CN110864946A - Device and method for measuring mercury content in flue gas - Google Patents
Device and method for measuring mercury content in flue gas Download PDFInfo
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Abstract
A device and method for measuring mercury content in flue gas, the device includes a flue gas sampling pretreatment module, an Ar gas storage cylinder, a mercury enrichment module, an electromagnetic induction heating module and a mercury content detection module; the mercury enrichment module comprises a quartz outer tube and metal iron inner tubes, a golden silk cake is arranged between every two adjacent metal iron inner tubes, and a golden silk ball column is arranged in each metal iron inner tube; the metal iron inner tube, the golden cake and the golden ball column form an enrichment area. Introducing the treated mercury-containing flue gas into an enrichment region to enable mercury in the flue gas to form a gold amalgam alloy; then the enrichment area generates eddy current by electromagnetic induction heating, so that mercury is thermally separated out; and then loading the mercury vapor separated out by pyrolysis into a mercury concentration detection module by using argon gas for measurement. The method has the advantages of efficient enrichment and rapid thermal desorption, and simultaneously considers the occurrence state of mercury in flue gas in the mercury enrichment module, and solves the problems of low enrichment efficiency, low thermal desorption speed, poor consistency and the like in the application of the existing mercury enrichment module.
Description
Technical Field
The invention relates to a device and a method for measuring mercury content in flue gas, in particular to a device and a method for realizing real-time and rapid detection of flue gas mercury by utilizing gold amalgam in a rapid thermal desorption mercury enrichment module heated by electromagnetic induction.
Background
Mercury and its compounds are toxic and harmful substances, and the micro-dose of mercury can cause great harm to human health and natural environments such as ecological water, soil, atmosphere and the like, and is difficult to completely eliminate, thus having attracted global wide attention. Mercury entering the atmosphere evolves into global pollutants under the action of atmospheric motion, and the environmental pollution of mercury is mostly generated by the release of mercury caused by human development and use of mercury. In addition to natural causes such as volcanic eruption, rock weathering and forest fire, artificial activities such as fossil fuel combustion, metal smelting, cement production and chlor-alkali industry have become important sources of mercury pollution in the atmosphere.
As China uses the most coal in the world every year, the total mercury emission accounts for more than 40% of the world, and in the coal-fired power plants with the most mercury emission, the mercury emitted into the atmosphere by flue gas is mainly elemental mercury Hg with the valence state of 00The elemental mercury is extremely insoluble in water, can stay in the atmosphere for years and spread to an environmental area far away from a release source, so that the elemental mercury Hg with the valence state of 0 in a coal-fired power plant is used0The continuous measuring method of the content is extremely important to research.
The existing method for measuring the mercury content of the flue gas mainly comprises a Cold Vapor Atomic Absorption Spectrum (CVAAS), an Atomic Emission Spectrum (AES), a cold atomic fluorescence spectrum (CVAFS) and the like, has the advantages of high detection sensitivity, low detection lower limit, no matrix interference, rapidness and the like compared with other measuring methods of the CVASF, and is suitable for measuring the trace and ultra-trace mercury in the flue gas. The ground state atoms of the mercury elements generate resonance absorption to the characteristic narrow-frequency radiation of the mercury atoms emitted by the light source, and the absorbance of the resonance absorption is in direct proportion to the concentration of the ground state atoms of the mercury elements to be detected in the vapor phase within a certain concentration range. The mercury atom vapor selectively absorbs 253.7nm ultraviolet light, the absorbance and the mercury concentration are in a linear relation in a lower concentration range, and the mercury-containing concentration of the gas is calculated according to the absorption of the mercury-containing gas to a spectral line.
With the improvement of the lower limit requirement of mercury detection, when trace and ultra-trace mercury detection is carried out, the original instruments and analysis technology cannot meet the detection requirement, in order to obtain an ideal detection result, the pretreated flue gas mercury is selected to be enriched, mercury is an alloy-amalgam which is extremely easy to form with most metals such as gold, silver, sodium, zinc and the like (except iron), and due to the performance characteristics of gold, the mercury has good stability in the atmosphere, is not easy to oxidize, is very soft and is easy to process. At normal temperature, mercury and gold form alloy-gold amalgam, most of the traditional enrichment modules are formed by filling gold-plated quartz sand, gold-plated glass balls, gold sand and the like into a quartz tube shell, heating a gold-plated material to thermally decompose mercury, and carrying the mercury into a cold atom fluorescent mercury analyzer by carrier gas to finish detection. However, the gold plating degree is different, the gold sand has different shapes, which results in large enrichment difference and inconsistent sensitivity, and the traditional heating mode of the mercury enrichment module winds the heating wire outside the mercury enrichment module and transmits the temperature to the inside of the mercury enrichment module from outside to inside, thereby resulting in long heating time, low efficiency and failure in well realizing on-line measurement of the mercury content in the flue gas.
Disclosure of Invention
The invention aims to provide a device and a method for measuring mercury content in flue gas, aiming at the problems of low enrichment efficiency, poor consistency, low heat release speed, poor measurement precision and the like in the prior art.
The technical scheme of the invention is as follows:
a device for measuring mercury content in flue gas is characterized in that: the device comprises a flue gas sampling pretreatment module, an Ar gas storage bottle, a mercury enrichment module, an electromagnetic induction heating module and a mercury content detection module; the mercury enrichment module comprises a quartz outer tube and a plurality of metal iron inner tubes arranged in the quartz outer tube, a gold cake is arranged between every two adjacent metal iron inner tubes, a gold wire ball column is arranged in each metal iron inner tube, and the metal iron inner tubes, the gold cakes and the gold wire ball columns form an enrichment area; the gas outlet of the flue gas sampling pretreatment module and the gas outlet of the Ar gas storage cylinder are respectively connected with two inlets of a three-way valve through a first electromagnetic valve and a second electromagnetic valve; the outlet of the three-way valve is connected with the inlet of the mercury enrichment module through a condenser, and the enrichment area of the mercury enrichment module is arranged in an electromagnetic induction coil of the electromagnetic induction heating module; and a gas outlet of the mercury enrichment module is connected with the mercury content detection module.
In the above technical solution, preferably, the diameter of the gold wire of the gold cake and the gold wire column is 0.03mm to 0.1 mm; the purity of the gold wire is higher than 99.99%. The diameter of an electromagnetic induction coil in the electromagnetic induction heating module is 18-25 mm, and the number of turns is 7-12. The number of the metal iron inner tubes is at least 5.
The invention provides a method for measuring mercury content in flue gas, which is characterized by comprising the following steps:
1) opening a first electromagnetic valve at one side of the flue gas sampling pretreatment module, closing a second electromagnetic valve at one side of the Ar gas storage bottle, and filtering dust and particulate matters in the flue gas by using the flue gas sampling pretreatment module to obtain mercury-containing flue gas;
2) introducing the mercury-containing flue gas into a condenser through a three-way valve, cooling the mercury-containing flue gas to 0-5 ℃, introducing the cooled mercury-containing flue gas into a mercury enrichment module, and controlling the flow rate of the flue gas to be 250 ml/min-5L/min;
3) in the enrichment module, the mercury-containing flue gas is contacted with the golden cake and the golden wire ball column in the enrichment area at normal temperature to form gold amalgam alloy, and the time for introducing the mercury-containing flue gas is 30-300 s;
4) closing the first electromagnetic valve, opening the electromagnetic induction heating module to enable the metallic iron inner tube in the enrichment zone to generate a vortex, controlling the temperature of the enrichment zone at 700-1100 ℃, and pyrolyzing mercury to separate out mercury vapor;
5) and opening the second electromagnetic valve, and loading the mercury vapor subjected to thermal decomposition into the mercury content detection module by using argon as carrier gas, so as to detect the content of mercury in the flue gas. Preferably, the flow rate of argon is between 250ml/min and 2.5L/min.
Compared with the prior art, the invention has the following advantages and prominent technical effects:
① the enrichment area of the invention is composed of a plurality of gold cake enrichment units and gold ball column enrichment units with specific forms, the diameter of the gold wire is controlled at 0.03 mm-0.1 mm by utilizing the characteristic of strong gold extensibility, the density and the surface area of the gold cake enrichment units and the gold ball column enrichment units are improved, the surface area and the density of the gold wire are greatly improved by utilizing the way of arranging a gold cake and a gold ball column repeatedly step by step, the mercury in the flue gas is fully and efficiently contacted and enriched with the gold cake and the gold ball column, the enrichment efficiency can reach more than 95%, the problems of large enrichment difference, inconsistent sensitivity and the like caused by filling enrichment materials such as gold-plated quartz sand, gold-plated glass ball, gold sand and the like in the traditional enrichment module are solved, the measurement precision is poor, ② uses electromagnetic induction heating, the electromagnetic induction coil makes the metal iron inner tube generate eddy current, the eddy current changes the electric energy into heat energy, the surface of the metal iron inner tube is rapidly heated and is mainly distributed on the surface, the skin depth exceeds 1mm, the metal inner tube is heated by the electromagnetic induction heating effect, the external heat-containing iron heat transfer effect is ensured, the metal inner tube is heated by the mode, the self-heating effect, the external heat-heating effect is increased, the metal-free heat-induced thermal effect detection module, the metal-induced thermal effect is realized by the external heat-induced thermal effect, the external heat-induced thermal effect is.
Drawings
FIG. 1 is a schematic diagram of a mercury detection device according to the present invention.
Fig. 2 is a schematic structural diagram of a mercury high efficiency enrichment unit of the present invention.
Fig. 3 is a graph of concentration signals for the same concentration of mercury content according to the present invention.
Fig. 4 is a linear plot of mercury content at different concentrations according to the present invention.
In the figure: 1-quartz outer tube; 2-supporting; 3-an enrichment zone; 4-metallic iron inner tube; 5-golden silk cake; 6-gold wire ball column; 7-an electromagnetic induction coil; 8-a flue gas sampling pretreatment module; 9-an electromagnetic induction heating module; 10-mercury content detection module; 11-Ar gas cylinder; 12-a mercury enrichment module; 13-three-way valve; 14-a condenser; 15A-a first solenoid valve; 15B-second solenoid valve.
Detailed Description
The present invention will now be described in more detail with reference to the accompanying drawings so that aspects of the invention and advantages thereof can be better understood.
Referring to fig. 1 and fig. 2, the device for measuring mercury content in flue gas provided by the invention comprises a flue gas sampling pretreatment module 8, an Ar gas storage cylinder 11, a mercury enrichment module 12, an electromagnetic induction heating module 9 and a mercury content detection module 10; the mercury enrichment module comprises a quartz outer tube 1 and a plurality of metal iron inner tubes 4 arranged in the quartz outer tube, a golden silk cake 5 is arranged between every two adjacent metal iron inner tubes, and a golden silk ball column 6 is arranged in each metal iron inner tube; the metal iron inner tube, the golden cake and the golden ball column form an enrichment area 3; the gas outlets of the flue gas sampling pretreatment module 8 and the Ar gas storage bottle 11 are respectively connected with two inlets of a three-way valve 13 through a first electromagnetic valve 15A and a second electromagnetic valve 15B, the outlet of the three-way valve is connected with the inlet of a mercury enrichment module 12 through a condenser 14, and the enrichment region 3 of the mercury enrichment module 12 is arranged in an electromagnetic induction coil 7 of an electromagnetic induction heating module; the gas outlet of the mercury enrichment module is connected with the mercury content detection module 10.
The mercury enrichment module comprises a quartz outer tube, a pair of bearings 2 are arranged inside a tube body of the quartz outer tube, an enrichment area is formed between the bearings, the enrichment area comprises metal iron inner tubes which are sequentially connected, gold cakes are tightly attached and added between two adjacent metal iron inner tubes, a gold wire ball column 6 is arranged in each metal iron inner tube, the diameter of a gold wire used in the enrichment area is 0.03-0.1 mm, and the gold wire used in the enrichment area is made into a cake shape and a column shape so as to increase the density and the surface area during smoke enrichment; the diameter of the gold wire cake and the gold wire ball column is 0.03 mm-0.1 mm; the purity of the gold wire should be higher than 99.99%.
One enrichment area is at least composed of five adjacent metal iron inner pipes, a golden silk cake is closely attached between the adjacent metal iron inner pipes 4, and a golden silk ball column is added in each metal iron inner pipe. The mercury-containing flue gas is firstly enriched after passing through the first golden silk cake in the enrichment area, then is enriched through the first golden silk column, and then passes through the golden silk cake and the next golden silk column, so that the enrichment efficiency is improved step by step, and the efficiency is improved to more than 95%.
The enrichment area in the mercury enrichment module is integrally placed in the center of an electromagnetic induction coil 7 of the electromagnetic induction heating module, the electromagnetic induction coil completely covers the whole enrichment area, the electromagnetic induction coil enables the metal iron inner pipe to generate eddy current, the eddy current enables electric energy to be converted into heat energy, and the surface of the metal iron inner pipe is rapidly heated. The eddy current is mainly distributed on the surface, the heating depth exceeds 1mm, and almost no current passes through the inner part of the metal iron inner tube, which is called as skin effect. The electromagnetic induction heating is to utilize the skin effect to quickly heat the surface of the metal iron inner tube by depending on the current heat effect, thereby improving the detection rate and ensuring the synchronism and accuracy of the measurement result to the maximum extent. The diameter of an induction coil in the electromagnetic induction heating module is generally 18-25 mm, and the number of turns is 7-12; the material is red copper.
The invention provides a method for measuring mercury content in flue gas, which comprises the steps of introducing the flue gas obtained after a flue gas sampling pretreatment module into a mercury enrichment module containing an enrichment area, and enabling mercury in the flue gas to be in contact with the enrichment area and be enriched to form a gold amalgam alloy; and then, generating eddy current in the enrichment region by an electromagnetic induction heating method, rapidly heating the enrichment region, thermally analyzing mercury in the enrichment region, loading analyzed mercury vapor into a mercury concentration detection module by argon carrier gas, and rapidly detecting the content of mercury in the flue gas.
The specific process steps are as follows:
1) opening a first electromagnetic valve 15A at one side of the flue gas sampling pretreatment module, closing a second electromagnetic valve 15B at one side of the Ar gas storage bottle, and filtering dust and particulate matters in the flue gas by using the flue gas sampling pretreatment module to obtain mercury-containing flue gas;
2) introducing the mercury-containing flue gas into a condenser 14 through a three-way valve, cooling the mercury-containing flue gas to 0-5 ℃, introducing the cooled mercury-containing flue gas into a mercury enrichment module 12, and controlling the flow rate of the flue gas to be 250 ml/min-5L/min;
3) in the enrichment module, the mercury-containing flue gas contacts the golden cake 5 and the golden silk ball column 6 in the enrichment area 3 at normal temperature to form gold amalgam alloy, and the time for introducing the mercury-containing flue gas is 30-300 s;
4) closing the first electromagnetic valve 15A, opening the electromagnetic induction heating module to enable the metallic iron inner tube 4 in the enrichment area 3 to generate a vortex, controlling the temperature of the enrichment area at 700-1100 ℃, and pyrolyzing mercury to separate out mercury vapor;
5) opening a second electromagnetic valve 15B, and loading mercury vapor obtained by thermal decomposition into a mercury content detection module by using argon as carrier gas, so as to detect the content of mercury in the flue gas; the flow rate of the argon is 250 ml/min-2.5L/min.
Example 1:
in combination with the integrated device as described in FIG. 1, mercury was added at a concentration of 20ng/m3The mercury-containing flue gas passes through a flue gas sampling pretreatment module at the flow rate of 1L/min, dust, particulate matters and the like in the flue gas are filtered, the mercury gas in the mercury-containing flue gas is cooled by a condenser, then introducing into a mercury enrichment module containing 4 gold wire cakes and 3 gold wire ball columns as an enrichment region for enrichment, introducing mercury-containing flue gas for 60s, stopping enrichment, starting an electromagnetic induction heating module, heating the enrichment region by using a 9-turn electromagnetic induction coil for 70s at 700-900 ℃, stopping electromagnetic induction heating, introducing 300ml/min argon carrier gas, loading the mercury separated out by pyrolysis into a mercury content detection module by using argon, the results of the experiments shown in fig. 3 were obtained, and a consistent concentration result was obtained with a relative error of less than 3% with respect to the concentration signal for 13 experiments. :
example 2:
in combination with the integrated device as described in FIG. 1, mercury was added at a concentration of 20ng/m3The mercury-containing flue gas passes through a flue gas sampling pretreatment module at different flow rates, the flow rate range of the mercury-containing flue gas is 250 mL/min-2L/min, the flow rate interval of each experiment is increased by 250mL/min, dust, particulate matters and the like in the flue gas are filtered, the mercury gas in the mercury-containing flue gas is cooled by a condenser, then the mercury-containing flue gas is introduced into a mercury enrichment module which takes 4 golden silk cakes and 3 golden silk spherocolumns as an enrichment area for enrichment, the time of introducing the mercury-containing flue gas is 60s, after the enrichment is stopped, an electromagnetic induction heating module is started, a 9-turn electromagnetic induction coil is utilized to heat the enrichment area, the heating time is 70s, the temperature is controlled to be 700-900 ℃, after the electromagnetic induction heating is stopped, 300mL/min argon carrier gas is introduced, and the mercury gas is thermally analyzed and analyzed outThe obtained mercury is loaded into the mercury content detection module, and the experimental result shown in fig. 4 is obtained, the intensity of the relative concentration signal is increased along with the linear increase of the flow, and the accuracy of the linear fitting is higher than 98.5%.
Claims (6)
1. A device for measuring mercury content in flue gas is characterized in that: the device comprises a flue gas sampling pretreatment module (8), an Ar gas storage bottle (11), a mercury enrichment module (12), an electromagnetic induction heating module (9) and a mercury content detection module (10); the mercury enrichment module comprises a quartz outer tube (1) and a plurality of metal iron inner tubes (4) arranged in the quartz outer tube, a golden silk cake (5) is arranged between every two adjacent metal iron inner tubes (4), a golden silk ball column (6) is arranged in each metal iron inner tube, and the metal iron inner tubes (4), the golden silk cakes (5) and the golden silk ball columns (6) form an enrichment area (3); the gas outlet of the flue gas sampling pretreatment module and the gas outlet of the Ar gas storage bottle are respectively connected with two inlets of a three-way valve (13) through a first electromagnetic valve (15A) and a second electromagnetic valve (15B); an outlet of the three-way valve is connected with an inlet of a mercury enrichment module (12) through a condenser (14), and an enrichment area of the mercury enrichment module (12) is arranged in an electromagnetic induction coil (7) of the electromagnetic induction heating module; the gas outlet of the mercury enrichment module is connected with a mercury content detection module (10).
2. The apparatus for measuring mercury content in a flue gas according to claim 1, wherein: the diameter of the gold wire cake and the gold wire ball column is 0.03 mm-0.1 mm; the purity of the gold wire is higher than 99.99%.
3. The apparatus for measuring mercury content in a flue gas according to claim 1, wherein: the diameter of an electromagnetic induction coil (7) in the electromagnetic induction heating module is 18-25 mm, and the number of turns is 7-12.
4. A device for measuring the mercury content in flue gases according to any one of claims 1 to 3, characterized in that: the number of the metal iron inner tubes is at least 5.
5. A method for measuring the mercury content in flue gases using the device according to any of claims 1-4, characterized in that the method comprises the following steps:
1) opening a first electromagnetic valve (15A) on one side of the flue gas sampling pretreatment module, closing a second electromagnetic valve (15B) on one side of the Ar gas storage bottle, and filtering dust and particulate matters in the flue gas by using the flue gas sampling pretreatment module to obtain mercury-containing flue gas;
2) introducing the mercury-containing flue gas into a condenser (14) through a three-way valve, cooling the mercury-containing flue gas to 0-5 ℃, introducing the cooled mercury-containing flue gas into a mercury enrichment module (12), and controlling the flow rate of the flue gas to be 250 ml/min-5L/min;
3) in the enrichment module, the mercury-containing flue gas contacts with the golden cake (5) and the golden ball column (6) in the enrichment area (3) at normal temperature to form gold amalgam alloy, and the time for introducing the mercury-containing flue gas is 30-300 s;
4) closing the first electromagnetic valve (15A), opening the electromagnetic induction heating module to enable the metal iron inner tube (4) in the enrichment area (3) to generate eddy current, controlling the temperature of the enrichment area at 700-1100 ℃, and pyrolyzing mercury to separate out mercury vapor;
5) and opening a second electromagnetic valve (15B), and loading mercury vapor obtained by thermal decomposition into a mercury content detection module by using argon as carrier gas, thereby detecting the content of mercury in the flue gas.
6. The method for measuring the mercury content in the flue gas as claimed in claim 5, wherein the flow rate of the argon in the step 5) is 250ml/min to 2.5L/min.
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| CN114544744A (en) * | 2022-02-15 | 2022-05-27 | 西安西热锅炉环保工程有限公司 | Rapid mercury measurement method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114544744A (en) * | 2022-02-15 | 2022-05-27 | 西安西热锅炉环保工程有限公司 | Rapid mercury measurement method |
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