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CN112414796A - Integrated acquisition system and method for polymorphic ammonia of fixed pollution source - Google Patents

Integrated acquisition system and method for polymorphic ammonia of fixed pollution source Download PDF

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Publication number
CN112414796A
CN112414796A CN202011471476.5A CN202011471476A CN112414796A CN 112414796 A CN112414796 A CN 112414796A CN 202011471476 A CN202011471476 A CN 202011471476A CN 112414796 A CN112414796 A CN 112414796A
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China
Prior art keywords
screw
box body
sampling gun
ammonia
heat tracing
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CN202011471476.5A
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Chinese (zh)
Inventor
石爱军
孙成一
闫静
王志平
李国傲
郭明星
罗志云
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Beijing Municipal Research Institute of Environmental Protection
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Beijing Municipal Research Institute of Environmental Protection
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Priority to CN202011471476.5A priority Critical patent/CN112414796A/en
Publication of CN112414796A publication Critical patent/CN112414796A/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
    • 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
    • G01N1/2208Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with impactors
    • 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
    • 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
    • G01N1/24Suction devices
    • 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)
    • 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
    • G01N2001/2282Devices for withdrawing samples in the gaseous state with cooling means

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention relates to the technical field of monitoring of environmental pollutants, in particular to an integrated acquisition system and method for polymorphic ammonia of a fixed pollution source. The integrated collection system of polymorphic ammonia of fixed pollution source includes: the sampling head is provided with a heat tracing sampling gun with a filtering membrane, and the box body is connected with a smoke outlet of the heat tracing sampling gun; a snakelike condenser pipe is arranged in the box body, and an inlet of the snakelike condenser pipe is connected with a smoke outlet of the heat tracing sampling gun; a semiconductor refrigerating sheet is arranged on the snakelike condensation pipe, and a radiating fan is arranged in the center of a spiral body formed by the snakelike condensation pipe; the bottom of the box body is connected with a first screw absorption and collection bottle and a second screw absorption and collection bottle; the condensate outlet of the serpentine condenser pipe enters a first screw absorption collecting bottle, non-condensable gas in the first screw absorption collecting bottle enters a second screw absorption collecting bottle, and the non-condensable gas in the second screw absorption collecting bottle is discharged through a smoke outlet of the box body. The invention can collect three forms of ammonia at the same time.

Description

Integrated acquisition system and method for polymorphic ammonia of fixed pollution source
Technical Field
The invention relates to the technical field of monitoring of environmental pollutants, in particular to an integrated acquisition system and method for polymorphic ammonia of a fixed pollution source.
Background
Ammonia exists in 3 forms in the smoke of a fixed pollution source, wherein 1 is gaseous ammonia, 2 is ammonia on particles (particle state and adsorption state), and 3 is ammonia dissolved in aerogel (condensable state). The national standard method has the advantages of small flow sampling, secondary impact dilute sulfuric acid absorption, simple and convenient monitoring and sampling device and high field sampling speed. The defects mainly comprise: firstly, the sampling pipeline is not accompanied by heat, and water vapor in high-temperature flue gas in the sampling pipeline is easy to condense and form dew, so that the test result is low; secondly, the sampling with small flow rate can not realize the constant-speed sampling of the particles, can not measure the ammonia or ammonium salt on the particles and dissolved in small drops, and can not distinguish the existing state of the escaping ammonia in the flue gas; thirdly, the sample gas collection amount is small (10-45L), so that the representative deficiency of the monitoring data is caused.
Disclosure of Invention
In view of this, the technical problem to be solved by the present invention is to provide an integrated collection system and method for polymorphic ammonia in a stationary pollution source, which can effectively collect polymorphic ammonia in flue gas.
The invention provides an integrated acquisition system for polymorphic ammonia of a fixed pollution source, which comprises:
a box body; the box body is provided with a sampling gun connecting port and a smoke outlet; a first screw and a second screw are arranged at the bottom of the box body;
the smoke outlet of the heat tracing sampling gun is connected with the box body through a sampling gun connecting port; a sampling head of the heat tracing sampling gun is provided with a filtering membrane;
a snakelike condenser pipe is arranged in the box body, and an inlet of the snakelike condenser pipe is connected with a smoke outlet of the heat tracing sampling gun through a sampling gun connecting port; a semiconductor refrigerating sheet is arranged on the serpentine condenser pipe; a cooling fan is arranged in the center of a spiral body formed by the snake-shaped condensation pipe;
the bottom of the box body is connected with a first screw absorption and collection bottle through a first screw; the bottom of the box body is connected with a second screw absorption and collection bottle through a second screw;
the condensate outlet of the serpentine condenser pipe enters a first screw absorption collecting bottle through a first screw, non-condensable gas in the first screw absorption collecting bottle enters a second screw absorption collecting bottle and is connected with the second screw absorption collecting bottle, and the non-condensable gas in the second screw absorption collecting bottle is discharged through a smoke outlet of the box body.
Preferably, the top of the box body is further provided with heat dissipation holes.
Preferably, a touch screen and a power socket are arranged on the outer side of the box body, and a circuit system is arranged in the box body;
the touch screen receives and transmits the electric signal through a circuit system;
the semiconductor refrigerating sheet receives and transmits an electric signal through a circuit system;
the heat dissipation fan receives an electrical signal through a circuit system.
Preferably, the method further comprises the following steps: pitot tubes and smoke temperature lines;
the pitot tube is used for adjusting the flue gas flow rate of the heat tracing sampling gun;
the smoke temperature line is used for controlling the smoke temperature of the heat tracing sampling gun.
Preferably, the method further comprises the following steps:
the gas inlet is connected with the flue gas outlet of the box body;
a cumulative flow meter having a gas inlet connected to the gas outlet of the dryer;
and the gas inlet is connected with the gas outlet of the accumulation flowmeter.
The invention also provides an integrated acquisition method of polymorphic ammonia of a fixed pollution source, which comprises the following steps:
A) sampling smoke in a flue through a heat tracing sampling gun, wherein a sampling head of the heat tracing sampling gun is provided with a filtering membrane; collecting ammonia or ammonium salt in a particle state on the filter membrane;
B) condensing the flue gas collected in the step A) in a serpentine condenser pipe to obtain condensate, wherein condensable ammonia or ammonium salt is collected in the condensate; in the sampling process, the temperature of the heat tracing sampling gun is maintained at 115-125 ℃; the temperature of the condensed gas is not more than 30 ℃;
C) and the condensed non-condensable gas is subjected to primary sulfuric acid solution impact absorption treatment and secondary sulfuric acid solution impact absorption treatment in sequence, and gaseous ammonia is collected.
Preferably, in the step A), the volume of the sample is 0.5-2 m under the standard condition3
Preferably, in step B), the temperature of the first absorption treatment is room temperature;
the temperature of the second absorption treatment is room temperature.
Preferably, in the step B), the concentration of the sulfuric acid solution subjected to the first absorption treatment is 0.1 mol/L;
the concentration of the sulfuric acid solution subjected to the second absorption treatment was 0.1 mol/L.
The invention provides an integrated acquisition system for polymorphic ammonia of a fixed pollution source, which comprises: a box body; the box body is provided with a sampling gun connecting port and a smoke outlet; a first screw and a second screw are arranged at the bottom of the box body; the smoke outlet of the heat tracing sampling gun is connected with the box body through a sampling gun connecting port; a sampling head of the heat tracing sampling gun is provided with a filtering membrane; a snakelike condenser pipe is arranged in the box body, and an inlet of the snakelike condenser pipe is connected with a smoke outlet of the heat tracing sampling gun through a sampling gun connecting port; a semiconductor refrigerating sheet is arranged on the serpentine condenser pipe; a cooling fan is arranged in the center of a spiral body formed by the snake-shaped condensation pipe; the bottom of the box body is connected with a first screw absorption and collection bottle through a first screw; the bottom of the box body is connected with a second screw absorption and collection bottle through a second screw; a condensate outlet of the serpentine condenser pipe enters a first screw absorption and collection bottle through a first screw, and non-condensable gas in the first screw absorption and collection bottle enters a second screwThe port absorption collecting bottle is connected, and the non-condensable gas in the second screw port absorption collecting bottle is discharged through a smoke outlet of the box body. The invention can simultaneously collect ammonia in three forms, and fills the blank of the existing monitoring method. In addition, the collection method provided by the invention has large collection amount, and the collection amount of the smoke can be 1-2 m3The method has the advantages of data representativeness and good accuracy.
Drawings
FIG. 1 is a front view of an integrated capture system for polymorphic ammonia from a stationary source, according to an embodiment of the present invention;
FIG. 2 is a top view of an integrated capture system for polymorphic ammonia from a stationary source, according to an embodiment of the present invention;
FIG. 3 is a diagram of an integrated system for capturing polymorphic ammonia from a stationary source according to another embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides an integrated acquisition system for polymorphic ammonia of a fixed pollution source, which comprises:
a box body; the box body is provided with a sampling gun connecting port and a smoke outlet; a first screw and a second screw are arranged at the bottom of the box body;
the smoke outlet of the heat tracing sampling gun is connected with the box body through a sampling gun connecting port; a sampling head of the heat tracing sampling gun is provided with a filtering membrane;
a snakelike condenser pipe is arranged in the box body, and an inlet of the snakelike condenser pipe is connected with a smoke outlet of the heat tracing sampling gun through a sampling gun connecting port; a semiconductor refrigerating sheet is arranged on the serpentine condenser pipe; a cooling fan is arranged in the center of a spiral body formed by the snake-shaped condensation pipe;
the bottom of the box body is connected with a first screw absorption and collection bottle through a first screw; the bottom of the box body is connected with a second screw absorption and collection bottle through a second screw;
the condensate outlet of the serpentine condenser pipe enters a first screw absorption collecting bottle through a first screw, non-condensable gas in the first screw absorption collecting bottle enters a second screw absorption collecting bottle and is connected with the second screw absorption collecting bottle, and the non-condensable gas in the second screw absorption collecting bottle is discharged through a smoke outlet of the box body.
FIG. 1 is a front view of an integrated capture system for polymorphic ammonia from a stationary source, according to one embodiment of the present invention. Fig. 2 is a top view of an integrated collection system for polymorphic ammonia from a stationary source, according to an embodiment of the present invention. The device comprises a heat tracing sampling gun 1, a box 2, a first screw absorbing and collecting bottle 3, a second screw absorbing and collecting bottle 4, a pitot tube 5, a smoke temperature line 6, a first screw plug 7, a second screw plug 8, a serpentine condenser pipe 2-1, a semiconductor refrigeration sheet 2-2, a cooling fan 2-3, a heat dissipation hole 2-4, a touch screen 2-5, a transformer 2-6, a circuit board 2-7 and a power socket 2-8.
The integrated collection system for polymorphic ammonia of a fixed pollution source comprises a box body 2. The box body is provided with a sampling gun connecting port and a smoke outlet; the bottom of box is provided with first screw and second screw. The position of the sampling gun connection port is not particularly limited, and in some embodiments, the sampling gun connection port is disposed at an upper portion of an outer sidewall of the case. The shape of the box 2 is not particularly limited, and in some embodiments of the present invention, the box 2 is a rectangular parallelepiped. The material of the box body is not limited in particular, and aluminum alloy, PVC or stainless steel can be adopted. In some embodiments of the invention, the dimensions of the tank are 30cm by 50cm by 30 cm.
The integrated collection system for polymorphic ammonia of the fixed pollution source further comprises a heat tracing sampling gun 1. In the invention, the smoke outlet of the heat tracing sampling gun is connected with the box body through the sampling gun connecting port. And a filtering membrane is arranged on the sampling head of the heat tracing sampling gun. In some embodiments of the invention, a sampling head is connected to the air inlet end of the heat tracing sampling gun, and the sampling head is provided with a sampling nozzle and a filtering membrane. In some embodiments of the invention, the filter membrane is mounted to the sampling head of the heat traced sampling gun by a removable filter membrane clip. In some embodiments of the present invention, the heat trace sampling gun is used to collect waste gas from a stationary pollution source, which may be flue gas.
In some embodiments of the present invention, the sampling nozzle diameter of the heat trace sampling gun may be selected in accordance with standard GB/T16157-1996.
In certain embodiments of the invention, the filtration membrane pore size may be selected according to the standard GB/T16157-1996.
The structure and source of the heat tracing sampling gun are not particularly limited, and the heat tracing sampling gun known by the person skilled in the art can be adopted and can be generally sold in the market.
In certain embodiments of the invention, the integrated capture system for stationary pollution source polymorphic ammonia further comprises a pitot tube 5. The pitot tube is used for adjusting the flue gas flow rate of the heat tracing sampling gun. The arrangement position of the pitot tube is not specially limited, and the flue gas flow rate of the heat tracing sampling gun can be adjusted. The installation mode of the pitot tube is not limited in particular, and constant-speed tracking sampling can be realized by adopting the installation mode known by the person skilled in the art. The type of the pitot tube is not particularly limited, and the pitot tube may be generally commercially available.
In certain embodiments of the present invention, the integrated collection system for polymorphic ammonia from a stationary source of pollution further comprises a smoke temperature line 6. The smoke temperature line is used for controlling the smoke temperature of the heat tracing sampling gun. The smoke temperature line is not specially limited in arrangement position, and the smoke temperature of the heat tracing sampling gun can be controlled.
In the invention, a snakelike condenser pipe 2-1 is arranged in the box body, and the inlet of the snakelike condenser pipe is connected with the smoke outlet of the heat tracing sampling gun through a sampling gun connecting port. The serpentine condenser tube is used for rapidly cooling flue gas and collecting condensable ammonia. In certain embodiments of the invention, the serpentine condenser tube is used to rapidly cool the flue gas to no more than 30 ℃.
In some embodiments of the present invention, the pipe diameter of the serpentine condenser pipe 2-1 is 8 mm. In certain embodiments of the present invention, the serpentine condenser tube 2-1 has a helix height of 12 cm. In certain embodiments of the present invention, the serpentine condenser tube 2-1 has a toroid diameter of 8 mm. In some embodiments of the present invention, the serpentine condenser tube 2-1 is made of glass or quartz. In certain embodiments of the present invention, the serpentine condenser tube 2-1 may be generally commercially available.
In the invention, a semiconductor refrigerating sheet 2-2 is arranged on the snakelike condensation pipe 2-1. In some embodiments of the invention, the semiconductor chilling plates have a format size of 10mm by 1 mm. The distance between two adjacent semiconductor refrigeration pieces is 3-5 mm. In some embodiments of the present invention, the semiconductor chilling plates 2-2 may be generally commercially available.
In the invention, a radiating fan 2-3 is arranged in the center of a spiral body formed by the snakelike condensation pipe 2-1. In some embodiments of the invention, the heat dissipation fan 2-3 is arranged at the bottom of the center of the spiral body. In some embodiments of the present invention, the heat dissipation fan 2-3 is coaxially disposed with the spiral coil of the serpentine shaped condensation duct 2-1. In some embodiments of the invention, the cooling fan 2-3 has a diameter of 5 cm. In some embodiments of the present invention, the heat dissipation fans 2 to 3 may be generally commercially available.
In the invention, the bottom of the box body is connected with a first screw absorption and collection bottle 3 through a first screw; the bottom of the box body is connected with a second screw absorbing and collecting bottle 4 through a second screw. The condensate outlet of the serpentine condenser pipe 2-1 enters a first screw absorption and collection bottle 3 through a first screw, non-condensable gas in the first screw absorption and collection bottle 3 enters a second screw absorption and collection bottle 4, and the non-condensable gas in the second screw absorption and collection bottle 4 is discharged through a smoke outlet of the box body.
In some embodiments of the invention, the first screw-top absorption collector bottle is provided with a first screw-top plug 7. And a condensate outlet pipe of the serpentine condenser pipe 2-1 penetrates through the first screw plug 7 to enter the first screw absorption collecting bottle 3, and the first absorption treatment is carried out in the first screw absorption collecting bottle 3. In some embodiments of the present invention, the first screw-top absorption and collection bottle 3 is filled with sulfuric acid solution, and the concentration of the sulfuric acid solution is 0.1 mol/L.
In some embodiments of the present invention, the first screw plug 7 is further provided with a first non-condensable gas outlet pipe, and the non-condensable gas after the first absorption treatment enters the second screw absorption collecting bottle 4 through the first non-condensable gas outlet pipe on the first screw plug 7.
In some embodiments of the invention, the second screw-top absorption collection bottle is provided with a second screw-top plug 8. And a first non-condensable gas outlet pipe extending from the first screw plug 7 penetrates through the second screw plug 8 to enter the second screw absorption collecting bottle 4, and a second absorption treatment is carried out in the second screw absorption collecting bottle 4. In some embodiments of the present invention, the second screw absorption and collection bottle 4 is filled with sulfuric acid solution, and the concentration of the sulfuric acid solution is 0.1 mol/L.
In some embodiments of the present invention, the second screw plug 8 is further provided with a second non-condensable gas outlet pipe, and the non-condensable gas after the second absorption treatment is discharged through a flue gas outlet of the tank.
According to the invention, the first screw plug 7 and the second screw plug 8 are arranged to improve the air tightness of the air passage.
In some embodiments of the invention, heat dissipation holes 2-4 are further arranged at the top of the box body for heat dissipation. The invention has no special limit to the position and the area of the heat dissipation hole and can be determined according to the actual situation. In some embodiments of the invention, the area of the louvers is 5cm by 5 cm.
In some embodiments of the invention, a touch screen 2-5 and a power socket 2-8 are arranged on the outer side of the box body, and a circuit system is arranged in the box body. In some embodiments of the present invention, the touch screen receives and transmits electrical signals through circuitry. In some embodiments of the invention, the semiconductor chilling plates receive and transmit electrical signals through circuitry. In some embodiments of the present invention, the heat dissipation fan receives an electrical signal through circuitry.
In some embodiments of the invention, the circuitry includes a transformer 2-6 and a circuit board 2-7. The transformer is used for converting voltage into adaptive voltage of the semiconductor refrigeration sheet and the fan, and transmitting current to each electric appliance through the circuit board. The present invention is not limited to the type and source of the circuit board, and may be commercially available. The invention has no special limitation on the type and the source of the transformer, and the transformer can be generally sold in the market.
In some embodiments of the invention, the integrated collection system for polymorphic ammonia from a stationary source of contamination further comprises a dryer 9, as shown in fig. 3. FIG. 3 is a diagram of an integrated system for capturing polymorphic ammonia from a stationary source according to another embodiment of the present invention. Wherein, 9 is a dryer, 10 is an accumulation flow meter, and 11 is an air pump.
In some embodiments of the invention, the gas inlet of the dryer is connected to the flue gas outlet of the cabinet. The dryer is used for removing redundant water vapor in the flue gas. The structure and source of the dryer are not particularly limited in the present invention, and the dryer may be constructed as known to those skilled in the art, and may be generally commercially available.
In certain embodiments of the present invention, the integrated capture system for stationary pollution source polymorphic ammonia further comprises a cumulative flow meter 10, as shown in FIG. 3. The gas inlet of the accumulation flowmeter is connected with the gas outlet of the dryer. The cumulative flow meter is used for recording the flow. The source of the cumulative flowmeter is not particularly limited, and the cumulative flowmeter may be generally commercially available.
In some embodiments of the present invention, the integrated system for collecting polymorphic ammonia from a stationary source further comprises a suction pump 11, as shown in fig. 3. And a gas inlet of the air pump is connected with a gas outlet of the accumulation flowmeter.
The invention also provides an integrated collection method for fixed pollution source polymorphic ammonia by adopting the integrated collection system, which comprises the following steps:
A) sampling smoke in a flue through a heat tracing sampling gun, wherein a sampling head of the heat tracing sampling gun is provided with a filtering membrane; collecting ammonia or ammonium salt in a particle state on the filter membrane;
B) condensing the flue gas collected in the step A) in a serpentine condenser pipe to obtain condensate, wherein condensable ammonia or ammonium salt is collected in the condensate; in the sampling process, the temperature of the heat tracing sampling gun is maintained at 115-125 ℃; the temperature of the condensed gas is not more than 30 ℃;
C) and the condensed non-condensable gas is subjected to primary sulfuric acid solution impact absorption treatment and secondary sulfuric acid solution impact absorption treatment in sequence, and gaseous ammonia is collected.
In some embodiments of the invention, in the step A), the temperature of the heat tracing sampling gun is maintained at 110-130 ℃ during the sampling process. In certain embodiments of the invention, in step a), the temperature of the heat tracing sampling gun is maintained at 120 ℃ during the sampling. In some embodiments of the invention, the sampling time is 60-90 min.
In certain embodiments of the invention, the filter membrane is a quartz membrane or a teflon filter membrane.
In the invention, the flue gas in the flue is sampled by the heat tracing sampling gun, and granular ammonia or ammonium salt, mainly ammonium nitrate, ammonium sulfate and other ammonium salts, is collected on the filtering membrane. In some embodiments of the invention, after the collection method is complete, the filtered particulate filter membrane is rinsed with 100mL of deionized water and transferred to a first 500mL volumetric flask; and (3) rinsing the filter tip of the sampling gun by using deionized water, transferring the rinsed solution into the same volumetric flask, and diluting the solution to a constant volume of 500mL by using the deionized water to obtain a rinsing solution, namely a first sample. The present invention can directly measure the obtained first sample by an ion selective electrode method.
In certain embodiments of the invention, the temperature of the condensed gas in step a) does not exceed 30 ℃. In certain embodiments, the temperature of the condensed gas in step a) is 28 ℃.
In some implementations of the inventionIn the example, in the step A), the volume of the sample is 0.5-2 m under the standard condition3. In certain embodiments, the volume of the sample is 0.9m under standard conditions3
In certain embodiments of the invention, the temperature of the first sulfuric acid solution impact absorption treatment in step B) is room temperature.
In certain embodiments of the invention, the temperature of the second sulfuric acid solution impact absorption treatment in step B) is room temperature.
In certain embodiments of the present invention, in step B), the concentration of the sulfuric acid liquor subjected to the first sulfuric acid liquor impact absorption treatment is 0.1 mol/L.
In certain embodiments of the present invention, in the step B), the concentration of the sulfuric acid solution subjected to the second sulfuric acid solution impact absorption treatment is 0.1 mol/L.
In some embodiments of the invention, drying is further included after the second shock absorbing treatment of the sulfuric acid solution. The drying is used to remove excess water vapor from the flue gas.
In the invention, gaseous ammonia is collected in the absorption liquid after the two times of absorption treatment. The resulting absorption solution was transferred to a 2 nd 500mL volumetric flask and fixed to volume using deionized water to obtain a second sample. The present invention can directly measure the obtained first sample by an ion selective electrode method.
In some embodiments of the present invention, after the integrated acquisition method is finished, the method further includes:
and (3) rinsing the pipeline and the sampling gun by using deionized water, recovering ammonia adsorbed in the pipeline of the device and the sampling gun, transferring the ammonia and the ammonia into a 3 rd 500mL volumetric flask together, and fixing the volume by using the deionized water to obtain a third sample. The present invention can directly measure the obtained third sample by an ion selective electrode method.
The method can simultaneously collect ammonia in three forms, and fills the blank of the existing detection method. In addition, the collection method provided by the invention has large collection amount, and the collection amount of the smoke can be 1-2 m3The method has the advantages of data representativeness and good accuracy.
In order to further illustrate the present invention, the following will describe the integrated collection method and system for polymorphic ammonia from a stationary source in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
An integrated collection system employing a stationary source of contamination polymorphic ammonia as shown in figure 3, comprising:
a box body (made of stainless steel, and in a cuboid shape, the size is 30cm multiplied by 50cm multiplied by 30 cm); the box body is provided with a sampling gun connecting port and a smoke outlet; a first screw and a second screw are arranged at the bottom of the box body;
the smoke outlet of the heat tracing sampling gun is connected with the box body through a sampling gun connecting port; the gas inlet end of the heat tracing sampling gun is connected with a sampling head, and the sampling head is provided with a sampling nozzle and a filtering membrane;
the pitot tube is used for adjusting the flue gas flow rate of the heat tracing sampling gun and realizing constant-speed tracking sampling;
the smoke temperature line is used for controlling the smoke temperature of the heat tracing sampling gun;
a snake-shaped condensing pipe (the pipe diameter of the snake-shaped condensing pipe is 8mm, the height of the spiral body is 12cm, and the diameter of the spiral body is 8cm) is arranged in the box body, and an inlet of the snake-shaped condensing pipe is connected with a flue gas outlet of the heat tracing sampling gun through a sampling gun connecting port; semiconductor refrigeration pieces (the specification size is 10mm multiplied by 1mm, and the distance between two adjacent semiconductor refrigeration pieces is 3-5 mm) are arranged on the serpentine condensation pipe; a cooling fan is arranged in the center of the spiral body formed by the snake-shaped condensation pipe (the cooling fan is arranged at the bottom of the center of the spiral body, and the diameter of the cooling fan is 5 cm);
the bottom of the box body is connected with a first screw absorption and collection bottle through a first screw; the bottom of the box body is connected with a second screw absorption and collection bottle through a second screw; a condensate outlet of the serpentine condenser pipe enters a first screw absorption and collection bottle through a first screw, non-condensable gas in the first screw absorption and collection bottle enters a second screw absorption and collection bottle, and the non-condensable gas in the second screw absorption and collection bottle is discharged through a smoke outlet of the box body;
a first screw plug is arranged on the bottle mouth of the first screw absorption collecting bottle in a matched manner, a condensate outlet pipe of the serpentine condenser pipe penetrates through the first screw plug and enters the first screw absorption collecting bottle, a first non-condensable gas outlet pipe is further arranged on the first screw plug, and non-condensable gas subjected to primary absorption treatment enters a second screw absorption collecting bottle through the first non-condensable gas outlet pipe on the first screw plug;
a second screw plug is arranged on the bottle mouth of the second screw absorption and collection bottle in a matching manner, and a first non-condensable gas outlet pipe extending out of the first screw plug penetrates through the second screw plug and enters the second screw absorption and collection bottle; a second non-condensable gas outlet pipe is further arranged on the second screw plug, and the non-condensable gas after the second absorption treatment is discharged through a flue gas outlet of the box body;
the touch screen and the power socket are arranged on the outer side of the box body, the circuit system is arranged in the box body, the touch screen receives and transmits electric signals through the circuit system, the semiconductor refrigerating sheet receives and transmits the electric signals through the circuit system, and the cooling fan receives the electric signals through the circuit system;
the gas inlet is connected with the flue gas outlet of the box body;
a cumulative flow meter having a gas inlet connected to the gas outlet of the dryer;
and the gas inlet is connected with the gas outlet of the accumulation flowmeter.
The integrated acquisition method comprises the following steps:
1) sampling the flue gas in the flue by a heat tracing sampling gun, filtering the flue gas entering the heat tracing sampling gun, and then condensing the flue gas in a snake-shaped condensing pipe, wherein the temperature of the condensed gas is 28 ℃, so as to obtain condensable ammonia or ammonium salt; in the sampling process, the temperature of the heat tracing sampling gun is maintained at 120 ℃; the sampling time is 70min, and the sampling volume is 0.9m under standard condition3(ii) a Collecting ammonia or ammonium salt in a particle state on the filter membrane;
2) and after the condensed non-condensable gas is subjected to primary absorption treatment by sulfuric acid solution with the concentration of 0.1mol/L at room temperature, and is subjected to secondary absorption treatment by sulfuric acid solution with the concentration of 0.1mol/L at room temperature, and then the condensed non-condensable gas is dried.
Separately detecting NH in the filtered filter membrane and the absorption liquid4+The content of (a).
The filter was dried in a desiccator for 24h, then taken out and weighed using an electronic balance 0.01mg (AB265-S, MettlerToledo), the filter rinsed with 100mL of deionized water, and transferred to the first 500mL volumetric flask; and (3) rinsing the filter tip of the sampling gun by using deionized water, transferring the rinsed solution into the same volumetric flask, and diluting the solution to a constant volume of 500mL by using the deionized water to obtain a rinsing solution, namely a first sample. Transferring the absorption liquid into a 2 nd 500mL volumetric flask and using deionized water for constant volume to obtain a second sample; after the sample collection is finished, the deionized water is used for rinsing the pipeline and the heat tracing sampling gun, ammonia adsorbed in the device pipeline and the sampling gun is recovered, and the ammonia is transferred to a 3 rd 500mL volumetric flask together and is subjected to constant volume by using the deionized water to obtain a third sample. The resulting first, second and third samples were subjected to direct measurement using an ion selective electrode method.
The invention can simultaneously collect three forms of ammonia, and the ammonia is used as the concentration of total escaping ammonia in the waste gas after being summed, thereby making up the blank of the existing monitoring method.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (9)

1.一种固定污染源多形态氨的一体化采集系统,包括:1. An integrated collection system for fixed pollution source polymorphic ammonia, comprising: 箱体;箱体设置有采样枪连接口和烟气出口;箱体的底部设置有第一螺口和第二螺口;a box body; the box body is provided with a sampling gun connection port and a flue gas outlet; the bottom of the box body is provided with a first screw opening and a second screw opening; 伴热采样枪,所述伴热采样枪的烟气出口通过采样枪连接口与所述箱体连接;所述伴热采样枪的采样头设置有过滤膜;a heat tracing sampling gun, the flue gas outlet of the heat tracing sampling gun is connected to the box body through the connection port of the sampling gun; the sampling head of the heat tracing sampling gun is provided with a filter membrane; 在所述箱体中设置有蛇形冷凝管,所述蛇形冷凝管的进口通过采样枪连接口与所述伴热采样枪的烟气出口相连;在所述蛇形冷凝管上设置有半导体制冷片;在所述蛇形冷凝管形成的螺旋体中心设置有散热风扇;A serpentine condenser tube is arranged in the box, and the inlet of the serpentine condenser tube is connected with the flue gas outlet of the heat tracing sampling gun through the connection port of the sampling gun; a semiconductor is arranged on the serpentine condenser tube a cooling fin; a cooling fan is arranged in the center of the spiral body formed by the serpentine condenser pipe; 所述箱体的底部通过第一螺口与第一螺口吸收收集瓶相连;所述箱体的底部通过第二螺口与第二螺口吸收收集瓶相连;The bottom of the box body is connected with the first screw mouth absorbing and collecting bottle through the first screw mouth; the bottom of the box body is connected with the second screw mouth absorbing and collecting bottle through the second screw mouth; 蛇形冷凝管的冷凝液出口通过第一螺口进入第一螺口吸收收集瓶,所述第一螺口吸收收集瓶中的不凝气体进入第二螺口吸收收集瓶相连,所述第二螺口吸收收集瓶相连中的不凝气体通过箱体的烟气出口排出。The condensate outlet of the serpentine condenser tube enters the first screw mouth absorption collection bottle through the first screw mouth, the non-condensable gas in the first screw mouth absorption collection bottle enters the second screw mouth absorption collection bottle and is connected to The non-condensable gas in the connection of the screw suction collection bottle is discharged through the flue gas outlet of the box. 2.根据权利要求1所述的一体化采集系统,其特征在于,在所述箱体的顶部还设置有散热孔。2 . The integrated collection system according to claim 1 , wherein a heat dissipation hole is further provided on the top of the box. 3 . 3.根据权利要求1所述的一体化采集系统,其特征在于,在所述箱体的外侧设置有触控屏和电源插口,在所述箱体的内部设置有电路系统;3 . The integrated acquisition system according to claim 1 , wherein a touch screen and a power socket are arranged outside the box body, and a circuit system is arranged inside the box body; 3 . 所述触控屏通过电路系统接收和传递电信号;The touch screen receives and transmits electrical signals through the circuit system; 所述半导体制冷片通过电路系统接收和传递电信号;The semiconductor refrigeration chip receives and transmits electrical signals through the circuit system; 所述散热风扇通过电路系统接收电信号。The cooling fan receives electrical signals through the circuit system. 4.根据权利要求1所述的一体化采集系统,其特征在于,还包括:皮托管和烟温线;4. The integrated collection system according to claim 1, further comprising: a pitot tube and a smoke temperature line; 所述皮托管用于调节伴热采样枪的烟气流速;The pitot tube is used to adjust the flue gas flow rate of the heat tracing sampling gun; 所述烟温线用于控制伴热采样枪的烟气温度。The flue gas temperature line is used to control the flue gas temperature of the heat tracing sampling gun. 5.根据权利要求1所述的一体化采集系统,其特征在于,还包括:5. The integrated acquisition system according to claim 1, characterized in that, further comprising: 气体进口与所述箱体的烟气出口相连的干燥器;a dryer whose gas inlet is connected to the flue gas outlet of the box; 气体进口与所述干燥器的气体出口相连的累积流量计;a cumulative flow meter connected to the gas inlet of the dryer; 气体进口与所述累积流量计的气体出口相连的抽气泵。A suction pump whose gas inlet is connected to the gas outlet of the accumulating flowmeter. 6.一种固定污染源多形态氨的一体化采集方法,包括以下步骤:6. An integrated method for collecting polymorphic ammonia from a fixed pollution source, comprising the following steps: A)通过伴热采样枪对烟道内的烟气进行采样,所述伴热采样枪的采样头设置有过滤膜;在所述过滤膜上采集到颗粒态的氨或铵盐;A) Sampling the flue gas in the flue through a heat tracing sampling gun, the sampling head of the heat tracing sampling gun is provided with a filter membrane; the particulate ammonia or ammonium salt is collected on the filter membrane; B)步骤A)采集的烟气进入蛇形冷凝管进行冷凝,得到的冷凝液中采集到可凝态的氨或铵盐;所述采样的过程中,伴热采样枪的温度维持在115~125℃;冷凝后的气体温度不超过30℃;B) The flue gas collected in step A) enters the serpentine condensation tube for condensation, and condensable ammonia or ammonium salt is collected in the obtained condensate; during the sampling process, the temperature of the heat tracing sampling gun is maintained at 115~ 125℃; the gas temperature after condensation does not exceed 30℃; C)所述冷凝后的不凝气体依次经过第一次硫酸液冲击吸收处理和第二次硫酸液冲击吸收处理,采集到气态氨。C) The condensed non-condensable gas is subjected to the first sulfuric acid liquid shock absorption treatment and the second sulfuric acid liquid shock absorption treatment in turn, and gaseous ammonia is collected. 7.根据权利要求6所述的一体化采集方法,其特征在于,步骤A)中,采样的体积在标况下为0.5~2m37 . The integrated collection method according to claim 6 , wherein in step A), the sampled volume is 0.5-2 m 3 under standard conditions. 8 . 8.根据权利要求6所述的一体化采集方法,其特征在于,步骤B)中,所述第一次吸收处理的温度为室温;8. The integrated collection method according to claim 6, wherein in step B), the temperature of the first absorption treatment is room temperature; 所述第二次吸收处理的温度为室温。The temperature of the second absorption treatment is room temperature. 9.根据权利要求6所述的一体化采集方法,其特征在于,步骤B)中,进行第一次吸收处理的硫酸液的浓度为0.1mol/L;9. The integrated collection method according to claim 6, wherein in step B), the concentration of the sulfuric acid liquid for the first absorption treatment is 0.1 mol/L; 进行第二次吸收处理的硫酸液的浓度为0.1mol/L。The concentration of the sulfuric acid liquid subjected to the second absorption treatment was 0.1 mol/L.
CN202011471476.5A 2020-12-14 2020-12-14 Integrated acquisition system and method for polymorphic ammonia of fixed pollution source Pending CN112414796A (en)

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CN110398398A (en) * 2019-07-10 2019-11-01 东南大学 A classification sampling system and method suitable for ammonia emission in high-humidity flue gas

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017071515A1 (en) * 2015-10-29 2017-05-04 清华大学 Device and method enabling industrial coal-fired boiler to concurrently absorb nox and so2
CN108362530A (en) * 2018-03-25 2018-08-03 华电电力科学研究院有限公司 A kind of high humidity gas liquid-solid phase object sampling apparatus and the method for sampling
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