CN115792079A - Method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas - Google Patents
Method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas Download PDFInfo
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- 239000003546 flue gas Substances 0.000 title claims abstract description 59
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 58
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 52
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 230000005494 condensation Effects 0.000 claims abstract description 36
- 238000009833 condensation Methods 0.000 claims abstract description 36
- 238000005070 sampling Methods 0.000 claims abstract description 28
- 150000002500 ions Chemical class 0.000 claims abstract description 20
- 239000010453 quartz Substances 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 8
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 8
- 238000010521 absorption reaction Methods 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 239000011324 bead Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012494 Quartz wool Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 244000088401 Pyrus pyrifolia Species 0.000 description 1
- 235000001630 Pyrus pyrifolia var culta Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention relates to the technical field of waste gas treatment, and discloses a method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas. The method comprises the following steps: collecting a sample to be detected from the coal-fired flue gas of a flue by adopting a collecting device, and detecting SO in the sample to be detected by adopting an ion chromatography and a nano-reagent spectrophotometry 4 2‑ And NH 4 + The concentration of ions is determined, and then the concentrations of ammonium sulfate and ammonium bisulfate in coal-fired flue gas are determined according to detection results, wherein the acquisition device comprises a heating sampling gun, a heating quartz filter, a constant-temperature oil bath system and a condensation reactor, the air inlet end of the heating sampling gun is placed in a flue, the heating sampling gun, the heating quartz filter and the condensation reactor are sequentially connected, and the condensation reactor is placed in the constant-temperature oil bath system. According to the technical scheme of the invention, ammonium sulfate and ammonium bisulfate in the coal-fired flue gas can be collected, and quantitative separation is realizedAnd (5) analyzing and detecting.
Description
Technical Field
The invention relates to the technical field of waste gas treatment, in particular to a method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas.
Background
Nitrogen oxides are one of main atmospheric pollutants of a coal-fired power plant, the requirements of the nation on pollution control are continuously improved at present, wherein NOx emission limits of 50mg/m are regulated in the atmospheric pollutant emission Standard of the Heat-engine plant (DB/37 664-2019) of Shandong province and the atmospheric pollutant emission Standard of the coal-fired power plant (DB/32 4148-2021) of Jiangsu province 3 。
The Selective Catalytic Reduction (SCR) is the most widely used flue gas denitration technology worldwide at present. The principle is that the flue gas enters an SCR reactor, and ammonia is injected into NO-containing gas as a reducing agent in an oxygen-containing atmosphere through a catalyst X In the flue gas, NO is generated under the action of a metal catalyst X Is reduced to N 2 And H 2 O, its main reaction is as follows:
4NO+4NH 3 +O 2 →4N 2 +6H 2 O (1)
2NO 2 +4NH 3 +O 2 →3N 2 +6H 2 O (2)
in most boiler flue gases, a certain amount of ammonia escapes from the denitration outlet. Meanwhile, part of SO in the coal-fired flue gas 2 Will oxidize into SO 3 . Under certain conditions, SO 3 Ammonium sulfate and ammonium bisulfate can be generated with unreacted escaping ammonia and water vapor. Ammonium sulfate and ammonium bisulfate are produced simultaneously, and the production distribution of the ammonium sulfate and the ammonium bisulfate depends on NH 3 /SO 3 Molar ratio of NH 3 /SO 3 When the molar ratio is more than 2, the ammonium sulfate is a main product; when NH is present 3 /SO 3 When the molar ratio is less than 1, the product is mainly ammonium bisulfate.
The melting point of ammonium sulfate is 280 ℃ and the melting point of ammonium bisulfate is 147 ℃. Ammonium sulfate can cover the original active site on the catalyst, so that pore channels are blocked, and the adsorption of acid and alkali sites on reaction gas is hindered; in the air preheater, ammonium bisulfate is in the process of converting from liquid state to solid state, has viscosity and acidity, can adhere to a large amount of fly ash, causes the phenomena of blockage and corrosion of the air preheater, influences the safety of a system and increases the energy consumption for operation. According to the prior literature, the current research on ammonium sulfate salts is obviously more inclined to ammonium bisulfate, and the research on ammonium sulfate is lacked. Meanwhile, in practical application, how to collect ammonium sulfate and ammonium bisulfate in coal-fired flue gas still has no mature sampling method and device for flue gas collection.
Disclosure of Invention
The invention aims to solve the problem that the ammonium sulfate and ammonium bisulfate in coal-fired flue gas can not be collected, analyzed and detected in the prior art, and provides a method for measuring the ammonium sulfate and the ammonium bisulfate in the coal-fired flue gas.
In order to achieve the above object, the present invention provides a method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas, which comprises: collecting a sample to be detected from the coal-fired flue gas of a flue by adopting a collecting device, and detecting SO in the sample to be detected by adopting an ion chromatography and a nano-reagent spectrophotometry 4 2- And NH 4 + Ion concentration, then confirm ammonium sulfate and ammonium bisulfate's concentration in the coal-fired flue gas according to the testing result, wherein, collection system is including heating sampling rifle, heating quartz filter, thermostatic oil bath system and condensation reactor, the inlet end of heating sampling rifle is put into the flue, the heating sampling rifle heating quartz filter with the condensation reactor connects gradually, the condensation reactor is arranged in among the thermostatic oil bath system.
Preferably, the temperature of the heating sampling gun is controlled to be 320 +/-5 ℃.
Preferably, the temperature of the heated quartz filter is controlled to be 320 ± 5 ℃.
Preferably, the oil bath temperature of the constant temperature oil bath system is 120-260 ℃.
Preferably, the condensation reactor is filled with glass beads or quartz wool.
Preferably, the glass beads have a diameter of 1 to 5mm.
Preferably, the collecting device further comprises a first absorption device and a second absorption device, wherein the first absorption device is used for treating the gas discharged from the condensation reactor and absorbing SO in the gas 3 (ii) a The second absorption device is used for treating the gas discharged from the first absorption device and absorbing NH in the gas 3 。
Preferably, the first absorption device contains an aqueous isopropanol solution, preferably an aqueous isopropanol solution with a concentration of 75-85 wt%.
Preferably, the second absorption device contains hydrochloric acid solution, preferably hydrochloric acid solution with the concentration of 0.05-0.2 mol/L.
Preferably, the process of collecting the sample to be tested comprises: the condensate was washed out of the condensation reactor with deionized water to obtain a wash liquid.
Preferably, the specific process of determining the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the detection result is as follows:
(I) SO detected by ion chromatography and spectrophotometry with Nassner reagent based on the volume of the washing solution 4 2- And NH 4 + Calculating SO in the washing liquid by ion concentration 4 2- Ions and NH 4 + The amount of ions;
(II) calculating the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the following formula, wherein M =2a-b
N＝b-a
Wherein a is SO in the washing liquid 4 2- Amount of ions, mol;
b is NH in the washing liquid 4 + Amount of ions, mol;
m is the amount of ammonium bisulfate in mol;
n is the amount of ammonium sulfate, mol;
v is the volume of the coal-fired flue gas extracted by sampling in a standard state, L;
According to the technical scheme of the invention, ammonium sulfate and ammonium bisulfate in the coal-fired flue gas can be collected, and quantitative analysis and detection can be realized.
Drawings
Fig. 1 is a schematic structural diagram of an acquisition device used in the method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas according to the present invention.
Description of the reference numerals
1-heating a sampling gun; 2. heating the quartz filter; 3. a constant temperature oil bath system; 4. condensing the reactor; 5. a first absorption device; 6. a second absorption device; 7. a gas flow meter; 8. a pressure gauge; 9, a thermometer; 10. a fan.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and these ranges or values should be understood to encompass values close to these ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the description of the present application, the terms "first", "second" are used for descriptive purposes only and are not to be construed as indicating relative importance or as implicitly indicating the number of technical features indicated. Thus, unless stated otherwise, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature; "plurality" means two or more. The terms "comprises" and "comprising," and any variations thereof, are intended to cover a non-exclusive inclusion, such that one or more other features, integers, steps, operations, elements, components, and/or combinations thereof may be present or added.
The method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas comprises the following steps: collecting a sample to be detected from coal-fired flue gas of a flue by adopting a collecting device, and detecting SO in the sample to be detected by adopting an ion chromatography method and a Nassner reagent spectrophotometry method 4 2- And NH 4 + And determining the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the detection result.
In the invention, as shown in fig. 1, the collecting device comprises a heating sampling gun 1, a heating quartz filter 2, a constant temperature oil bath system 3 and a condensation reactor 4, wherein the gas inlet end of the heating sampling gun 1 is placed in a flue, the heating sampling gun 1, the heating quartz filter 2 and the condensation reactor 4 are connected in sequence, and the condensation reactor 4 is placed in the constant temperature oil bath system 3.
In the specific implementation process, the temperature of the heating sampling gun 1 is controlled to be 320 +/-5 ℃, and the temperature of the heating quartz filter 2 is controlled to be 320 +/-5 ℃. By controlling the temperature of the heating sampling gun 1 and the heating quartz filter 2, ammonium bisulfate or ammonium sulfate can be prevented from being generated and condensed before the condensation reactor. The constant temperature oil bath system 3 is used for heating the condensation reactor 4, and preferably, the oil bath temperature of the constant temperature oil bath system 3 is 120-260 ℃.
In the collecting device, glass beads or quartz wool is filled in the condensation reactor 4 for trapping ammonium bisulfate and ammonium sulfate. The glass beads may have a diameter of 1-5mm, most preferably 2mm. In the present invention, the length of the condensation reactor 4 is set to be enough to ensure sufficient heating and sufficient constant temperature residence time, so that the temperature of the flue gas at the tail end of the condensation reactor is consistent with the temperature of the constant temperature oil bath.
In the collecting device, preferably, the collecting device further comprises a first absorption device 5 and a second absorption device 6, the first absorption device 5 is used for treating the gas discharged from the condensation reactor 4 to absorb SO in the gas 3 (ii) a The second absorption device 6 is used for treating the gas discharged from the first absorption device 5 and absorbing NH in the gas 3 . In a specific embodiment, the first absorption device 5 contains an aqueous isopropanol solution, preferably an aqueous isopropanol solution with a concentration of 75-85wt%, and most preferably an aqueous isopropanol solution with a concentration of 80 wt%; the second absorption device 6 contains hydrochloric acid solution, preferably hydrochloric acid solution with concentration of 0.05-0.2mol/L, and most preferably hydrochloric acid solution with concentration of 0.1 mol/L.
In the collecting device, it is preferable that the collecting device further comprises a gas flow meter 7, a pressure gauge 8 and a temperature gauge 9 for detecting the flow rate, pressure and temperature of the gas discharged from the second absorption device 6, respectively, to determine the sampling volume of the coal-fired flue gas.
In the collecting device, the collecting device also comprises a fan 10 which is used for overcoming the resistance of a flue and a sampling system and ensuring that the flue gas is collected and measured at a certain flow.
In the method of the present invention, the step of collecting the sample to be tested comprises: and washing out condensate from the condensation reactor 4 by using deionized water to obtain washing liquid serving as a sample to be tested.
In the method, the specific process of determining the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the detection result comprises the following steps:
(I) SO detected by ion chromatography and spectrophotometry with Nassner reagent based on the volume of the washing solution 4 2- And NH 4 + Calculating SO in the washing liquid by ion concentration 4 2- Ions and NH 4 + The amount of ions;
(II) calculating the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the following formula, wherein M =2a-b
N＝b-a
Wherein a is SO in the washing liquid 4 2- Amount of ions, mol;
b is NH in the washing liquid 4 + Amount of ions, mol;
m is the amount of ammonium bisulfate, mol;
n is the amount of ammonium sulfate, mol;
v is the volume L of the coal-fired flue gas sampled in a standard state;
According to the method, the constant-temperature oil bath system can accurately control the temperature of the condensation reactor 4, and effectively ensures the condensation effect. The condensation reactor is preferably a straight pipe made of quartz, and the reactor is filled with glass beads with the diameter of about 2mm, so that the specific surface area can be increased, and the condensation of ammonium sulfate and ammonium bisulfate is promoted. Heating sampling rifle 1 with heating quartz filter 2 all corresponds and is provided with heating system, through the temperature control with the flue gas about 320 ℃, can prevent that ammonium bisulfate or ammonium sulfate in the flue gas from generating and before condensation reactorAnd the particles in the flue gas can be filtered by arranging a quartz filter device. In addition, due to excess NH 3 Will react with the formed ammonium bisulfate for the second time to generate ammonium sulfate and excessive SO 3 The ammonium bisulfate is also reacted with the ammonium sulfate to generate the ammonium bisulfate, and the ammonium bisulfate have a mutual conversion relationship, so a certain reaction time is ensured in an experiment, and reaction products are not immediately cleaned after the introduction of the flue gas is stopped, so that the reaction is completely ensured.
The following examples further illustrate the measuring methods of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the present invention. The embodiments are implemented on the premise of the technical scheme of the invention, and detailed implementation modes and specific operation processes are given, but the scope of the invention is not limited to the following embodiments.
The experimental procedures in the following examples are, unless otherwise specified, conventional in the art. The experimental materials used in the following examples are commercially available unless otherwise specified.
The collecting device adopted in the following embodiment comprises a heating sampling gun 1, a heating quartz filter 2, a constant-temperature oil bath system 3, a condensation reactor 4, a first absorption bottle 5, a second absorption bottle 6, a gas flowmeter 7, a pressure gauge 8, a temperature gauge 9 and a fan 10, wherein the gas inlet end of the heating sampling gun 1 is placed in a flue, the condensation reactor 4 is placed in the constant-temperature oil bath system 3, the heating sampling gun 1, the heating quartz filter 2, the condensation reactor 4, the first absorption bottle 5, the second absorption bottle 6, the gas flowmeter 7 and the fan 10 are sequentially connected, the pressure gauge 8 and the temperature gauge 9 are arranged in the gas flowmeter 7, wherein the condensation reactor 4 is a quartz straight pipe, and glass beads with the diameter of 2mm are filled in the condensation reactor 4; the first absorption bottle 5 contains an aqueous isopropanol solution with a concentration of 80wt%, and the second absorption bottle 6 contains a hydrochloric acid solution with a concentration of 0.1 mol/L.
Example 1
The simulation coal-fired flue gas that this embodiment adopted carries out ammonium bisulfate and ammonium sulfate collection efficiency experiment. Respectively weighing 1.0g of ammonium bisulfate and 1.0g of ammonium sulfate, placing the ammonium bisulfate and the ammonium sulfate at specified positions for quantitative gas distribution, and heatingAt a temperature of 350 ℃ by using N 2 As carrier gas, the simulated gas is carried into the collecting device.
The collection device is adopted to collect the flue gas, specifically, the temperature of the inlet flue gas is stabilized to 320 ℃, the heating sampling gun 1 is opened, the temperature of the heating sampling gun 1 is adjusted to 320 ℃, the flow is adjusted to 1L/min, and the temperature of the heating quartz filter 2 is adjusted to 320 ℃. The condensation reactor 4 was heated by means of a constant temperature oil bath, the temperature of which was adjusted to 175 ℃.
After sampling was completed, the condensation product in the condensation reactor was washed out with 100mL of deionized water to obtain a washing liquid. Analyzing SO in the washing solution by ion chromatography and Nashi reagent spectrophotometry respectively 4 2- Ions and NH 4 + The concentration of the ions. According to volume and SO of the washing solution 4 2- Ion, NH 4 + Calculating the ion concentration to obtain SO in the washing liquid 4 2- Ion, NH 4 + The amount of (c). Then the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas are calculated according to the following formula,
M＝2a-b
N＝b-a
wherein a is SO in the washing liquid 4 2- Amount of ions, mol;
b is NH in the washing liquid 4 + Amount of ions, mol;
m is the amount of ammonium bisulfate, mol;
n is the amount of ammonium sulfate, mol;
v is the volume L of the coal-fired flue gas sampled in a standard state;
The experiment was repeated ten times according to the above procedure, and the results of the ten times of measurements are shown in table 1 below.
TABLE 1
| Recovery ratio of ammonium sulfate (%) | Recovery ratio of ammonium bisulfate (%) | |
| |
91.4 | 93.3 |
| Experiment 2 | 92.2 | 91.6 |
| |
90.8 | 91.9 |
| |
93.6 | 90.8 |
| |
92.0 | 92.6 |
| |
92.3 | 93.1 |
| Experiment 7 | 88.4 | 91.6 |
| Experiment 8 | 89.1 | 92.2 |
| |
94.2 | 89.5 |
| |
90.4 | 92.8 |
As can be seen from the data in Table 1, according to the method for measuring ammonium sulfate and ammonium bisulfate in coal-fired flue gas, the quantitative analysis and detection of ammonium sulfate and ammonium bisulfate in coal-fired flue gas can be realized, and the detection result is accurate and stable.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
1. Fire coalA method for measuring ammonium sulfate and ammonium bisulfate in flue gas is characterized by comprising the following steps: collecting a sample to be detected from the coal-fired flue gas of a flue by adopting a collecting device, and detecting SO in the sample to be detected by adopting an ion chromatography and a nano-reagent spectrophotometry 4 2- And NH 4 + Ion concentration, then determining the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the detection result,
the collecting device comprises a heating sampling gun (1), a heating quartz filter (2), a constant-temperature oil bath system (3) and a condensation reactor (4), wherein the air inlet end of the heating sampling gun (1) is placed in a flue, the heating sampling gun (1), the heating quartz filter (2) and the condensation reactor (4) are sequentially connected, and the condensation reactor (4) is placed in the constant-temperature oil bath system (3).
2. The method according to claim 1, characterized in that the temperature of the heated sampling gun (1) is controlled to 320 ± 5 ℃.
3. The method according to claim 1, characterized in that the temperature of the heated quartz filter (2) is controlled to 320 ± 5 ℃.
4. The process according to claim 1, characterized in that the oil bath temperature of the thermostatic oil bath system (3) is 120-260 ℃.
5. A method according to any one of claims 1-4, characterized in that the condensation reactor (4) is filled with glass beads or quartz wool.
6. The method of claim 5, wherein the glass beads have a diameter of 1-5mm.
7. The method according to any one of claims 1 to 4, wherein the collecting device further comprises a first absorbing device (5) and a second absorbing device (6), the first absorbing device (5) being adapted to react from the condensationThe gas discharged from the device (4) is treated to absorb SO in the gas 3 (ii) a The second absorption device (6) is used for treating the gas discharged from the first absorption device (5) and absorbing NH in the gas 3 。
8. A process according to claim 7, characterized in that said first absorption means (5) contains an aqueous isopropanol solution, preferably an aqueous isopropanol solution with a concentration of 75-85% by weight.
9. The method according to claim 7, characterized in that the second absorption device (6) contains a hydrochloric acid solution, preferably a hydrochloric acid solution with a concentration of 0.05-0.2 mol/L.
10. The method of claim 1, wherein collecting the test sample comprises: washing the condensate from the condensation reactor (4) with deionized water to obtain a wash liquid.
11. The method according to claim 10, wherein the specific process of determining the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the detection result is as follows:
(I) According to the volume of the washing solution and SO detected by ion chromatography and spectrophotometry with a Nashin reagent 4 2- And NH 4 + Calculating SO in the washing liquid by ion concentration 4 2- Ions and NH 4 + The amount of ions;
(II) calculating the concentrations of ammonium sulfate and ammonium bisulfate in the coal-fired flue gas according to the following formula,
M＝2a-b
N＝b-a
wherein a is SO in the washing liquid 4 2- Amount of ions, mol;
b is NH in the washing liquid 4 + Amount of ions, mol;
m is the amount of ammonium bisulfate in mol;
n is the amount of ammonium sulfate, mol;
v is the volume L of the coal-fired flue gas sampled in a standard state;
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| CN117890166A (en) * | 2024-03-14 | 2024-04-16 | 山西泰瑞祥科技有限公司 | Air pollution monitoring device |
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