CN103086461A - Method for treating oxytetracycline-containing wastewater by adopting low-temperature plasma technology - Google Patents
Method for treating oxytetracycline-containing wastewater by adopting low-temperature plasma technology Download PDFInfo
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Abstract
The invention discloses a method for treating oxytetracycline-containing wastewater by adopting a low-temperature plasma technology. The method comprises the following steps of: putting the oxytetracycline-containing wastewater in a reaction vessel of a corona discharge reaction device, wherein a pin-type hollow high-voltage electrode and a plate-type grounding electrode are arranged in the reaction vessel and the water floods the plate-type grounding electrode and the pin-type hollow high-voltage electrode; introducing air into the pin-type hollow high-voltage electrode; introducing electric current input by a high-frequency electric source into the pin-type hollow high-voltage electrode to carry out corona discharge; and producing low-temperature plasma to treat the oxytetracycline-containing wastewater and degrade the oxytetracycline in the wastewater. The method disclosed by the invention has the advantages that the oxytetracycline in the wastewater is oxidized by adopting.OH produced in the high-voltage discharge and no any oxidant or catalyst is needed to be added, so that the operation is simple and the oxytetracycline removing rate is high.
Description
Technical field
The invention belongs to field of waste water treatment, be specifically related to a kind of lower temperature plasma technology that adopts and process the method containing terramycin wastewater.
Background technology
Terramycin (ocytetracycline, OTC) is a kind of tetracycline antibiotics, as antiseptic-germicide and somatomedin, is extensively hanged down and is applied in treatment and herding and aquaculture.Yet because its waste water is the organic waste water that a kind of high chroma, difficult degradation and bio-toxicity are higher, when a large amount of directly discharge meeting serious harm water body environments, at present both at home and abroad relatively less to the technology of its improvement and certain limitation arranged, therefore, study a kind of new and effective treatment technology extremely urgent.At present, the technique that terramycin is processed is main mainly with supporting technique well greatly, mostly still adopts activated sludge process and biological filter etc., and the technology of domestic current employing is mainly by following several classes:
Aerobic biological treatment process: be mainly the innovation alternative techniques of early stage traditional activated sludge process and the exploitation seventies, as biological contact oxidation process, deep well aeration, biological fluidized bed etc.But, because the terramycin trade effluent is high concentrated organic wastewater, the aerobic process water inlet time need to be diluted several times and even become hundred times stoste, and clear water, power consumption be large, cause processing cost very high, the actual treatment rate is also lower, so this technique is eliminated gradually.
Although the experimental study of anaerobe art breading terramycin wastewater is more, because its design to high efficiency anaerobic reactor, operation study are inadequate, lack the research to the contained compound anaerobe of its waste water toxic action.
Pre-treatment-anaerobic-aerobic combination process: current more common technique, but the conditional request due to its high anaerobic and aerobic reactor, higher to its construction production and equipment requirements, toxicity and the degradation characteristic of the intermediate product of fermentating metabolism lack research simultaneously, are also to enjoy to query and words all the time.
Membrane separation process and absorption rule are because mother liquor middle and high concentration organism makes film vulnerable to pollution, flux decline serious, also relatively less on using.
Photocatalysis technology is considered to a kind of less energy-consumption treatment technology that application prospect is arranged very much at present, but because its quantum yield is low, need the restricted condition such as catalyzer, range of application is also narrower.
Ozonation is comparatively obvious to the terramycin degradation effect, but has increased cost because it need to add catalyzer, uses ozone also can affect to environment simultaneously.
As can be seen here, all there is certain deficiency in the technique of at present terramycin being processed, therefore find a kind of efficient, simple, avoid the method for secondary pollution extremely urgent.In water, the Low Temperature Plasma Treating technology is a kind of high-level oxidation technology, has the advantages such as processing efficiency is high, non-selectivity, non-secondary pollution, so will likely become the developing direction that following high concentrated organic wastewater is processed.
Summary of the invention
The objective of the invention is on the basis of currently available technology, provide a kind of more efficient, operation is simpler, employing lower temperature plasma technology that secondary pollution is little is processed the method containing terramycin wastewater.
Purpose of the present invention can reach by following measures:
A kind of lower temperature plasma technology that adopts is processed the method containing terramycin wastewater, to containing the waste water of terramycin, join in the reaction vessel of corona discharge reaction unit, the inside of described reaction vessel is provided with pin type hollow high voltage electrode and plate-type grounding electrode, and the water surface did not have described plate-type grounding electrode and pin type hollow high voltage electrode, first air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing terramycin wastewater, the degraded of terramycin in waste water (is oxidized to CO by the terramycin in waste water
2, water and simple organic), the voltage peak of described high frequency electric source electric discharge is 8000 ~ 12000(AC sine waveform), current peak is 20 ~ 50mA, the discharge frequency of generation is 2.5 ~ 30kHz.
Of the present invention is laboratory simulation waste water containing terramycin wastewater, and has selected top condition for different concentration ranges.
The spacing of described pin type hollow high voltage electrode and plate-type grounding electrode is 6 ~ 10cm, is preferably 8 cm.
The described concentration containing terramycin in terramycin wastewater is 100 ~ 250mg/L, is preferably 150 ~ 200 mg/L.
Low-temperature plasma is 1 ~ 12min to the time of being processed containing terramycin wastewater, is preferably 6 ~ 10min.
The described pH containing terramycin wastewater is 2 ~ 10, is preferably 2 ~ 4 or 10 ~ 11.
The described flow that is passed into the air in described pin type hollow high voltage electrode is preferably 0.01 ~ 0.1m
3/ h, be preferably 0.01 ~ 0.05m
3/ h.
The output rating of described high frequency electric source is preferably 20 ~ 500 W.
The air be passed in described pin type hollow high voltage electrode can be dry air, can be also wet air, preferably adopts wet air.The wet air here refers to the moistening air of process from water, and the present invention is to being that the humidity of air there is no specific requirement.
The OH that the present invention utilizes electrion to produce carries out oxide treatment to the terramycin in waste water, does not need to add any oxygenant and catalyzer, simple to operate.
A kind of water treatment device that above-mentioned corona discharge reaction unit is known to the skilled person, mainly comprise high frequency electric source and the inner reaction vessel that is provided with pin type hollow high voltage electrode and plate-type grounding electrode, described high frequency electric source earthing pole with positive pole, with plate-type grounding electrode, with pin type hollow high voltage electrode, be connected respectively, the hollow structure of described pin type hollow high voltage electrode for passing into air in reaction vessel.
The mechanism of action of corona discharge is near the point electrode very large in radius-of-curvature, because local electric field strength surpasses the ionisation of gas field intensity, gas is ionized, thereby corona discharge occurs.Can see light when corona occurs around electrode, and with fizz.Cause a series of physics, chemical effect in the plasma channel injected water of energy by discharge generation, comprised the release of UV, shockwave, and free radical (OH, H, O), H
2o
2and O
3the generation of contour active substance.Plasma body ionizes liquid water molecules in airborne vaporous water molecule and solution all can produce OH, H.
beneficial effect of the present invention:
The high reactivity material that the present invention utilizes electrion to produce carries out oxide treatment to the terramycin in waste water, reaction unit is simple, easy handling, and do not need to add any oxygenant and catalyzer in reaction process, can effectively process the waste water under different condition.Meanwhile, this technology can be processed the multiple compound waste water mixed, and can significantly reduce the Pollutant levels in waste water, and final product is pollution-free, and cost is comparatively cheap.Especially can be applied to the processing of the organic waste water that current industrial high chroma, difficult degradation and bio-toxicity are higher, be acknowledged as comparatively advanced a kind of technology with thering is the development and application prospect in environmental area at present.
The accompanying drawing explanation
Fig. 1 is a kind of simple corona discharge reaction unit structural representation that this experiment adopts.
In figure, 1-high frequency electric source, 2-reaction vessel, 3-plate-type grounding electrode, 4-pin type hollow high voltage electrode, 5-air flowmeter, 6-electromagnetic air pump, 7-sealing is containing water bottle, 8-cooling water inlet, 9-cooling water outlet, 10-gas inlet, 11-ventilating pit, 12-interlayer.
Embodiment
The corona discharge reaction unit that following each embodiment adopts as shown in Figure 1, comprise high frequency electric source 1 and the inner reaction vessel 2 that is provided with plate-type grounding electrode 3 and pin type hollow high voltage electrode 4, the earthing pole of described high frequency electric source 1 with anodal respectively be located at reaction vessel 2 in plate-type grounding electrode 3 with pin type hollow high voltage electrode 4, be connected, the vertical lower that described pin type hollow high voltage electrode 4 is located in plate-type grounding electrode 3.Described reaction vessel 2 is provided with interlayer 12(for passing into water quench reaction vessel 2), water coolant enters interlayer 12 by cooling water inlet 8, by cooling water outlet 9, is flowed out.Pin type hollow high voltage electrode 4 is connected with air flowmeter 5 by pipeline, and air flowmeter 5 is connected with electromagnetic air pump 6 again, and the gas of electromagnetic air pump 6 passes into via gas inlet 10 containing water bottle 7 from sealing.
The high frequency electric source 1 adopted in the embodiment of the present invention, for the CTP-2000K discharge power supply that Nanjing Su Man Electronics Co., Ltd. produces, can be regulated by voltate regulator voltage and the power of high frequency electric source, thereby controls the electric current of output.The voltage of the high frequency electric source that voltate regulator is regulated and power range are respectively 0 ~ 220V and 0 ~ 500 W.The voltage peak of its electric discharge is 8000 ~ 12000V (AC sine waveform), and current peak is 20 ~ 50mA, and the discharge frequency of generation is 2.5kHz ~ 30kHz.
In the embodiment of the present invention, adopt synthetic glass to make cylindric reaction vessel 2, bottom surface diameter 5cm, high 10cm.Pin type hollow high voltage electrode 4 adopts No. 7 hollow draw points, connects the power supply high-pressure stage, and air enters reaction vessel by the hollow draw point.Plate type electrode (4cm
2) adopt stainless steel plate to make and ground connection.Ground-electrode is located at the needle electrode vertical direction.Reaction vessel upper bottom surface plug is made a call to two holes, and one is ventilating pit 11, another hand-hole that is plate type electrode.The bottom surface plug is directly passed by pin type hollow high voltage electrode, and gas is at first by seal strip plug wide-necked bottle, and ventpipe one end is gas inlet, and the other end of ventpipe inserts in wide-necked bottle.Can discharge water as required or not discharge water in its bottle, when discharging water, the other end of ventpipe submerges in water, so that enter the interior gas of bottle from gas inlet, becomes wet air.
In figure, the pin type high voltage electrode connects the high frequency electric source positive pole by plain conductor, and plate type electrode connects the power ground utmost point by plain conductor.Reaction vessel, under meter, electromagnetic air pump and wide-necked bottle are connected by emulsion tube.Air enters in pneumatic pump through the distilled water (increase atmospheric moisture) in wide-necked bottle, through under meter, is passed in hollow pin type high voltage electrode subsequently, finally from the outlet of reaction vessel upper end, discharges.Can control air flow quantity by under meter.In discharge process, air and waste water solution are ionized at the high voltage electrode tip, and the plasma body of generation enters in water, reacts.The active substance be not consumed is got rid of from reaction vessel upper end ventilating pit 11 with air as ozone.
The water sample that will contain terramycin passes in reaction vessel, and water sample need not have plate-type grounding electrode.The measuring method of terramycin content is that the high performance liquid chromatography that hewlette-packard is produced detects.
One, adopt different starting point concentrations to process containing the terramycin water sample
150,200,250mg/L(pH is respectively 2.82 concentration is respectively:, 2.44,2.13) pass in the reaction vessel of corona discharge reaction unit as shown in Figure 1 containing terramycin water sample 100mL, and the water surface did not have plate-type grounding electrode and pin type hollow high voltage electrode, first wet air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing the terramycin water sample, the terramycin in waste water is degraded; Output power of power supply is 64W, and the sparking voltage peak value is about 10000V, and maximum discharge current is about 30mA, and discharge frequency is about 15kHz.Pin type hollow high voltage electrode and plate type electrode spacing 8mm, air passes into reaction vessel by electromagnetic air pump 6 after humidification, and air flow quantity is 0.05m
3/ h, in the situation that discharge time 10min, the clearance of terramycin is respectively 97.32%, 92.32%, 88.84% after testing.The treatment effect that the starting point concentration that contains the terramycin water sample is 150 ~ 250mg/L all can reach more than 92%, is preferably 150 ~ 200mg/L.
Two, adopt the different reaction times to process containing the terramycin water sample
By concentration, be 200mg/L(pH=2.44) pass in the reaction vessel of corona discharge reaction unit as shown in Figure 1 containing terramycin water sample 100mL, and the water surface did not have plate-type grounding electrode and pin type hollow high voltage electrode, first wet air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing the terramycin water sample, the terramycin in waste water is degraded; Output power of power supply is 64 W, and the sparking voltage peak value is about 10000V, and maximum discharge current is about 30mA, and discharge frequency is about 15kHz.Pin type hollow high voltage electrode and plate type electrode spacing 10mm, air passes into reaction vessel by electromagnetic air pump 6 after humidification, and air flow quantity is 0.05 m
3/ h, in the situation that different discharge time be: 2,4,6,8,10min, the clearance of terramycin is respectively 39.87%, 63.44%, 77.22%, 86.48% and 92.68% after testing.The treatment effect that reaction times is 6 ~ 12min all can reach more than 70% or 70%.
Three, adopt different output ratings to process containing the terramycin water sample
By concentration, be 200mg/L(pH=2.44) pass in the reaction vessel of corona discharge reaction unit as shown in Figure 1 containing terramycin water sample 100mL, and the water surface did not have plate-type grounding electrode and pin type hollow high voltage electrode, first wet air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing the terramycin water sample, the terramycin in waste water is degraded; Output power of power supply is respectively 32,64,80W, and the sparking voltage peak value is about 10000V, and maximum discharge current is about 30mA, and discharge frequency is about 15kHz.Needle electrode and plate type electrode spacing 8mm, air passes into reaction vessel by pneumatic pump after humidification, and air flow quantity is 0.05m
3/ h, in the situation that be 10min discharge time, the clearance of terramycin is respectively 79.13%, 92.25%, 98.44% after testing.
Four, adopt different pH values to process containing the terramycin water sample
The terramycin water sample 100mL that is 200mg/L by concentration passes in the reaction vessel of corona discharge reaction unit as shown in Figure 1, and the water surface did not have plate-type grounding electrode and pin type hollow high voltage electrode, first wet air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing the terramycin water sample, the terramycin in waste water is degraded; The adjustment pH value of solution is: 4,7,10, and output power of power supply is respectively 64W, and the sparking voltage peak value is about 10000V, and maximum discharge current is about 30mA, and discharge frequency is about 15kHz.Needle electrode and plate type electrode spacing 8mm, air passes into reaction vessel by pneumatic pump after aqueous solution humidification, and air flow quantity is 0.05m
3/ h, in the situation that be 10min discharge time, the clearance of terramycin is respectively 85.25%, 80.50%, 87.45% after testing.When approaching neutrality, the clearance of terramycin is slightly low.Acid or alkaline solution is conducive to improve the clearance of terramycin.
Five, adopt different air flow quantitys to process containing the terramycin water sample
By concentration, be 200mg/L(pH=2.44) terramycin water sample 100mL pass in the reaction vessel of corona discharge reaction unit as shown in Figure 1, and the water surface did not have plate-type grounding electrode and pin type hollow high voltage electrode, first wet air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing the terramycin water sample, the terramycin in waste water is degraded; Output power of power supply is respectively 64W, and the sparking voltage peak value is about 10000V, and maximum discharge current is about 30mA, and discharge frequency is about 15kHz.Needle electrode and plate type electrode spacing 8mm, pass into reaction vessel by pneumatic pump after air moistening, and air flow quantity is respectively 0.02,0.05,0.1m
3/ h, in the situation that be 10min discharge time, the clearance of terramycin is respectively 89.03%, 92.28%, 94.80% after testing.
embodiment 1
Select top condition and carry out wastewater treatment: be 200mg/L(pH=2.44 by concentration) terramycin water sample 100mL pass in the reaction vessel of corona discharge reaction unit as shown in Figure 1, and the water surface did not have plate-type grounding electrode and pin type hollow high voltage electrode, first wet air is passed in described pin type hollow high voltage electrode, then the electric current that high frequency electric source is inputted passes into described pin type hollow high voltage electrode and carries out corona discharge, produce low-temperature plasma to being processed containing the terramycin water sample, the terramycin in waste water is degraded; Output power of power supply is respectively 64W, and the sparking voltage peak value is about 10000V, and maximum discharge current is about 30mA, and discharge frequency is about 15kHz.Needle electrode and plate type electrode spacing 8mm, pass into reaction vessel by pneumatic pump after air moistening, and air flow quantity is respectively 0.05m
3/ h, in the situation that be 10min discharge time, the clearance of terramycin is 92.35% after testing, the clearance of process test of many times terramycin under these processing condition is more than 92%, effect stability, and the terramycin clearance is high.
Compare aerobic biological treatment process and anaerobe technique, this experiment reaction times is short, process identical waste water, obvious processing effect, the capital cost of this experiment simultaneously is lower, greatly reduces expected cost, and processing is workable, can according to the water inlet waste water different appropriate change parameters, thereby reach good treatment effect.
Compare membrane separation process, the final product environmentally safe of the method, effect is remarkable, cost is low, to equipment require low, workable.
Compare Ozonation and photocatalysis technology, react without any need for catalyzer, obvious processing effect, cost is lower by contrast, and needs to add catalyzer in Ozonation and photocatalysis technology reaction, and the concentration numbers magnitude of processing is generally all 10
-2below, and the general treatment time more than one hour, treatment effect also is difficult to reach more than 90%.
Therefore, in current terramycin treatment technology, the Low Temperature Plasma Treating technology combines multiple advantage, is with a wide range of applications, and this technology is also the following leading trend at environmental technology field simultaneously.
Claims (8)
1. one kind adopts lower temperature plasma technology to process the method containing terramycin wastewater, it is characterized in that containing the waste water of terramycin, joining in the reaction vessel of corona discharge reaction unit, be provided with pin type hollow high voltage electrode and plate-type grounding electrode in described reaction vessel, and the water surface did not have described plate-type grounding electrode and pin type hollow high voltage electrode, first air is passed in described pin type hollow high voltage electrode, then the electric current of high frequency electric source input is passed into to described pin type hollow high voltage electrode and carry out corona discharge, produce low-temperature plasma to being processed containing terramycin wastewater, terramycin in waste water is degraded, the voltage peak of described high frequency electric source electric discharge is 8000 ~ 12000, and current peak is 20 ~ 50mA, and the discharge frequency of generation is 2.5 ~ 30kHz.
2. employing lower temperature plasma technology according to claim 1 is processed the method containing terramycin wastewater, it is characterized in that the spacing of described pin type hollow high voltage electrode and plate-type grounding electrode is 6 ~ 10cm, is preferably 8 cm.
3. employing lower temperature plasma technology according to claim 1 is processed the method containing terramycin wastewater, it is characterized in that the described concentration containing terramycin in terramycin wastewater is 100 ~ 250mg/L, is preferably 150 ~ 200 mg/L.
4. employing lower temperature plasma technology according to claim 1 is processed the method containing terramycin wastewater, it is characterized in that low-temperature plasma is 1 ~ 12min to the time of being processed containing terramycin wastewater, is preferably 6 ~ 10min.
5. employing lower temperature plasma technology according to claim 1 is processed the method containing terramycin wastewater, it is characterized in that the described pH containing terramycin wastewater is 2 ~ 10, is preferably 2 ~ 4 or 10 ~ 11.
6. employing lower temperature plasma technology according to claim 1 is processed the method containing terramycin wastewater, it is characterized in that the described flow that is passed into the air in described pin type hollow high voltage electrode is 0.01 ~ 0.2m
3/ h, be preferably 0.02 ~ 0.1m
3/ h.
7. employing lower temperature plasma technology according to claim 1 is processed the method containing terramycin wastewater, and the output rating that it is characterized in that described high frequency electric source is 20 ~ 500 W.
8. process the method containing terramycin wastewater according to the described employing lower temperature plasma technology of claim 1 or 6, it is characterized in that the described air be passed in described pin type hollow high voltage electrode is wet air.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310678A (en) * | 2014-10-17 | 2015-01-28 | 南京大学 | Continuous catalytic plasma water pollution purification device |
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| CN104671357A (en) * | 2015-01-26 | 2015-06-03 | 南京大学 | Method for degrading dimethyl phthalate by virtue of cooperation of low-temperature plasma and bismuth tungstate catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310678A (en) * | 2014-10-17 | 2015-01-28 | 南京大学 | Continuous catalytic plasma water pollution purification device |
| CN104310678B (en) * | 2014-10-17 | 2016-01-20 | 南京大学 | A kind of continous way catalyze plasma water pollutions refining plant |
| CN104445812A (en) * | 2014-11-14 | 2015-03-25 | 中原工学院 | Treatment method of waste liquor obtained after alcohol mother liquor purifying in doxycycline hydrochloride production |
| CN104445812B (en) * | 2014-11-14 | 2016-04-27 | 中原工学院 | The treatment process of the rear waste liquid of ethanol mother liquor purification in Vibramycin hydrochloride production |
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| CN105036251A (en) * | 2015-06-26 | 2015-11-11 | 南京大学 | Device for efficiently degrading high-concentration organic polluted wastewater by corona discharge plasma |
| CN105174415A (en) * | 2015-10-10 | 2015-12-23 | 北京阳光欣禾科技有限公司 | Plasma advanced oxidation complete technology for waste water treatment |
| CN106746078A (en) * | 2016-12-14 | 2017-05-31 | 合肥工业大学 | A kind of pretreatment unit of high concentration organism P wastewater |
| CN111470592A (en) * | 2020-04-15 | 2020-07-31 | 中国人民解放军军事科学院防化研究院 | Device for degrading hazardous chemical substances by single-needle-plate gas-liquid underwater discharge plasma |
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