CN117288888A - System and method for sampling and testing oxysulfide in catalytic regeneration flue gas - Google Patents
System and method for sampling and testing oxysulfide in catalytic regeneration flue gas Download PDFInfo
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- CN117288888A CN117288888A CN202210694167.7A CN202210694167A CN117288888A CN 117288888 A CN117288888 A CN 117288888A CN 202210694167 A CN202210694167 A CN 202210694167A CN 117288888 A CN117288888 A CN 117288888A
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000003546 flue gas Substances 0.000 title claims abstract description 116
- 238000012360 testing method Methods 0.000 title claims abstract description 89
- 238000005070 sampling Methods 0.000 title claims abstract description 35
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 22
- 230000008929 regeneration Effects 0.000 title claims abstract description 22
- 238000011069 regeneration method Methods 0.000 title claims abstract description 22
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 25
- 239000000779 smoke Substances 0.000 claims abstract description 41
- 238000010521 absorption reaction Methods 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910052815 sulfur oxide Inorganic materials 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 85
- 239000006096 absorbing agent Substances 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 32
- 229920000557 Nafion® Polymers 0.000 claims description 25
- 238000001179 sorption measurement Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000010998 test method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 52
- 239000003570 air Substances 0.000 description 36
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 13
- 238000001514 detection method Methods 0.000 description 11
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000012080 ambient air Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- 125000000542 sulfonic acid group Chemical group 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007791 dehumidification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000126 substance Substances 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
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D49/00—Separating dispersed particles from gases, air or vapours by other methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
- G01N1/2258—Sampling from a flowing stream of gas in a stack or chimney
-
- 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
- G01N21/17—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
- G01N1/2258—Sampling from a flowing stream of gas in a stack or chimney
- G01N2001/2261—Sampling from a flowing stream of gas in a stack or chimney preventing condensation (heating lines)
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a sampling test system and a sampling test method for sulfur oxides in catalytic regeneration flue gas, wherein the system comprises a heating smoke gun, a first connecting pipeline, a second connecting pipeline, a first flowmeter, a third flowmeter and SO 2 Test unit and SO x Total test unit, x=2 or 3; wherein the heating smoke gun distributes collected smoke to a first connecting pipeline and a second connecting pipeline, and the first connecting pipeline is sequentially provided with a first flowmeter and SO 2 The test unit is provided with a third flowmeter and an SO (SO) in sequence on the second connecting pipeline x A total amount test unit;the SO x The total amount testing unit is used for adding absorption liquid into the flue gas to remove SO x Conversion to SO 4 2‑ And is used for measuring SO 4 2‑ The concentration of (2) and the volume of absorption liquid added; the SO 2 The test unit is used for measuring SO in the flue gas 2 Is a concentration of (3). The system of the invention ensures that the test result is more accurate and stable, the operation is convenient, and the practicability is high.
Description
Technical Field
The invention belongs to the field of gas detection, and relates to a sampling and testing system and method for sulfur oxides in catalytic regeneration flue gas.
Background
SO is carried out by the catalytic cracking device by adopting a wet desulfurization process 2 The emission reduction is realized, but because the flue gas heat exchanger is canceled, the regenerated flue gas is directly discharged to the atmosphere after desulfurization, so that the discharged flue gas has the characteristics of low flue gas temperature, high humidity and the like, and colored smoke plumes of different degrees appear in the discharged flue gas. In the atmosphere, sulfur trioxide is a major component of secondary aerosols and is also a major cause of acid rain formation. At present, a great deal of research considers that the cause of blue smoke plume is due to the higher SO content in the smoke 3 And the like can coagulate particulate matters and SO in flue gas 3 PM in the ambient air due to the condensable particulate matters 2.5 The effect of (2) is more pronounced. Thus, for devices with blue plume appearance, SO should be performed 3 Is reduced in emission by depth; blue smoke plume does not appear, and the SO in the smoke is also dealt with 3 Measurements were made and their effect on the surrounding atmosphere quality was analyzed.
At present, the main test methods of sulfur trioxide at home and abroad are a control condensation method, an isopropyl alcohol absorption method, a gas spectrum analysis method and the like. Wherein SO is 3 Is of the absorption spectrum of (a)SO 2 The absorption spectra of the (2) are similar, and when the spectrum analysis is directly carried out on the discharged smoke, the spectrum analysis equipment can not accurately measure SO 3 Concentration. The isopropyl alcohol absorption method is also a sampling measurement method recommended in developed countries such as U.S. EPA and Japanese JIS. But the sampling process of the isopropyl alcohol absorption method is affected by various factors, such as SO 2 Is oxidized after being dissolved in isopropanol solution, takes a long time to be sent to a laboratory for detection after sampling is completed, and dilution of the isopropanol solution during detection can cause SO 3 2- Oxidized, resulting in higher values.
Disclosure of Invention
In view of the above problems, an object of the present invention is to: the system and the method for sampling and testing the sulfur oxides in the catalytic regeneration flue gas are reliable and stable in structure, high in accuracy and high in automation degree, and can effectively solve the problem of sulfur trioxide detection.
In order to achieve the above object, the present invention provides the following technical solutions:
a sampling and testing system for sulfur oxides in catalytic regeneration flue gas comprises a heating smoke gun, a first connecting pipeline, a second connecting pipeline, a first flowmeter, a third flowmeter and SO 2 Test unit and SO x Total test unit, x=2 or 3;
the heating smoke gun is used for detecting smoke collected in a sampling environment, the heating smoke gun distributes the collected smoke to a first connecting pipeline and a second connecting pipeline, and the first connecting pipeline is sequentially provided with a first flowmeter and an SO (SO) 2 The test unit is provided with a third flowmeter and an SO (SO) in sequence on the second connecting pipeline x A total amount test unit;
the SO x The total amount testing unit is used for adding absorption liquid into the flue gas to remove SO x Conversion to SO 4 2- And is used for measuring SO 4 2- The concentration of (2) and the volume of absorption liquid added;
the SO 2 The test unit is used for measuring SO in the flue gas 2 Is a concentration of (3).
Preferably, the flue gas of the heating smoke gun is distributed to the first connecting pipeline and the second connecting pipeline through the first air pump.
Preferably, synchronization is set between the first flowmeter and the third flowmeter, and the intake air amounts of the first flowmeter and the third flowmeter are kept the same.
Preferably, the SO 2 The test unit comprises a Nafion tube dryer and a first SO which are connected in sequence 2 A measuring instrument;
wherein, the Nafion tube dryer is connected with the output of first flowmeter.
Preferably, the SO 2 The test unit further comprises a first SO 2 The tester is connected with the first activated carbon adsorption unit and the third air pump in sequence.
Preferably, the SO 2 The test unit further comprises an air compressor, a silica gel drying unit, a second activated carbon adsorption unit, a particulate filter and a second flowmeter which are connected in sequence;
and the output end of the second flowmeter is connected with a Nafion tube dryer.
Preferably, the absorption liquid is NaOH solution and KMnO 4 A solution.
Preferably, the SO x The total amount test unit comprises SO x Absorber, naOH reservoir, fourth flowmeter, KMnO 4 Reservoir, fifth flow meter, pH detector and SO 4 2- A detector;
wherein the SO x The absorber is connected with the output end of the third flowmeter, and the NaOH storage is connected with SO through the fourth flowmeter x Absorber connection, KMnO 4 The reservoir is connected with SO through a fifth flowmeter x Absorber connection, pH detector and SO 4 2- The detectors are all with SO x The absorber is connected.
Preferably, the SO x The total amount test unit also comprises a test agent and an SO x Second SO with absorber connected in turn 2 The device comprises a detector, a third activated carbon adsorption unit and a fourth air pump.
Preferably, the SO x An air-equalizing pore plate is arranged in the absorber.
Preferably, the third flowmeter is connected with a second SO 2 An interlocking device is arranged between the detectors, if the second SO 2 The detector detects SO 2 The concentration, the third flowmeter is immediately turned off.
A method for sampling and testing sulfur oxides in catalytic regeneration flue gas comprises the following specific steps:
the flue gas is collected by adopting a heating smoke gun which distributes the collected flue gas to a first connecting pipeline and a second connecting pipeline, and the air inflow of the first connecting pipeline and the air inflow of the second connecting pipeline are controlled to be the same through a first flowmeter arranged on the first connecting pipeline and a third flowmeter arranged on the second connecting pipeline; simultaneously, recording the time of introducing the flue gas into the first connecting pipeline and the second connecting pipeline as t;
the flue gas entering the first connecting pipeline sequentially enters the first flowmeter and the SO 2 The test unit obtains the volume V of the smoke in the time t based on the first flowmeter 1 Adopting SO 2 SO of the flue gas is measured by the test unit 2 Concentration C 1 ，
The flue gas entering the second connecting pipeline sequentially enters the third flowmeter and the SO x A total amount test unit; by SO x The absorption liquid in the total amount test unit is used for introducing SO x Conversion to SO 4 2- And measure SO 4 2- Is of concentration C 2 And the volume of the absorption liquid added is V, wherein x=2 or 3;
calculating to obtain SO in the flue gas of the second connecting pipeline within time t x Total amount is N 1 ＝C 2 X V, SO in the flue gas of the first connecting pipeline within time t 2 Total amount is N 2 ＝C 1 ×V 1 SO in the flue gas of the first connecting pipeline or the second connecting pipeline in time t 3 Total n=n 1 －N 2 SO in flue gas 3 Concentration c=n/V 1 。
Preferably, the absorption liquid is NaOH solution and KMnO 4 Solution, measuring the volume of NaOH solution added into the flue gas to be V 2 Adding KMnO into flue gas 4 Bulk of solutionThe product is V 3 The volume of the added absorption liquid is v=v 2 +V 3 。
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts SO 2 The test unit measures SO in the first connecting pipeline 2 Concentration of SO in flue gas is measured 2 Concentration C 1 Obtaining the volume V of the flue gas in the time t based on the first flowmeter 1 Obtaining SO in the flue gas 2 Total N 2 ＝C 1 ×V 1 The method comprises the steps of carrying out a first treatment on the surface of the The invention adopts SO x The total amount test unit measures SO in the solution 4 2- Concentration C of (2) 2 And adding the volume V of the absorption liquid to obtain SO in the flue gas 3 And SO 2 Total N 1 ＝C 2 X V; by combining it with SO 2 Total N 2 Comparing SO within the time t of availability 3 The method can effectively avoid SO in the sampling and testing process 2 The factors such as oxidation cause errors, improve the test accuracy, make the result more accurate stable, convenient operation, the practicality is high.
2. The invention adopts a Nafion tube dryer to contain SO 3 The flue gas is dried and dehumidified, the drying gas is directly collected from the ambient air, the gas collected from the air is compressed by an air compressor, a silica gel drying unit is dried and dehumidified, an activated carbon adsorption unit is purified, a particulate filter filters particulate matters in the gas, the drying and cleaning of the air are ensured, finally, the drying gas is introduced into an external sleeve of a Nafion tube dryer after the flow rate is controlled by a second flowmeter, and the SO can be ensured to be dehumidified 3 The service life of the nafion tube is prolonged, and the accuracy of data in the measuring process is improved;
in addition, the sulfonic acid group in the Nafion molecular structure has higher hydrophilicity, the moisture absorbed by the Nafion tube wall is transferred from one sulfonic acid group to the other sulfonic acid group, finally reaches the tube wall at the other side and is taken away by the dry back-blowing gas, SO that the Nafion tube dryer has higher selectivity, condensed water is not separated out in a mode of selective gaseous dehumidification of the Nafion tube dryer through the Nafion membrane, and SO is avoided 2 ，SO 3 DissolvingResulting in measurement errors and corrosion of equipment due to acidic substances generated after dissolution.
3. The invention uses the synchronous arrangement of the first flowmeter and the third flowmeter to ensure that the flows in the two flue gas measuring pipelines (the first connecting pipeline and the second connecting pipeline) are the same, thereby improving the detection accuracy.
4. The invention adopts NaOH solution and KMnO 4 The solution is absorption solution, SO x Conversion to SO 4 2- Specifically, the NaOH solution absorbs SO in the second connecting line 3 And SO 2 With SO 3 And SO 2 Dissolving the generated H 2 SO 4 、H 2 SO 3 The reaction generates more stable Na 2 SO 4 、Na 2 SO 3 And NaHSO 3 After that KMnO is added 4 Solution Na 2 SO 3 And NaHSO 3 Oxidation to stable Na 2 SO 4 Avoid Na 2 SO 3 And NaHSO 3 With subsequent SO 2 Is introduced into the reactor, the reaction reaches equilibrium, and SO is caused 2 Absorption stagnates, improves the detection precision.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a sample testing system according to the present invention.
In the figure: 1. heating the smoke gun; 2. a first air pump; 3. a first flowmeter; 4. a Nafion tube dryer;5. first SO 2 A measuring instrument; 6. a first activated carbon adsorption unit; 7. a third air pump; 8. a second air pump; 9. a second flowmeter; 10. a particulate filter; 11. a second activated carbon adsorption unit; 12. a silica gel drying unit; 13. an air compressor; 14. a third flowmeter; 15. SO (SO) x An absorber; 16. a gas-equalizing pore plate; 17. a pH detector; 18. SO (SO) 4 2- A detector; 19. a NaOH reservoir; 20. a fourth flow meter; 21. a fifth flowmeter; 22. KMnO 4 A reservoir; 23. second SO 2 A measuring instrument; 24. a third activated carbon adsorption unit; 25. and a fourth air pump.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in FIG. 1, the invention discloses a sampling and testing system for sulfur oxides in catalytic regeneration flue gas, which comprises a heating smoke gun 1, a first connecting pipeline, a second connecting pipeline, a first flowmeter 3, a third flowmeter 14 and SO 2 Test unit and SO x Total test unit, x=2 or 3;
the heating smoke gun 1 is used for detecting smoke in a sampling environment to collect the smoke, the heating smoke gun 1 distributes the collected smoke to a first connecting pipeline and a second connecting pipeline, and the first connecting pipeline is sequentially provided with a first flowmeter 3 and an SO (SO) 2 The test unit is provided with a third flowmeter 14 and SO in sequence on the second connecting pipeline x A total amount test unit;
the SO x The total amount testing unit is used for adding absorption liquid into the flue gas to remove SO x Conversion to SO 4 2- And is used for measuring SO 4 2- The concentration of (2) and the volume of absorption liquid added;
SO 2 the test unit is used for measuring SO in the flue gas 2 Is a concentration of (3).
The invention adopts SO 2 The test unit measures SO in the first connecting pipeline 2 Concentration of SO in flue gas is measured 2 Concentration C 1 The volume V of the flue gas within a time t (here, the time of introducing the flue gas to the first connecting pipeline and the second connecting pipeline is t) is obtained based on the first flowmeter 1 Obtaining SO in the flue gas 2 Total N 2 ＝C 1 ×V 1 The method comprises the steps of carrying out a first treatment on the surface of the The invention adopts SO x The total amount test unit measures SO in the solution 4 2- Concentration C of (2) 2 And adding the volume V of the absorption liquid in the time t to obtain SO in the flue gas 3 And SO 2 Total N 1 ＝C 2 X V; by combining it with SO 2 Total N 2 Comparing SO within the time t of availability 3 The method can effectively avoid SO in the sampling and testing process 2 The factors such as oxidation cause errors, improve the test accuracy, make the result more accurate stable, convenient operation, the practicality is high.
Preferably, the heating smoke gun 1 distributes the collected smoke to the first connecting pipeline and the second connecting pipeline through the first air pump 2.
Preferably, synchronization is set between the first flowmeter 3 and the third flowmeter 14, and the intake air amounts of both are kept the same; the invention uses the synchronous arrangement of the first flowmeter 3 and the third flowmeter 14 to ensure that the flows in the two flue gas measuring pipelines (the first connecting pipeline and the second connecting pipeline) are the same, thereby improving the detection accuracy.
Preferably, the SO 2 The test unit comprises a Nafion tube dryer 4 and a first SO which are connected in sequence 2 A measuring instrument 5; wherein the Nafion tube dryer 4 is connected to the output of the first flowmeter 3. The invention adopts the Nafion tube dryer 4 to dry and dehumidify the flue gas, and adopts the first SO after the flue gas is dried and dehumidified 2 Measurement of SO by the measuring instrument 5 2 The accuracy of the test is improved.
Preferably, the SO 2 The test unit further comprises a first SO 2 First living organism with measuring instrument 5 connected in turnA charcoal adsorption unit 6 and a third air pump 7. Tested for SO 2 The flue gas after concentration is absorbed and purified by the first activated carbon absorption unit 6 and then is discharged into the atmosphere through the third air pump 7, so that the pollution to the atmosphere is avoided.
Preferably, the SO 2 The test unit further comprises an air compressor 13, a silica gel drying unit 12, a second activated carbon adsorption unit 11, a particulate filter 10 and a second flowmeter 9 which are connected in sequence; wherein the output end of the second flowmeter 9 is connected with the Nafion tube dryer 4. The Nafion tube dryer 4 of the invention directly collects the gas for drying from the ambient air, the gas collected from the air is compressed by the air compressor 13, the silica gel drying unit 12 is dried and dehumidified, the activated carbon adsorption unit 11 is purified, the particulate matter in the gas is filtered by the particulate matter filter 10, the drying and cleaning of the air are ensured, finally the gas for drying in the outer sleeve of the Nafion tube dryer 4 is introduced after the flow rate is controlled by the second flowmeter 9, SO that the SO can be ensured while the dehumidification is ensured 3 And the service life of the Nafion tube dryer 4 is prolonged, the accuracy of data in the measuring process is improved, and the flowing direction of the drying air is opposite to the flowing direction of the flue gas when the device is used. A second air pump 8 is arranged at the air outlet of the Nafion tube dryer 4.
Preferably, the absorption liquid is NaOH solution and KMnO 4 Solution of SO x The total amount test unit comprises SO x Absorber 15, naOH reservoir 19, fourth flowmeter 20, KMnO 4 Reservoir 22, fifth flow meter 21, pH detector 17 and SO 4 2- A detector 18; wherein the SO x The absorber 15 is connected to the output of the third flowmeter 14, and the NaOH reservoir 19 is connected to the SO via a fourth flowmeter 20 x Absorber 15 is connected to KMnO 4 The reservoir 22 is connected with SO via a fifth flowmeter 21 x Absorber 15 is connected, pH detector 17 and SO 4 2- The detectors 18 are all connected with SO x Absorber 15 is connected.
The invention adopts NaOH solution and KMnO 4 The solution is absorption solution, SO x Conversion to SO 4 2- Specifically, the NaOH solution absorbs SO in the second connecting line 3 And SO 2 With SO 3 And SO 2 Dissolving the generated H 2 SO 4 、H 2 SO 3 The reaction generates more stable Na 2 SO 4 、Na 2 SO 3 And NaHSO 3 After that KMnO is added 4 Solution Na 2 SO 3 And NaHSO 3 Oxidation to stable Na 2 SO 4 Avoid Na 2 SO 3 And NaHSO 3 With subsequent SO 2 Is introduced into the reactor, the reaction reaches equilibrium, and SO is caused 2 Absorption stagnates, improves the detection precision. By providing the fourth flowmeter 20 and the fifth flowmeter 21, the NaOH solution and KMnO can be measured 4 The volume of the solution added was calculated by recording the addition time. By arranging SO 4 2- A detector 18 for detecting SO in the solution 4 2- Is a concentration of (2); by setting the pH detector 17 for determining the addition of KMnO 4 When the pH value of the solution is lower than 9, which is detected by the pH detector 17, the fifth flowmeter 21 is started, and KMnO is used 4 Reservoir 22 to SO x KMnO is added dropwise into absorber 15 4 A solution.
Preferably, the SO x The total amount test unit also comprises a test agent and an SO x Second SO with absorber 15 connected in sequence 2 A detector 23, a third activated carbon adsorption unit 24 and a fourth air pump 25.
By arranging a second SO 2 Detector 23, when the second SO 2 The detector 23 detects SO 2 The third flowmeter 14 is immediately turned off to stop the flow of flue gas into the second connecting line, thereby ensuring the flow of SO x The flue gas in the absorber 15 is totally converted into SO 4 2- Thereby ensuring the accuracy of the detection result. Into a second SO 2 The flue gas of detector 23 after the purification of third active carbon adsorption unit 24, in the atmospheric air through fourth air pump 25, avoided the pollution to the atmosphere.
Preferably, the SO x An air-equalizing orifice 16 is arranged in the absorber 15, specifically, the air-equalizing orifice 16 is fixed on SO x The inner wall of the absorber 15 is uniformly provided with mesh holes on a gas-equalizing pore plate 16, and in the second connecting pipeline, the flue gas passes through the third flow rateMeter 14 controls flow rate into SO x The absorber 15 is evenly distributed under the action of the air-equalizing pore plate 16.
Preferably, the third flowmeter 14 is coupled with a second SO 2 An interlocking device is arranged between the detectors 23, if a second SO 2 The detector 23 detects SO 2 The concentration, the third flowmeter 14 is immediately turned off. The design idea here is: first at SO x An amount of NaOH solution is added to absorber 15 for absorbing SO x When the second SO 2 The detector 23 detects SO 2 When the absorption of NaOH solution is saturated, the automatic interlock closes the third flowmeter 14 and the flow is to SO x KMnO is added to absorber 15 4 Solution oxidation of all SO 3 2- And HSO 3 - Is SO 4 2- . This ensures the passage into the SO x The flue gas in the absorber 15 is totally converted into SO 4 2- Thereby ensuring the accuracy of the detection result.
The invention also discloses a method for sampling and testing the oxysulfide in the catalytic regeneration flue gas, which comprises the following specific steps:
the flue gas is collected by adopting a heating smoke gun 1 to be detected in a sampling environment, the heating smoke gun 1 distributes the collected flue gas to a first connecting pipeline and a second connecting pipeline, and the air inflow of the first connecting pipeline and the air inflow of the second connecting pipeline are controlled to be the same through a first flowmeter 3 arranged on the first connecting pipeline and a third flowmeter 14 arranged on the second connecting pipeline; simultaneously, recording the time of introducing the flue gas into the first connecting pipeline and the second connecting pipeline as t;
the flue gas entering the first connecting pipe sequentially enters the first flowmeter 3 and the SO 2 The test unit obtains the volume V of the flue gas in time t based on the first flowmeter 3 1 Adopting SO 2 SO of the flue gas is measured by the test unit 2 Concentration C 1 ，
The flue gas entering the second connecting pipeline sequentially enters the third flowmeter 14 and the SO x A total amount test unit; by SO x The total amount testing unit adds absorption liquid into the flue gas to add SO x Conversion to SO 4 2 And measure SO4 2- Is of concentration C 2 And the volume of the absorption liquid added is V, wherein x=2 or 3;
calculating to obtain SO in the flue gas of the second connecting pipeline within time t x Total amount is N 1 ＝C 2 X V, SO in the flue gas of the first connecting pipeline within time t 2 Total amount is N 2 ＝C 1 ×V 1 SO in the flue gas of the first connecting pipeline or the second connecting pipeline in time t 3 Total n=n 1 －N 2 SO in flue gas 3 Concentration c=n/V 1 。
Preferably, the absorption liquid is NaOH solution and KMnO 4 Solution, measuring the volume of NaOH solution added into the flue gas to be V 2 Adding KMnO into flue gas 4 The volume of the solution is V 3 The volume of the added absorption liquid is v=v 2 +V 3 。
The invention adopts NaOH solution and KMnO 4 The solution is absorption solution, SO x Conversion to SO 4 2- Specifically, the NaOH solution absorbs SO in the second connecting line 3 And SO 2 With SO 3 And SO 2 Dissolving the generated H 2 SO 4 、H 2 SO 3 The reaction generates more stable Na 2 SO 4 、Na 2 SO 3 And NaHSO 3 After that KMnO is added 4 Solution Na 2 SO 3 And NaHSO 3 Oxidation to stable Na 2 SO 4 Avoid Na 2 SO 3 And NaHSO 3 With subsequent SO 2 Is introduced into the reactor, the reaction reaches equilibrium, and SO is caused 2 Absorption stagnates, improves the detection precision.
The following is an example of a test for sampling sulfur dioxide and sulfur trioxide in flue gas at the outlet of a wet desulfurization system of a catalytic cracking device, and the specific process of the test method of the invention is as follows:
before the S1 test starts, the fourth flowmeter 20 is started and the NaOH storage 21 is used for supplying SO x NaOH solution with concentration of 2mol/L is dripped into the absorber 15, then the air compressor 13 is started, and the dry gas collecting ambient air passes through the silica gel drying unit 12And after the active carbon adsorption unit 11 purifies and the particulate filter 10 removes filterable particulate matters, the particulate matters enter the sleeve of the Nafion tube dryer 4 through the second flowmeter 9 by controlling the flow rate, and the flowing direction of the drying air is opposite to the flowing direction of the flue gas.
S2, placing the heating smoke gun 1 in a smoke flue, wherein the smoke is provided with negative pressure by a first air pump 2 and enters two connecting pipelines (a first connecting pipeline and a second connecting pipeline) through the heating smoke gun 1, and the sampling flow of the heating smoke gun 1 is 1L/min; recording the time of introducing the flue gas into the first connecting pipeline and the second connecting pipeline as t.
S3, controlling the air inlet flow to be 0.5L/min through the first flowmeter 3 by the flue gas entering the first connecting pipeline; obtaining the volume V of the flue gas in time t based on the first flowmeter 3 1 (specifically, the volume of the flue gas is equal to the time t multiplied by the flow rate of the first flowmeter 3), and the flue gas is dehumidified in the Nafion tube dryer 4 and then introduced into the first SO 2 A measuring instrument 5 for obtaining SO in the flue gas 2 Concentration C 1 SO SO in the flue gas of the first connecting pipeline in time t 2 Total amount is N 2 ＝C 1 ×V 1 。
S4, after the measurement of the flue gas in the first connecting pipeline is completed, the flue gas is purified by the first activated carbon adsorption unit 6 and then discharged by the third air pump 7;
s5, the flue gas entering the second connecting pipeline is controlled to flow through the third flowmeter 14 to be the same as that of the first flowmeter 3, namely, the flue gas flows inwards SO x The volume of the flue gas introduced into the absorber 15 is V 1 The method comprises the steps of carrying out a first treatment on the surface of the Flue gas enters SO x The absorber 15 is used for uniformly distributing the flue gas under the action of the gas-equalizing pore plate 16, absorbing the flue gas by NaOH solution, and starting the fifth flowmeter 21 when the pH value detected by the pH detector 17 is lower than 9, and measuring KMnO 4 Reservoir 22 to SO x KMnO is added dropwise into absorber 15 4 Solution of SO 2 Dissolving the generated SO 3 2- And HSO 3 - Oxidation to stable SO 4 2- ；
SO 4 2- The detector 18 detects SO in the solution 4 2- Concentration C 2 The NaOH solution volume V is obtained based on the fourth flowmeter 20 2 (specifically, naOH is dissolved thereinThe liquid volume is equal to the flow rate measured by the fourth flow meter 20 times the time of NaOH solution addition), KMnO is obtained based on the fifth flow meter 21 4 Volume of solution V 3 (specifically, KMnO herein 4 The solution volume is equal to the flow measured by the fourth flow meter 20 multiplied by KMnO 4 The time of solution addition), SO the SO in the flue gas x Total amount is N 1 ＝C 2 ×(V 2 +V 3 )。
S6 flue gas in second connecting pipeline is in SO x Absorbing in absorber 15 and introducing a second SO 2 In the measuring instrument 23, if SO can be measured 2 The concentration is programmed to automatically shut down the third flowmeter 14.
S7 according to the test result, SO 3 Total amount is n=n 1 －N 2 Concentration of c=n/V 1 。
Although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (13)
1. A sampling and testing system for sulfur oxides in catalytic regeneration flue gas is characterized by comprising a heating smoke gun (1), a first connecting pipeline, a second connecting pipeline, a first flowmeter (3), a third flowmeter (14) and SO 2 Test unit and SO x Total test unit, x=2 or 3;
the heating smoke gun (1) is used for detecting smoke in a sampling environment to collect the smoke, the heating smoke gun (1) distributes the collected smoke to a first connecting pipeline and a second connecting pipeline, and the first connecting pipeline is sequentially provided with a first flowmeter (3) and an SO (SO) 2 The test unit is provided with a third flowmeter (14) and SO (SO) in sequence on the second connecting pipeline x A total amount test unit;
the SO x The total amount testing unit is used for adding absorption liquid into the flue gas to remove SO x Conversion to SO 4 2- And is used for measuring SO 4 2- The concentration of (2) and the volume of absorption liquid added;
the SO 2 The test unit is used for measuring SO in the flue gas 2 Is a concentration of (3).
2. A catalytic regeneration flue gas sampling test system according to claim 1, wherein the flue gas of the heating lance (1) is distributed via a first air pump (2) to a first connection line and a second connection line.
3. A catalytic regeneration flue gas sampling test system according to claim 1 or 2, wherein synchronization is provided between the first flowmeter (3) and the third flowmeter (14), and the intake air amounts of both are kept the same.
4. A catalytic regeneration flue gas sampling test system according to claim 1, wherein the SO 2 The test unit comprises a Nafion tube dryer (4) and a first SO which are connected in sequence 2 A measuring instrument (5);
wherein the Nafion tube dryer (4) is connected with the output end of the first flowmeter (3).
5. The catalytic regeneration flue gas sampling test system according to claim 4, wherein the SO 2 The test unit further comprises a first SO 2 The tester (5) is sequentially connected with a first activated carbon adsorption unit (6) and a third air pump (7).
6. The catalytic regeneration flue gas sampling test system according to claim 4, wherein the SO 2 The test unit further comprises an air compressor (13), a silica gel drying unit (12), a second activated carbon adsorption unit (11), a particulate filter (10) and a second flowmeter (9) which are connected in sequence;
the output end of the second flowmeter (9) is connected with the Nafion tube dryer (4).
7. The catalytic regeneration flue gas sampling test system according to claim 1, wherein the absorption liquid is NaOH solution and KMnO 4 A solution.
8. The catalytic regeneration flue gas sampling test system according to claim 7, wherein the SO x The total amount test unit comprises SO x Absorber (15), naOH reservoir (19), fourth flowmeter (20), KMnO 4 A reservoir (22), a fifth flowmeter (21), a pH detector (17) and SO 4 2- A detector (18);
wherein the SO x The absorber (15) is connected with the output end of the third flowmeter (14), and the NaOH storage (19) is connected with SO through the fourth flowmeter (20) x Absorber (15) is connected with KMnO 4 The reservoir (22) is connected with SO through a fifth flowmeter (21) x An absorber (15) is connected, the pH detector (17) and SO 4 2- The detectors (18) are all connected with SO x The absorber (15) is connected.
9. The catalytic regeneration flue gas sampling test system according to claim 8, wherein the SO x The total amount test unit also comprises a test agent and an SO x Second SO with absorber (15) connected in turn 2 The device comprises a detector (23), a third activated carbon adsorption unit (24) and a fourth air pump (25).
10. The catalytic regeneration flue gas sampling test system according to claim 8, wherein the SO x An air-equalizing pore plate (16) is arranged in the absorber (15).
11. A catalytic regeneration flue gas sampling test system according to claim 9, wherein the third flowmeter (14) is in communication with the second SO 2 An interlocking device is arranged between the detectors (23), if a second SO 2 The detector (23) detects SO 2 Concentration of then thirdThe flowmeter (14) is immediately shut off.
12. A method for sampling and testing sulfur oxides in catalytic regeneration flue gas is characterized by comprising the following specific steps:
the flue gas is collected by adopting a heating smoke gun (1) to explore a sampling environment, the heating smoke gun (1) distributes the collected flue gas to a first connecting pipeline and a second connecting pipeline, and the air inflow of the first connecting pipeline and the air inflow of the second connecting pipeline are controlled to be the same through a first flowmeter (3) arranged on the first connecting pipeline and a third flowmeter (14) arranged on the second connecting pipeline; simultaneously, recording the time of introducing the flue gas into the first connecting pipeline and the second connecting pipeline as t;
the flue gas entering the first connecting pipeline sequentially enters the first flowmeter (3) and the SO 2 The test unit obtains the volume V of the flue gas in the time t based on the first flowmeter (3) 1 Adopting SO 2 SO of the flue gas is measured by the test unit 2 Concentration C 1 ，
The flue gas entering the second connecting pipeline sequentially enters a third flowmeter (14) and SO x A total amount test unit; by SO x The absorption liquid in the total amount test unit is used for introducing SO x Conversion to SO 4 2- And measure SO 4 2- Is of concentration C 2 And the volume of the absorption liquid added is V, wherein x=2 or 3;
calculating to obtain SO in the flue gas of the second connecting pipeline within time t x Total amount is N 1 ＝C 2 X V, SO in the flue gas of the first connecting pipeline within time t 2 Total amount is N 2 ＝C 1 ×V 1 SO in the flue gas of the first connecting pipeline or the second connecting pipeline in time t 3 Total n=n 1 －N 2 SO in flue gas 3 Concentration c=n/V 1 。
13. The method for sampling sulfur oxides in catalytic regeneration flue gas according to claim 12, wherein the absorption liquid is NaOH solution and KMnO 4 Solution, measuring the volume of NaOH solution added into the flue gas to be V 2 To the cigaretteAdding KMnO into the gas 4 The volume of the solution is V 3 The volume of the added absorption liquid is v=v 2 +V 3 。
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| CN202210694167.7A CN117288888A (en) | 2022-06-17 | 2022-06-17 | System and method for sampling and testing oxysulfide in catalytic regeneration flue gas |
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| CN202210694167.7A CN117288888A (en) | 2022-06-17 | 2022-06-17 | System and method for sampling and testing oxysulfide in catalytic regeneration flue gas |
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