CN114397257A - H2S corrosivity and adsorption analytical characteristic synchronous monitoring system - Google Patents
H2S corrosivity and adsorption analytical characteristic synchronous monitoring system Download PDFInfo
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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
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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
- G01N21/03—Cuvette constructions
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Abstract
The invention provides a H2S corrosion and adsorption analytical characteristic synchronous monitoring system, mixing different concentrations of H by mass flowmeter2S gas is introduced into an anti-corrosion gas chamber and an anti-adsorption gas chamber, different porous metal materials can be placed in the anti-corrosion gas chamber, different adsorption materials are placed in a quartz spiral tube of the anti-adsorption gas chamber, and the gas chamber communication is based on TDLAS high-precision H2S on-line measuring system for monitoring H in air chamber in real time2The concentration of S is changed, and H can be synchronously treated by changing the conditions of temperature, humidity, pressure and the like of the two air chambers2Research on S corrosion mechanism and adsorption analytical characteristics is realized by combining static monitoring and dynamic monitoring to establish a compensation model for realizing the purpose of realizing the H close to the wall surface of the water wall of the pulverized coal boiler2And S gas high-fidelity pretreatment and online monitoring lay a foundation.
Description
Technical Field
The invention relates to the technical field of gas monitoring, in particular to an H2S corrosivity and adsorption analytical characteristic synchronous monitoring system.
Background
In recent years, the ultra-low emission and energy-saving reconstruction of the coal-fired power plant in China are comprehensively implemented, the coal-fired unit adopts the modes of 'low-nitrogen combustion' and 'anoxic combustion' to inhibit the generation of nitrogen oxides, so that the ultra-low emission standard is achieved, and various governments propose a series of subsidies such as 'near zero emission' and the like in order to better implement the 'ultra-low emission' policyThe policy is fed back to the power plant, the economic burden of the power plant is reduced in a short period, but with the steady promotion of the policy of 'ultra-low emission', difficult and miscellaneous diseases such as increase of ammonia escape rate, blockage of an air preheater and the like begin to influence the operation of the unit, but sulfur in pulverized coal or SO generated by combustion reaction2Will be partially converted into H2S, under the working condition of medium and high load, H2S is mainly concentrated in the near-wall surface area of the water-cooled wall, and H is generated in the local strong reducing atmosphere of the hearth2S is used as a strong corrosive gas, and when the concentration of the S is higher (such as more than 100 ppm), the S can cause strong corrosion to the water wall and can cause strong corrosion to the near wall surface H of the boiler water wall2S is particularly important for realizing on-line monitoring, H2S gas is dissolved in water, has strong corrosivity, and transmission pipelines of different materials, temperatures and humidity are all aligned to H2S has different degrees of adsorption, cannot ensure high-fidelity transmission of sample gas, and has great difficulty in on-line monitoring.
H2S is a flammable acidic gas under the standard condition, is colorless, smells of smelly eggs at low concentration, is extremely toxic, is dissolved in water and has strong corrosivity. In order to ensure the safe operation of the thermal power generating unit and realize the online monitoring of the near wall surface of the water wall of the pulverized coal boiler, an experimental system needs to be built to solve the problem of H2S, synchronously monitoring and analyzing the corrosivity and adsorption analytical characteristics of the gas, establishing a compensation model, and realizing the purpose of detecting the wall surface H close to the water wall of the pulverized coal boiler2And (4) high-fidelity pretreatment and online monitoring of S gas.
The prior art has the following disadvantages:
1. near wall surface H of water-cooled wall of pulverized coal fired boiler hearth2S on-line monitoring system adopts extraction type sampling method, because of H2S has strong corrosivity and adsorption characteristics, is dissolved in water, and puts higher requirements on a traditional extraction type sampling pretreatment monitoring system, and the existing monitoring system cold drying method mostly adopts a high-temperature heat tracing polytetrafluoroethylene tube combined with a condensing device for sampling pretreatment, so that high-fidelity sample gas cannot be obtained;
2. sample preprocessing system is not paired with H2S gas is used for establishing an empirical model of temperature, humidity and the like, surface corrosion rate and corrosion depth and analyzing material absorption of different materials at different temperatures and different humidityThe ability to determine the optimum material and optimum set temperature, no H build-up2And accurately and quantitatively analyzing the loss by using an S adsorption analysis compensation model.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
The invention aims to provide a hydrogen (H)2S corrosivity and adsorption analytical characteristic synchronous monitoring system capable of synchronously realizing H2S, researching the corrosivity and the adsorption analysis characteristic, establishing a compensation model to realize the H-shaped near wall surface of the water-cooled wall of the pulverized coal boiler2And S gas high-fidelity pretreatment and online monitoring lay a foundation.
An embodiment of one aspect of the application provides an H2The S-corrosion and adsorption analytical characteristic synchronous monitoring system comprises a gas distribution system and H2The system comprises an S monitoring system, a corrosivity monitoring system and an adsorption analysis monitoring system, wherein the gas distribution system is communicated with H connected in parallel through a main pipeline2The system comprises an S monitoring system, a corrosivity monitoring system and an adsorption analysis monitoring system, wherein parallel branches are communicated with one another, and each parallel branch is provided with a control valve.
In some embodiments, a temperature adjustment mechanism is also included for adjusting the temperature of the corrosion prevention plenum in the corrosion monitoring system and the temperature of the adsorption prevention plenum in the adsorption desorption monitoring system.
In some embodiments, the system further comprises a blowback system for blowing back the internal pipeline of the whole system after each monitoring is finished, and the blowback system is communicated with the main pipeline.
In some embodiments, the gas distribution system comprises N2Gas source and H2S gas source, and connected with mass flow meter, N2Gas source and H2S gas sources are gathered on the main pipeline through a gas circuit, and N is2And H2And a filtering device is communicated with the main pipeline before the S enters each monitoring system.
In some embodiments, the H2The S monitoring system comprises a signal generator, a laser driver, a laser collimator, a beam splitter, a planar gold-plated reflector, and a cavity enhancerThe system comprises an optical path pool, an interferometer, a first detector, a second detector and a data processing unit;
the signal generator emits low-frequency triangular waves and high-frequency sine waves which are superposed and coupled to enter the laser driver to drive the laser, light beams are irradiated to the surface of the beam splitter through the laser collimator to form reflected light and transmitted light, the reflected light of the beam splitter is irradiated to the plane gold-plated reflecting mirror to enter the interferometer and the first detector in sequence to carry out frequency spectrum calibration, the transmitted light of the beam splitter enters the cavity enhancement optical path pool, the cavity enhancement optical path pool carries the vacuum gauge, the emergent light enters the second detector to obtain photoelectric signals, and the first detector and the second detector are connected to the data processing unit to carry out H processing2And (4) monitoring and analyzing the S concentration on line.
In some embodiments, the corrosion monitoring system includes an anti-corrosion gas chamber having a replaceable metallic material to be tested disposed therein, the anti-corrosion gas chamber carrying a vacuum gauge and a hygrometer.
In some embodiments, the adsorption analytical monitoring system includes an anti-adsorption gas chamber with an adsorption device built in, the anti-adsorption gas chamber carrying a vacuum gauge and a hygrometer.
In some embodiments, the temperature adjustment mechanism is a temperature-adjustable high-temperature box, the corrosion-resistant air chamber and the adsorption-resistant air chamber are both arranged in the temperature-adjustable high-temperature box, and the vacuum gauge and the hygrometer which are arranged on the corrosion-resistant air chamber and the adsorption-resistant air chamber are both arranged outside the temperature-adjustable high-temperature box.
In another aspect, an embodiment of the present application provides a method as described above2The static monitoring method of the S corrosivity and adsorption analytical characteristic synchronous monitoring system comprises the following steps:
S1，N2gas source and H2S gas source is proportioned by a mass flow meter and passes through a filtering device to obtain H with different concentrations2S gas;
s2, when monitoring H2S, when the mixture is corrosive, the pipelines between the anti-corrosion air chamber and the cavity-enhanced optical path pool are communicated to form a loop, and the pipelines in front of and behind the back-blowing system and the adsorption-resistant air chamber are closed, so that the proportioned H2S gas synchronously enters an anti-corrosion gas chamber and a cavity enhanced optical path pool and can pass through the temperatureAdjusting the temperature of the high temperature box to change the temperature of the anti-corrosion air chamber, and monitoring the pressure, humidity and concentration change in the anti-corrosion air chamber in real time to obtain H2S, the relationship between the corrosion rate and the corrosion depth of the gas to different material types at different temperatures and different humidities;
when monitoring H2When S adsorbs the analytic characteristic, the pipeline between the anti-adsorption air chamber and the cavity enhanced optical path pool is communicated to form a loop, and the pipeline in front of and behind the back flushing system and the anti-corrosion air chamber is closed, so that the proportioned H2S gas synchronously enters the anti-adsorption gas chamber and the cavity enhanced optical path pool, the temperature of the anti-adsorption gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, the humidity and the concentration change in the anti-adsorption gas chamber are monitored in real time, and H is obtained2S, the relationship between adsorption and analysis of gas on the surfaces of different materials at different temperatures and different humidities;
and S3, opening a back-flushing pump and an exhaust device to perform system integral purging after each monitoring is finished.
In the third embodiment of the present application, a H is provided2The dynamic monitoring method of the S corrosion and adsorption analytical characteristic synchronous monitoring system comprises the following steps:
S1，N2gas source and H2S gas source is proportioned by a mass flow meter and passes through a filtering device to obtain H with different concentrations2S gas;
s2, when monitoring H2S, when the gas is corrosive, the pipelines among the anti-corrosion gas chamber, the cavity enhanced optical path pool and the exhaust device are communicated, the pipelines in front of and behind the back-blowing system and the adsorption-preventing gas chamber are closed, and the pipeline between the cavity enhanced optical path pool and the main pipeline is closed, so that the proportioned H2S gas sequentially enters the anti-corrosion gas chamber, the cavity enhanced optical path pool and the exhaust device, the temperature of the anti-corrosion gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, humidity and concentration change in the anti-corrosion gas chamber is monitored in real time, and H is obtained2S, the relationship between the corrosion rate and the corrosion depth of the gas to different material types at different temperatures and different humidities;
when monitoring H2When S adsorbs the analytic characteristic, will prevent adsorbing the pipeline intercommunication between air chamber, chamber reinforcing optical path pond and the exhaust apparatus, closeClose the pipeline in front of and behind the blowback system and the anti-corrosion air chamber, close the pipeline between the cavity enhanced optical path pool and the main pipeline, so that the H after proportioning2S gas sequentially enters the anti-adsorption gas chamber, the cavity enhanced optical path pool and the exhaust device, the temperature of the anti-adsorption gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, humidity and concentration change in the anti-adsorption gas chamber is monitored in real time, and H is obtained2S, the relationship between adsorption and analysis of gas on the surfaces of different materials at different temperatures and different humidities;
when monitoring H2S corrosivity and monitoring H2When S adsorption analysis characteristic is synchronously carried out, pipelines among the anti-corrosion air chamber, the anti-adsorption air chamber, the cavity enhanced optical path pool and the exhaust device are communicated, and a back flushing system and a pipeline between the cavity enhanced optical path pool and a main pipeline are closed, so that the proportioned H2S gas simultaneously enters an anti-corrosion air chamber and an anti-adsorption air chamber, then the gas is gathered and sequentially enters a cavity enhanced optical path pool and an exhaust device, the temperature of the anti-corrosion air chamber and the anti-adsorption air chamber is changed through a temperature-adjustable high-temperature box, the pressure, humidity and concentration changes in the anti-corrosion air chamber and the anti-adsorption air chamber are monitored in real time, and H is obtained2The relationship between the corrosivity and adsorption and analysis characteristics of S gas to different materials at different temperatures and different humidities.
And S3, opening a back-flushing pump and an exhaust device to perform system integral purging after each monitoring is finished.
The invention has the beneficial effects that:
1. based on the laser absorption spectroscopy (TLDAS) technology, a WM-DAS algorithm is adopted to combine with the development of a cavity enhanced gas absorption cell with an optical path of more than 500m, and a monitoring system is set up to realize real-time high-precision H2S, online monitoring is carried out, and static monitoring and dynamic monitoring are combined;
2. high-precision online monitoring through TDLAS (tunable diode laser absorption spectroscopy) and synchronous deep research H2S gas corrodes different material types under different temperature and different humidity and the relation of corrosion rate and corrosion depth establishes H2S, a high-temperature corrosion rate model;
3. high-precision online monitoring through TDLAS (tunable diode laser absorption spectroscopy) and synchronous deep research H2S gas is at different temperature and different humidityAnd establishing an adsorption and analysis compensation model according to the relationship between adsorption and analysis of the surfaces of different materials, and laying a foundation for realizing sampling pretreatment of high-precision online monitoring.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent from and readily appreciated by reference to the following description of the embodiments taken in conjunction with the accompanying drawings,
wherein:
FIG. 1 is a drawing H in the present embodiment2S, a schematic diagram of a static monitoring method of a synchronous monitoring system for corrosivity and adsorption analytical characteristics;
FIG. 2 is a drawing H in the example of the present application2S, a schematic diagram of a dynamic monitoring method of a synchronous monitoring system for corrosivity and adsorption analytical characteristics;
reference numerals:
1-N2gas source, 2-H2S gas source, 3-mass flow meter, 4-filter, 5-back-blowing pump, 6-1-first needle valve, 6-2-second needle valve, 6-3-third needle valve, 6-4-fourth needle valve, 6-5-fifth needle valve, 6-6-sixth needle valve, 6-7-seventh needle valve, 6-8-eighth needle valve, 7-corrosion-resistant air chamber, 8-adsorption-resistant air chamber, 9-metal material, 10-spiral adsorption device, 11-temperature adjustable high-temperature box, 12-vacuum gauge, 13-hygrometer, 14-signal generator, 15-laser driver, 16-laser, 17-laser collimator, 18-beam splitter, 19-plane gold-plated reflector, 20-cavity enhanced optical path pool, 21-interferometer, 22-1-first detector, 22-2-second detector and 23-data processing unit.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
H of an embodiment of the present invention is described below with reference to the drawings2Corrosive and adsorptive characteristics of SSexual synchronism monitoring system.
An embodiment of one aspect of the application provides an H2S corrosivity and adsorption analysis characteristic synchronous monitoring system, as shown in figure 1, comprises gas distribution system, corrosivity monitoring system, adsorption analysis monitoring system, temperature-adjustable high-temperature box, back-flushing system and TDLAS-based high-precision H2S monitoring system, gas distribution system is through trunk line intercommunication H2S monitoring system, corrosivity monitoring system and adsorption analysis monitoring system, H2The three branches of the S monitoring system, the corrosivity monitoring system and the adsorption analysis monitoring system are communicated in parallel, and each parallel branch is provided with a control valve.
The gas distribution system comprises N2Gas source 1 (N)2Standard gas) and H2S gas source 2 (H)2S standard gas) and respectively connected with a mass flow meter 3 for proportioning, N2Gas sources 1 and H2 S gas source 2 is gathered on the main pipeline through a gas circuit, and N is2And H2And a main pipeline before the S enters each monitoring system is communicated with a filtering device 4, and a high-precision filter element is arranged in the filtering device 4 and is used for filtering the gas after proportioning.
The back-blowing system is a back-blowing pump 5, a branch of the back-blowing pump 5 is communicated with the main pipeline and used for blowing the internal pipeline of the whole system after each monitoring is finished, and a needle valve 6-1 is arranged on the branch and used for controlling the on-off of the back-blowing pump 5.
The corrosivity monitoring system comprises an anti-corrosion air chamber 7, wherein a porous metal material 9 for monitoring is arranged in the anti-corrosion air chamber 7, the metal material 9 can be replaced, the anti-corrosion air chamber 7 is provided with a vacuum gauge 12 and a hygrometer 13, and the internal pressure and humidity of the anti-corrosion air chamber 7 can be monitored in real time. And a second needle valve 6-2 and a fourth needle valve 6-4 are respectively arranged on the front pipeline and the rear pipeline of the anti-corrosion air chamber 7 and are used for controlling the on-off of the pipelines of the anti-corrosion air chamber 7.
The adsorption analysis monitoring system comprises an adsorption-prevention air chamber 8, a spiral adsorption device 10 is arranged in the adsorption-prevention air chamber 8, a quartz spiral tube can be adopted, different adsorption materials can be loaded in the spiral adsorption device 10, and the adsorption materials can be replaced. The spiral adsorption device 10 is in a spiral pipe shape and is used for increasing the contact area. Connecting it to gas pipeline in front and back mode H2And introducing the S gas into the spiral adsorption device 10 for monitoring. The adsorption-preventing gas chamber 8 is equipped with a vacuum gauge 12 and a hygrometer 13. And a third needle valve 6-3 and a fifth needle valve 6-5 are respectively arranged on the front pipeline and the rear pipeline of the adsorption-preventing air chamber 8 and are used for controlling the on-off of the pipelines of the adsorption-preventing air chamber 8.
In some specific embodiments, the spiral adsorption device 10 is made of stainless steel, teflon, quartz, etc., and these materials also have adsorption function and plasticity, and can be directly used for monitoring adsorption and desorption. An inert powdered adsorbent material, such as activated carbon or copper oxide, may be used, and may be placed in the spiral adsorbent device 10 for monitoring the adsorption and desorption.
The anti-corrosion air chamber 7 and the anti-adsorption air chamber 8 are both arranged in the temperature-adjustable high-temperature box 11. The temperature-adjustable high-temperature box 11 is used for adjusting the temperature in the anti-corrosion air chamber 7 and the anti-adsorption air chamber 8. The needle valve, the vacuum gauge 12, and the hygrometer 13 mounted in the corrosion prevention chamber 7 and the adsorption prevention chamber 8 are all disposed outside the temperature-adjustable high-temperature tank 11.
A six-gauge needle valve 6-6 is arranged on the pipeline of the cavity enhanced optical path cell 20 and used for controlling the connection and disconnection with an exhaust device (not shown in the attached figure 1). A seventh needle valve 6-7 is arranged on a pipeline between the main pipeline and the cavity enhanced optical path pool 20, and a pipeline between the main pipeline and the cavity enhanced optical path pool 20 is positioned between the sixth needle valve 6-6 and the cavity enhanced optical path pool 20.
When the metal material 9 in the corrosion prevention air chamber 7 needs to be replaced, or the adsorbing material in the adsorption prevention air chamber 8 needs to be replaced, all needle valves are closed.
H2The S monitoring system comprises a signal generator 14, a laser driver 15, a laser 16, a laser collimator 17, a beam splitter 18, a planar gold-plated reflecting mirror 19, a cavity enhanced optical path cell 20, an interferometer 21, a first detector 22-1, a second detector 22-2 and a data processing unit 23. H2The front pipeline and the rear pipeline of the S monitoring system are respectively provided with a seven needle valve 6-7 and an eight needle valve 6-8 for controlling H2And S, monitoring the on-off of the system.
The application also provides an H2Corrosion by SThe synchronous monitoring method for the sex and adsorption analytical characteristics comprises static measurement and dynamic measurement.
A static measurement method comprises the following steps:
as shown in FIG. 1, the direction of the arrow is H2The flow direction of the S gas. When monitoring H2When S is corrosive, the system adopts N2Standard gas and H2S standard gas is proportioned by respective mass flow meters 3 and passes through a high-precision filter element of a filter device 4 to obtain pure and dry H with different concentrations2And S, opening a second needle valve 6-2, a fourth needle valve 6-4, a seventh needle valve 6-7 and an eighth needle valve 6-8, closing a first needle valve 6-1, a third needle valve 6-3, a fifth needle valve 6-5 and a sixth needle valve 6-6, communicating pipelines between the anti-corrosion air chamber 7 and the cavity enhanced optical path pool 20 to form a loop, and closing pipelines in front of and behind the back-blowing pump 5, the exhaust device and the anti-adsorption air chamber 8. So that the H after proportioning2S gas synchronously enters the anti-corrosion gas chamber 7 and the cavity-enhanced optical path pool 20, the anti-corrosion gas chamber 7 is provided with the vacuum gauge 12 and the hygrometer 13, and the internal pressure and humidity of the anti-corrosion gas chamber 7 can be monitored in real time. The temperature inside the corrosion prevention gas chamber 7 is changed by the temperature-adjustable high-temperature tank 11. The concentration change in the anti-corrosion air chamber 7 can be monitored in real time by the synchronous cavity-entering enhanced optical path pool 20, and H is deeply researched2S gas is used for establishing the relation between the corrosion rate and the corrosion depth of different material types under different temperatures and different humidities to establish H2And S, a high-temperature corrosion rate model.
When monitoring H2When S adsorption analysis characteristic is adopted, N is adopted by the system2Standard gas and H2S standard gas is proportioned by respective mass flow meters 3 and passes through a high-precision filter element of a filter device 4 to obtain pure and dry H with different concentrations2And S, opening a third needle valve 6-3, a fifth needle valve 6-5, a seventh needle valve 6-7 and an eighth needle valve 6-8, closing a first needle valve 6-1, a second needle valve 6-2, a fourth needle valve 6-4 and a sixth needle valve 6-6, communicating pipelines between the anti-adsorption air chamber 8 and the cavity enhanced optical path pool 20 to form a loop, and closing pipelines in front of and behind the back-flushing pump 5, the exhaust device and the anti-corrosion air chamber 7. So that the H after proportioning2The S gas synchronously enters the anti-adsorption gas chamber 8 and the cavity enhanced optical path cell 20. The adsorption-preventing gas chamber 8 is provided with a vacuum gauge 12 and a hygrometer 13, and can be used for real-time measurementThe pressure and humidity inside the adsorption prevention air chamber 8 are monitored, and the temperature inside the adsorption prevention air chamber 8 is changed by the temperature-adjustable high-temperature box 11. The concentration change in the anti-adsorption air chamber 8 can be monitored in real time by the synchronous cavity-entering enhanced optical path pool 20, and H is deeply researched2And S, establishing an adsorption and analysis compensation model according to the relation between adsorption and analysis of the gas on the surfaces of different materials at different temperatures and different humidities.
After the monitoring is finished, the back-flushing pump 5 and the exhaust device can be opened to carry out the integral purging of the system, and the internal working condition of the system is ensured to meet the experimental requirements. The specific operation is as follows: and (3) continuously keeping the opened needle valve in the monitoring process, opening the first needle valve 6-1 and the sixth needle valve 6-6, purging the whole pipeline, and discharging gas into an exhaust device.
II, a dynamic measurement method:
as shown in fig. 2, the direction of the arrow is H2The flow direction of the S gas. When monitoring H2When S is corrosive, the system adopts N2Standard gas and H2S standard gas is proportioned by respective mass flow meters 3 and passes through a high-precision filter element of a filter device 4 to obtain pure and dry H with different concentrations2And S, opening a second needle valve 6-2, a fourth needle valve 6-4, a sixth needle valve 6-6 and an eighth needle valve 6-8, closing a first needle valve 6-1, a third needle valve 6-3, a fifth needle valve 6-5 and a seventh needle valve 6-7, communicating pipelines among the anti-corrosion air chamber 7, the cavity enhancement optical path pool 20 and the exhaust device to form a serial passage, and closing pipelines in front of and behind the back-blowing pump 5 and the anti-adsorption air chamber 8. So that the H after proportioning2The S gas sequentially enters the anti-corrosion gas chamber 7, the cavity enhanced optical path pool 20 and the exhaust device. The anti-corrosion air chamber 7 is provided with a vacuum gauge 12 and a hygrometer 13, so that the internal pressure and humidity of the anti-corrosion air chamber 7 can be monitored in real time, and after being monitored by the cavity enhanced optical path pool 20, the gas directly enters the exhaust device. The temperature inside the corrosion prevention gas chamber 7 is changed by the temperature-adjustable high-temperature tank 11. The concentration change in the anti-corrosion gas chamber 7 can be monitored in real time after entering the cavity enhanced optical path cell 20, dynamic measurement is realized, and H is deeply researched2S gas is used for establishing the relation between the corrosion rate and the corrosion depth of different material types under different temperatures and different humidities to establish H2And S, a high-temperature corrosion rate model.
When monitoring H2When S adsorption analysis characteristic is adopted, N is adopted by the system2Standard gas and H2S standard gas is proportioned by respective mass flow meters 3 and passes through a high-precision filter element of a filter device 4 to obtain pure and dry H with different concentrations2S gas, opening a needle valve 6-3 No. three, a needle valve 6-5 No. five, a needle valve 6-6 No. six and a needle valve 6-8 No. eight, closing a needle valve 6-1 No. two, a needle valve 6-2 No. four and a needle valve 6-7 No. seven, communicating pipelines among the anti-adsorption air chamber 8, the cavity enhancement optical path pool 20 and the exhaust device to form a serial passage, closing pipelines in front of and behind the back-flushing pump 5 and the anti-corrosion air chamber 7, and closing a pipeline between the cavity enhancement optical path pool 20 and a main pipeline. So that the H after proportioning2The S gas sequentially enters the anti-adsorption gas chamber 8, the cavity enhanced optical path pool 20 and the exhaust device. The anti-adsorption air chamber 8 is provided with a vacuum gauge 12 and a hygrometer 13, so that the internal pressure and humidity of the anti-adsorption air chamber 8 can be monitored in real time, and after being monitored by the cavity enhanced optical path pool 20, gas directly enters the exhaust device. The temperature inside the adsorption preventing gas chamber 8 is changed by the temperature-adjustable high-temperature tank 11. The concentration change in the anti-adsorption air chamber 8 can be monitored in real time after entering the cavity enhanced optical path pool 20, dynamic measurement is realized, and H is deeply researched2And S, establishing an adsorption and analysis compensation model according to the relation between adsorption and analysis of the gas on the surfaces of different materials at different temperatures and different humidities.
When monitoring H2S corrosivity and monitoring H2When S adsorption analysis characteristic is synchronously performed, the gas distribution system, the front needle valve and the rear needle valve of the anti-corrosion gas chamber, the front needle valve and the rear needle valve of the anti-adsorption gas chamber and H can be synchronously opened2S, monitoring needle valves of a front needle valve, a rear needle valve and an exhaust system of the system, namely opening a second needle valve 6-2, a third needle valve 6-3, a fourth needle valve 6-4, a fifth needle valve 6-5, a sixth needle valve 6-6 and an eighth needle valve 6-8, closing a first needle valve 6-1 and a seventh needle valve 6-7, and communicating pipelines among an anti-corrosion air chamber 7, an anti-adsorption air chamber 8, a cavity enhancement optical path pool 20 and an exhaust device. Proportioning different concentrations of H by a mass flowmeter 32And S gas synchronously enters the anti-corrosion gas chamber 7 and the anti-adsorption gas chamber 8, and then is gathered and enters the cavity enhanced optical path pool 20 and the exhaust device. At a certain moment, the monitored data in the cavity enhanced optical path cell 20 is the data in the anti-corrosion gas chamber 7And the data is also the data in the anti-adsorption air chamber 8, so that synchronous monitoring is realized. The temperature of the anti-corrosion air chamber 7 and the anti-adsorption air chamber 8 is changed through the temperature-adjustable high-temperature box 11, the pressure, humidity and concentration changes in the anti-corrosion air chamber 7 and the anti-adsorption air chamber 8 are monitored in real time, and H can be synchronously realized2And (3) researching corrosion mechanisms and adsorption analytical characteristics of different materials by the S gas under working conditions of different temperatures and humidities, and establishing a compensation model.
And after the monitoring is finished, the back-flushing pump 5 can be opened to carry out the integral purging of the system, so that the internal working condition of the system is ensured to meet the experimental requirements. The specific operation is as follows: and (3) continuously keeping the opened needle valves in the monitoring process, opening the first needle valve 6-1 and the seventh needle valve 6-7, and purging the whole pipeline.
The vacuum gauge 12 in the present embodiment is a high-precision vacuum gauge.
The principle of the technical implementation of the scheme is as follows: based on H2S high-temperature corrosion physical and chemical mechanism research, design and construction H2S corrosivity and adsorption characteristic synchronous monitoring experiment system, different concentrations of H are proportioned at the front end of the system through a mass flow meter2S gas is switched by a needle valve (or an electromagnetic valve) to change the concentration H of the gas into different concentrations2The S gas is sent into a self-grinding temperature-adjustable high-temperature box 11 in a plurality of times, and the temperature-adjustable high-temperature box 11 comprises a porous metal material and a spiral pipeline. (1) The corrosion mechanism is researched: high selective absorption and avoidance of H2O and CO2Interfering H2S spectral line, developing a cavity enhanced gas absorption cell with an optical length of more than 500m, and monitoring H in the material corrosion process by combining a cavity enhanced TDLAS technology2The concentration change trend of S, and the chemical corrosion rate and H of different materials in the temperature-adjustable high-temperature box 11 are quantitatively analyzed2And (3) analyzing the surface characterization of the material by combining the relation of factors such as the concentration, the temperature, the humidity and the like and the scanning electron microscope, and establishing an empirical model of the temperature, the humidity and the like, the surface corrosion rate and the corrosion depth. (2) Study of adsorption characteristics: the experiment system can synchronously adopt the cavity enhanced TDLAS technology to monitor H before and after entering the spiral pipeline in a time-sharing manner2S concentration, obtaining the relation of concentration changing along with time, quantitatively calculating the adsorption capacity of the material through the area enclosed by two concentration curves, and analyzingDetermining the adsorption capacity of different materials and materials at different temperatures, determining the optimal material and optimal set temperature, and establishing H2S adsorption analysis compensation model for increasing H2And S, preprocessing the measurement precision.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. H2The S corrosivity and adsorption analytical characteristic synchronous monitoring system is characterized by comprising a gas distribution system and H2The system comprises an S monitoring system, a corrosivity monitoring system and an adsorption analysis monitoring system, wherein the gas distribution system is communicated with H connected in parallel through a main pipeline2The system comprises an S monitoring system, a corrosivity monitoring system and an adsorption analysis monitoring system, wherein parallel branches are communicated with one another, and each parallel branch is provided with a control valve.
2. H according to claim 12The system is characterized by further comprising a temperature adjusting mechanism for adjusting the temperature of an anti-corrosion air chamber in the corrosion monitoring system and the temperature of an anti-adsorption air chamber in the adsorption analysis monitoring system.
3. H according to claim 12S corrosion and adsorption analytical characteristic synchronous monitoring system, characterized by also including the blowback system that is used for blowing and sweeping whole body system internal pipeline after the monitoring is finished each time, and the blowback system communicates on the trunk line.
4. H according to claim 12S corrosivity and adsorption analytical characteristic synchronous monitoring system, characterized in that, the gas distribution system includes N2Gas source and H2S gas source, and connected with mass flow meter, N2Gas source and H2S gas sources are gathered on the main pipeline through a gas circuit, and N is2And H2And a filtering device is communicated with the main pipeline before the S enters each monitoring system.
5. According to claim 1H is as described2S corrosivity and adsorption analytical characteristic synchronous monitoring system, characterized in that, H2The S monitoring system comprises a signal generator, a laser driver, a laser collimator, a beam splitter, a plane gold-plated reflecting mirror, a cavity enhanced optical path cell, an interferometer, a first detector, a second detector and a data processing unit;
the signal generator emits low-frequency triangular waves and high-frequency sine waves which are superposed and coupled to enter the laser driver to drive the laser, light beams are irradiated to the surface of the beam splitter through the laser collimator to form reflected light and transmitted light, the reflected light of the beam splitter is irradiated to the plane gold-plated reflecting mirror to enter the interferometer and the first detector in sequence to carry out frequency spectrum calibration, the transmitted light of the beam splitter enters the cavity enhancement optical path pool, the cavity enhancement optical path pool carries the vacuum gauge, the emergent light enters the second detector to obtain photoelectric signals, and the first detector and the second detector are connected to the data processing unit to carry out H processing2And (4) monitoring and analyzing the S concentration on line.
6. H according to claim 12The system is characterized by comprising an anti-corrosion air chamber, wherein a replaceable metal material to be detected is arranged in the anti-corrosion air chamber, and the anti-corrosion air chamber is provided with a vacuum gauge and a hygrometer.
7. H according to claim 12S corrosivity and adsorption analysis characteristic synchronous monitoring system, its characterized in that, adsorption analysis monitoring system includes prevents that the adsorption chamber embeds has adsorption equipment, prevents that the adsorption chamber carries on vaccum meter and hygrometer.
8. H according to claim 12The system is characterized in that the temperature adjusting mechanism is a temperature-adjustable high-temperature box, the anti-corrosion air chamber and the anti-adsorption air chamber are both arranged in the temperature-adjustable high-temperature box, and the vacuum gauge and the hygrometer which are carried on the anti-corrosion air chamber and the anti-adsorption air chamber are both arranged outside the temperature-adjustable high-temperature box.
9. A H according to any one of claims 1 to 82The static monitoring method of the S corrosion and adsorption analytical characteristic synchronous monitoring system is characterized by comprising the following steps:
S1，N2gas source and H2S gas source is proportioned by a mass flow meter and passes through a filtering device to obtain H with different concentrations2S gas;
s2, when monitoring H2S, when the mixture is corrosive, the pipelines between the anti-corrosion air chamber and the cavity-enhanced optical path pool are communicated to form a loop, and the pipelines in front of and behind the back-blowing system and the adsorption-resistant air chamber are closed, so that the proportioned H2S gas synchronously enters the anti-corrosion gas chamber and the cavity-enhanced optical path pool, the temperature of the anti-corrosion gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, humidity and concentration change in the anti-corrosion gas chamber is monitored in real time, and H is obtained2S, the relationship between the corrosion rate and the corrosion depth of the gas to different material types at different temperatures and different humidities;
when monitoring H2When S adsorbs the analytic characteristic, the pipeline between the anti-adsorption air chamber and the cavity enhanced optical path pool is communicated to form a loop, and the pipeline in front of and behind the back flushing system and the anti-corrosion air chamber is closed, so that the proportioned H2S gas synchronously enters the anti-adsorption gas chamber and the cavity enhanced optical path pool, the temperature of the anti-adsorption gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, the humidity and the concentration change in the anti-adsorption gas chamber are monitored in real time, and H is obtained2S, the relationship between adsorption and analysis of gas on the surfaces of different materials at different temperatures and different humidities;
and S3, opening a back-flushing pump and an exhaust device to perform system integral purging after each monitoring is finished.
10. A H according to any one of claims 1 to 82The dynamic monitoring method of the S corrosion and adsorption analytical characteristic synchronous monitoring system is characterized by comprising the following steps:
S1，N2gas source and H2S gas source is proportioned by a mass flow meter and passes through a filtering device to obtain H with different concentrations2S gas;
s2, when monitoring H2S, when the gas is corrosive, the pipelines among the anti-corrosion gas chamber, the cavity enhanced optical path pool and the exhaust device are communicated, the pipelines in front of and behind the back-blowing system and the adsorption-preventing gas chamber are closed, and the pipeline between the cavity enhanced optical path pool and the main pipeline is closed, so that the proportioned H2S gas sequentially enters the anti-corrosion gas chamber, the cavity enhanced optical path pool and the exhaust device, the temperature of the anti-corrosion gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, humidity and concentration change in the anti-corrosion gas chamber is monitored in real time, and H is obtained2S, the relationship between the corrosion rate and the corrosion depth of the gas to different material types at different temperatures and different humidities;
when monitoring H2When S adsorbs the analytic characteristic, the pipelines among the anti-adsorption air chamber, the cavity enhanced optical path pool and the exhaust device are communicated, the pipelines in front of and behind the back flushing system and the anti-corrosion air chamber are closed, and the pipeline between the cavity enhanced optical path pool and the main pipeline is closed, so that the proportioned H2S gas sequentially enters the anti-adsorption gas chamber, the cavity enhanced optical path pool and the exhaust device, the temperature of the anti-adsorption gas chamber is changed through the temperature-adjustable high-temperature box, the pressure, humidity and concentration change in the anti-adsorption gas chamber is monitored in real time, and H is obtained2S, the relationship between adsorption and analysis of gas on the surfaces of different materials at different temperatures and different humidities;
when monitoring H2S corrosivity and monitoring H2When S adsorption analysis characteristic is synchronously carried out, pipelines among the anti-corrosion air chamber, the anti-adsorption air chamber, the cavity enhanced optical path pool and the exhaust device are communicated, and a back flushing system and a pipeline between the cavity enhanced optical path pool and a main pipeline are closed, so that the proportioned H2S gas simultaneously enters an anti-corrosion air chamber and an anti-adsorption air chamber, then the gas is gathered and sequentially enters a cavity enhanced optical path pool and an exhaust device, the temperature of the anti-corrosion air chamber and the anti-adsorption air chamber is changed through a temperature-adjustable high-temperature box, the pressure, humidity and concentration changes in the anti-corrosion air chamber and the anti-adsorption air chamber are monitored in real time, and H is obtained2The relationship between the corrosivity and adsorption and analysis characteristics of S gas to different materials at different temperatures and different humidities.
And S3, opening a back-flushing pump and an exhaust device to perform system integral purging after each monitoring is finished.
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