Device and method for measuring concentration of organic amine in waste gas after carbon capture

Abstract

The invention provides a device and a method for measuring the concentration of organic amine in waste gas after carbon capture. The measuring device comprises a gas sampling gun, a pre-filter, a first absorption device, a second absorption device, a dryer, an air extractor and an ion chromatography device which are sequentially connected through pipelines along the gas trend, the gas inlet end of the gas sampling gun extends into the industrial waste gas runner, the gas outlet end of the gas sampling gun is connected with the gas inlet end of the pre-filter, and the outer wall of the gas sampling gun is coated with an electric heating structure. By limiting the measuring device and the measuring method, the concentration of the organic amine in the outlet waste gas of the organic amine chemical absorption method carbon capture system can be detected and analyzed, data support is provided for controlling volatilization and escape of the organic amine in the carbon capture process, and pollution of the organic amine to the ambient atmosphere is reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of industrial carbon capture, and relates to a device and a method for measuring the concentration of organic amines in waste gas after carbon capture. Background Art

[0002] Organic amine chemical absorption carbon capture technology has received much attention and application in the chemical, electric power, metallurgical and other industries. When the waste gas leaves the carbon capture system, it usually carries a certain amount of organic amine absorbent, which will form strong carcinogens after being discharged into the atmosphere, posing a huge threat to human health. Accurate determination of the concentration of organic amines in waste gas after carbon capture is the key to controlling the emission of organic amines.

[0003] Organic amine absorbents are usually volatile, and their content in the exhaust gas after carbon capture is affected by multiple factors such as temperature, pressure, humidity and composition. The organic amines exist in the exhaust gas in the form of droplets, gas and aerosol. The content in the exhaust gas at the outlet of the carbon capture system is 0.5-5 mg / m 3 Due to the lack of suitable online detection devices, the current detection and analysis of organic amine concentrations in gases often adopts an offline method, that is, sampling on site and then sending it to the laboratory for detection and analysis.

[0004] The prior art solution discloses a method and application for measuring the concentration of gas-phase organic amines, which uses an excess of acidic solution to absorb organic amines in waste gas or air, and then performs acid-base titration on the absorption liquid. The amount of organic amine substance is obtained by calculating the difference between the amount of hydrogen ions in the acidic solution and the amount of hydroxide ions consumed in the alkaline solution, and the gas-phase organic amine concentration is calculated in combination with the volume of the gas sampling.

[0005] The prior art solution also discloses a gaseous organic amine collection device and method, in which a filter head A, a first gas washing bottle, a second gas washing bottle, a one-way valve, a filter head B and an air pump are arranged in sequence along the gas flow direction. The gas washing bottle is filled with an inorganic acid solution that can absorb organic amines. The organic amines in the absorption solution are determined by titration, and the concentration of the gaseous organic amines is calculated in combination with the sampling volume of the air pump.

[0006] At present, there are methods for measuring and analyzing the concentration of organic amines in the field of atmospheric environmental protection. However, since the composition of industrial waste gas is more complex than that of air and the test environment is more severe, the existing methods for measuring the concentration of organic amines in the air are not suitable for testing the concentration of organic amines in industrial waste gas. The solid particulate matter, moisture and other impurity gases contained in industrial waste gas are greater than those in the air. At the same time, when industrial waste gas is extracted from the flue, its parameters such as pressure and temperature will change, causing the existence form of organic amines to change, resulting in certain measurement errors. In addition, with the iterative upgrade of organic amine absorbents, the sampling and analysis technology used in the existing technical solutions is not applicable to the measurement of the concentration of organic amines in the exhaust gas at the outlet of the carbon capture system. For example, for composite amine solutions, it is difficult to distinguish the concentrations of different effective components by titration. Therefore, it is urgent to design a measuring device and method for the concentration of organic amines in exhaust gas after carbon capture to overcome the defects of the existing technology and meet the needs of practical applications. Summary of the invention

[0007] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a measuring device and method for the concentration of organic amines in exhaust gas after carbon capture. In the present invention, by limiting the measuring device, the concentration of organic amines in the exhaust gas at the outlet of the organic amine chemical absorption carbon capture system can be detected and analyzed, providing data support for controlling the volatilization and escape of organic amines in the carbon capture process, and reducing the pollution of organic amines to the ambient atmosphere.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a device for measuring the concentration of organic amines in exhaust gas after carbon capture, the device comprising a gas sampling gun, a pre-filter, at least two groups of absorption devices, a dryer and a gas extraction device connected in sequence along the direction of the gas;

[0010] The air inlet end of the gas sampling gun extends into the industrial waste gas flow channel, the air outlet end is connected to the air inlet end of the pre-filter, and the outer wall of the gas sampling gun is covered with an electric heating structure;

[0011] Each group of the absorption devices is connected in series.

[0012] In the present invention, by limiting the measuring device, the concentration of organic amines in the exhaust gas at the outlet of the organic amine chemical absorption carbon capture system can be detected and analyzed, providing data support for controlling the volatilization and escape of organic amines during the carbon capture process, and reducing the pollution of organic amines to the ambient atmosphere.

[0013] It should be noted that, in view of the characteristics of industrial waste gas, the present invention designs a gas sampling and measuring device with complete functions, easy operation and accurate measurement, that is, a combination of a gas sampling gun, a pre-filter, at least two groups of absorption devices, a dryer and a vacuum device, and proposes a corresponding operating method, which realizes the accurate measurement of the escape concentration of organic amines in industrial waste gas, provides data support for the performance evaluation of the carbon capture system absorbent, and lays the foundation for controlling the emission of organic pollutants.

[0014] It should be noted that the specific model and structure of the gas sampling gun are not particularly limited in the present invention, and those skilled in the art can make adaptive adjustments according to actual conditions. The air inlet end of the gas sampling gun should be designed to face the airflow. By heating the gas sampling gun, the organic amines in the exhaust gas can be converted into a gaseous state, which can reduce the content of organic amines in the form of droplets or aerosols and reduce gas sampling errors.

[0015] It should be noted that the pre-filter of the present invention is located after the gas sampling gun, which can not only effectively filter the solid particles in the gas, but also prevent the organic amines in the form of droplets and aerosols from adhering to the filter material.

[0016] It should be noted that the at least two groups of absorption devices in the present invention may be, for example, 2 groups, 3 groups, 4 groups, 5 groups, 6 groups, etc., but are not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0017] As a preferred technical solution of the present invention, the electric heating structure includes a temperature measuring device, a temperature controller and an electric heating sleeve which are electrically connected in sequence, and the electric heating sleeve is sleeved on the outer wall of the gas sampling gun.

[0018] Preferably, one end of the temperature measuring device is arranged in the gas sampling gun.

[0019] It should be noted that the internal structure of the sampling gun in the present invention can be a straight pipe section, which can enhance the heat exchange effect between the inner wall of the sampling gun and the flue gas, while ensuring daily cleaning and maintenance. The straight pipe section is provided with an insert, such as a tie, a spiral coil, a wound wire, a spiral spring, etc.

[0020] It should be noted that the working principle of the electric heating structure in the present invention includes a temperature measuring device extending into the tail of the gas sampling gun, converting the temperature into an electrical signal and inputting it into a temperature controller. The temperature controller timely adjusts the power of the electric heating sleeve to make the temperature inside the gas sampling gun about 150°C, which can not only convert all the organic amines in the exhaust gas into a gaseous state, but also prevent the industrial exhaust gas in the gas sampling gun from condensing and corroding due to the lowering of temperature.

[0021] As a preferred technical solution of the present invention, the filter material used in the pre-filter is quartz wool or alkali-free glass wool.

[0022] It should be noted that the present invention does not limit the filling amount of quartz wool or alkali-free glass wool, the purpose of which is to prevent solid particles in industrial waste gas from entering the absorption liquid and affecting the subsequent measurement of organic amine concentration.

[0023] As a preferred technical solution of the present invention, the at least two groups of absorption devices include a first absorption device and a second absorption device.

[0024] Preferably, the first absorption device comprises a first absorption bottle, in which a first absorption solvent is arranged.

[0025] Preferably, the first absorption solvent is a dilute sulfuric acid solution or a dilute hydrochloric acid solution.

[0026] As a preferred technical solution of the present invention, the second absorption device includes a second absorption bottle, and the second absorption solvent is arranged in the second absorption bottle.

[0027] Preferably, the second absorption solvent is a dilute sulfuric acid solution or a dilute hydrochloric acid solution.

[0028] It should be noted that the first absorption solvent and the second absorption solvent in the present invention can be the same or different, and the two can independently select any one of dilute sulfuric acid solution or dilute hydrochloric acid solution; wherein, the first absorption bottle can be filled with 75 ml of dilute sulfuric acid solution, the solution concentration is 0.05 mol per liter, and the first absorption bottle adopts a standard frosted mouth and has good sealing; the second absorption bottle is filled with 75 ml of dilute sulfuric acid solution, the solution concentration is 0.05 mol per liter, and the second absorption bottle adopts a standard frosted mouth and has good sealing. Furthermore, the concentration and volume of the first absorption solvent and the second absorption solvent can be adaptively adjusted according to actual conditions.

[0029] It should be noted that, in order to absorb the organic amines in the exhaust gas as much as possible, the present invention mainly uses an inorganic acid solution as an absorbent and adopts a multi-stage porous absorption bottle as a main absorption device.

[0030] As a preferred technical solution of the present invention, a moisture absorbent is arranged in the dryer.

[0031] It should be noted that the present invention does not specifically limit the specific structure of the dryer, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0032] Preferably, the desiccant is color-changing silica gel or spherical molecular sieve.

[0033] It should be noted that the desiccant in the present invention can absorb water vapor in the gas to protect the sampling pump, and specifically, any one of color-changing silica gel or spherical molecular sieve can be selected.

[0034] As a preferred technical solution of the present invention, the air extraction device includes a sampling pump and an air extraction pipeline which are sequentially connected along the direction of the gas.

[0035] It should be noted that the sampling pump is designed in the present invention because its working flow rate is adjustable, the suction pressure can overcome the pressure of the flow channel and the sampling system, and ensure sufficient gas sampling volume, wherein the sampling pump suction flow rate operates stably in the range of 0 to 20 liters per minute, and the sampling gas volume can be adjusted as needed; the present invention does not specifically limit the specific model of the sampling pump, and technical personnel in this field can make adaptive adjustments according to actual conditions.

[0036] Preferably, a gas flow meter is provided on the air extraction pipeline, and the gas flow meter is used to measure the volume of the sampled gas.

[0037] It should be noted that the specific model of the gas flow meter in the present invention is not particularly limited, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0038] Preferably, a thermometer and a pressure gauge are also provided on the air extraction pipeline to measure the temperature and pressure of the sampled gas.

[0039] It should be noted that the specific models of the thermometer and the pressure gauge in the present invention are not particularly limited, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0040] In a second aspect, the present invention provides a method for measuring the concentration of organic amines in exhaust gas after carbon capture, wherein the measuring method is performed using the measuring device described in the first aspect.

[0041] As a preferred technical solution of the present invention, the measuring method comprises:

[0042] (1) Filling the pre-filter with filter material, adding the first absorption solvent and the second absorption solvent into the first absorption bottle and the second absorption bottle respectively, and adding a moisture absorbent into the dryer;

[0043] (2) Connect the outlet end of the gas sampling gun to the electric heater, pre-filter, first absorption bottle, second absorption bottle, dryer, sampling pump and gas flow meter in sequence along the direction of the gas, and check the air tightness of the measuring device;

[0044] (3) Turn on the electric heater to heat the gas sampling gun. After the temperature reaches the set value, extend the gas inlet end of the gas sampling gun into the industrial waste gas flow channel;

[0045] (4) Turn on the sampling pump, adjust the air flow rate to the set value, set the air extraction time, record the air extraction temperature and air extraction pressure, and when the air extraction time is reached, turn off the sampling pump and record the air extraction volume displayed by the gas flow meter;

[0046] (5) Rinse the gas sampling gun, collect and mix the solution in the first absorption bottle and the solution in the second absorption bottle, mix the rinse solution with the mixed solution again, dilute it, and record the volume of the diluted solution;

[0047] (6) The diluted solution is quantitatively analyzed by an ion chromatography device, the volume concentration of each effective component is recorded, and the component mass of the organic amine, the gas sampling volume under standard conditions, and the organic amine concentration in the industrial waste gas under standard conditions are calculated in turn.

[0048] It should be noted that, in order to solve the problem that it is difficult to measure the amount of organic amine pollutants carried in the exhaust gas after passing through the carbon capture system, the present invention proposes a device and method for measuring the concentration of organic amines in the exhaust gas after carbon capture, wherein the gas sampling gun used heats the gas during the sampling process, and the organic amines in the exhaust gas are converted into gas in the form of the gas, thereby achieving complete absorption of the organic amines; by arranging the pre-filter at the rear end of the gas sampling gun, it is possible to effectively filter the solid particulate matter in the exhaust gas and ensure the smooth passage of the gaseous organic amines; the absorption liquid analysis device used adopts cation chromatography, which only requires diluting the absorbent, without the need for complicated extraction and derivatization processes, and can also avoid the problems of large measurement errors caused by acid-base titration.

[0049] As a preferred technical solution of the present invention, in step (3), the temperature setting value is 100-150°C, for example, it can be 100°C, 105°C, 110°C, 115°C, 120°C, 125°C, 130°C, 135°C, 140°C, 145°C, 150°C, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0050] The temperature setting value in the present invention is 100-150°C because within this range, the water vapor in the exhaust gas will not condense or the organic amine will not overheat and decompose. If it is not within this range, inaccurate measurement may occur; when the temperature is less than 100°C, the water vapor in the exhaust gas will condense and precipitate, and the organic amine molecules will be absorbed by the condensed water and adhere to the inner wall of the pipeline without being absorbed by the absorption liquid; when the temperature is greater than 150°C, the organic amine may overheat and decompose, resulting in inaccurate measurement.

[0051] Preferably, in step (4), the set value for adjusting the exhaust air flow rate is 30 to 40 L / min, for example, it can be 30 L / min, 32 L / min, 34 L / min, 36 L / min, 38 L / min, 40 L / min, etc., but is not limited to the listed values, and other unlisted values ​​within this numerical range are also applicable.

[0052] Preferably, in step (4), the set value of the pumping time is greater than 40 min, for example, it can be 41 L / min, 42 L / min, 44 L / min, 50 L / min, 58 L / min, 60 L / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0053] Preferably, in step (5), the rinse gas sampling gun is rinsed with high-purity water.

[0054] Preferably, in step (5), the dilution treatment is performed in the following manner:

[0055] A certain multiple of high-purity water is added to the solution after the rinse solution and the mixed solution are mixed again for dilution.

[0056] Preferably, the certain multiple is 5 to 10 times, for example, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0057] The certain multiple in the present invention is 5 to 10 times because the measurement results of ion chromatography can be more accurate within this range. If it is not within this range, the detection results may deviate greatly. This is because when the dilution multiple is small, the sample components are highly complex and the solution pH is acidic, which does not meet the neutral requirement; when the dilution multiple is high, it may be less than the detection limit and the measurement data is inaccurate.

[0058] Preferably, in step (6), the ion chromatography device uses a cation chromatography column.

[0059] It should be noted that the present invention can accurately and quantitatively analyze the mixed organic amine components in the exhaust gas by adopting the cation chromatography method, wherein the model of the cation chromatography column adopted can be adaptively adjusted according to the actual situation.

[0060] Compared with the prior art, the present invention has the following beneficial effects:

[0061] In the present invention, by limiting the measuring device and the measuring method, the concentration of organic amines in the exhaust gas at the outlet of the organic amine chemical absorption carbon capture system can be detected and analyzed, providing data support for controlling the volatilization and escape of organic amines during the carbon capture process, and reducing the pollution of organic amines to the ambient atmosphere. BRIEF DESCRIPTION OF THE DRAWINGS

[0062] Figure 1 A schematic diagram of the structure of a device for measuring the concentration of organic amines in exhaust gas after carbon capture provided by a specific embodiment of the present invention;

[0063] Among them, 1-gas sampling gun; 2-electric heating jacket; 3-pre-filter; 4-first absorption device; 5-second absorption device; 6-dryer; 7-sampling pump; 8-thermometer; 9-pressure gauge; 10-gas flow meter. DETAILED DESCRIPTION

[0064] It should be understood that, in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0065] It should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "disposed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood by specific circumstances.

[0066] Those skilled in the art should understand that the present invention necessarily includes necessary pipelines, conventional valves and general pump equipment for realizing a complete process, but the above content does not belong to the main inventive point of the present invention. Those skilled in the art can add layouts on their own based on the process flow and equipment structure selection, and the present invention does not make special requirements and specific limitations on this.

[0067] The technical solution of the present invention is further described below with reference to the accompanying drawings and through specific implementation methods.

[0068] In one embodiment, the present invention provides a device for measuring the concentration of organic amines in exhaust gas after carbon capture, such as Figure 1As shown, the measuring device includes a gas sampling gun 1, a pre-filter 3, at least two groups of absorption devices, a dryer 6 and an exhaust device which are connected in sequence along the direction of the gas; the air inlet end of the gas sampling gun 1 extends into the industrial waste gas flow channel, and the air outlet end is connected to the air inlet end of the pre-filter 3, and the outer wall of the gas sampling gun 1 is covered with an electric heating structure; each group of absorption devices is connected in series.

[0069] It should be noted that, in view of the characteristics of industrial waste gas, the present invention designs a gas sampling and measuring device with complete functions, convenient operation and accurate measurement, that is, a combination of a gas sampling gun 1, a pre-filter 3, at least two groups of absorption devices, a dryer 6 and a vacuum device, and proposes a corresponding operation method, thereby achieving accurate measurement of the escape concentration of organic amines in industrial waste gas, providing data support for the performance evaluation of the carbon capture system absorbent, and laying a foundation for controlling the emission of organic pollutants.

[0070] It should be noted that the specific model and structure of the gas sampling gun 1 are not particularly limited in the present invention, and those skilled in the art can make adaptive adjustments according to actual conditions. The air inlet end of the gas sampling gun 1 should be designed to face the airflow. By heating the gas sampling gun 1, the organic amines in the exhaust gas can be converted into a gaseous state, which can reduce the content of organic amines in the form of droplets or aerosols and reduce gas sampling errors.

[0071] It should be noted that the pre-filter 3 of the present invention is located after the gas sampling gun 1, which can not only effectively filter the solid particles in the gas, but also prevent the organic amines in the form of droplets and aerosols from adhering to the filter material.

[0072] In one embodiment, the electric heating structure includes a temperature measuring device, a temperature controller and an electric heating jacket 2 which are electrically connected in sequence, and the electric heating jacket 2 is sleeved on the outer wall of the gas sampling gun 1 .

[0073] In one embodiment, one end of the temperature measuring device is disposed in the gas sampling gun 1 .

[0074] It should be noted that the working principle of the electric heating structure in the present invention includes a temperature measuring device extending into the tail of the gas sampling gun 1, converting the temperature into an electrical signal and inputting it into a temperature controller. The temperature controller timely adjusts the power of the electric heating sleeve 2 to make the temperature inside the gas sampling gun 1 about 150°C, which can not only convert all the organic amines in the exhaust gas into a gaseous state, but also prevent the industrial exhaust gas in the gas sampling gun 1 from condensing and corroding due to the decrease in temperature.

[0075] In one embodiment, the filter material used in the pre-filter 3 is quartz wool or alkali-free glass wool.

[0076] It should be noted that the present invention does not limit the filling amount of quartz wool or alkali-free glass wool, the purpose of which is to prevent solid particles in industrial waste gas from entering the absorption liquid and affecting the subsequent measurement of organic amine concentration.

[0077] In one embodiment, the at least two groups of absorption devices include a first absorption device 4 and a second absorption device 5 .

[0078] In one embodiment, the first absorption device 4 comprises a first absorption bottle, in which a first absorption solvent is arranged.

[0079] In one embodiment, the first absorption solvent is a dilute sulfuric acid solution or a dilute hydrochloric acid solution.

[0080] In one embodiment, the second absorption device 5 comprises a second absorption bottle, in which a second absorption solvent is arranged.

[0081] In one embodiment, the second absorption solvent is a dilute sulfuric acid solution or a dilute hydrochloric acid solution.

[0082] It should be noted that the first absorption solvent and the second absorption solvent in the present invention can be the same or different, and the two can independently select any one of dilute sulfuric acid solution or dilute hydrochloric acid solution; wherein, the first absorption bottle can be filled with 75 ml of dilute sulfuric acid solution, the solution concentration is 0.05 mol per liter, and the first absorption bottle adopts a standard frosted mouth and has good sealing; the second absorption bottle is filled with 75 ml of dilute sulfuric acid solution, the solution concentration is 0.05 mol per liter, and the second absorption bottle adopts a standard frosted mouth and has good sealing. Furthermore, the concentration and volume of the first absorption solvent and the second absorption solvent can be adaptively adjusted according to actual conditions.

[0083] It should be noted that, in order to absorb the organic amines in the exhaust gas as much as possible, the present invention mainly uses an inorganic acid solution as an absorbent and adopts a multi-stage porous absorption bottle as a main absorption device.

[0084] In one embodiment, a moisture absorbent is disposed in the dryer 6 .

[0085] It should be noted that the present invention does not specifically limit the specific structure of the dryer 6, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0086] In one embodiment, the moisture absorbent is color-changing silica gel or spherical molecular sieve.

[0087] It should be noted that the desiccant in the present invention can absorb water vapor in the gas to protect the sampling pump 7, and specifically, any one of color-changing silica gel or spherical molecular sieve can be selected.

[0088] In one embodiment, the air extraction device includes a sampling pump 7 and an air extraction pipeline which are sequentially connected along the direction of the gas.

[0089] It should be noted that the sampling pump 7 is designed in the present invention because its working flow rate is adjustable, the suction pressure can overcome the pressure of the flow channel and the sampling system, and ensure sufficient gas sampling volume, wherein the suction flow rate of the sampling pump 7 works stably in the range of 0 to 20 liters per minute, and the sampling gas volume can be adjusted as needed; the present invention does not specifically limit the specific model of the sampling pump 7, and technical personnel in this field can make adaptive adjustments according to actual conditions.

[0090] In one embodiment, a gas flow meter 10 is provided on the gas extraction pipeline, and the gas flow meter 10 is used to measure the volume of the sampled gas.

[0091] It should be noted that the specific model of the gas flow meter 10 in the present invention is not particularly limited, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0092] In one embodiment, a thermometer 8 and a pressure gauge 9 are also provided on the gas extraction pipeline to measure the temperature and pressure of the sampled gas.

[0093] It should be noted that the specific models of the thermometer 8 and the pressure gauge 9 in the present invention are not particularly limited, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0094] In another specific embodiment, the present invention provides a method for measuring the concentration of organic amines in exhaust gas after carbon capture, and the measurement method is performed using the above-mentioned measurement device.

[0095] In one embodiment, the measuring method comprises:

[0096] (1) Fill the pre-filter 3 with filter material, add the first absorption solvent and the second absorption solvent to the first absorption bottle and the second absorption bottle respectively, and add the moisture absorbent to the dryer 6;

[0097] (2) Connect the outlet end of the gas sampling gun 1 to the electric heater, the pre-filter 3, the first absorption bottle, the second absorption bottle, the dryer 6, the sampling pump 7 and the gas flow meter 10 in sequence along the gas flow direction, and check the air tightness of the measuring device;

[0098] (3) turning on the electric heater to heat the gas sampling gun 1, and after the temperature reaches the set value, extending the air inlet end of the gas sampling gun 1 into the industrial waste gas flow passage;

[0099] (4) Turn on the sampling pump 7, adjust the air extraction flow rate to the set value, set the air extraction time, record the air extraction temperature and air extraction pressure, and when the air extraction time is reached, turn off the sampling pump 7 and record the air extraction volume displayed by the gas flow meter 10;

[0100] (5) Rinse the gas sampling gun 1, collect and mix the solution in the first absorption bottle and the solution in the second absorption bottle, mix the rinse solution with the mixed solution again, dilute it, and record the volume of the diluted solution;

[0101] (6) The diluted solution is quantitatively analyzed by an ion chromatography device, the volume concentration of each effective component is recorded, and the component mass of the organic amine, the gas sampling volume under standard conditions, and the organic amine concentration in the industrial waste gas under standard conditions are calculated in turn.

[0102] In one embodiment, in step (3), the temperature setting value is 100-150°C, for example, it can be 100°C, 105°C, 110°C, 115°C, 120°C, 125°C, 130°C, 135°C, 140°C, 145°C, 150°C, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0103] In one embodiment, in step (4), the set value of the exhaust air flow rate is adjusted to 30-40 L / min, for example, it can be 30 L / min, 32 L / min, 34 L / min, 36 L / min, 38 L / min, 40 L / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0104] In one embodiment, in step (4), the set value of the vacuum time is greater than 40 min, for example, it can be 41 L / min, 42 L / min, 44 L / min, 50 L / min, 58 L / min, 60 L / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0105] In one embodiment, in step (5), the gas sampling gun 1 is rinsed with high-purity water.

[0106] In one embodiment, in step (5), the dilution process is performed by:

[0107] A certain multiple of high-purity water is added to the solution after the rinse solution and the mixed solution are mixed again for dilution.

[0108] In one embodiment, the certain multiple is 5 to 10 times, for example, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0109] In one embodiment, in step (6), the ion chromatography device uses a cation chromatography column.

[0110] It should be noted that the present invention can accurately and quantitatively analyze the mixed organic amine components in the exhaust gas by adopting the cation chromatography method, wherein the model of the cation chromatography column adopted can be adaptively adjusted according to the actual situation.

[0111] Example 1

[0112] This embodiment provides a device for measuring the concentration of organic amines in exhaust gas after carbon capture, wherein:

[0113] The measuring device comprises a gas sampling gun 1, a pre-filter 3, a first absorption device 4, a second absorption device 5, a dryer 6 and an exhaust device which are sequentially connected by pipelines along the direction of the gas; the air inlet end of the gas sampling gun 1 extends into the industrial waste gas flow channel, the air outlet end is connected to the air inlet end of the pre-filter 3, and the outer wall of the gas sampling gun 1 is covered with an electric heating structure; each group of absorption devices is connected in series.

[0114] The electric heating structure comprises a temperature measuring device, a temperature controller and an electric heating sleeve 2 which are electrically connected in sequence. The electric heating sleeve 2 is sleeved on the outer wall of the gas sampling gun 1 , and one end of the temperature measuring device is arranged inside the gas sampling gun 1 .

[0115] The filter material used in the pre-filter 3 is quartz wool.

[0116] The first absorption device 4 comprises a first absorption bottle, in which a dilute sulfuric acid solution is arranged. The second absorption device 5 comprises a second absorption bottle, in which a dilute sulfuric acid solution is arranged.

[0117] A desiccant is arranged in the dryer 6, and the desiccant is color-changing silica gel.

[0118] The air extraction device comprises a sampling pump 7 and an air extraction pipeline which are sequentially connected along the direction of the gas. A gas flow meter 10, a thermometer 8 and a pressure gauge 9 are arranged on the air extraction pipeline.

[0119] A method for measuring the concentration of organic amines in exhaust gas after carbon capture in this embodiment includes:

[0120] (1) Fill the pre-filter 3 with quartz wool, add dilute sulfuric acid solution to the first absorption bottle and the second absorption bottle, and add color-changing silica gel to the dryer 6;

[0121] (2) Connect the outlet end of the gas sampling gun 1 to the electric heater, the pre-filter 3, the first absorption bottle, the second absorption bottle, the dryer 6, the sampling pump 7 and the gas flow meter 10 in sequence along the gas flow direction, and check the air tightness of the measuring device;

[0122] (3) Turn on the electric heater to heat the gas sampling gun 1. After the temperature reaches 100° C., extend the gas inlet end of the gas sampling gun 1 into the industrial waste gas flow passage;

[0123] (4) Turn on the sampling pump 7, adjust the air flow rate to 30 L / min, and set the air extraction time to 50 min. Record the air extraction temperature and air extraction pressure. After the air extraction time is reached, turn off the sampling pump 7 and record the air extraction volume displayed by the gas flow meter 10;

[0124] (5) Rinse the gas sampling gun 1, collect and mix the solution in the first absorption bottle and the solution in the second absorption bottle, mix the rinse solution with the mixed solution again, dilute it, and record the volume of the diluted solution;

[0125] (6) The diluted solution is quantitatively analyzed by an ion chromatography device, the volume concentration of each effective component is recorded, and the component mass of the organic amine, the gas sampling volume under standard conditions, and the organic amine concentration in the industrial waste gas under standard conditions are calculated in turn.

[0126] In step (5), the dilution process is performed in the following manner:

[0127] Add 5 times of high-purity water to the solution after the rinse solution and the mixed solution are mixed again to dilute it.

[0128] In step (6), the ion chromatography device uses a cation chromatography column.

[0129] Example 2

[0130] This embodiment provides a device for measuring the concentration of organic amines in exhaust gas after carbon capture, wherein:

[0131] The measuring device comprises a gas sampling gun 1, a pre-filter 3, a first absorption device 4, a second absorption device 5, a dryer 6 and an exhaust device which are sequentially connected by pipelines along the direction of the gas; the air inlet end of the gas sampling gun 1 extends into the industrial waste gas flow channel, the air outlet end is connected to the air inlet end of the pre-filter 3, and the outer wall of the gas sampling gun 1 is covered with an electric heating structure; each group of absorption devices is connected in series.

[0132] The electric heating structure comprises a temperature measuring device, a temperature controller and an electric heating sleeve 2 which are electrically connected in sequence. The electric heating sleeve 2 is sleeved on the outer wall of the gas sampling gun 1 , and one end of the temperature measuring device is arranged inside the gas sampling gun 1 .

[0133] The filter material used in the pre-filter 3 is alkali-free glass wool.

[0134] The first absorption device 4 comprises a first absorption bottle, in which a dilute hydrochloric acid solution is arranged. The second absorption device 5 comprises a second absorption bottle, in which a dilute hydrochloric acid solution is arranged.

[0135] The dryer 6 is provided with a spherical molecular sieve.

[0136] The air extraction device comprises a sampling pump 7 and an air extraction pipeline which are sequentially connected along the direction of the gas. A gas flow meter 10, a thermometer 8 and a pressure gauge 9 are arranged on the air extraction pipeline.

[0137] A method for measuring the concentration of organic amines in exhaust gas after carbon capture in this embodiment includes:

[0138] (1) Fill the pre-filter 3 with alkali-free glass wool, add dilute hydrochloric acid solution to the first absorption bottle and the second absorption bottle, and add spherical molecular sieves to the dryer 6;

[0139] (2) Connect the outlet end of the gas sampling gun 1 to the electric heater, the pre-filter 3, the first absorption bottle, the second absorption bottle, the dryer 6, the sampling pump 7 and the gas flow meter 10 in sequence along the gas flow direction, and check the air tightness of the measuring device;

[0140] (3) Turn on the electric heater to heat the gas sampling gun 1. After the temperature reaches 150° C., extend the gas inlet end of the gas sampling gun 1 into the industrial waste gas flow passage;

[0141] (4) Turn on the sampling pump 7, adjust the air flow rate to 40 L / min, and set the air extraction time to 40 min. Record the air extraction temperature and air extraction pressure. After the air extraction time is reached, turn off the sampling pump 7 and record the air extraction volume displayed by the gas flow meter 10.

[0142] (5) Rinse the gas sampling gun 1, collect and mix the solution in the first absorption bottle and the solution in the second absorption bottle, mix the rinse solution with the mixed solution again, dilute it, and record the volume of the diluted solution;

[0143] (6) The diluted solution is quantitatively analyzed by an ion chromatography device, the volume concentration of each effective component is recorded, and the component mass of the organic amine, the gas sampling volume under standard conditions, and the organic amine concentration in the industrial waste gas under standard conditions are calculated in turn.

[0144] In step (5), the dilution process is performed in the following manner:

[0145] Add 10 times of high-purity water to the solution after the rinse solution and the mixed solution are mixed again to dilute it.

[0146] In step (6), the ion chromatography device uses a cation chromatography column.

[0147] Comparative Example 1

[0148] This comparative example provides a device for measuring the concentration of an organic amine, wherein:

[0149] A filter head A, a first gas washing bottle, a second gas washing bottle, a one-way valve, a filter head B and an air pump are arranged in sequence along the gas flow direction. The gas washing bottle is filled with an inorganic acid solution capable of absorbing organic amines, and the organic amines in the absorption solution are determined by titration.

[0150] The organic amine concentration of the measuring device used in the above examples and comparative examples was measured with a gas flow rate of 40 L / min and a time of 40 min. The results are shown in Table 1 below:

[0151] Table 1 Organic amine measurement results of the measuring devices of the embodiment and the comparative example

[0152]

[0153]

[0154] It can be seen from Table 1 above that the accuracy of the measuring device in the present invention is higher than that of the measuring device in the comparative example. This is because the gas sampling gun used in the present invention heats the gas during the sampling process, and by converting the form of organic amines in the exhaust gas into gas, the complete absorption of organic amines can be achieved; by setting the pre-filter 3 at the rear end of the gas sampling gun 1, it is possible to effectively filter the solid particulate matter in the exhaust gas and ensure the smooth passage of gaseous organic amines; the absorption liquid analysis device used adopts cation chromatography, which only requires diluting the absorbent, without the need for complicated extraction and derivatization processes, and can also avoid the problems of large measurement errors caused by acid-base titration.

[0155] In summary, the present invention can detect and analyze the concentration of organic amines in the exhaust gas at the outlet of the organic amine chemical absorption carbon capture system by limiting the measuring device and the measuring method, provide data support for controlling the volatilization and escape of organic amines during the carbon capture process, and reduce the pollution of organic amines to the ambient atmosphere.

[0156] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention are within the protection scope and disclosure scope of the present invention.

Claims

1. A device for measuring the concentration of organic amines in exhaust gas after carbon capture, characterized in that: The measuring device comprises a gas sampling gun, a pre-filter, at least two groups of absorption devices, a dryer and a gas extraction device which are sequentially connected by pipelines along the direction of the gas; The air inlet end of the gas sampling gun extends into the industrial waste gas flow channel, the air outlet end is connected to the air inlet end of the pre-filter, and the outer wall of the gas sampling gun is covered with an electric heating structure; Each group of the absorption devices is connected in series.

2. The measuring device according to claim 1, characterized in that The electric heating structure comprises a temperature measuring device, a temperature controller and an electric heating sleeve which are electrically connected in sequence, and the electric heating sleeve is sleeved on the outer wall of the gas sampling gun; Preferably, one end of the temperature measuring device is arranged in the gas sampling gun.

3. The measuring device according to claim 1 or 2, characterized in that: The filter material used in the pre-filter is quartz wool or alkali-free glass wool.

4. The measuring device according to any one of claims 1 to 3, characterized in that: The at least two groups of absorption devices include a first absorption device and a second absorption device; Preferably, the first absorption device comprises a first absorption bottle, in which a first absorption solvent is arranged; Preferably, the first absorption solvent is a dilute sulfuric acid solution or a dilute hydrochloric acid solution.

5. The measuring device according to claim 4, characterized in that The second absorption device comprises a second absorption bottle, and the second absorption solvent is arranged in the second absorption bottle; Preferably, the second absorption solvent is a dilute sulfuric acid solution or a dilute hydrochloric acid solution.

6. The measuring device according to any one of claims 1 to 5, characterized in that: A moisture absorbent is provided in the dryer; Preferably, the desiccant is color-changing silica gel or spherical molecular sieve.

7. The measuring device according to any one of claims 1 to 6, characterized in that: The gas extraction device comprises a sampling pump and a gas extraction pipeline which are sequentially connected along the direction of the gas; Preferably, a gas flow meter is provided on the gas extraction pipeline, and the gas flow meter is used to measure the volume of the sampled gas; Preferably, a thermometer and a pressure gauge are also provided on the air extraction pipeline to measure the temperature and pressure of the sampled gas.

8. A method for measuring the concentration of organic amines in exhaust gas after carbon capture, characterized in that: The measuring method is performed using the measuring device described in any one of claims 1 to 7.

9. The measuring method according to claim 8, characterized in that: The measuring method comprises: (1) Filling the pre-filter with filter material, adding the first absorption solvent and the second absorption solvent into the first absorption bottle and the second absorption bottle respectively, and adding a moisture absorbent into the dryer; (2) Connect the outlet end of the gas sampling gun to the electric heater, pre-filter, first absorption bottle, second absorption bottle, dryer, sampling pump and gas flow meter in sequence along the direction of the gas, and check the air tightness of the measuring device; (3) Turn on the electric heater to heat the gas sampling gun. After the temperature reaches the set value, extend the gas inlet end of the gas sampling gun into the industrial waste gas flow channel; (4) Turn on the sampling pump, adjust the air flow rate to the set value, set the air extraction time, record the air extraction temperature and air extraction pressure, and when the air extraction time is reached, turn off the sampling pump and record the air extraction volume displayed by the gas flow meter; (5) Rinse the gas sampling gun, collect and mix the solution in the first absorption bottle and the solution in the second absorption bottle, mix the rinse solution with the mixed solution again, dilute it, and record the volume of the diluted solution; (6) The diluted solution is quantitatively analyzed by an ion chromatography device, the volume concentration of each effective component is recorded, and the component mass of the organic amine, the gas sampling volume under standard conditions, and the organic amine concentration in the industrial waste gas under standard conditions are calculated in turn.

10. The measuring method according to claim 9, characterized in that: In step (3), the temperature setting value is 100-150° C.; Preferably, in step (4), the set value of adjusting the exhaust air flow rate is 30 to 40 L / min; Preferably, in step (4), the set value of the air extraction time is greater than 40 minutes; Preferably, in step (5), the rinse gas sampling gun is rinsed with high-purity water; Preferably, in step (5), the dilution treatment is performed in the following manner: Add a certain multiple of high-purity water to the solution after the rinse solution and the mixed solution are mixed again for dilution; Preferably, the certain multiple is 5 to 10 times; Preferably, in step (6), the ion chromatography device uses a cation chromatography column.

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