CN111135770A - Experimental research device and method for generation characteristics of catalytic synergistic discharge active ingredients - Google Patents

Experimental research device and method for generation characteristics of catalytic synergistic discharge active ingredients Download PDF

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CN111135770A
CN111135770A CN201911412690.0A CN201911412690A CN111135770A CN 111135770 A CN111135770 A CN 111135770A CN 201911412690 A CN201911412690 A CN 201911412690A CN 111135770 A CN111135770 A CN 111135770A
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discharge
water
gas
voltage electrode
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CN111135770B (en
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张清阳
陈秉岩
王进华
耿镇
唐颖
马昕悦
钱俊成
蒋永锋
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Jiangsu Guowang Technology Co ltd
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Changzhou Campus of Hohai University
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Abstract

The invention discloses a device and a method for experimental research on generation characteristics of catalytic synergistic discharge active ingredients, and discloses a device and a method for experimental research on generation characteristics of discharge liquid-phase active ingredients under the coordination of ultrasound, catalysis, ultraviolet and ozone by changing input parameters of a catalytic region such as the type of gas introduced into the catalytic region and ultrasonic electric power at the bottom of a catalyst cavity. The invention utilizes the gas-liquid two-phase discharge to generate plasma to directly contact with the atomized liquid drops, increases the contact area, is more favorable for fixing nitrogen, and the liquid obtained by reaction can be directly applied to plant fertilization, and the system can stably run near the optimal energy efficiency ratio, and the fertilization is more stable and adjustable.

Description

Experimental research device and method for generation characteristics of catalytic synergistic discharge active ingredients
Technical Field
The invention relates to an experimental research device and method for generating characteristics of active ingredients of a discharge liquid phase under the synergistic effect of ultrasound, catalysis, ultraviolet and ozone by changing input parameters of a catalytic region such as the type of gas introduced into the catalytic region and ultrasonic electric power at the bottom of a catalyst cavity, and belongs to the technical field of high-voltage electrode discharge.
Background
The existing nitrogen fixation technologies include a haber method industrial ammonia synthesis technology, a synthetic nitric acid method and a chemical simulation biological nitrogen fixation method. The industrial ammonia synthesis and nitric acid synthesis methods have high energy consumption and large pollution, chemical simulation of biological nitrogen fixation is still in an experimental research stage, and the method is not put into practical application and has low yield. The natural thunder and lightning can ionize the air to generate nitrogen oxides which are dissolved in water to generate nitrate and nitrite. The nitrogen oxides can be generated by 1.6 multiplied by 10 per year in the world through lightning discharge7Ton, and the atmospheric pressure plasma discharge phenomenon is similar to natural thunder and lightning, and the discharge excites the molecular ionization to generate a series of chemical processes to generate HNO-rich gasx、NOx、·OH、H2O2、O3And O, etc.
The gas-liquid two-phase sliding arc discharge plasma technology is a novel low-temperature plasma technology, and integrates physical and chemical effects such as oxidation, acid effect, ultraviolet irradiation and the like. Gas-liquid two-phase discharge plasma in or in contact with water generates a large amount of active species (also called active species) such as HNO due to electron impact and ultraviolet radiationx、NOx、·OH、H2O2、O3And O, etc., and the active ingredients can be widely applied to the fields of agricultural production, environmental protection, material processing, biomedicine, etc. The gas-liquid two-phase sliding arc plasma has the advantages of simple structure, convenience in use, low energy efficiency and the like, and has wide prospects in the aspect of nitrogen fixation.
Disclosure of Invention
The invention provides an experimental research device and method for generating characteristics of active ingredients of a discharge liquid phase under the synergistic effect of ultrasound, catalysis, ultraviolet and ozone by changing input parameters of a catalytic region such as the type of gas introduced into the catalytic region and ultrasonic electric power at the bottom of a catalyst cavity. The technical scheme of the invention is as follows:
a high-voltage electrode discharge reactor comprises a first air inlet, a second air inlet, a first water inlet, a second water inlet, an air outlet, a water outlet, an atomizing nozzle, a cyclone blade, a metal gasket, a high-voltage electrode, a quartz tube, a catalyst cavity, a metal bottom plate, an annular ultrasonic transducer, a low-voltage electrode, a load TiO2The quartz ball and the fixing sleeve;
the discharge reactor is divided into three areas, namely an atomization area, a discharge area and a synergistic action area;
the atomizing nozzle and the area below the atomizing nozzle form an atomizing area, the first air inlet is positioned at the top of the atomizing nozzle, and the first water inlet is positioned on the side wall of the atomizing nozzle;
the metal gasket, the high-voltage electrode, the quartz tube and the low-voltage electrode form a discharge area, wherein the metal gasket is externally connected with a high-voltage power supply, the metal gasket is internally contacted with the high-voltage electrode, the low-voltage electrode is grounded to realize discharge between the two electrodes, a sealing ring and a hoop are arranged on the outer side of the metal gasket, the cyclone blade and the low-voltage electrode are coaxially arranged, are positioned right above the low-voltage electrode and are axially positioned in the center of the two metal gaskets;
the catalyst cavity, the quartz balls and the annular ultrasonic transducer at the bottom form an ultraviolet ray, ultrasonic wave and catalyst synergistic action area; the catalyst cavity is wrapped outside the quartz tube, the quartz pellets are filled inside the catalyst cavity, the annular ultrasonic transducer is located below the catalyst cavity and also wrapped outside the quartz tube, the second water inlet and the second air outlet are located at the top of the catalyst cavity, the second air inlet and the second water outlet are located at the bottom of the catalyst cavity, the metal bottom plate is located at the bottom of the catalyst cavity, and the bottom of the quartz tube is provided with the fixing sleeve.
Preferably, the low voltage electrode has a spiral structure.
Preferably, the high-voltage electrode comprises a metal sleeve, a shuttle-shaped electrode and blades, wherein the shuttle-shaped electrode is positioned in the metal sleeve, and the periphery of the shuttle-shaped electrode is connected with the inner wall of the metal sleeve through the blades in an inclined design.
Preferably, the fixing sleeve is a hollow cylinder, a plurality of screw holes for fixing the low-voltage electrode are formed in the lower portion of the side wall of the cylinder, a plurality of screw holes for adjusting the electrode spacing are formed in the upper portion of the side wall of the cylinder, and the bottom of the spiral low-voltage electrode is coaxially placed in the quartz tube after being fixed on the fixing sleeve.
Preferably, TiO of the above-mentioned quartz pellet2The loading process comprises the following steps:
selecting quartz pellets with the grain size of 0.50-5.00mm to be fired into porous quartz pellets, then immersing the pellets into butyl titanate alcohol solution, slowly lifting upwards, using a fan to blow to promote alcohol volatilization, enabling the solution to generate a titanic acid film on the surfaces of the quartz pellets, then placing the porous quartz pellets in a furnace with the temperature of 350-2A film.
An experimental research device for generating characteristics of active components of a discharge liquid phase under the coordination of ultrasound, catalysis, ultraviolet and ozone by changing input parameters of a catalytic region such as the type of gas introduced into the catalytic region and the ultrasonic electric power at the bottom of a catalyst cavity, wherein the device comprises a buffer gas chamber A, a buffer gas chamber B, a separation box, an ultrasonic power supply, an oscilloscope, a high-voltage alternating current/pulse power supply, a transformer and the high-voltage electrode discharge reactor;
the inlet of the buffer air chamber A supplies air through a plurality of air sources, and the outlet of the buffer air chamber A is connected with the first air inlet of the discharge reactor; the inlet of the buffer air chamber B supplies air through a plurality of air sources, the outlet of the buffer air chamber B is connected with a second air inlet of the discharge reactor through an air pump, the outlet of the buffer air chamber B is also connected with a separation box, a solution collected by the discharge area is placed in a water tank A in the separation box, and a solution to be detected, which is collected by the discharge area and stored in the water tank A in the separation box, is connected with a second water inlet through a liquid pump; the water to be treated in the water tank C is connected with a first water inlet through a liquid pump, a water outlet is connected with the water tank B, and the water tank B stores the solution collected by the catalytic zone;
the metal gasket is connected with the output end of a high-voltage alternating current/pulse power supply, the low-voltage electrode is grounded, discharge is carried out between the two electrodes, and the high-voltage alternating current/pulse power supply is connected with a commercial power through a transformer and is also connected with an oscilloscope; the oscilloscope is respectively connected with the high-voltage probe and the current probe to acquire voltage and current data, and the ultrasonic power supply supplies power to the annular piezoelectric transducer.
An experimental method for the generation characteristics of gas types in different catalytic regions on discharge liquid-phase active ingredients under the coordination of ultrasound, catalysis, ultraviolet rays and ozone utilizes the device, and comprises the following steps:
(7-1) setting the flow of water and gas in a discharge area;
(7-2) setting the flow rate of water and gas in the catalytic zone;
(7-3) setting the voltage of the high-voltage alternating current/pulse power supply;
(7-4) ultrasonic electric power setting;
(7-5) changing the gas species in the catalytic zone
The type of gas is selected by controlling the on-off of the valve group, and single gas or mixed gas is selected;
(7-6) active ingredient assay
After the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of active ingredients, and calculating the yield of the active ingredients in a discharge period by combining the discharge time;
(7-7) acquisition of electric signals
Collecting voltage and current signals by using a high-voltage probe and a current probe, transmitting the voltage and current signals to an oscilloscope, and storing voltage and current data;
(7-8) energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (7-7) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a full width at half maximum method; the energy efficiency ratio is obtained by dividing the generation amount of the active ingredients in one discharge period by the energy in one discharge period;
(7-9) image rendering
And then, taking the gas species introduced into the catalytic zone as an abscissa, and respectively taking the active ingredient generation amount and the energy efficiency ratio as an ordinate to draw a bar chart.
An experimental method for generating characteristics of liquid-phase active ingredients in a catalytic zone by different ultrasonic electric powers under the synergistic effect of ultrasound, catalysis, ultraviolet rays and ozone utilizes the device, and comprises the following steps:
(8-1) setting the flow of water and gas in a discharge area;
(8-2) setting the flow rate of water and gas in the catalytic zone;
(8-3) setting the voltage of the high-voltage alternating current/pulse power supply;
(8-4) ultrasonic electric Power setting
Setting an ultrasonic power supply to change ultrasonic electric power according to a well-drawn ultrasonic electric power experimental point;
(8-5) active ingredient assay
After the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of active ingredients, and calculating the yield of the active ingredients in a discharge period by combining the discharge time;
(8-6) acquisition of electric signals
Collecting voltage and current signals by using a high-voltage probe and a current probe, transmitting the voltage and current signals to an oscilloscope, and storing voltage and current data;
(8-7) energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (8-6) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a full width at half maximum method; the energy efficiency ratio is obtained by dividing the generation amount of the active ingredients in one discharge period by the energy in one discharge period;
(8-8) image rendering
And then, drawing a bar chart by taking the ultrasonic electric power as an abscissa and the active ingredient generation amount and the energy efficiency ratio as an ordinate.
The invention achieves the following beneficial effects:
patent CN102583278A discloses a device design of fixed nitrogen system nitric acid of dielectric barrier discharge, but the device utilizes and need get into secondary reactor and water reaction again after discharging and producing plasma, the fixed nitrogen inefficiency and the nitric acid solution that obtains still need have further process flow and can use, but this patent utilizes the rotatory sliding arc discharge of gas-liquid two-phase discharge to produce plasma and atomizing liquid drop direct contact, increased area of contact, be more favorable to fixed nitrogen gas, and the liquid that obtains of reaction can directly be applied to the plant fertilization.
Patent CN205812485U discloses a sliding arc discharge plasma jet device, but the strong ultraviolet energy generated by discharge is not fully utilized, the patent designs a gas-liquid two-phase rotating sliding arc discharge device, the shell of a primary reactor is a quartz tube, the strong ultraviolet generated by discharge penetrates through the quartz tube to enter a peripheral secondary reactor and is mixed with load TiO2The quartz ball catalysis of the film and the ultrasonic synergy of the bottom are more sufficient in reaction.
Patent CN105294175A discloses a slip arc discharge nitrogen fixation generating device for foliage dressing of facility agriculture, utilizes high-pressure discharge to arouse that air produces plasma and water mixture and produces nitrogenous solution, but this device combines ultrasonic system cooperative catalyst to make active ingredient concentration higher in the in-service use, and the fertilization is more stable, adjustable.
Patent CN109621715A discloses a sliding arc plasma organic matter treatment device combined with a catalyst, which utilizes high-voltage discharge to excite air to generate plasma and fill the catalyst to treat organic matter, but the device combines an ultrasonic system to cooperate with the catalyst in a secondary reactor to make the concentration of active ingredients higher and the fertilization more stable and adjustable.
Drawings
FIG. 1 is a schematic diagram of a high voltage electrode discharge reactor;
FIG. 2 is a diagram of the atomization zone of the discharge reactor;
FIG. 3 is a structural view of a quartz tube;
FIG. 4 is a block diagram of a low voltage electrode;
FIG. 5 is a structural diagram of a high voltage electrode;
fig. 6 is a structural view of the fixing sleeve;
FIG. 7 is a block diagram of the first embodiment;
FIG. 8 is a flowchart of the second embodiment;
FIG. 9 is a flowchart of the third embodiment.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
As shown in fig. 1, a high voltage electrode discharge reactor comprises a first air inlet 1, a second air inlet 2, a first water inlet 3, a second water inlet 4, an air outlet 5, a water outlet 6, an atomizing nozzle 7, a cyclone blade 8, a metal gasket 9, a high voltage electrode 10, a quartz tube 11, a catalyst cavity 12, a metal bottom plate 13, an annular ultrasonic transducer 14, a low voltage electrode 15, a load TiO 152The quartz ball 16 and the fixing sleeve 17;
the discharge reactor is divided into three areas, namely an atomization area, a discharge area and a synergistic action area;
the atomizing nozzle 7 and the area below the atomizing nozzle form an atomizing area, the first air inlet 1 is positioned at the top of the atomizing nozzle, and the first water inlet 3 is positioned on the side wall of the atomizing nozzle 7;
the discharge area is composed of a metal gasket 9, a high-voltage electrode 10, a quartz tube 11 and a low-voltage electrode 15, wherein the metal gasket is externally connected with a high-voltage power supply, the inside of the metal gasket is contacted with the high-voltage electrode 10, the low-voltage electrode 15 is grounded to realize discharge between the two electrodes, and a sealing ring 18 and a hoop 19 are arranged on the outer side of the metal gasket 9; the cyclone blade 8 is coaxially arranged with the low-voltage electrode 15, is positioned right above the low-voltage electrode 15, and is axially positioned in the center of the two metal gaskets 9.
The catalyst cavity 12, the quartz ball 16 and the annular ultrasonic transducer 14 at the bottom form an ultraviolet ray, ultrasonic wave and catalyst synergistic action area; the catalyst cavity 12 is wrapped outside the quartz tube 11, the quartz balls 16 are filled inside the catalyst cavity 12, the annular ultrasonic transducer 14 is located below the catalyst cavity 12 and also wrapped outside the quartz tube 11, the second water inlet 4 and the second air outlet 5 are located at the top of the catalyst cavity, the second air inlet 2 and the second water outlet 6 are located at the bottom of the catalyst cavity 12, the metal bottom plate 13 is located at the bottom of the catalyst cavity 12, and the bottom of the quartz tube 11 is provided with the fixing sleeve 17.
As shown in fig. 2, the atomization zone structure of the discharge reactor. The atomizing nozzle can generate water mist, the model can be selected from BD30-316SS of PNR company, the key parameter of the nozzle is the water mist cone angle theta, and the water mist is distributed in a solid cone shape. The nozzle is screwed into the upper part of the sleeve, the height from the tip to the bottom of the sleeve is h, the inner diameter of the sleeve is d, and h, d and theta have the following relations:
Figure BDA0002350389330000061
fig. 3 shows a quartz tube for placing a helical low voltage electrode with an inner diameter d.
The calculation procedure is designed for dimension d as follows:
Figure BDA0002350389330000062
Q=Ql+Qg(3)
Figure BDA0002350389330000063
Figure BDA0002350389330000064
in the above formula, v is the flow rate of water mist, Q is the total flow rate of water and gas, and Q islIs the water flow rate, QgThe air flow is, the water content is P, and the cross-sectional area of the water mist passing part is S. S is calculated by empirically determining the optimum flow rate v and the optimum Q, and d is calculated by equation (4). Keeping Q unchanged in practical experiments, and changing Ql、QgThe optimal water content can be determined by experiments by changing the water content PThe parameters allow the maximum yield of active ingredient, which is the highest.
As shown in fig. 4, the low voltage electrode 15 has a spiral structure. The material can be selected from titanium, tungsten, nickel chromium and the like. The spiral electrode is selected because the discharge area can be reduced in the discharge process of the two electrodes, which is not beneficial to discharge, and the spiral electrode can enable the electric arc to rotate quickly, which is beneficial to discharge.
As shown in FIG. 5, the high voltage electrode 10 includes a metal sleeve 10-1, a shuttle-shaped electrode 10-2 and a blade 10-3, the shuttle-shaped electrode 10-2 is located in the metal sleeve 10-1, and the periphery of the shuttle-shaped electrode is connected with the inner wall of the metal sleeve 10-1 through the obliquely designed blade 10-3.
As shown in fig. 6, the fixing sleeve is a hollow cylinder, a plurality of screw holes for fixing the low-voltage electrode are arranged below the side wall of the cylinder, a plurality of screw holes for adjusting the electrode spacing are arranged above the side wall of the cylinder, and the bottom of the spiral low-voltage electrode is coaxially placed inside the quartz tube after being fixed on the fixing sleeve. In order to further improve the generation amount of liquid-phase active ingredients in a discharge region, a catalyst cavity is designed, the catalyst cavity is of a double-layer structure and made of quartz glass, and a supported catalyst TiO is filled in the catalyst cavity2The quartz beads are used as a catalyst, ultraviolet rays generated by discharge in a gas-liquid two-phase discharge area can almost completely penetrate through quartz glass and act on the surface of the catalyst, the bottom of a catalyst cavity is an annular metal bottom plate, a metal material can select aluminum with a good ultrasonic wave conduction effect, an annular ultrasonic transducer is tightly attached to the lower part of the metal bottom plate to generate ultrasonic waves, and solution containing ozone and recycled gas containing ozone collected by the discharge area are introduced into the catalyst cavity, so that a reaction environment with synergistic effects of catalysis, ultrasound, ultraviolet and ozone is constructed, and the aim of further improving the generation amount of liquid-phase active ingredients in the discharge area is fulfilled. The catalyst is provided with four openings, namely a water inlet, a water outlet, an air inlet and an air outlet, and the inside of the catalyst is filled with loaded TiO2The quartz beads, the catalyst supported on the beads are usually titanium dioxide, and Fe-TiO can also be used2Nickel or cobalt and the like are used as catalysts, and the quartz pellets can be replaced by alumina pellets, ceramic granules, activated carbon and the like. Titanium dioxide excited by ultraviolet rays generated by electric dischargeFurther reaction to produce active particles and increase the yield of active components in liquid phase.
TiO of the above-mentioned quartz pellet2The loading process comprises the following steps:
selecting quartz pellets with the grain size of 0.50-5.00mm to be fired into porous quartz pellets, then immersing the pellets into butyl titanate alcohol solution, slowly lifting upwards, using a fan to blow to promote alcohol volatilization, enabling the solution to generate a titanic acid film on the surfaces of the quartz pellets, then placing the porous quartz pellets in a furnace with the temperature of 350-2A film.
The first embodiment is as follows:
as shown in fig. 7, an experimental study device for generating characteristics of active ingredients in a discharge liquid phase by changing input parameters of a catalytic region such as the type of gas introduced into the catalytic region, ultrasonic electric power at the bottom of a catalyst cavity and the like under the coordination of ultrasound, catalysis, ultraviolet and ozone comprises a buffer gas chamber a, a buffer gas chamber B, a separation box, an ultrasonic power supply, an oscilloscope, a high-voltage alternating current/pulse power supply, a transformer and the high-voltage electrode discharge reactor;
the inlet of the buffer air chamber A supplies air through a plurality of air sources, and the outlet of the buffer air chamber A is connected with the first air inlet of the discharge reactor; the inlet of the buffer air chamber B supplies air through a plurality of air sources, the outlet of the buffer air chamber B is connected with a second air inlet of the discharge reactor through an air pump, the outlet of the buffer air chamber B is also connected with a separation box, the separation box is used for storing the solution collected by the discharge area, and the solution collected by the discharge area and stored in the water tank A in the separation box is connected with a second water inlet through a liquid pump; the water to be treated stored in the water tank C is connected with a first water inlet through a liquid pump, a water outlet is connected with the water tank B, and the solution collected by the catalytic zone is stored in the water tank B;
the metal gasket is connected with the output end of a high-voltage alternating current/pulse power supply, the low-voltage electrode is grounded, discharge is carried out between the two electrodes, and the high-voltage alternating current/pulse power supply is connected with a commercial power through a transformer and is also connected with an oscilloscope; the oscilloscope is respectively connected with the high-voltage probe and the current probe to acquire voltage and current data, and the ultrasonic power supply supplies power to the annular piezoelectric transducer.
Water sample to be treatedBy means of a liquid pump M1Pumping into the atomizing nozzle from the water inlet of the atomizing nozzle, and using a liquid flow meter FL for water flow1And (5) monitoring. The water tank A stores the water directly subjected to the discharge treatment, and the water in the water tank A is pumped by the liquid pump M2Pumping into catalyst cavity for second reaction to increase the content of active components in water, and liquid flowmeter FL for flow rate2For monitoring, a liquid pump can be selected from Passcalpump, MG1015AD-ZWX-90/24 and the like, and a liquid flowmeter can be selected from Gems, FT-210 and the like. The cylinders 1 to n store different kinds of gas, e.g. O2、N2Ar, etc. during the test, single gas can be selected, or a plurality of gases can be selected to be mixed and introduced into the air inlet of the atomizing nozzle, wherein the valve V1-VnFor regulating the type and the respective flow of gas directly into the interior of the discharge reactor, a gas flow meter FG monitors the total flow of gas. Valve V1’-Vn’The valve V' only has on-off function, and the total flow is the gas flowmeter FG connected in series with each gas cylinder1’-FGn’The sum of the flow rates, the gas flow meter can be selected from SIARGO, MF5706 and the like. The water vapor is converted into water mist under the action of the atomizing nozzle and enters the reactor to participate in the discharge reaction. The bottom of the reactor is extended into a separation box, the lower layer of the separation box is a water tank A, the solution collected by a discharge area is stored in the water tank A, and the upper layer of the separation box contains O after reaction3Gas of equal active composition, gas pump M3And pumping the upper layer gas into the buffer gas chamber, introducing the upper layer gas into the catalyst cavity for full utilization, and selecting the gas in the gas cylinder when selecting the gas source of the catalyst cavity, or selecting the gas after reaction, or mixing the gas and the gas for use.
Method for detecting amount of active ingredient produced
The present invention detects the amount of active ingredient produced by the absorbance method. Adding a certain amount of collected solution into a color reagent, fully mixing, standing, reacting the color reagent with the detected active component, detecting with an ultraviolet-visible spectrophotometer to obtain the characteristic peak of absorbance of the resultant, the wavelength of the characteristic peak is different from that of the original detected substance, and measuring the intensity of the characteristic peakCalculating to obtain the yield of the active ingredient to be detected. The color reaction can use ozone and nitrite nitrogen color reagent of the giga-swan. In addition, the amount of active ingredient produced can be measured directly by a liquid phase concentration meter, such as a Gieser and Swan ozone meter (GDYS-101SC2), a nitrite nitrogen meter (GDYS-101SX3), and a Kyoritsu chemical-check Lab. Corp hydrogen peroxide meter (DPM-H)2O2) (ii) a The concentration of the active ingredient can also be detected by spectroscopic detection, and a detection reagent is added into the collected solution containing active ingredient after discharge to calculate the concentration value by detecting the characteristic peak value of the reaction product, and NO is usedxFor example, NOxThe characteristic peak wavelength of the product after the reaction with the special NOx detection reagent of Changchong Geigao Xiao Swan instruments ltd is 530 nm.
Example two:
an experimental method for the generation characteristics of liquid-phase active components in a catalytic zone by different types of gases in the catalytic zone under the synergistic effect of ultrasound, catalysis, ultraviolet rays and ozone utilizes the device in the first embodiment, and comprises the following steps as shown in fig. 8:
(1) parameter water and gas flow are input into a discharge area; regulating liquid pump M1Valve group V1-VnAnd setting the water and air flow in the discharge area as optimal parameters.
The optimal parameters of the water-gas mixing ratio are obtained by an experimental method of discharge active ingredient generation characteristics of different water-gas mixing ratios, and the method comprises the following steps:
(1-1) setting water flow;
the total flow of water and gas is constant, water flow and gas flow experimental points are respectively calculated according to the water-gas mixing ratio experimental points, and the water flow is adjusted to reach a calculated value;
water-gas mixing ratio experimental points: and finding a critical value of the water-gas mixing ratio which can enable the discharge reactor to normally work, determining the number of the experiments, and equally dividing the interval formed by the critical water-gas mixing ratio to obtain the water-gas mixing ratio point which is the water-gas mixing ratio experiment point.
(1-2) an air flow setting;
the total flow of water and gas is constant, the water flow and the gas flow are respectively calculated according to the experimental points of the water-gas mixture ratio, and the gas flowmeter is adjusted to reach the calculated value.
(1-3) voltage setting;
determining an optimal voltage value, and adjusting an isolation transformer to enable the power supply to output the optimal voltage; the determination of the optimum voltage value is determined by the following steps (3-1) - (3-7).
(1-4) active ingredient assay
And after the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of the active ingredients, and calculating the yield of the active ingredients in one discharge period by combining the discharge time.
(1-5) acquisition of electric signals
And collecting voltage and current signals.
(1-6) energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (1-5) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a full-width half-maximum method; the energy efficiency ratio is obtained by dividing the amount of active ingredient produced during one discharge cycle by the energy of one discharge cycle.
(1-7) image rendering
And respectively drawing a bar chart by taking the water-gas mixing ratio as an abscissa and taking the active ingredient generation amount and the energy efficiency ratio as an ordinate.
(2) Inputting parameter water and gas flow setting in the catalytic zone; regulating liquid pump M2Valve group V1’-Vn’And setting the water and air flow in the catalytic zone as optimal parameters. The optimal parameters are researched by a control variable method, and only the water flow of the catalytic zone is changed to obtain the water flow corresponding to the optimal energy efficiency ratio, namely the water flow is optimal.
(3) High voltage ac/pulsed supply voltage setting; the high voltage ac/pulsed supply voltage is adjusted to optimum parameters.
The determination of the optimum parameters is obtained by an experimental method of the active ingredient generation characteristics of different supply voltages, comprising the following steps:
(3-1) setting water flow;
respectively calculating water flow and air flow according to the optimal water-air mixing ratio and the total water-air flow, and adjusting the flow to enable the water flow to reach a calculated value;
the optimal water-gas mixing ratio is as follows: and controlling a variable method, and only changing the water-gas mixing ratio to obtain the water-gas mixing ratio corresponding to the peak value of the optimal energy efficiency ratio, namely the optimal water-gas mixing ratio.
(3-2) air flow volume setting;
and respectively calculating water flow and gas flow according to the optimal water-gas mixing ratio and the total water-gas flow, and adjusting the gas flowmeter to reach a calculated value.
(3-3) voltage setting;
and determining voltage experiment points, finding a voltage critical value which can enable the discharge reactor to normally work, determining the number of the experiments, and equally dividing intervals formed by the critical voltage points to obtain the voltage points, namely the voltage experiment points.
(3-4) detecting active ingredients;
and after the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of the active ingredients, and calculating the yield of the active ingredients in one discharge period by combining the discharge time.
(3-5) acquisition of electric signals
And collecting voltage and current signals.
(3-6) energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (3-5) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a full width at half maximum method; the energy efficiency ratio is obtained by dividing the amount of active ingredient produced during one discharge cycle by the energy of one discharge cycle.
(3-7) image rendering
And drawing a bar chart by taking the voltage as an abscissa and the active ingredient generation amount and the energy efficiency ratio as an ordinate.
(4) Ultrasonic electric power setting; the ultrasonic electric power is set to the optimum parameters. The optimal parameters are researched by a control variable method, and only the ultrasonic electric power is changed to obtain the ultrasonic electric power corresponding to the optimal energy efficiency ratio of the catalytic zone, namely the optimal parameters.
(5) Changing the gas species in the catalytic zone
By controlling valve group V1’-Vn’The gas type can be selected by switching on and off, only one valve can be opened in a single experiment, a single gas can be selected, or a plurality of valves can be opened, and a mixed gas can be selected, but the total flow of the gas is kept consistent, and the single gas is taken as an example. Besides directly using the gas in the gas cylinder, the gas in the discharge area can be recycled.
(6) Active ingredient detection
And after the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of the active ingredients, and calculating the yield of the active ingredients in one discharge period by combining the discharge time.
(7) Electrical signal acquisition
And collecting voltage and current signals by using a high-voltage probe and a current probe, transmitting the voltage and current signals to an oscilloscope, and storing voltage and current data.
(8) Energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (7) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a half-peak full-width method; the energy efficiency ratio is obtained by dividing the amount of active ingredient produced during one discharge cycle by the energy of one discharge cycle.
(9) Image rendering
And then, taking the gas species introduced into the catalytic zone as an abscissa, and respectively taking the active ingredient generation amount and the energy efficiency ratio as an ordinate to draw a bar chart.
Example three:
an experimental method for the generation characteristics of liquid-phase active ingredients in a catalytic zone by different ultrasonic electric powers under the synergistic effect of ultrasound, catalysis, ultraviolet rays and ozone utilizes the device of the first embodiment and comprises the following steps as shown in figure 9:
(1) setting water and air flow in a discharge area; regulating liquid pump M1Valve group V1-VnSetting the water and air flow in the discharge area as the optimal parameters(ii) a The optimum parameters are the same as those in the second embodiment.
(2) Setting the flow of water and gas in the catalytic zone; regulating liquid pump M2Valve group V1’-Vn’Setting the water and gas flow rate in the catalytic area as the optimal parameters; the optimum parameters are the same as those in the second embodiment.
(3) High voltage ac/pulsed supply voltage setting; adjusting the high voltage/alternating current power supply voltage to an optimal parameter; the optimum parameters are the same as those in the second embodiment.
(4) Ultrasonic electrical power settings
Setting an ultrasonic power supply to change ultrasonic electric power according to a well-drawn ultrasonic electric power experimental point;
ultrasonic electric power experimental points: selecting an ultrasonic electric power interval, determining the number of experiments, and equally dividing the interval to obtain ultrasonic electric power points which are the experimental points.
(5) Active ingredient detection
And after the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of the active ingredients, and calculating the yield of the active ingredients in one discharge period by combining the discharge time.
(6) Electrical signal acquisition
And collecting voltage and current signals by using a high-voltage probe and a current probe, transmitting the voltage and current signals to an oscilloscope, and storing voltage and current data.
(7) Energy efficiency ratio calculation
Adopting an instantaneous power method, importing the voltage and current data acquired in the step (6) into Origin for data processing, drawing a power spectrogram, and calculating the energy of one power supply period by using a full width at half maximum method; the energy efficiency ratio is obtained by dividing the amount of active ingredient produced during one discharge cycle by the energy of one discharge cycle.
(8) Image rendering
And then, drawing a bar chart by taking the ultrasonic electric power as an abscissa and the active ingredient generation amount and the energy efficiency ratio as an ordinate.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (8)

1. A high voltage electrode discharge reactor, characterized by: the discharge reactor comprises a first air inlet, a second air inlet, a first water inlet, a second water inlet, an air outlet, a water outlet, an atomizing nozzle, a cyclone blade, a metal gasket, a high-voltage electrode, a quartz tube, a catalyst cavity, a metal bottom plate, an annular ultrasonic transducer, a low-voltage electrode and a load TiO2The quartz ball and the fixing sleeve;
the discharge reactor is divided into three areas, namely an atomization area, a discharge area and a synergistic action area;
the atomizing nozzle and the area below the atomizing nozzle form an atomizing area, the first air inlet is positioned at the top of the atomizing nozzle, and the first water inlet is positioned on the side wall of the atomizing nozzle;
the discharge area is composed of a metal gasket, a high-voltage electrode, a quartz tube and a low-voltage electrode, wherein the metal gasket is externally connected with a high-voltage power supply, the inside of the metal gasket is contacted with the high-voltage electrode, the low-voltage electrode is grounded to realize discharge between the two electrodes, and a sealing ring and a hoop are arranged on the outer side of the metal gasket; the cyclone blades and the low-voltage electrode are coaxially arranged, are positioned right above the low-voltage electrode and are axially positioned in the centers of the two metal gaskets;
the catalyst cavity, the quartz balls and the annular ultrasonic transducer at the bottom form an ultraviolet ray, ultrasonic wave and catalyst synergistic action area; the catalyst cavity is wrapped outside the quartz tube, the quartz pellets are filled inside the catalyst cavity, the annular ultrasonic transducer is located below the catalyst cavity and also wrapped outside the quartz tube, the second water inlet and the second air outlet are located at the top of the catalyst cavity, the second air inlet and the second water outlet are located at the bottom of the catalyst cavity, the metal bottom plate is located at the bottom of the catalyst cavity, and the bottom of the quartz tube is provided with the fixing sleeve.
2. A high voltage electrode discharge reactor according to claim 1, wherein said low voltage electrode is a spiral structure.
3. A high-voltage electrode discharge reactor as claimed in claim 1, wherein said high-voltage electrode comprises a metal sleeve, a shuttle-shaped electrode and blades, the shuttle-shaped electrode is located in the metal sleeve, and the periphery of the shuttle-shaped electrode is connected with the inner wall of the metal sleeve through the blades which are designed to be inclined.
4. The high voltage electrode discharge reactor as claimed in claim 2, wherein said sheath is a hollow cylinder, a plurality of screw holes are provided below the side wall of the cylinder for fixing the low voltage electrodes, a plurality of screw holes are provided above the side wall of the cylinder for adjusting the electrode spacing, and the bottom of said helical low voltage electrode is coaxially placed inside the quartz tube after being fixed on the sheath.
5. A high voltage electrode discharge reactor as claimed in claim 1, characterized in that said TiO of quartz pellets2The loading process comprises the following steps:
selecting quartz pellets with the grain size of 0.50-5.00mm to be fired into porous quartz pellets, then immersing the pellets into butyl titanate alcohol solution, slowly lifting upwards, using a fan to blow to promote alcohol volatilization, enabling the solution to generate a titanic acid film on the surfaces of the quartz pellets, then placing the porous quartz pellets in a furnace with the temperature of 350-2A film.
6. A catalytic synergistic discharge active ingredient generation characteristic experimental research device is characterized in that the device comprises a buffer air chamber A, a buffer air chamber B, a separating box, an ultrasonic power supply, an oscilloscope, a high-voltage alternating current/pulse power supply, a transformer and a high-voltage electrode discharge reactor according to claim 1;
the inlet of the buffer air chamber A supplies air through a plurality of air sources, and the outlet of the buffer air chamber A is connected with the first air inlet of the discharge reactor; the inlet of the buffer air chamber B supplies air through a plurality of air sources, the outlet of the buffer air chamber B is connected with a second air inlet of the discharge reactor through an air pump, the outlet of the buffer air chamber B is also connected with a separation box, a water tank A in the separation box stores the solution collected by the discharge area, and the water tank A in the separation box is connected with a second water inlet through a liquid pump; the water to be treated in the water tank C is connected with a first water inlet through a liquid pump, a water outlet is connected with the water tank B, and the water tank B stores the solution collected by the catalytic zone;
the metal gasket is connected with the output end of a high-voltage alternating current/pulse power supply, the low-voltage electrode is grounded, discharge is carried out between the two electrodes, and the high-voltage alternating current/pulse power supply is connected with a commercial power through a transformer and is also connected with an oscilloscope; the oscilloscope is respectively connected with the high-voltage probe and the current probe to acquire voltage and current data, and the ultrasonic power supply supplies power to the annular piezoelectric transducer.
7. A method for testing the generation characteristics of liquid-phase active components in a catalytic zone by different gas species in the catalytic zone, which is characterized by using the device of claim 6, and comprising the following steps:
(7-1) setting the flow of water and gas in a discharge area;
(7-2) setting the flow rate of water and gas in the catalytic zone;
(7-3) setting the voltage of the high-voltage alternating current/pulse power supply;
(7-4) ultrasonic electric power setting;
(7-5) changing the gas species in the catalytic zone
The type of gas is selected by controlling the on-off of the valve group, and single gas or mixed gas is selected;
(7-6) active ingredient assay
After the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of active ingredients, and calculating the yield of the active ingredients in a discharge period by combining the discharge time;
(7-7) acquisition of electric signals
Collecting voltage and current signals by using a high-voltage probe and a current probe, transmitting the voltage and current signals to an oscilloscope, and storing voltage and current data;
(7-8) energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (7-7) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a full width at half maximum method; the energy efficiency ratio is obtained by dividing the generation amount of the active ingredients in one discharge period by the energy in one discharge period;
(7-9) image rendering
And then, taking the gas species introduced into the catalytic zone as an abscissa, and respectively taking the active ingredient generation amount and the energy efficiency ratio as an ordinate to draw a bar chart.
8. An experimental method for the generation characteristics of liquid-phase active ingredients in a catalytic zone by different ultrasonic electric powers is characterized in that the device of claim 6 is utilized, and the method comprises the following steps:
(8-1) setting the flow of water and gas in a discharge area;
(8-2) setting the flow rate of water and gas in the catalytic zone;
(8-3) setting the voltage of the high-voltage alternating current/pulse power supply;
(8-4) ultrasonic electric power setting;
setting an ultrasonic power supply to change ultrasonic electric power according to a well-drawn ultrasonic electric power experimental point;
(8-5) active ingredient assay
After the discharge is finished, taking a certain amount of collected solution as a water sample to be detected, detecting the generation amount of active ingredients, and calculating the yield of the active ingredients in a discharge period by combining the discharge time;
(8-6) acquisition of electric signals
Collecting voltage and current signals by using a high-voltage probe and a current probe, transmitting the voltage and current signals to an oscilloscope, and storing voltage and current data;
(8-7) energy efficiency ratio calculation
Introducing the voltage and current data acquired in the step (8-6) into Origin for data processing by adopting an instantaneous power method, drawing a power spectrogram, and calculating the energy of one power supply period by using a full width at half maximum method; the energy efficiency ratio is obtained by dividing the generation amount of the active ingredients in one discharge period by the energy in one discharge period;
(8-8) image rendering
And then, drawing a bar chart by taking the ultrasonic electric power as an abscissa and the active ingredient generation amount and the energy efficiency ratio as an ordinate.
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