CN113805614A - Ozone gas concentration control system - Google Patents
Ozone gas concentration control system Download PDFInfo
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- CN113805614A CN113805614A CN202111023287.6A CN202111023287A CN113805614A CN 113805614 A CN113805614 A CN 113805614A CN 202111023287 A CN202111023287 A CN 202111023287A CN 113805614 A CN113805614 A CN 113805614A
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 210
- 238000010790 dilution Methods 0.000 claims abstract description 137
- 239000012895 dilution Substances 0.000 claims abstract description 137
- 238000007865 diluting Methods 0.000 claims abstract description 21
- 238000001514 detection method Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000002474 experimental method Methods 0.000 abstract description 6
- 238000011160 research Methods 0.000 abstract description 6
- 230000007246 mechanism Effects 0.000 abstract description 4
- 239000005427 atmospheric aerosol Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 129
- 239000003570 air Substances 0.000 description 39
- 230000001276 controlling effect Effects 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- 238000004088 simulation Methods 0.000 description 11
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000000443 aerosol Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000006385 ozonation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D11/00—Control of flow ratio
- G05D11/02—Controlling ratio of two or more flows of fluid or fluent material
- G05D11/13—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means
- G05D11/139—Controlling ratio of two or more flows of fluid or fluent material characterised by the use of electric means by measuring a value related to the quantity of the individual components and sensing at least one property of the mixture
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- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
The invention provides a concentration control system of ozone gas, and relates to the technical field of experimental research on reaction mechanism of atmospheric aerosol. The invention provides a concentration control system of ozone gas, which comprises an ozone generating system and an ozone diluting system, wherein the ozone diluting system comprises a zero gas generator, a first diluting bottle, a second diluting bottle, a first flow limiting pipe and a second flow limiting pipe. The ozone dilution system is connected with the ozone generation system, so that high-concentration ozone generated in the ozone generation system is diluted in a dilution bottle of the ozone dilution system in a grading manner, and low-concentration ozone which can be continuously and stably output and meets the requirements of experiments is obtained.
Description
Technical Field
The invention relates to the technical field of experimental research on atmospheric aerosol reaction mechanism, in particular to the field of ozone gas concentration control, and particularly relates to a system for controlling the ozone gas concentration.
Background
Atmospheric stratospheric ozone (O)3) Is a protective layer of the earth and can prevent ultraviolet rays from radiating to the ground, however, ozone near the ground is an atmospheric pollutant and affects human health. According to GB3095-2012 Standard on ambient air quality, the daily 8-hour mean value and the hourly mean value of ozone do not exceed a maximum of 60.7ppb and 93.5ppb (second level concentration limits). In recent years, researchers have found that near-surface ozone concentrations rise, sometimes even up to several hundred ppb, photochemically to the atmosphereChemical Process, PM2.5The concentration and the formation of secondary organic aerosol both have important effects.
Therefore, in the environmental monitoring and evaluation of ozone, besides the direct observation of the instrument, it is necessary to prepare a certain concentration of ozone in research work for simulating the ozone photochemical process, controlling experimental conditions such as concentration of ozone, experimental temperature, relative humidity, etc. to study the reaction mechanism of ozone in the aerosol formation and aging process in the atmosphere.
Ozone is easy to decompose and difficult to store, and generally follows the principle of 'preparing and using at present'. The ozone generation method mainly includes a high-voltage discharge method, an ultraviolet irradiation method (also referred to as a photochemical method), an electrolytic water method, and the like. Commercially available ozone generators, such as certain types of ozone generators, utilize the principle of high voltage discharge, with narrow high voltage pulses causing the gas to discharge, resulting in a high purity oxygen (O) gas2) The process for converting to ozone has an upper limit of ozone yield of 46.7ppm/h and an upper limit of concentration of 467 ppm. The basic principle is schematically shown as follows:
O2+ energy → 2O (1)
O+O2→O3 (2)
In the common flow tube (flow tube reactor) or smoke box (smoke chamber) simulation experiment, the research is generally carried out by adopting ozone (ppb level) which is close to the atmospheric concentration level or slightly higher than the atmospheric concentration level, and the initial ozone concentration generated by a plurality of ozone generators is ppm level, so the ozone concentration generated by the equipment is high, the fluctuation is large, and the equipment cannot be directly used for the simulation experiment for exploring the chemical reaction mechanism of the aerosol; on the other hand, the direct discharge of high concentration ozone is wasteful and not an economical experimental way.
Currently available ozone calibrators prepared by an ultraviolet irradiation method can quickly and stably generate low-concentration ozone (ppb level) and are commonly used for calibrating ozone detection equipment, but are not suitable for simulation experiments which are operated for a long time, and the experiments usually continuously provide ozone for several days or even dozens of days. The ultraviolet irradiation method has disadvantages of high energy consumption and low ozone concentration, and is not an optimal method for mass production of ozone and continuous supply of ozone.
In addition, the process of preparing ozone is influenced by factors such as the type of gas source, the flow rate of the gas, the power of the ozone generator, and the stability of the instrument. Therefore, in the research work of simulation experiments using ozone, it is necessary to develop a dilution apparatus and a concentration control method for ozone gas, which can dilute high-concentration ozone generated from various ozone generators, generate low-concentration ozone (less than 300ppb) without other interference components (without impurities such as metal particles) and maintain the low-concentration ozone at a stable concentration level to meet the requirements of simulation experiments.
Disclosure of Invention
The invention mainly aims to provide a concentration control system of ozone gas, which is used for diluting high-concentration ozone (ppm level) generated in an ozone generator by low-cost carrier gas to generate low-concentration ozone (ppb level) and keeping the concentration of the ozone at a stable level, thereby ensuring that chemical reaction simulation experiments can be continuously supplied.
In order to achieve the purpose, the invention provides a concentration control system of ozone gas, which comprises an ozone generating system and an ozone diluting system, wherein the ozone diluting system comprises a zero gas generator, a first diluting bottle, a second diluting bottle, a first flow limiting pipe and a second flow limiting pipe; the first dilution bottle and the second dilution bottle are respectively provided with an ozone inlet, an ozone outlet and a zero gas inlet; the ozone generating system is connected with the ozone inlet of the first dilution bottle; the zero gas generator is respectively connected with a zero gas inlet of the first dilution bottle and a zero gas inlet of the second dilution bottle; the ozone outlet of the first dilution bottle is connected with the ozone inlet of the second dilution bottle through the first flow limiting pipe; and an ozone outlet of the second dilution bottle is connected with an air inlet end of the second flow limiting pipe, and diluted ozone is discharged through an air outlet end of the second flow limiting pipe.
In the technical scheme of the invention, high-concentration ozone (ppm level) generated in the ozone generating system enters a first dilution bottle through an ozone inlet of the first dilution bottle, meanwhile, zero gas generated by a zero gas generator of the ozone dilution system enters the first dilution bottle through a zero gas inlet of the first dilution bottle, the ozone and the zero gas are mixed in the first dilution bottle, and the ozone is diluted for the first time; the ozone after the first dilution enters a second dilution bottle through a first flow limiting pipe, meanwhile, zero gas generated by a zero gas generator of the ozone dilution system also enters the second dilution bottle through a zero gas inlet of the second dilution bottle, the ozone after the first dilution and the zero gas are mixed in the second dilution bottle, the ozone is diluted for the second time, the concentration of the ozone after the second dilution is reduced to ppb level, and the ozone can be directly used for supplying a chemical reaction simulation experiment after being discharged through the second flow limiting pipe.
As a preferred embodiment of the system for controlling the concentration of ozone gas in the present invention, the ozone outlet of the first dilution bottle is further connected to a first pressure detection system, and the first pressure detection system is connected in parallel to the first flow limiting pipe; the ozone gas outlet of the second dilution bottle is further connected with a second pressure detection system and a first screwing valve, and the second pressure detection system, the second flow limiting pipe and the first screwing valve are connected in parallel.
According to the technical scheme, the air pressure in the first dilution bottle and the air pressure in the second dilution bottle can be respectively detected through the first pressure detection system and the second pressure detection system, an operator can judge whether the air pressure in the first dilution bottle and the air pressure in the second dilution bottle meet the preset condition according to the air pressure values detected by the first pressure detection system and the second pressure detection system, and the air pressure in the first dilution bottle is required to be larger than the air pressure in the second dilution bottle.
The first screwing valve is connected with an ozone gas outlet of the second dilution bottle, the second pressure detection system, the second flow limiting pipe and the first screwing valve are connected in parallel, and the first screwing valve can control the opening and closing of the air flow. When the first screwing valve is closed, the low-concentration ozone flowing out of the air outlet of the second dilution bottle is discharged through the flow limiting pipe; when the first screwing valve is opened, because the inner diameter of the flow limiting pipe is far smaller than the pipe diameter of the first screwing valve pipeline, at the moment, the low-concentration ozone flowing out of the air outlet of the second dilution bottle is directly discharged through the first screwing valve, and at the moment, the low-concentration ozone flowing out of the air outlet of the second dilution bottle is not discharged through the flow limiting pipe.
As a preferred embodiment of the system for controlling the concentration of ozone gas according to the present invention, the zero gas inlet of the first dilution bottle and the zero gas inlet of the second dilution bottle are connected in parallel, and at least one of a mass flow controller and a solenoid valve is further provided between the zero gas generator and the zero gas inlet of the first dilution bottle and between the zero gas generator and the zero gas inlet of the second dilution bottle.
According to the technical scheme, the zero gas inlet of the first dilution bottle is connected with the zero gas inlet of the second dilution bottle in parallel, so that the zero gas generated by the zero gas generator can respectively enter the first dilution bottle and the second dilution bottle. And a mass flow controller is further arranged between the zero gas generator and the zero gas inlet of the first dilution bottle and between the zero gas generator and the zero gas inlet of the second dilution bottle, so that the flow of the zero gas entering the first dilution bottle and the flow of the zero gas entering the second dilution bottle can be controlled. It should be noted that the number of the mass flow controllers can be adjusted according to actual conditions, for example, one mass flow controller can be respectively arranged in front of the first dilution bottle and the second dilution bottle, so that the zero-gas air inlet of the first dilution bottle and the zero-gas air inlet of the first dilution bottle can be independently controlled; the first dilution bottle and the second dilution bottle can be controlled by the same mass flow controller, and at the moment, the zero-gas air inlet of the first dilution bottle and the zero-gas air inlet of the first dilution bottle have the same flow.
In addition, in order to further ensure the controllability of the zero gas, a screwing valve can be additionally arranged between the zero gas generator and the zero gas inlet of the first dilution bottle and between the zero gas generator and the zero gas inlet of the second dilution bottle, and the on-off of the zero gas flow is controlled by the switch of the screwing valve. The position of the solenoid valve can also be adjusted to the actual situation, and normally, the solenoid valve is arranged between the zero gas generator and the mass flow controller.
In a preferred embodiment of the system for controlling a concentration of ozone gas according to the present invention, the first dilution bottle and the second dilution bottle are further provided with an exhaust port, and the exhaust port is connected to a needle valve.
According to the technical scheme, the first dilution bottle and the second dilution bottle are provided with the tail gas ports, the tail gas ports are connected with the needle valves, the content and the pressure of ozone in the dilution bottles can be adjusted by adjusting the opening and closing degrees of the needle valves, and redundant ozone or diluted ozone is discharged into the tail gas. In actual operation, an operator can adjust the air pressure of the first dilution bottle and the air pressure of the second dilution bottle according to the air pressure values detected by the first pressure detection system and the second pressure detection system and by adjusting the needle valve, so that the further adjustment of the air pressure in the dilution bottle is realized. The exhausted tail gas needs to pass through a fume hood to exhaust gas so as to prevent indoor air from being polluted.
As a preferred embodiment of the ozone gas concentration control system according to the present invention, a pipe diameter of the first flow restriction pipe is smaller than a diameter of an ozone outlet of the first dilution bottle, and a pipe diameter of the second flow restriction pipe is smaller than a diameter of an ozone outlet of the second dilution bottle.
The flow limiting pipe (comprising a first flow limiting pipe and a second flow limiting pipe) is used for limiting the flow of ozone at an air outlet in the system, the pipe diameter of the flow limiting pipe is smaller than the caliber of the ozone air outlet connected with the flow limiting pipe, the concentration of gas can be further diluted, and the length and the material of the flow limiting pipe can be selected according to actual conditions.
As a preferred embodiment of the system for controlling the concentration of ozone gas according to the present invention, each of the first pressure system and the second pressure system is composed of a pressure gauge and a solenoid valve.
According to the technical scheme, when the screwing valve is opened, the pressure gauge can detect the air pressure value in the corresponding dilution bottle in real time.
As a preferred embodiment of the system for controlling the concentration of ozone gas according to the present invention, 1 to 2 dilution bottles are further connected in series between the first dilution bottle and the second dilution bottle.
In the technical scheme of the invention, the number of the dilution bottles can be set according to the actual situation, if the concentration of ozone generated by the initial ozone generation system is too high, a plurality of dilution bottles can be added between the first dilution bottle and the second dilution bottle, but considering the simplicity of a connecting pipeline and the consumption of system pressure and instrument accessories, the whole system is recommended to be provided with no more than 4 dilution bottles.
It should be noted that the additional dilution bottles between the first dilution bottle and the second dilution bottle are also connected in series, and the structures of the dilution bottles are the same, and the connection mode is basically the same. And the ozone gas inlet of the added dilution bottle is connected with the ozone gas outlet of the previous dilution bottle, the zero gas inlet of the added dilution bottle is connected with the zero gas generator, the ozone gas outlet of the added dilution bottle is connected with the ozone gas inlet of the next dilution bottle, and the ozone gas outlet of the added dilution bottle is also connected with a pressure detection system.
As a preferred embodiment of the system for controlling the concentration of ozone gas of the present invention, the system for controlling the concentration further comprises an ozone detection system, wherein the ozone detection system is connected to the ozone dilution system; the ozone detection system comprises a flow tube and an ozone analyzer, wherein the air inlet end of the flow tube is connected with the air outlet end of the second flow limiting tube and the first screwing valve respectively, and the air outlet end of the flow tube is connected with the ozone analyzer.
In the technical scheme of the invention, diluted low-concentration ozone enters the flow pipe of the ozone detection system through the exhaust end of the second flow limiting pipe and/or the first screw valve, the flow pipe can be used as a container for chemical reaction of ozone and other substances, and gas after reaction in the flow pipe enters an ozone analysis instrument for analysis and test.
As a preferred embodiment of the system for controlling the concentration of ozone gas according to the present invention, the inlet end of the flow tube is further connected to the zero gas generator, and at least one of a mass flow controller and a solenoid valve is disposed between the inlet end of the flow tube and the zero gas generator.
In the technical scheme of the invention, the air inlet end of the flow pipe is connected with the zero gas generator, and the zero gas generated by the zero gas generator enters the flow pipe to further dilute the ozone flowing into the flow pipe from the second dilution bottle. Furthermore, a mass flow controller is arranged between the air inlet end of the flow pipe and the zero gas generator, so that the flow of the zero gas entering the flow pipe can be adjusted, and a screwing valve is arranged between the air inlet end of the flow pipe and the zero gas generator, so that the on-off of a gas path can be controlled.
Compared with the prior art, the invention has the beneficial effects that:
according to the technical scheme, the ozone generating system is connected with the ozone diluting system, so that high-concentration ozone generated in the ozone generating system is subjected to graded dilution in a diluting bottle of the ozone diluting system, and low-concentration ozone (<300ppb) which can be continuously and stably output and meets the requirements of experiments is obtained.
Drawings
FIG. 1 is a simplified flow chart of the operation of the ozone gas concentration control system of the present invention;
FIG. 2 is a schematic view of a system for controlling the concentration of ozone gas according to embodiment 1 of the present invention;
FIG. 3 is a schematic view of a dilution bottle of the ozone gas concentration control system of the present invention;
FIG. 4 shows O in Experimental example 1 of the present invention3A graph of concentration versus time;
FIG. 5 shows O in Experimental example 2 of the present invention3Graph of concentration versus time.
Wherein, the reference numbers in the structure of the concentration control system are as follows: 1-oxygen, 2-screw valve, 3-mass flow controller, 4-mass flow controller, 5-oxygen, 6-screw valve, 7-mass flow controller, 8-ozone generator, 9-first dilution bottle, 10-needle valve, 11-tail gas discharge port, 12-first flow limiting pipe, 13-screw valve, 14-pressure gauge, 15-second dilution bottle, 16-needle valve, 17-tail gas discharge port, 18-screw valve, 19-pressure gauge, 20-second flow limiting pipe, 21-first screw valve, 22-flow pipe, 23-tail gas discharge port, 24-ozone analyzer, 25-other analyzer;
the reference numerals in the dilution bottle structure are: a-ozone inlet, b-ozone outlet, c-zero inlet, d-tail gas port, and e-spare port.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
Fig. 2 shows a schematic structural diagram of a concentration control system of ozone gas in this embodiment, which includes an ozone generation system, an ozone dilution system, and an ozone detection system. Wherein the ozone generating system comprises oxygen 5, a screwing valve 6, a mass flow controller 7 and an ozone generator 8; the ozone diluting system comprises zero gas 1, a screwed valve 2, a mass flow controller 3, a mass flow controller 4, a first diluting bottle 9, a needle valve 10, a tail gas discharge port 11, a first flow limiting pipe 12, a screwed valve 13, a pressure gauge 14, a second diluting bottle 15, a needle valve 16, a tail gas discharge port 17, a screwed valve 18, a pressure gauge 19, a second flow limiting pipe 20 and a first screwed valve 21; the ozone detection system includes a flow tube 22, a tail gas 23, an ozone analyzer 24, and other analyzers 25.
In this embodiment, the zero gas 1 is air processed through steps of filtering, drying, purifying, and the like, and may be zero gas provided by any zero gas generator or zero gas stored in a high-pressure bottle. Common diluent gas can be high-purity nitrogen, purified zero air and the like;
the screw valves (2, 6, 13, 18, 21) are used for controlling the opening and closing of the gas flow, wherein the first screw valve 21 is substantially the same as the other 4 screw valves, and in the scheme, the connection relationship is named as the first screw valve for the sake of clarity; the first screw valve 21 is provided for supplying high-concentration ozone for a simulation experiment, so that new substances and other pollutants generated in the reaction of the simulation experiment can be removed quickly, the cleaning of a flow pipe is realized, and preparation is made for the next group of simulation experiments;
the needle valves (10, 16) are respectively used for adjusting the content and the pressure of ozone in the first dilution bottle and the second dilution bottle and discharging redundant ozone or diluted ozone into tail gas (11, 17);
the tail gas discharge ports (11, 17 and 23) are exhaust ports of tail gas in the system and are used for discharging redundant gas to the outside atmosphere and regulating the pressure of the system, and when the system works normally, all the tail gas discharge ports of the system pass through the fume hood to discharge gas so as to prevent indoor air from being polluted;
the oxygen 5 is the raw material gas for preparing ozone in the present invention, and high purity oxygen (purity is 99.999%) is usually used, and the gas can avoid the interference of other impurity gases when preparing ozone. Although zero gas can also be used as raw material gas for preparing ozone, researches find that nitrogen oxide (NOx) is easy to be introduced into the system, and the prepared ozone is not pure enough, thus being not beneficial to realizing the conditions required by simulation experiments;
the mass flow controllers (3, 4 and 7), which are abbreviated as MFCs in English, are used for controlling the flow of gas in the system, and the MFCs used in the system have different ranges at different connecting positions, wherein the MFCs used in the connecting positions 3,4 and 7 have the ranges of 10L/min, 50L/min and 1L/min respectively;
the ozone generator 8 is a commercially available ozone generator capable of continuously generating ozone at a high concentration (ppm level) at a stable power; the model of the ozone generator used in the invention is COM-AD-01-OEM, and can also be ozone generators of other brands;
the first dilution bottle 9 and the second dilution bottle 15 are two buffer bottles for diluting ozone in the embodiment, and the structural schematic diagram is shown in fig. 3, the dilution bottles are cylinders made of 304 or 316 type stainless steel, the diameter of each cylinder is 10cm, the height of each cylinder is 20cm, the volume of each cylinder is about 1.6L, each buffer bottle is provided with 5 holes, each hole is welded with a stainless steel pipe with the outer diameter of 1/4 inches and the length of about 1-2cm, and the stainless steel pipes are used for switching four-way valves or three-way valve ferrules so as to facilitate the inlet and the outlet of air flow; five hole sites on the buffer bottle are respectively: the ozone gas inlet a, the ozone gas outlet b, the zero gas inlet c, the tail gas port d and the spare port e are connected together to serve as the zero gas inlet or the spare ozone gas outlet;
the first flow limiting pipe 12 and the second flow limiting pipe 20 are two sections of air guide pipes made of Teflon materials, the length of each air guide pipe is 90cm, the outer diameter of each air guide pipe is 1/16, the flow of ozone at an air outlet in the system can be limited, and the dilution of the gas concentration can be completed;
the pressure gauges (14, 19) are commercially available hand-held pressure gauges, and may be other types of instruments capable of measuring gas pressure, which are respectively used for measuring the gas pressure at the ozone outlet of the first dilution bottle 9 and the second dilution bottle 15, and the system of the present invention needs to keep the gas pressure at the ozone outlet of the first dilution bottle 9 higher than the gas pressure at the ozone outlet of the second dilution bottle 15 during use. It should be noted that the invention can also use only one pressure gauge to test the pressure of two buffer bottles respectively;
the flow pipe 22 is a container for chemical reaction of ozone and other substances, and is also a container for further diluting ozone which has passed through the secondary dilution bottle in the experimental system; the flow tube used in the experimental device is a cylinder made of quartz, and the total volume is about 20L. It should be noted that the flow tube may be other vessels, shapes, or other sized volumes suitable for carrying out the ozonation reaction;
the ozone analyzer 24 is a commercially available ozone detecting instrument, and the instrument model used in the system of this embodiment is model number T400U O manufactured by Teledyne API corporation3An analyzer;
in the system of the embodiment, interfaces of other analyzers 25 are reserved, and if other detection instruments, such as a nitrogen oxide analyzer, need to be connected simultaneously during testing, the system can be directly connected for testing;
the system apparatus connections of this example were 1/4 inch teflon tubing and were connected using a shivialock (Swaglok)1/4 inch stainless steel bayonet, except as otherwise noted.
Experimental example 1
When the concentration control system of the embodiment 1 is used for carrying out an ozone concentration regulation experiment and starts to operate, all the screw valves (2, 6, 13, 18, 21) and the needle valves (10, 16) are in a closed state by default, all the tail gas discharge ports (11, 17, 23) are in an open state, and the specific operation steps are as follows: opening a screwed valve 2 of a zero gas 1, opening a screwed valve 6 of an oxygen 5, and respectively setting the flow rates of MFCs (3, 4 and 7) to be 5L/min, 10L/min and 0.5L/min; opening an ozone analyzer 24, starting to automatically record the concentration of ozone in the system after the instrument is stable, and operating for 3 hours because zero gas does not contain ozone, wherein the concentration is close to 0;
the ozone generator 8 is started, the ozone generation rate is set to be 20%, and the flow of a rotameter arranged on the ozone generator is slightly higher than 0.5L/min. It should be noted that the maximum ozone generation rate is 100%, although the output ozone concentration can be reduced by adjusting the generation rate down, the generation rate cannot be lower than 20%, otherwise the ozone concentration is very unstable; and due to the O required for the production of ozone2The flow rate is set to be 0.5L/min, and in order to avoid negative pressure, the flow meter of the instrument can be properly increased by 10 percent;
adjusting the opening and closing degree of the needle valves (10 and 16), opening the screw valves (13 and 18), and simultaneously reading the readings of corresponding pressure gauges (14 and 19) to ensure that the pressure of the dilution bottle 9 is higher than that of the dilution bottle 15, and the pressure ratio of the two is kept at 1.045;
the ozone generator 8 needs to be stabilized for 2-3h after being started, the pipeline of the whole system is fully diluted and needs about 5min, so the operation is carried out for 3-5h, and the diluted O is3The concentration is higher and is close to 450 ppb; when the operation is continued for 20.28h and the first screw-on valve 21 is opened, the gas bypasses the flow limiting pipe 20 and directly enters the flow pipe 22 from the 1/4-inch pipeline where the first screw-on valve 21 is located, and the ozone concentration rapidly rises and then tends to be stable. After an absolute time period of about 1.2h for the high concentration operation, i.e. from 20.28h to 21.48h, O is obtained3The average concentration was 1502.1. + -. 418.1ppb (note that, at the moment when this step was completed, O is present3The concentration will appear at one or two instantaneous high concentration values, which in the present experimental example can be as high as 4000ppb, but then the concentration drops immediately and tends to stabilize); then the first screw valve 21 is closed, the dilution condition of the system is kept unchanged, the equipment is continuously operated for 46h, and the high concentration data of the middle 1.2h are deducted, so that the O between 5h and 46h can be obtained3The average concentration was 151.7. + -. 11.1 ppb.
O in this example3As shown in FIG. 4, it can be seen from FIG. 4 that, by using the concentration control system of example 1, after the start-up of the ozone generator is stabilized, the whole experimental device system can rapidly and stably provide low-concentration ozone, and has the effect of rapidly switching to the high-concentration mode for use in the ozone generatorCleaning the flow tube.
Experimental example 2
The experimental example was the same as experimental example 1, and the concentration control system of example 1 was used to perform an ozone concentration adjustment experiment, and the experimental example changed the gas pressure of the dilution bottle in a short time by rapidly changing the opening and closing degree of the needle valves (10, 16), thereby accomplishing a plurality of changes in the dilution concentration.
O in this example3As shown in FIG. 5, the concentration changes with time were found to be 169. + -4.9 (19 h total data from 3.8 to 22.8h abscissa in FIG. 5), 86.0 + -1.9 (23.4 to 25.4h total 2h data), 65.4 + -0.6 (25.5 to 27.5h total 2h total data), 34.4 + -0.5 (27.6 to 29.6h total 2h total data) and 4.0 + -0.9 (27.6 to 29.6h total 2h total data) in the 4 dilution concentration points tested, respectively, as shown in FIG. 5. The test results show that the concentration control system in the embodiment 1 is adopted for ozone dilution, the stability of the system is good, and the diluted ozone can meet the experiment requirements.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The ozone gas concentration control system is characterized by comprising an ozone generating system and an ozone diluting system, wherein the ozone diluting system comprises a zero gas generator, a first diluting bottle, a second diluting bottle, a first flow limiting pipe and a second flow limiting pipe; the first dilution bottle and the second dilution bottle are respectively provided with an ozone inlet, an ozone outlet and a zero gas inlet; the ozone generating system is connected with the ozone inlet of the first dilution bottle; the zero gas generator is respectively connected with a zero gas inlet of the first dilution bottle and a zero gas inlet of the second dilution bottle; the ozone outlet of the first dilution bottle is connected with the ozone inlet of the second dilution bottle through the first flow limiting pipe; and an ozone outlet of the second dilution bottle is connected with an air inlet end of the second flow limiting pipe, and diluted ozone is discharged through an air outlet end of the second flow limiting pipe.
2. The ozone gas concentration control system of claim 1, wherein the ozone outlet of the first dilution bottle is further connected with a first pressure detection system, and the first pressure detection system is connected with the first flow limiting pipe in parallel; the ozone gas outlet of the second dilution bottle is further connected with a second pressure detection system and a first screwing valve, and the second pressure detection system, the second flow limiting pipe and the first screwing valve are connected in parallel.
3. The system for controlling concentration of ozone gas as claimed in claim 1, wherein the zero gas inlet of the first dilution bottle is connected in parallel with the zero gas inlet of the second dilution bottle, and at least one of a mass flow controller and a solenoid valve is further provided between the zero gas generator and the zero gas inlet of the first dilution bottle and the zero gas inlet of the second dilution bottle.
4. The system for controlling concentration of ozone gas as claimed in claim 1, wherein the first dilution bottle and the second dilution bottle are further provided with an exhaust port, and the exhaust port is connected with a needle valve.
5. The system for controlling concentration of ozone gas as claimed in claim 1, wherein a pipe diameter of the first flow restriction pipe is smaller than a diameter of an ozone outlet port of the first dilution bottle, and a pipe diameter of the second flow restriction pipe is smaller than a diameter of an ozone outlet port of the second dilution bottle.
6. The system for controlling concentration of ozone gas according to claim 2, wherein the first pressure system and the second pressure system each consist of a pressure gauge and a solenoid valve.
7. The system for controlling concentration of ozone gas as claimed in claim 1, wherein 1-2 dilution bottles are further connected in series between the first dilution bottle and the second dilution bottle.
8. The system for controlling concentration of ozone gas as claimed in any one of claims 1 to 7, further comprising an ozone detection system, wherein the ozone detection system is connected to the ozone dilution system.
9. The system for controlling concentration of ozone gas according to claim 8, wherein the ozone detecting system comprises a flow tube and an ozone analyzer, wherein an inlet end of the flow tube is connected to an outlet end of the second flow limiting tube and the first solenoid valve, respectively, and an outlet end of the flow tube is connected to the ozone analyzer.
10. The system for controlling concentration of ozone gas as claimed in claim 9, wherein the inlet end of the flow tube is further connected to the zero gas generator, and at least one of a mass flow controller and a solenoid valve is disposed between the inlet end of the flow tube and the zero gas generator.
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