CN114460038B - Device and method for on-line monitoring concentration of sulfur trioxide - Google Patents
Device and method for on-line monitoring concentration of sulfur trioxide Download PDFInfo
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- CN114460038B CN114460038B CN202111674390.7A CN202111674390A CN114460038B CN 114460038 B CN114460038 B CN 114460038B CN 202111674390 A CN202111674390 A CN 202111674390A CN 114460038 B CN114460038 B CN 114460038B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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Abstract
The invention discloses a device and a method for on-line monitoring of sulfur trioxide concentration, wherein the device comprises a sampling module, a detection module, a gas analysis tank module and a data processing module; the sampling module is used for externally sampling the gas to be detected and the standard gas, and guiding the gas into the gas analysis pool module for storage; the detection module is used for carrying out optical detection on the gas to be detected or the standard gas in the gas analysis tank module; the data processing module is connected with the detection module, processes and calculates the data detected by the detection module and then outputs a measurement result; the method comprises the steps of firstly obtaining a standard zero gas characteristic value through optical detection and calculation, and then establishing methane and SO to be detected 3 The corresponding relation of the gas concentration is calibrated by the completed methane gas concentration and the characteristic value in the range, thereby obtaining SO 3 A correspondence table of gas concentration and measured optical characteristic values; finally, the SO to be measured is measured in actual detection 3 Acquiring SO to be measured by using the gas optical characteristic value and the established corresponding relation table 3 Concentration value of gas.
Description
Technical Field
The invention relates to a device for on-line monitoring of sulfur trioxide concentration, and also relates to a monitoring method adopting the device, belonging to the field of monitoring of coal-fired flue gas pollutants.
Background
Sulfur trioxide (SO) produced in industrial processes 3 ) Mainly from sulfur acid making industry, pyrite acid making industry, coal-fired power plant, petroleum refining industry, and other industrial enterprises using coal as raw material or fuel, such as steel and cement industry, etc. SO in coal-fired flue gas 3 And the sulfuric acid is reacted with water vapor to generate sulfuric acid, and when the temperature is reduced to be lower than the acid dew point, the sulfuric acid is condensed and adhered to the wall of the flue, so that the wall surface is corroded at low temperature. The sulfuric acid mist aerosol is easy to further react to generate secondary particulate sulfate, and is the heavy weight of PM2.5 in the atmosphereOne of the sources is. SO (SO) 3 The concentration measurement has very important significance on the economical efficiency, safety and environmental protection of the operation of the devices of the production enterprises such as the coal-fired power plants. On-line monitoring of SO 3 The concentration provides powerful data support for enterprises to improve the production process, prevent equipment corrosion, control acid mist emissions exceeding standards and the like.
SO at present 3 The detection method of the gas concentration mainly comprises a condensation control method, a salt absorption method, an isopropyl alcohol absorption method, a laser absorption spectrum method and the like. The off-line measurement method mainly comprises a condensation control method, a salt absorption method and the like, but has long measurement period, cannot reflect the working condition characteristics in real time, has complex detection equipment and flow, and has large human error. The online measurement method mainly comprises an online monitoring method based on isopropanol absorption, a laser absorption spectrometry and the like, and is mainly used for carrying out periodic calibration by combining a sulfur trioxide generator, so that the online measurement method is easy to be influenced by conversion rate, and is complex in operation and long in calibration time.
Disclosure of Invention
The invention aims to: the invention aims to provide a device for on-line monitoring of the concentration of sulfur trioxide; another object of the present invention is to provide a method for on-line monitoring of sulfur trioxide concentration using the above device, which uses methane standard gas to indirectly calibrate SO in combination with spectral database characteristics 3 Concentration of SO 3 And (5) monitoring the concentration on line in real time.
The technical scheme is as follows: the device for on-line monitoring of the concentration of sulfur trioxide comprises a sampling module, a detection module, a gas analysis pool module and a data processing module; the sampling module is used for externally sampling the gas to be detected and the standard gas, and guiding the gas into the gas analysis pool module for storage; the detection module is used for carrying out optical detection on the gas to be detected or the standard gas in the gas analysis tank module; the data processing module is connected with the detection module, processes and calculates the data detected by the detection module and then outputs a measurement result.
The gas analysis tank module comprises a gas analysis tank, a vacuum pump and a temperature control device; the vacuum pump is connected with the gas analysis tank and provides a negative pressure environment for the gas analysis tank; the temperature control device provides a high-temperature environment for the gas analysis tank.
The sampling module comprises a multi-way valve and a sampling heat tracing pipe; the multi-way input ends of the multi-way valve are respectively connected with nitrogen input, methane standard gas input and SO to be tested 3 The output end of the multi-way valve is connected with the gas analysis tank through the sampling heat tracing pipe.
The detection module comprises a laser, a photoelectric detector and a driving device; the laser emitted by the laser passes through two ends of the gas analysis tank and is received by the photoelectric detector; the driving device is connected with the laser and modulates the wavelength of the laser.
The data processing module comprises a data acquisition end, a central processing unit and a communication module; and the central processing unit acquires signals output by the photoelectric detector through the data acquisition end, processes the data and finally sends measurement result data to an external system through the communication module.
The method for monitoring the concentration of sulfur trioxide on line by adopting the device comprises the following steps: firstly, standard zero gas characteristic values are obtained through optical detection and calculation, and then methane and SO to be detected are established through calculation 3 The corresponding relation of the gas concentration is calibrated by the obtained methane gas concentration and the characteristic value in the range, thereby obtaining SO 3 A correspondence table of gas concentration and measured optical characteristic values; finally, the SO to be measured is measured in actual detection 3 Acquiring SO to be measured by using the gas optical characteristic value and the established corresponding relation table 3 Concentration value of gas.
The method specifically comprises the following steps:
(1) Switching the multi-way valve, and introducing nitrogen (equivalent SO) 3 The concentration is zero and marked as C 0 ) Introducing the sample heat tracing pipe into a gas analysis pool, completing zero gas calibration through a laser, a photoelectric detector and a data processing module, and calculating an optical characteristic value S under a zero gas state 0 ；
(2) Build-up of methane and SO 3 Equivalent concentration relationship R1 between;
(3) Switching the multi-pass valve, and introducing methane standard gas (equivalent SO is obtained by utilizing the equivalent concentration relation R1) 3 Concentration of C 1 ) Introducing the sample heat tracing pipe into a gas analysis tank, completing range calibration through a laser, a photoelectric detector and a data processing module, and calculating concentration C 1 Corresponding optical characteristic value S 1 The method comprises the steps of carrying out a first treatment on the surface of the Obtaining a plurality of concentrations C within the range according to a fixed step length n Corresponding characteristic value S n Build-up of SO 3 A correspondence table T2 of the density and the optical characteristic value;
(4) Switching a multi-way valve to access an actual SO to be tested 3 The gas is subjected to online concentration monitoring, an optical characteristic value S is detected and calculated through a laser, a photoelectric detector and a data processing module, and is substituted into a relation table T2 to be interpolated to obtain SO to be detected 3 Concentration value C.
The method for calculating the optical characteristic value S is as follows:
the driving device generates a low-frequency scanning waveform electric signal and superimposes a high-frequency modulation waveform (usually a sine wave) to realize the tuning of the output wavelength of the laser; by demodulating the absorption intensity of the photodetector, a harmonic signal on the high-frequency modulation frequency component is extracted, and in the case of weak absorption (absorbance < 0.05), the nonlinear intensity modulation term is ignored at small modulation depths (i 2 And 0), the optical characteristic value is calculated by the following formula:
wherein S is an optical characteristic value, i 1 For the linear term amplitude and the nonlinear term amplitude of the light intensity modulation,is a linear function, P is pressure, X is gas component concentration, L is optical path length, S (T) is spectral line intensity, and the ratio of the pressure to the optical path length is +.>The wave number is the central wave number of the laser light, and a is the modulation depth.
Wherein in the step (2), methane and SO are established 3 The equivalent concentration relation between the two satisfies the following formula:
wherein X is the gas concentration, S is the strong spectral line,as a linear function +.>The wave number is the central wave number of the laser light, and a is the modulation depth; establishing methane and SO from the above equation 3 Equivalent concentration relationship between the two.
The beneficial effects are that: according to the monitoring method, the relation between methane and sulfur trioxide is established through spectral line parameters, so that the equivalent calibration concentration is calculated, and the monitoring method is convenient, quick, stable and reliable; meanwhile, methane is used as intermediate gas, so that the tedious links of operation of the sulfur trioxide generator and calibration by a condensation control method are avoided, the calibration period is greatly shortened, and human errors are reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of the device of the present invention;
FIG. 2 is SO 3 And CH (CH) 4 Simulated absorbance based on a spectral database.
Detailed Description
As shown in FIG. 1, the device for on-line monitoring of the concentration of sulfur trioxide comprises a sampling module, a detection module, a gas analysis tank module and a data processing module; the sampling module is used for externally sampling the gas to be detected and the standard gas, and guiding the gas into the gas analysis tank module for storage; the detection module is used for carrying out optical detection on the gas to be detected or the standard gas in the gas analysis tank module; the data processing module is connected with the detection module, processes and calculates the data detected by the detection module and then outputs a measurement result.
The gas analysis tank module comprises a gas analysis tank 6, a vacuum pump 4 and a temperature control device 3; the gas analysis tank 6 is a transparent cavity at two ends and stores the gas to be tested and the standard gas, and the vacuum pump 4 is connected with the gas analysis tank 6 and provides a negative pressure environment for the gas analysis tank 6; the temperature control device 3 provides a high temperature environment for the gas analysis cell 6.
The sampling module comprises a multi-way valve 1 and a sampling heat tracing pipe 2; the multi-way input end of the multi-way valve 1 is respectively connected with nitrogen input, methane standard gas input and SO to be detected 3 The output end of the multi-way valve 1 is connected with the gas analysis tank 6 through the sampling heat tracing pipe 2.
The detection module comprises a laser 5, a photoelectric detector 8 and a driving device 51; the laser emitted by the laser 5 passes through two ends of the gas analysis tank 6 and is received by the photoelectric detector 8; the driving device 51 is connected to the laser 5 and modulates the wavelength of the laser 5.
The data processing module 7 comprises a data acquisition end, a central processing unit and a communication module; the central processing unit acquires signals output by the photoelectric detector 8 through the data acquisition end, processes the data and finally sends measurement result data to an external system through the communication module.
The gas analysis cell 6 maintains a negative pressure high temperature environment of 60hPa and 220 ℃ through the vacuum pump 4 and the temperature control device 3. The temperature control device 3 comprises a multi-path temperature controller and is used for maintaining the high temperature of the sampling heat tracing pipe 2220 ℃ and avoiding condensation loss of sulfur trioxide and sulfuric acid steam during sampling.
The invention discloses a method for on-line monitoring of sulfur trioxide concentration, which specifically comprises the following steps:
step 1, switching the multi-way valve 1, and introducing nitrogen (equivalent SO) 3 The concentration is zero and marked as C 0 ) The gas is introduced into a gas analysis tank 6 through a sampling heat tracing pipe 2, zero gas calibration is completed through a laser 5, a photoelectric detector 8 and a data processing module 7, and an optical characteristic value S under a zero gas state is calculated 0 The method comprises the steps of carrying out a first treatment on the surface of the The optical characteristic value calculation principle is as follows:
wavelength modulation spectroscopy is typically performed by superimposing a high frequency modulation waveform (typically a sine wave) on a low frequency scanning waveform electrical signal, and inputting the superimposed waveform to a temperature current driver to achieve tuning of the output wavelength of the laser. The wavelength modulation spectrum technology can reduce the interference of low-frequency noise in a measuring system and improve the measuring sensitivity. And the harmonic signals on the high-frequency modulation frequency components are extracted by demodulating the absorption light intensity, so that the measurement of the gas parameters is realized.
When a high frequency modulation signal is introduced to the output wavelength of the laser, the variation of the laser output wavelength with time can be expressed as:
wherein, the liquid crystal display device comprises a liquid crystal display device,the wave number is the central wave number of the laser light, a is the modulation depth, and f is the modulation frequency;
the laser output intensity can be expressed as:
wherein the method comprises the steps ofIs the direct current of the laser light intensity, i m Linear term amplitude and nonlinear term amplitude for light intensity modulation,/->The phase difference between the frequency modulation and the light intensity modulation is represented by f, which is the modulation frequency; nonlinear light intensity modulation is typically frequency doubled, so the above equation can be simplified as:
the light intensity transmittance of the absorption line can be expressed as:
alpha (v) is absorbance, expressed as:
wherein S (T) is strong spectral line and is related to temperature;is a linear function, P is pressure, X is gas component concentration, and L is optical path length.
The transmittance of the wavelength modulation spectrum is an even function of 2pi ft, the fourier cosine expansion is:
wherein, the liquid crystal display device comprises a liquid crystal display device,the coefficients representing the nth order harmonics are specifically expressed as:
multiplying the transmitted light intensity signal with a sine reference signal and a cosine reference signal with the frequency of mf respectively, performing digital phase locking processing, and obtaining an X component and a Y component of a primary harmonic signal and a secondary harmonic signal of an absorption signal through a low-pass filter:
the 1f normalized 2f signal can eliminate the influence of photoelectric amplification coefficient of the detection system and the interference of light intensity variation caused by other non-absorption factors.
At the spectral line center frequency, the odd term for Hk is 0. In the case of weak absorption (alpha (v) < 0.05), the nonlinear intensity modulation term is negligible at small modulation depths (i 2 =0), the WMS-2f/1f signal at the center of the line can be simplified expressed as an optical eigenvalue:
from the above, P 2f/1f The gas parameter information such as pressure, temperature, component concentration and the like is contained. When the pressure, temperature and optical path length of the instrument analysis cell are known, the on-line measurement of the concentration of the target gas component can be realized by combining the calibration database.
Step 2, establishing methane and SO by calculation 3 Equivalent concentration relationship R1 between; to realize CH 4 Indirect SO calibration of spectral line 3 The equivalent concentration relationship between the two is required to be established, as shown in figure 2, and the immediate SO is screened out 3 And CH (CH) 4 The absorption spectrum line can enable the laser to scan two absorption peaks at the same time, and the difference between the light intensity modulation amplitude and the modulation depth of the laser near the two spectrum lines can be ignored due to the close proximity of the spectrum linesSlightly less, when the optical characteristic values are equal, then CH 4 And SO 3 The equivalent concentration relation is shown in the formula (15):
combining (15) with high-resolution spectrum database parameter simulation, when the temperature of an analysis cell is 220 ℃, the pressure is 60hPa, and the optical path length is 80cm, CH 4 And SO 3 Equivalent concentrations are shown in Table 1, using equivalent concentrations of CH 4 SO can be completed 3 0-100mg/m of gas 3 Is defined by the calibration of (a).
Table 1 shows CH 4 And SO 3 Equivalent concentration meter
| SO 3 Concentration (mg/m) 3 ) | 0 | 20 | 40 | 60 | 80 | 100 |
| Equivalent CH 4 (％) | 0 | 0.2095 | 0.4190 | 0.6285 | 0.8380 | 1.0475 |
Step 3, switching the multi-way valve 1, and introducing methane standard gas (obtaining equivalent SO by utilizing the equivalent concentration relation R1) 3 Concentration of C 1 ) The gas is introduced into a gas analysis tank 6 through a sampling heat tracing pipe 2, the range calibration is completed through a laser 5, a photoelectric detector 8 and a data processing module 7, and the concentration C is calculated 1 Corresponding optical characteristic value S 1 The method comprises the steps of carrying out a first treatment on the surface of the Obtaining a plurality of concentrations C within the range according to a fixed step length n Corresponding characteristic value S n (the calculation method is the same as step 1), and SO is established 3 A correspondence table T2 of the density and the optical characteristic value;
step 4, switching the multi-way valve 1, and accessing the SO to be actually tested 3 The gas is subjected to online concentration monitoring, an optical characteristic value S is detected and calculated through a laser 5, a photoelectric detector 6 and a data processing module 7 (the calculation method is the same as step 1), and the optical characteristic value S is substituted into a relation table T2 to be interpolated to obtain SO to be detected 3 Concentration value C.
Claims (6)
1. An on-line monitoring sulfur trioxide concentration's device, its characterized in that: the device comprises a sampling module, a detection module, a gas analysis pool module and a data processing module; the sampling module is used for externally sampling the gas to be detected and the standard gas, and guiding the gas into the gas analysis pool module for storage; the detection module is used for carrying out optical detection on the gas to be detected or the standard gas in the gas analysis tank module; the data processing module is connected with the detection module, processes and calculates the data detected by the detection module and then outputs a measurement result; the sampling module comprises a multi-way valve and a sampling heat tracing pipe; the multi-way input ends of the multi-way valve are respectively connected with nitrogen input, methane standard gas input and SO to be tested 3 The output end of the multi-way valve is connected with the gas analysis tank through the sampling heat tracing pipe;
the method for monitoring the concentration of sulfur trioxide on line by adopting the device comprises the following steps:
(1) Switching the multi-way valve, introducing nitrogen and equivalent SO 3 The concentration is zero and marked as C 0 Introducing the sample heat tracing pipe into a gas analysis pool, completing zero gas calibration through a laser, a photoelectric detector and a data processing module, and calculating an optical characteristic value S under a zero gas state 0 ；
(2) Calculation to establish methane and SO 3 Equivalent concentration relationship R1 between;
(3) Switching the multi-way valve, introducing methane standard gas, and obtaining equivalent SO by using an equivalent concentration relation R1 3 Concentration of C 1 Introducing the sample heat tracing pipe into a gas analysis pool, completing range calibration through a laser, a photoelectric detector and a data processing module, and calculating SO (SO) 3 Concentration C 1 Corresponding optical characteristic value S 1 The method comprises the steps of carrying out a first treatment on the surface of the Obtaining a plurality of concentrations C within the range according to a fixed step length n Corresponding characteristic value S n Build-up of SO 3 A correspondence table T2 of the density and the optical characteristic value;
(4) Switching a multi-way valve to access an actual SO to be tested 3 The gas is subjected to online concentration monitoring, an optical characteristic value S is detected and calculated through a laser, a photoelectric detector and a data processing module, and is substituted into a relation table T2 to be interpolated to obtain SO to be detected 3 Concentration value C.
2. The apparatus for on-line monitoring of sulfur trioxide concentration according to claim 1, characterized in that: the gas analysis tank module comprises a gas analysis tank, a vacuum pump and a temperature control device; the vacuum pump is connected with the gas analysis tank and provides a negative pressure environment for the gas analysis tank; the temperature control device provides a high-temperature environment for the gas analysis tank.
3. The apparatus for on-line monitoring of sulfur trioxide concentration according to claim 1, characterized in that: the detection module comprises a laser, a photoelectric detector and a driving device; the laser emitted by the laser passes through two ends of the gas analysis tank and is received by the photoelectric detector; the driving device is connected with the laser and modulates the wavelength of the laser.
4. The apparatus for on-line monitoring of sulfur trioxide concentration according to claim 1, characterized in that: the data processing module comprises a data acquisition end, a central processing unit and a communication module; and the central processing unit acquires signals output by the photoelectric detector through the data acquisition end, processes the data and finally sends measurement result data to an external system through the communication module.
5. The apparatus for on-line monitoring of sulfur trioxide concentration according to claim 1, characterized in that: the calculation method of the optical characteristic value S is as follows:
generating a low-frequency scanning waveform electric signal through a driving device and superposing a high-frequency modulation waveform to tune the output wavelength of the laser; extracting harmonic signals on the high-frequency modulation frequency components by demodulating the absorption light intensity of the photoelectric detector; at small modulation depths, the nonlinear intensity modulation term is ignored and the optical characteristic value is calculated by the following formula:
wherein S is an optical characteristic value, i 1 Is the linear term amplitude of the light intensity modulation,is a linear function, P is pressure, X is gas component concentration, L is optical path length, S (T) is spectral line intensity, and the ratio of the pressure to the optical path length is +.>The wave number is the central wave number of the laser light, and a is the modulation depth.
6. The apparatus for on-line monitoring of sulfur trioxide concentration according to claim 1, characterized in that: in step (2), methane and SO 3 The equivalent concentration relation between the two components meets the following requirementsThe following formula is given:
wherein X is the gas concentration, S is the strong spectral line,as a linear function +.>The wave number is the central wave number of the laser light, and a is the modulation depth.
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