CN101863526A - Method and device for degrading pollutants through ultraviolet catalytic wet oxidation - Google Patents
Method and device for degrading pollutants through ultraviolet catalytic wet oxidation Download PDFInfo
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Abstract
The invention discloses a method for rapidly and efficiently degrading pollutants through ultraviolet catalytic wet oxidation at the normal temperature and normal pressure and designs a typical device for implementing the method. In the method, ultraviolet light, an oxidant and a catalyst are introduced into a reaction system; and a wet oxidation reaction can be performed under the mild conditions of normal temperature and normal pressure by utilizing the synergistic catalytic oxidation of the ultraviolet light, the oxidant and the catalyst. Compared with the traditional catalytic wet oxidation method which needs to be implemented under the reaction conditions of high temperature and high pressure, the method can be implemented under the conditions of a temperature of between 25 and 80 DEG C and normal pressure, wherein organic pollutants in high-concentration toxic and hazardous waste water can be decomposed to be harmless components such as carbon dioxide (CO2), water and the like through the high oxidizing property; and the removal rate of chemical oxygen demand (COD) chromium (Cr) after the treatment of a plurality of representative high-concentration organic waste water can reach over 95 percent, and the biochemical property can be improved obviously. The method has the advantages of mild reaction, high treating efficiency, complete degradation, clean and environmental-friendly process, energy conservation and wide application prospect.
Description
Technical field
The present invention discloses a kind of method for oxidation and device, and particularly a kind of Catalytic Wet Oxidation method and device that adopts ultraviolet to strengthen is used for sewage treatment area, particularly is applied to the removal of organic pollutant in the high density poisonous and harmful waste water.
Background technology
Along with the develop rapidly of industry such as oil, chemical industry and pharmacy, the handling problem of high-concentration hardly-degradable waste water becomes the focus and the difficult point of countries in the world research.At present, trade effluent has had new characteristics: Pollutant levels are higher on the one hand; Pollutant component is more complicated on the other hand, and this just causes traditional pollutent method of wastewater treatment efficiency to reduce, and adopts the pollutent waste water of handling high density, difficult degradation such as methods such as Coagulation Method, biochemical process, absorption method, physico-chemical process, is difficult to reach emission standard.Therefore, the research of new and effective wastewater processing technology is extremely urgent.
Wet type air oxidation technology (Wet Air Oxidation, be called for short WAO) be under high temperature (150-350 ℃) and high pressure (0.5-20MPa), as oxygenant, is the chemical process of inorganicss such as carbonic acid gas and water or organic molecule with the organic pollutant oxygenolysis with air or pure oxygen.Nineteen forty-four, the F.J.Zimmermann of the U.S. proposed the WAO technology, also claimed the Annemarie Zimmermann method.First WAO being used to handle papermaking black liquor wastewater in 1958, is 150-350 ℃ in temperature of reaction, and pressure is under the 5-20MPa condition, waste water COD
CrDegradation rate reaches more than 90%.
Although WAO is the technology of a kind of effective processing high density, poisonous and harmful, bio-refractory organic waste water, but because it carries out under High Temperature High Pressure, inevitably have a lot of weak points: (1) because reaction requires to carry out under high temperature, highly compressed condition, operation easier is big, poor stability; (2) require reactor material to have high temperature resistant, highly compressed characteristic, not only make the device systems one-time investment big, and the selection of the system of giving causes difficulty; (3) owing to must keep the reaction conditions of high temperature and high pressure, running cost costliness in the reaction.Higher reaction pressure also can increase the power consumption of air compressor machine in addition, increases the regular job expense of this process; 4) even under very high temperature, to some organism such as polychlorobiphenyl, the removal effect of small molecules carboxylic acid is also undesirable, is difficult to accomplish complete oxidation.Therefore, for the improvement of traditional WAO technology with improve extremely important.
Because there is above defective in the WAO technology, along with the progress of pollutent wastewater processing technology, based on the WAO technology, some new wet-type oxidation degradation methods have appearred again, catalyzer is incorporated in this field, formed a kind of new technology---Catalytic Wet Oxidation technology (Catalytic Wet Oxidation is called for short CWO), by adding suitable catalyzer in reaction process, temperature of reaction and pressure are reduced, can effectively improve oxidative decomposition capacity, fast reaction speed shortens the reaction times.Catalytic wet hydrogen peroxide oxidation technology (Catalytic Wet Peroxide Oxidation is called for short CWPO) is on the basis of catalytic wet air oxidation process, and oxygenant is replaced by H
2O
2Waste water is degraded.Though catalytic wet hydrogen peroxide oxidation technology has improved the waste water degradation rate greatly, but still need under the severe condition of High Temperature High Pressure, to carry out, do not avoid the fatal shortcoming of wet oxidation technology fully, make this The Application of Technology and popularization be subjected to very big restriction.
Summary of the invention
Carry out under the condition at the above-mentioned wet oxidation Technology Need High Temperature High Pressure of mentioning of the prior art, the shortcoming that requirement condition is relatively harsher, the invention provides a kind of new wet oxidation method, it utilizes ultraviolet ray as intensified condition, add catalyzer and carry out wet oxidation, this high-level oxidation technology can be carried out at normal temperatures and pressures, and for realizing that this method has designed a kind of exemplary device.
In order to solve the problem of conventional catalyst wet oxidation technology degradation condition harshness, ultraviolet catalytic wet-type oxidation technology (UV-Catalytic Wet Oxidation Process is called for short UV-CWOP) has been proposed.Process characteristic is by introduce UV-light, oxygenant and catalyzer (one or more appraise at the current rate transition metal or metal oxide) in reaction system, with their concerted catalysis oxygenizement, under the mild conditions of normal temperature and pressure, organic pollutant in the high density poisonous and harmful waste water is resolved into CO
2With harmless composition such as water, and deodorizing simultaneously, decolouring and sterilization and disinfection, thereby reach the purpose of purifying liquid waste.
The technical scheme that the present invention solves its technical problem employing is: a kind of method of degrading pollutants through ultraviolet catalytic wet oxidation, method for oxidation comprise following reaction conditions:
A, the pH value of waste water is adjusted to certain limit,, it is adjusted to a certain numerical value between the 3-10 according to the catalyst type difference according to the characteristic of waste water characteristic and catalyzer;
The original COD of B, the pending waste water of foundation
CrValue adds oxygenant;
C, add catalyzer according to oxidant content, the mol ratio of catalyzer and oxygenant is 1: 5-1: between 200;
D, UV-irradiation is arranged;
E, temperature of reaction are 25 ℃-80 ℃;
F, reaction pressure are normal pressure;
G, reaction times are 5-300min.
A kind of device of realizing aforesaid method, this device comprises the reaction tank that splendid attire waste water is used, be provided with ultraviolet source in the reaction tank, the reaction tank bottom is provided with aerating apparatus, the reaction tank top is provided with and is used for the medicine storage tank that storage catalyst is used, and also is provided with the chemicals dosing plant that is communicated with the medicine storage tank in the reaction tank, is provided with control device in the reaction tank, be provided with measuring cell in the reaction tank, the reaction tank outside is equipped with the liquid level instrument.
The technical scheme that the present invention solves its technical problem employing further comprises:
Described catalyzer is the combination of one or more appraise at the current rate transiting state metal ion or oxide compounds.
The described transiting state metal that appraises at the current rate is copper, iron, manganese or zinc.
Described catalyzer adopts a kind of as carrier in aluminum oxide, titanium dioxide, silica gel or the gac.
Described oxygenant is one or more the combination in air, oxygen, ozone, hydrogen peroxide, the Peracetic Acid.
Described method is according to the difference of catalyzer form, and reaction can be a homogeneous phase or heterogeneous.
Described reaction tank material adopts corrosion resistant material.
Described ultraviolet source is low pressure ultraviolet lamp or middle pressure ultraviolet lamp.
Kind of waste water among the present invention comprises organic used water difficult to degradate such as electroplating wastewater, printing ink wastewater, surface active agent wastewater, dyeing waste water, phenolic wastewater;
The invention has the beneficial effects as follows: (1) needs to compare with the reaction conditions of high pressure (0.5-20MPa) at high temperature (150-350 ℃) with the conventional catalyst wet oxidation process, the inventive method is because the introducing of ultraviolet ray and catalyzer can make wet oxidation reaction carry out under the mild conditions of normal temperature and pressure.
(2) catalyzer of the present invention is the transiting state metals that appraise at the current rate such as Cu, Fe, Mn, Zn, is the common industrial catalystic material, and wide material sources are cheap.After catalyzed reaction finished, particle shape catalyzer was realized separating of catalyzer and waste water easily, can reclaim it, was difficult for running off.
(3) oxygenant of the present invention is one or more the combination in air, oxygen, ozone, hydrogen peroxide, the Peracetic Acid, and low price is easy to use.In addition because the adding of UV-light makes the utilization ratio of oxygenant obviously improve, so with traditional Catalytic Wet Oxidation reacting phase ratio, the throwing amount of having saved oxygenant.
(4) introduce UV-light and catalyzer in the reaction system simultaneously, utilize their concerted catalysis oxygenizement, organic pollutant in the high density poisonous and harmful waste water is resolved into CO
2With harmless compositions such as water, and has the effect of deodorizing, decolouring and sterilization and disinfection simultaneously.
To sum up, the method for the invention technology have reaction temperature and, processing efficiency height, degraded thoroughly, the technology cleaning is green and save plurality of advantages such as the energy, has very high practical value, have a extensive future.
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is a structural principle synoptic diagram of the present invention.
Among the figure, 1-reaction tank, 2-ultraviolet source, 3-aerating apparatus, 4-chemicals dosing plant, 5-medicine storage tank, 6-housing, 7-panel, 8-measuring cell, 9-liquid level instrument, 10-water-in, 11-water outlet.
Embodiment
Present embodiment is the preferred embodiment for the present invention, and other all its principles are identical with present embodiment or proximate with basic structure, all within protection domain of the present invention.
Please referring to accompanying drawing 1, main body of the present invention is a reaction tank 1, and reaction tank 1 is used for splendid attire waste water and waste water is handled, in the present embodiment, reaction tank 1 adopts corrosion resistant material to process, and makes it be difficult for by the corrosion of the chemical substance in the waste water and has certain heat resistance.Be provided with ultraviolet source 2 in the reaction tank 1, in the present embodiment, ultraviolet source 2 is low pressure ultraviolet lamp or middle pressure ultraviolet lamp.Reaction tank 1 bottom is provided with aerating apparatus 3, the waste water that is used in reaction tank 1 feeds oxidation gas, as air, oxygen etc., reaction tank 1 top is provided with and is used for the medicine storage tank 5 that storage catalyst is used, be placed with catalyzer in the medicine storage tank 5, also be provided with chemicals dosing plant 4 in the reaction tank 1, can be by chemicals dosing plant 4 with in the waste water in the input of the catalyzer in the medicine storage tank 5 reaction tank 1.Reaction tank 1 is provided with housing 6, in the present embodiment, adopts PLC as control device, and PLC is arranged in the housing 6, and for easy to operate, reaction tank 1 is provided with panel 7, and panel 7 and housing 6 interior PLC are connected, and can carry out parameter input etc. by panel 7.Be provided with measuring cell 8 in the reaction tank 1, can be by meter etc. at measuring cell 8 places to reaction pressure, temperature, pH value, redox potential, the isoparametric on-line monitoring constantly of specific conductivity, reaction tank 1 outside is equipped with liquid level instrument 9, by the constantly monitoring of liquid level instrument 9 realizations to liquid level.
Ultraviolet catalytic wet oxidation method among the present invention, method for oxidation comprises following reaction conditions:
A, the pH value of waste water is adjusted to certain limit according to the characteristic of waste water characteristic and catalyzer, according to the catalyst type difference, it is adjusted to a certain numerical value between the 3-10, and this numerical value is by the pH stability and the interval decision of preferable catalytic activity pH of catalyst themselves;
The original COD of B, the pending waste water of foundation
CrValue adds oxygenant, and in the present embodiment, oxidant content is by COD in the waste water
CrValue is calculated 0.5-1.1 times of the theoretical consumption of gained, in addition, complexity according to the degraded of contaminated wastewater thing, the oxygenant consumption is also different, when it more needs more oxygenant during difficult degradation, in the present embodiment, oxygenant can be selected one or more the combination in air, oxygen, ozone, hydrogen peroxide, the Peracetic Acid for use;
C, add catalyzer according to oxidant content, the mol ratio of catalyzer and oxygenant is 1: 5-1: between 200, in the present embodiment, catalyzer is the combination of one or more appraise at the current rate transiting state metal ion or oxide compounds, the transiting state metal that appraises at the current rate specifically can be selected copper, iron, manganese or zinc for use, in the present embodiment, catalyzer can adopt a kind of as carrier in aluminum oxide, titanium dioxide, silica gel or the gac;
D, UV-irradiation (in the present embodiment, promptly opening ultra-violet lamp) is arranged;
E, temperature of reaction are 25 ℃-80 ℃;
F, reaction pressure are normal pressure;
G, reaction times are 5-300min.
In the inventive method, according to the difference of catalyzer form, reaction can be a homogeneous phase or heterogeneous.When catalyzer adopted metal oxide, reaction system was heterogeneous, promptly contains suspended solids in the reaction soln; When catalyzer adopted metal ion, reaction system was a homogeneous phase, does not promptly contain suspended solids in the reaction soln.
In the method for the present invention, pass through before the qualified discharge to filter or coagulating sedimentation Separation and Recovery catalyzer.
Below will the present invention will be further described with several specific exampless:
Example one: adopt the present invention's nitrification copper of degrading to electroplate useless tank liquor:
Get 4 liters of certain Electroplate Factory actual nitrification copper electroplating wastewaters (through measuring its COD
CrConcentration is 10032mg/L) put into reaction tank 1, regulate pH value to 7, and adding concentration is that 30% hydrogen peroxide (makes H
2O
2Concentration is 10g/L) and self-control Cu be nanocatalyst (making concentration is 5g/L), adopt the mechanical stirring mode to stir, open the 80W ultraviolet lamp and start reaction, carry out oxidative degradation.The COD of different degradation times
CrMeasurement result shows that the reaction times is that the CODCr degradation rate of 30min, 90min and 150min sample is respectively 18.2%, 49.1%, 99.1%, last water outlet COD
CrBe 90.3mg/L.
If other conditions are the same, but turn off ultraviolet lamp, the COD of 30min, 60min and 150min sample
CrDegradation rate is respectively 6.1%, 15.4%, 21.5%, is starkly lower than method of the present invention.
Example two: adopt the present invention's printing ink wastewater of degrading:
Get a certain amount of certain actual printing ink waste water (its COD of Electroplate Factory
CrConcentration is 26192mg/L), regulate pH value to 3.5 and carry out the pre-treatment of acid out coagulating sedimentation, get 4L supernatant liquor (its COD afterwards
CrConcentration is 10372mg/L) put into reactor, and add 30% hydrogen peroxide and (make H
2O
2Concentration is 10g/L) and self-control Fe, Cu be ionic catalyst (making Fe, Cu content be respectively 1g/L and 0.5g/L), adopt the air aeration of 50L/min, open the 80W ultraviolet lamp and start reaction, carry out oxidative degradation.The COD of different degradation times
CrMeasurement result shows that the reaction times is the COD of 30min, 90min and 120min sample
CrDegradation rate is respectively 30.6%, 85.0%, 99.6% last water outlet COD
CrBe 41.5mg/L.In addition, BOD behind the processing 90min
5/ CODcr rises to 0.36 from 0.21 of former water, and biodegradability obviously improves.
Example three: adopt the present invention's surface active agent wastewater of degrading:
Get 4 liters of certain Electroplate Factory's surface active agent wastewater (its COD
CrConcentration is 12032mg/L) put into reactor, regulate pH value to 6.5, and add Peracetic Acid (making concentration is 11g/L), self-control Fe, P are granule type nanocatalyst (making concentration is 2.5g/L), the air aeration of employing 50L/min, open the 80W ultraviolet lamp and start reaction, carry out oxidative degradation.The CODCr measurement result of different degradation times shows that the reaction times is the COD of 30min, 90min and 150min sample
CrDegradation rate is respectively 18.2%, 49.1%, 99.8%, last water outlet COD
CrBe 24.1mg/L; After handling 90min, sampling records BOD
5/ CODcr rises to 0.35 from 0.12 of former water, and biodegradability obviously improves.
If other conditions are the same, but turn off ultraviolet lamp, the COD of 30min, 60min and 150min sample
CrDegradation rate is respectively 6.1%, 15.4%, 21.5%, is starkly lower than the inventive method.In addition, catalyzer can reclaim once more and utilize, and experimental data shows that repeated use can not reduce catalyst activity.
Example four: adopt the present invention's sulfation copper plating tank liquid of degrading:
Get 4 liters of certain Electroplate Factory actual sulfation copper electroplating wastewaters (its COD concentration is 28350mg/L) and put into reactor, regulate pH value to 7, and add 30% hydrogen peroxide (making concentration is 20g/L), self-control loading type particulate state Fe, P are nanocatalyst (making concentration be 2.5g/L), adopt the O that contains of 50L/min
3Air aeration is opened the 80W ultraviolet lamp and is started reaction, carries out oxidative degradation.The COD of different degradation times
CrMeasurement result shows that the reaction times is the COD of 60min, 120min and 240min sample
CrDegradation rate is respectively 20.2%, 48.3%, 99.7%, last water outlet COD
CrBe 85mg/L.In addition, this catalyzer can reclaim once more and utilize, and experimental data shows that repeated use can not reduce catalyst activity.
Claims (10)
1. the method for a degrading pollutants through ultraviolet catalytic wet oxidation is characterized in that, described method comprises following reaction conditions:
A, the pH value of waste water is adjusted to certain limit,, it is adjusted to a certain numerical value between the 3-10 according to the catalyst type difference according to the characteristic of waste water characteristic and catalyzer;
The original COD of B, the pending waste water of foundation
CrValue adds oxygenant;
C, add catalyzer according to oxidant content, the mol ratio of catalyzer and oxygenant is 1: 5-1: between 200;
D, UV-irradiation is arranged;
E, temperature of reaction are 25 ℃-80 ℃;
F, reaction pressure are normal pressure;
G, reaction times are 5-300min.
2. the method for degrading pollutants through ultraviolet catalytic wet oxidation according to claim 1, it is characterized in that: described catalyzer is the combination of one or more appraise at the current rate transiting state metal ion or oxide compounds.
3. the method for degrading pollutants through ultraviolet catalytic wet oxidation according to claim 2, it is characterized in that: the described transiting state metal that appraises at the current rate is copper, iron, manganese or zinc.
4. according to the method for claim 1 or 2 or 3 described degrading pollutants through ultraviolet catalytic wet oxidation, it is characterized in that: described catalyzer adopts a kind of as carrier in aluminum oxide, titanium dioxide, silica gel or the gac.
5. according to the method for claim 1 or 2 or 3 described degrading pollutants through ultraviolet catalytic wet oxidation, it is characterized in that: described oxygenant is one or more the combination in air, oxygen, ozone, hydrogen peroxide, the Peracetic Acid.
6. the method for degrading pollutants through ultraviolet catalytic wet oxidation according to claim 1, it is characterized in that: waste water comprises organic used water difficult to degradate such as electroplating wastewater, printing ink wastewater, surface active agent wastewater, dyeing waste water or phenolic wastewater;
7. according to the method for claims 1 or 3 described degrading pollutants through ultraviolet catalytic wet oxidation, it is characterized in that: according to the difference of catalyzer form, reaction can be a homogeneous phase or heterogeneous.
8. device of realizing the method for claim 1, it is characterized in that: described device comprises the reaction tank that splendid attire waste water is used, be provided with ultraviolet source in the reaction tank, the reaction tank bottom is provided with aerating apparatus, the reaction tank top is provided with and is used for the medicine storage tank that storage catalyst is used, and also is provided with the chemicals dosing plant that is communicated with the medicine storage tank in the reaction tank, is provided with control device in the reaction tank, be provided with measuring cell in the reaction tank, the reaction tank outside is equipped with the liquid level instrument.
9. device according to claim 8 is characterized in that: described reaction tank material adopts corrosion resistant material.
10. device according to claim 8 is characterized in that: described ultraviolet source is low pressure ultraviolet lamp or middle pressure ultraviolet lamp.
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