quartzy agitator [13] is gone up loaded Cu/TiO
2Catalyzer, doping 1.0%, simultaneously, quartzy agitator speed with 20r/m under motor [12] drives is rotated.Temperature in the waste water reaction chamber is less than 100 ℃, normal pressure.Carry out water outlet discharging [7] through wastewater outlet, TOC reduces 50%.The waste water of discharging is handled [8] once again through refluxing, residue TOC10mg/L.
The device for the treatment of waste water by microwave photocatalysis, comprise microwave reaction stove [10], waste water reaction chamber [11] and electrodeless lamp [17], microwave reaction stove [10] is laid waste water reaction chamber [11] in the chamber, set up annular fixer [14] on the projection [18] of waste water reaction chamber [11] inwall, electrodeless lamp [17] inserts in the aperture of annular fixer [14], quartzy agitator [13] places waste water reaction chamber [11], and the opening on top, beam warp waste water reaction chamber [11] and microwave reaction stove [10] top links to each other with outer buttons rotating motor [12] in the quartzy agitator [13].Microwave reaction stove [10] two side is built-in with wave guide [16] and 10 magnetrons [15], and the power of each magnetron is 1kW, and the electrodeless lamp height is 1/2 of waste water reaction chamber [a 11] height.Quartzy agitator [13] is a coaxial multipage quartz plate, places the open circles central authorities of the fixer that goes in ring, and its axle links to each other with rotating machine [12] by the opening on waste water reaction chamber [11] and microwave reaction stove [10] top.The waste water reaction chamber interior walls is raised with 6 projections [18], and waste water reaction chamber loam cake is removable vent cover, and 6 apertures are arranged on the annular fixer [14], and electrodeless lamp [17] inserts in the aperture of annular fixer [14].After the making method of electrodeless lamp [17] is draws air to 2.5～5.0kPa, charge into rare gas elementes such as 0.5～2.0kPa argon gas, helium, and drip 1～10 of mercury metal, finally sealed.Waste water reaction chamber [11] is heat-resisting, corrosion resistant materials such as tetrafluoroethylene, polystyrene, pottery, and microwave reaction stove [10] inwall adopts stainless material or material nickeliferous, aluminium.
Claims (10)
1. the method for a treating waste water by microwave photocatalysis, comprise the grid removal of impurities, staticly settle, pH regulator, it is characterized in that waste water is through the laggard device of going into the microwave light treating wastewater through catalysis of connected of above-mentioned preliminary treatment, carry out microwave and photo catalysis, in the device of described treating waste water by microwave photocatalysis, the temperature of waste water remains on below 100 ℃, and the microwave-excitation electrodeless lamp produces ultraviolet-visible light, and the irradiation nanocatalyst, realize the purification of waste water.
2. method according to claim 1 is characterized in that the pH value of waste water is controlled at 2～10, and is off-limits, carries out pH regulator with soda acid.
3. method according to claim 2 is characterized in that the residence time of waste water in the device for the treatment of waste water by microwave photocatalysis is 20～40 minutes, and pressure is normal pressure.
4. according to each described method in the claim 1～3, the nanocatalyst that it is characterized in that microwave and photo catalysis is pure semiconductor material TiO
2, ZnO or CdS, or the composite catalyst of the material doped metal oxide of described pure semiconductor, the mass percent of blended metal oxide is 0.1%～5.0%, described metal oxide is the metal oxide of Cu, Fe, Ag, Cd, Zn, Mn, Co or Ni.
5. method according to claim 1, the device of wherein said treating waste water by microwave photocatalysis, comprise microwave reaction stove [10], waste water reaction chamber [11] and electrodeless lamp [17], it is characterized in that laying waste water reaction chamber [11] in microwave reaction stove [10] chamber, set up annular fixer [14] on the projection [18] of waste water reaction chamber [11] inwall, electrodeless lamp [17] inserts in the aperture of annular fixer [14], quartzy agitator [13] places waste water reaction chamber [11], and the opening on top, beam warp waste water reaction chamber [11] and microwave reaction stove [10] top links to each other with outer buttons rotating motor [12] in the quartzy agitator [13].
6. method according to claim 5, it is characterized in that microwave reaction stove [10] two side is built-in with wave guide [16] and 5～20 magnetrons [15], the power of each magnetron is 0.5～2.0kW, and the electrodeless lamp height is not less than 2/3 of waste water reaction chamber [11] height.
7. method according to claim 6, it is characterized in that quartzy agitator [13] is a coaxial multipage quartz plate, place the open circles central authorities of the fixer that goes in ring, the axle of this quartz agitator links to each other with rotating machine [12] by the opening on waste water reaction chamber [11] and microwave reaction stove [10] top.
8. according to claim 5 or 6 or 7 described methods, it is characterized in that the waste water reaction chamber interior walls is raised with 3～9 projections [18], waste water reaction chamber loam cake is removable vent cover, and 4～8 apertures are arranged on the annular fixer [14], and electrodeless lamp [17] inserts in the aperture of annular fixer [14].
9. according to claim 5 or 6 or 7 described methods, after the making method that it is characterized in that electrodeless lamp [17] is draws air to 2.5～5.0kPa, charges into 0.5～2.0kPa argon gas or helium, and drip 1～5 of mercury metal, finally sealed.
10. according to claim 5 or 6 or 7 described methods, it is characterized in that waste water reaction chamber [11] is heat-resisting, corrosion resistant material tetrafluoroethylene, polystyrene or pottery, microwave reaction stove [10] inwall adopts stainless material or material nickeliferous, aluminium.
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| CN101857283B (en) * | 2010-06-18 | 2012-07-04 | 江苏技术师范学院 | Device for treating waste water with microwave electrodeless excimer lamp and gas distributing system for lamp |
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