CN111624060A - Flue gas sulfur trioxide sampling equipment and method - Google Patents

Flue gas sulfur trioxide sampling equipment and method Download PDF

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Publication number
CN111624060A
CN111624060A CN202010582670.4A CN202010582670A CN111624060A CN 111624060 A CN111624060 A CN 111624060A CN 202010582670 A CN202010582670 A CN 202010582670A CN 111624060 A CN111624060 A CN 111624060A
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China
Prior art keywords
gas
liquid
inlet
reactor
flue gas
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Pending
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CN202010582670.4A
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Chinese (zh)
Inventor
赵瀚辰
付康丽
姚明宇
郭中旭
杨成龙
杨嵩
程广文
李阳
蔡铭
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Xian Thermal Power Research Institute Co Ltd
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Xian Thermal Power Research Institute Co Ltd
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Priority to CN202010582670.4A priority Critical patent/CN111624060A/en
Publication of CN111624060A publication Critical patent/CN111624060A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • G01N1/2202Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2205Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/48Sulfur compounds
    • B01D53/50Sulfur oxides
    • B01D53/501Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • G01N1/2202Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • G01N1/2247Sampling from a flowing stream of gas
    • G01N1/2258Sampling from a flowing stream of gas in a stack or chimney
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/02Other waste gases
    • B01D2258/0283Flue gases
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • G01N1/2247Sampling from a flowing stream of gas
    • G01N1/2258Sampling from a flowing stream of gas in a stack or chimney
    • G01N2001/2261Sampling from a flowing stream of gas in a stack or chimney preventing condensation (heating lines)

Abstract

The invention relates to a boiler flue gas component detection technology, in particular to a flue gas sulfur trioxide sampling device and a method. The device comprises a heating smoke gun arranged in a flue, and a micro-channel gas-liquid reactor, a gas-liquid separator and a drying bottle which are sequentially connected and arranged in a low-temperature box; the micro-channel gas-liquid reactor comprises a spiral reaction part, wherein the input end of the spiral reaction part is provided with a gas inlet and a liquid inlet in parallel, and the output end of the spiral reaction part is provided with a mixing outlet; the input end of the heating pipe is inserted into the flue, and the output end of the heating pipe enters the low-temperature box and then is connected with the gas inlet of the microchannel gas-liquid contact reactor; the mixing outlet of the microchannel gas-liquid reactor is connected with the inlet of the gas-liquid separator; a liquid outlet of the gas-liquid separator is connected with a liquid inlet of the microchannel gas-liquid contact reactor through a liquid circulating pump, and a gas outlet of the gas-liquid separator is connected with an inlet of the drying bottle;the outlet of the drying bottle is sequentially provided with a flowmeter and an air pump. The invention has higher absorption efficiency and strong detection accuracy, and can effectively improve SO3The acquisition accuracy of (2).

Description

Flue gas sulfur trioxide sampling equipment and method
Technical Field
The invention relates to a boiler flue gas component detection technology, in particular to a flue gas sulfur trioxide sampling device and a method.
Background
The boiler flue gas contains a plurality of pollutants, and with implementation of domestic boiler atmospheric pollutant emission standards and vigorous popularization of ultralow emission modification of coal-fired power plants, the traditional atmospheric pollutants comprise SO2、NOxAnd smoke, etc., are effectively controlled. However, atmospheric haze is not significantly improved, and researchers in the industry have also shifted their focus to other trace contaminants, including SO3. As shown in the United States Environmental Protection Agency (USEPA) report, SO3And sulfuric acid aerosols may cause a number of health problems, also a direct cause of acid rain, while the primary source of primary condensable PM2.5 in boiler flue gas is also SO3,SO3Is SO2More than 10 times of the amount of the sulfuric acid, is very easy to combine with water to form sulfuric acid mist, and is difficult to be removed by the existing environment-friendly equipment. Therefore, coal-fired power plant to SO3Control and detection are imperative. In addition, there have been 22 weeks in the United states to combat SO in coal-fired power plant flue gas3The emission limit value is limited, and national development and reform committee, environmental protection department and national energy agency of China also issue an action plan for energy conservation, emission reduction, upgrade and modification of coal and electricity (2014-2020), wherein SO reduction is also mentioned3The discharge of unconventional pollutants indicates that China pays more attention to SO3And (4) controlling the emission.
Due to SO3Sulfuric acid has special steam physical and chemical properties, SO3Is always a difficult problem in the industry, and the existing SO3The sampling detection technology has complex operation, various devices and SO pair3The collection rate of (A) is unstable, SO3The accuracy and repeatability of the detection are not ideal.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the flue gas sulfur trioxide sampling equipment and the method, which have the advantages of reasonable structural design, simplicity in operation, higher absorption efficiency and strong detection accuracy, and can effectively improve SO3The acquisition accuracy of (2).
The invention is realized by the following technical scheme:
a sampling device for sulfur trioxide in flue gas comprises a heating smoke gun arranged in a flue, and a micro-channel gas-liquid reactor, a gas-liquid separator and a drying bottle which are sequentially connected and arranged in a low-temperature box;
the micro-channel gas-liquid reactor comprises a spiral reaction part, wherein the input end of the spiral reaction part is provided with a gas inlet and a liquid inlet in parallel, and the output end of the spiral reaction part is provided with a mixing outlet;
the input end of the heating smoke gun is inserted into the flue, and the output end of the heating smoke gun enters the low-temperature box and then is connected with the gas inlet of the micro-channel gas-liquid contact reactor; the mixing outlet of the microchannel gas-liquid reactor is connected with the inlet of the gas-liquid separator; the liquid outlet of the gas-liquid separator is connected with the liquid inlet of the microchannel gas-liquid contact reactor through a liquid circulating pump, and the gas outlet of the gas-liquid separator is connected with the inlet of the drying bottle; and the outlet of the drying bottle is sequentially provided with a flowmeter and an air pump.
Furthermore, the inner diameter of the spiral reaction part of the micro-channel gas-liquid reactor is less than 2mm, the spiral thread rotates left or right, the tooth height is less than 1mm, and the thread pitch is less than 3 mm.
Furthermore, the input end of the spiral reaction part is provided with a gas inlet and a liquid inlet which are arranged in parallel, and the spiral reaction part is of a T-shaped or Y-shaped structure.
Furthermore, the micro-channel gas-liquid reactor is made of glass fiber, PPSF or PETG materials through 3D printing processing.
Furthermore, a one-way valve is arranged between the liquid outlet of the gas-liquid separator and the liquid inlet of the microchannel gas-liquid contact reactor.
Further, a drying agent comprising allochroic silica gel or calcium chloride is filled in the drying bottle.
A method for sampling sulfur trioxide in flue gas comprises the following steps,
step one, starting an air pump for sampling, heating the flue gas by a high-temperature heating smoke pipe, and then carrying out SO (SO) treatment on the flue gas3Or after the sulfuric acid is converted into sulfuric acid vapor, dust is filtered out through high temperature at the tail part, enters a low-temperature box and is absorbed by absorption liquid in a microchannel gas-liquid reactor to be converted into sulfate ions, and a gas-liquid mixture is formed;
step two, separating the gas-liquid mixture after the gas-liquid mixture enters a gas-liquid separator, passing the clean flue gas through a dryer and then through a flowmeter to obtain the accumulated flue gas volume, and re-entering the liquid into the microchannel gas-liquid reactor through a liquid circulating pump to continuously enrich sulfate ions;
step three, after sampling is finished, sulfate ions in the absorption liquid are detected through a chloranilate barium method, a barium chromate method or an ion chromatography method, and SO in the flue gas is calculated according to the amount of the absorption liquid and the accumulated flue gas amount3And (4) concentration.
Further, in the step 1, 80% isopropanol water solution is adopted as the absorption liquid, and the circulating liquid amount of the absorption liquid is less than 3 mL/min.
Further, the heating temperature of the heating smoking pipe is more than 250 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
the device can greatly improve SO by adopting the micro-channel gas-liquid contact reactor3The absorption efficiency of the reactor is particularly the sulfuric acid fog drops which are difficult to absorb, the volume of the microchannel gas-liquid contact reactor is small, and the reactor adopts a high molecular inert material, so that the sealing problem is avoided; the threaded inner wall of the micro-channel gas-liquid contact reactor can enhance fluid disturbance and enhance gas-liquid transmissionQuality, increase SO3The absorption rate of (a); meanwhile, as the microchannel gas-liquid contact reactor is adopted, the circulating flow of the absorption liquid entering the microchannel gas-liquid contact reactor is smaller, and a small amount of absorption liquid is used for circulating absorption under the same flue gas flow, SO that the collected SO is improved3The concentration of the sample is improved, the acquisition precision is improved, the equipment is simple, and the repeatability is strong.
The method adopts the micro-channel gas-liquid reactor to ensure that the absorption liquid is fully contacted with the flue gas, thereby improving SO3By means of absorption liquid recirculation, enrichment of the absorption liquid in SO3The content and the collection rate are stable, and the measurement precision can be effectively improved.
Drawings
FIG. 1 is a system block diagram of the present invention.
In the figure: the device comprises a heating smoke gun 1, a micro-channel gas-liquid contact reactor 2, a low-temperature box 3, a gas-liquid separator 4, a liquid circulating pump 5, a drying bottle 6, a flowmeter 7, an air pump 8 and a one-way valve 9.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
The invention relates to a sampling device for sulfur trioxide in flue gas, which comprises a heating smoke gun 1, a microchannel gas-liquid contact reactor 2, a low-temperature box 3, a gas-liquid separator 4, a liquid circulating pump 5, a drying bottle 6, a flowmeter 7, an air pump 8 and a one-way valve 9;
as shown in fig. 1, the input end of the heating smoke gun 1 is inserted into a flue, the output end of the heating smoke gun enters a low-temperature box 3 and then is connected with a gas inlet of a microchannel gas-liquid contact reactor 2, a mixed outlet of the microchannel gas-liquid reactor 2 is connected with a gas-liquid separator 4, a gas outlet of the gas-liquid separator 4 is connected with a drying bottle 6, an outlet of the drying bottle 6 is connected with an air extracting pump 8, and a liquid outlet of the gas-liquid separator 4 is connected with a liquid inlet of the microchannel gas-liquid contact reactor 2 through a liquid circulating pump 5;
the inner diameter of a spiral reaction part of the micro-channel gas-liquid reactor 2 is smaller than 2mm, the spiral internal thread can rotate left and right, the tooth height is smaller than 1mm, the thread pitch is smaller than 3mm, high-precision 3D printing processing is adopted, and materials such as glass fiber, PPSF or PETG are selected; the input end of the spiral reaction part is provided with a gas inlet and a liquid inlet which are arranged in parallel and adopt a T-shaped or Y-shaped structure;
the gas-liquid separator 4 is used for separating a gas-liquid mixture of the flue gas and the absorption liquid after the reaction is finished, the separated absorption liquid is stored at the bottom of the gas-liquid separator 4 and enters the microchannel gas-liquid reactor 2 again through being connected with a liquid circulating pump to absorb the flue gas again; the gas-liquid separator 4 is located inside the low-temperature box, so that water vapor in the air can be removed;
the drying bottle 6 is used for further removing water vapor in the smoke and can be filled with drying agents such as allochroic silica gel and calcium chloride.
Preferably, the heating smoke gun 1 can heat the smoke to more than 250 ℃, so as to avoid filtering out condensed sulfuric acid fog drops when filtering fly ash particles.
The invention relates to a method for sampling sulfur trioxide in flue gas, which comprises the following steps,
step 1, starting an air pump 8 for sampling, heating the flue gas by a high-temperature heating smoke gun 1, and then carrying out SO (sulfur dioxide) treatment on the flue gas3After sulfuric acid is converted into sulfuric acid vapor, dust is filtered out through high temperature at the tail part, enters a low-temperature box 3 and is absorbed by absorption liquid in a micro-channel gas-liquid reactor 2 to be converted into sulfate ions, and a gas-liquid mixture is formed;
step 2, separating the gas-liquid mixture after the gas-liquid mixture enters a gas-liquid separator 4, obtaining the accumulated flue gas amount through a flow meter 7 after the clean flue gas passes through a dryer 6, and enabling the liquid to reenter the micro-channel gas-liquid reactor 2 through a liquid circulating pump 5 to continuously enrich sulfate ions;
step 3, after sampling is finished, detecting sulfate ions in the absorption liquid by methods such as a chloranilic acid barium method, a barium chromate method, an ion chromatography and the like, and calculating SO in the flue gas according to the absorption liquid amount and the accumulated flue gas amount3And (4) concentration.
Preferably, in step 1, the absorption liquid is 80% isopropanol water solution, SO that the SO content can be improved3Absorption efficiency of (3) avoiding SO2Dissolved in the absorption liquid to interfere with the measurement, absorptionThe liquid collecting circulation liquid amount is less than 3 mL/min.
Preferably, in step 1, the heating temperature of the heating smoke gun 1 is greater than 250 ℃, so that the phenomenon of filtering out condensed sulfuric acid mist drops during filtering fly ash particles can be effectively avoided.

Claims (9)

1. A flue gas sulfur trioxide sampling device is characterized by comprising a heating smoke gun (1) arranged in a flue, and a micro-channel gas-liquid reactor (2), a gas-liquid separator (4) and a drying bottle (6) which are sequentially connected and arranged in a low-temperature box (3);
the micro-channel gas-liquid reactor (2) comprises a spiral reaction part, wherein the input end of the spiral reaction part is provided with a gas inlet and a liquid inlet in parallel, and the output end is provided with a mixing outlet;
the input end of the heating smoke gun (1) is inserted into the flue, and the output end of the heating smoke gun enters the low-temperature box (3) and then is connected with the gas inlet of the micro-channel gas-liquid contact reactor (2); the mixing outlet of the micro-channel gas-liquid reactor (2) is connected with the inlet of the gas-liquid separator (4); the liquid outlet of the gas-liquid separator (4) is connected with the liquid inlet of the microchannel gas-liquid contact reactor (2) through a liquid circulating pump (5), and the gas outlet of the gas-liquid separator (4) is connected with the inlet of the drying bottle (6); the outlet of the drying bottle (6) is sequentially provided with a flowmeter (7) and an air pump (8).
2. The sampling device for sulfur trioxide in flue gas according to claim 1, characterized in that the inner diameter of the spiral reaction part of the microchannel gas-liquid reactor (2) is less than 2mm, the spiral thread is left-handed or right-handed, the thread height is less than 1mm, and the thread pitch is less than 3 mm.
3. The sampling equipment for sulfur trioxide in flue gas according to claim 1, characterized in that the gas inlet and the liquid inlet, which are arranged in parallel at the input end of the spiral reaction part, are of a T-shaped or Y-shaped structure.
4. The sampling equipment for sulfur trioxide in flue gas according to claim 1, characterized in that the microchannel gas-liquid reactor (2) is made of glass fiber, PPSF or PETG material by 3D printing process.
5. The flue gas sulfur trioxide sampling device according to claim 1 or 4, characterized in that a one-way valve (9) is further arranged between the liquid outlet of the gas-liquid separator (4) and the liquid inlet of the microchannel gas-liquid contact reactor (2).
6. The sampling equipment for sulfur trioxide in flue gas according to claim 1, characterized in that the drying bottle (6) is filled with a drying agent comprising allochroic silica gel or calcium chloride.
7. A method for sampling sulfur trioxide in flue gas, which is based on the equipment of any one of claims 1 to 6, is characterized by comprising the following steps,
step 1, starting an air pump (8) for sampling, heating the flue gas by a high-temperature heating smoke gun (1), and then adding SO in the flue gas3Or after the sulfuric acid is converted into sulfuric acid vapor, dust is filtered out through high temperature at the tail part, enters the low-temperature box (3), and is absorbed by absorption liquid in the micro-channel gas-liquid reactor (2) to be converted into sulfate ions, and a gas-liquid mixture is formed;
step 2, separating the gas-liquid mixture after the gas-liquid mixture enters a gas-liquid separator (4), obtaining the accumulated smoke gas amount through a flow meter (7) after the clean smoke gas passes through a dryer (6), and enabling the liquid to reenter the microchannel gas-liquid reactor (2) through a liquid circulating pump (5) to continuously enrich sulfate ions;
step 3, after sampling is finished, detecting sulfate ions in the absorption liquid by a chloranilate barium method, a barium chromate method or an ion chromatography method, and calculating to obtain SO in the flue gas according to the absorption liquid amount and the accumulated flue gas amount3And (4) concentration.
8. The method for sampling sulfur trioxide in flue gas according to claim 7, wherein in the step 1, an 80% isopropanol aqueous solution is adopted as the absorption liquid, and the circulating liquid amount of the absorption liquid is less than 3 mL/min.
9. The sampling method of sulfur trioxide in flue gas according to claim 7, characterized in that in step 1, the heating temperature of the heating smoke gun (1) is more than 250 ℃.
CN202010582670.4A 2020-06-23 2020-06-23 Flue gas sulfur trioxide sampling equipment and method Pending CN111624060A (en)

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CN202010582670.4A CN111624060A (en) 2020-06-23 2020-06-23 Flue gas sulfur trioxide sampling equipment and method

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Application Number Priority Date Filing Date Title
CN202010582670.4A CN111624060A (en) 2020-06-23 2020-06-23 Flue gas sulfur trioxide sampling equipment and method

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115105928A (en) * 2022-07-05 2022-09-27 南京大学 Promoting CO 2 Decarburization device and method for absorbing mass transfer rate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115105928A (en) * 2022-07-05 2022-09-27 南京大学 Promoting CO 2 Decarburization device and method for absorbing mass transfer rate
CN115105928B (en) * 2022-07-05 2023-12-26 南京大学 Promoting CO 2 Decarbonization device and method for absorbing mass transfer rate

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