CN110514485A - A kind of stationary source mercury in flue gas sampling apparatus - Google Patents
A kind of stationary source mercury in flue gas sampling apparatus Download PDFInfo
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- CN110514485A CN110514485A CN201910943697.9A CN201910943697A CN110514485A CN 110514485 A CN110514485 A CN 110514485A CN 201910943697 A CN201910943697 A CN 201910943697A CN 110514485 A CN110514485 A CN 110514485A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
- G01N1/2258—Sampling from a flowing stream of gas in a stack or chimney
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
- G01N2001/2217—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption using a liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2247—Sampling from a flowing stream of gas
- G01N1/2258—Sampling from a flowing stream of gas in a stack or chimney
- G01N2001/2261—Sampling from a flowing stream of gas in a stack or chimney preventing condensation (heating lines)
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N2001/2282—Devices for withdrawing samples in the gaseous state with cooling means
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Abstract
The present invention relates to a kind of stationary source mercury in flue gas sampling apparatuses, including constant temperature sampling gun, temperature filtration case, ice bath absorption bottle case, dehumidification device, sampling controller and sampling aspiration pump;The outlet of the constant temperature sampling gun connects with the entrance of the temperature filtration case, the outlet of the temperature filtration case connects with the entrance of the ice bath absorption bottle case, the outlet of the ice bath absorption bottle case is connected with the entrance of the dehumidification device, the outlet of the dehumidification device is connected with the entrance of the sampling controller, described to be also connected with the sampling aspiration pump using controller.Three kinds of different diatom soil matrix complex solid adsorbents that the present invention is placed in ice bath trap the mercury of different shape in stationary source flue gas respectively, diatom soil matrix complex solid adsorbent has biggish specific surface area and silicone hydroxyl abundant, there is very strong chelating effect to mercury, improves the collecting efficiency of mercury in flue gas.And collection in worksite is easy to operate, and the adsorbent for having adopted sample can save 30 days at room temperature.
Description
Technical field
The present invention relates to environmental monitoring technology field, especially a kind of stationary source mercury in flue gas sampling apparatus.
Background technique
Mercury is one of strongest heavy metal contaminants of toxicity, and the characteristic with biological accumulation and biomagnification has simultaneously
High volatile and property easy to migrate are easy the accumulation in biology and cause lesion.China and United Nations Environment Programme, world health group
It knits, mercury is classified as priority pollutants by the mechanisms such as European Union and Environmental Protection Agency.Existing Mercury In The Air emission inventory table
Bright, artificial source occupies very big specific gravity, coal fired power generation, burning city domestic garbage and medical waste in the mercury emissions source in the whole world
Burning belongs to very important artificial mercury emissions source.
Corresponding laws and regulations are formulated in order to monitor and prevent and treat the most of developed countries of mercury pollution, 2011, the U.S. mentioned
Chu Liao thermal power plant mercury and other pollutant emission standard drafts add for 2006 wherein being strict with mercury control rate reaches 91%
It puts on airs and has issued coal-burning power plant's mercury emissions standard, the control rate of discharge requires to reach 60%.European Union proposes " heavy metal within 2011
Protocol revision case ", it is specified that coal-burning power plant's atmosphere mercury emissions are limited to 0.03 mg/m3.2013, " Minamata pact " was outputed
The inventory for closing limitation mercury emissions, is the limitation to mercurous class product first.In July, 2011, " thermal power plant is big for Environmental Protection Department approval
Gas pollutant emission standard " in for the first time mercury and mercuric compounds are increased in thermal power plant's atmosphere pollution item controlled, it is desirable that
Coal-burning boiler mercury emissions limit value is 0.03mg/m3, and provide the discharge standard of execution mercury and mercuric compounds from January 1st, 2015.
In 2014, China has issued Industrial Boiler atmosphere pollutants emission standards (GB13271-2014), it is specified that all boilers execute
0.05mg/m3The emission limit of Mercury In The Air.
Mercury in flue gas exists in the form of 3 kinds, i.e. element mercury Hg0, oxidation state mercury Hg2+With particle mercury Hgp.Different shape
Mercury has different property in the environment.Hg0、Hg2+It is present in flue gas for gaseous form, HgpThe overwhelming majority can by dedusting,
The trapping removal of the flue gas purification devices such as wet desulphurization.Hg2+It is water-soluble, it is also easy to be adsorbed by particulate matter, is easy to trap and control
System is released in atmosphere and mainly causes Local anesthesia;Hg2 +Hg can be reduced to by being heated to 800 DEG C or so0.Elementary gas
Mercury (Hg0) not soluble in water and highly volatile, it is difficult to it controls, long transmission distance, effect on environment is big, but Hg0It can be by catalysis oxidation
For Hg2+.If being discharged into atmosphere, Hg2+And HgpAtmospheric residence time only has several days, Hg0It can then stop 1 year or more.Gas mercury
Accurate Determining is targeted control Mercury In The Air and the premise for formulating Mercury In The Air discharge standard.
Environmental Protection Department is with reference to U.S.'s test and materialogy meeting (American Society for Testing and
Materials, ASTM) Ontario method (Ontario Hydro Method, OH method) and Environmental Protection Agency (United
States Environmental Protection Agency, US EPA) EPA Method 29, formulated HJ 543-
2009 " the measurement cold atomic absorbent spectrophotometries (provisional) of stationary source exhaust gas mercury " and HJ 917-2017 are " fixed dirty
Measurement activated carbon adsorption/thermal cracking atomic absorption spectrophotometry of dye source exhaust gas gaseous mercury ".HJ 543-2009 is " fixed dirty
The measurement cold atomic absorbent spectrophotometry (provisional) of dye source exhaust gas mercury " connect 2 each dress 10mL on sampling apparatus
0.1mol/L KMnO4-10% H2SO4The bubble absorption tube or impact absorbing bottle of (volume fraction) acquire mercury in flue gas.Scene is surveyed
HJ 543-2009 is in terms of measurement range, measurement accuracy and accuracy of measurement for examination discovery, there is also some problems: 1. this method
Failed call carries out heat tracing to sampling pipe, therefore as flue-gas temperature constantly reduces in sampling pipeline, will lead to mercury in sampling pipe
Condensation, absorption on line, so that measurement result is relatively low;2. the non-ice bath of this method absorbing liquid, absorbing liquid temperature after sampling for a long time
It increases, is unfavorable for mercury absorption;3. this method, using the conventional gaseous pollutant method of sampling, the common sampling gun inner wall used is
Metal material, it is easy to Adsorption of Mercury, disturbed test result;4. the absorbing liquid type of this method only has one kind, therefore can not measure
The form of mercury;5. although being only required when analyzing this method uses two absorption tubes and merging the absorbing liquid in 2 absorption tubes
Post analysis does not formulate method of quality control;6. stationary source includes coal-burning power plant, Industrial Boiler, coloured smelting factory, cement
All kinds of pollution sources such as factory, steel plant, the smoke properties of these discharge of pollutant sources is there is very big difference, in HJ 543-2009
The method of sampling be not suitable for it is above-mentioned institute it is active.For example, SO in the flue gas that nonferrous metallurgical process generates2Concentration is significantly larger than
Coal-fired flue-gas, the SO of flue gas middle and high concentration2Absorption bottle can be entered and form SO3 2-Ion, gaseous elementary mercury meeting in flue gas and absorbs
SO in liquid3 2-Ionic reaction, interference measurement results.Only there are two KMnO is housed by HJ 543-20094/H2SO4The absorption of solution
Bottle, the configuration are only applicable to the lower flue gas of acidic gas concentration, sour gas energy and KMnO in flue gas4Reaction is reduced and is inhaled
Receive trapping of the liquid to mercury.Since HJ 543-2009 has more problem during the test, do not have in China also wide
General application.HJ 917-2017 there are the problem of: the SO in 1. flue gases2、NOxCapture of the meeting inhibitory activity charcoal to mercury, therefore only fit
For installing denitration-dedusting-sulfur removal technology coal-burning power plant additional;2. the low flue position (dedusting of particle concentration can only be acquired
Afterwards), because high dirt can block fine grain active carbon, so as to cause can not normal sample;3. expensive active carbon is adopted
Sample adsorption tube cannot be reused, it usually needs live preliminary experiment, testing cost are high.
Summary of the invention
To solve the above problems, the object of the present invention is to provide a kind of stationary source mercury in flue gas sampling apparatus,
It is realized in the embodiment of the present invention using following scheme: a kind of stationary source mercury in flue gas sampling apparatus, including perseverance is provided
Warm sampling gun, temperature filtration case, ice bath absorption bottle case, dehumidification device, sampling controller and sampling aspiration pump;The constant temperature sampling
The sampling head of rifle protrudes into flue, and the outlet of the constant temperature sampling gun connects with the entrance of the temperature filtration case, the constant temperature
The outlet of Rose Box connects with the entrance of the ice bath absorption bottle case, the outlet of the ice bath absorption bottle case and the dehumidification device
Entrance be connected, the outlet of the dehumidification device is connected with the entrance of the sampling controller, it is described use controller also connect
Connect the sampling aspiration pump;14 absorption bottles are housed, 7 absorption bottles are cascaded to be adopted for one group in the ice bath absorption bottle case
Sample, 14 absorption bottles are for once carrying out two groups of Parallel Samplings;Series connection numbers difference for one group of 7 absorption bottles from left to right
Are as follows: the first absorption bottle, the second absorption bottle, third absorption bottle, the 4th absorption bottle, the 5th absorption bottle, the 6th absorption bottle, the 7th absorb
Bottle, first absorption bottle, second absorption bottle, the third absorption bottle are provided with for trapping oxidation state mercury in flue gas
Diatomite base composite absorbent, the 4th absorption bottle are provided with the compound suction of diatom soil matrix for absorbing acid gas in flue gas
Attached dose;5th absorption bottle, the 6th absorption bottle, the 7th absorption bottle are provided with for trapping elementary gas in flue gas
The diatomite base composite absorbent of mercury.
In one embodiment of the invention, the preparation method of the diatomite base composite absorbent is prepared using following steps:
Step S1: by 30-45 parts of diatomite and 5-10 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S2: when preparing the diatomite base composite absorbent for trapping oxidation state mercury, the potassium chloride that 1mol/L is added is molten
6-17 parts of liquid or 10-20 parts of 8-15 parts of 1mol/L calcium chloride solution or 1mol/L potassium hydroxide solution or 1mol/L
8-22 parts of calcium hydroxide solution;
When preparing the diatomite base composite absorbent for absorbing sour gas, it is slow that 1mol/L citric acid-sodium citrate is added
10-20 parts of fliud flushing or 1.13g/ml hydrogen peroxide and 6-17 parts of 10% nitric acid mixed solution or 1mol/L hydrosulphuric acid solution
8-20 parts;
When preparation is used for the diatomite base composite absorbent of trapping gaseous element mercury, 5% liquor potassic permanganate and 18.4 is added
6-17 parts of mol/L sulfuric acid mixed solution or 5% potassium bichromate and 8-15 parts of 18.4 mol/L sulfuric acid mixed solutions or 5% potassium chlorate
Solution and 10-20 parts of 18.4 mol/L sulfuric acid mixed solutions or 5% ferrate solution and 18.4 mol/L sulfuric acid mixed solutions
8-22 parts;It carries out being heated to 120 DEG C after solution is added, and sealing stirring 1h at such a temperature;
Step S3: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, it is clear to remove upper layer
Liquid, room temperature are dried;
Step S4: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
In one embodiment of the invention, temperature filtration case temperature in sampling process is maintained at 120 DEG C, prevents mercury cold
It is solidifying;Fiber is housed in the filter cylinder of filter in the temperature filtration case, is used for arrested particles state mercury.
Beneficial effects of the present invention: three kinds of different diatom soil matrix complex solid adsorbents that the present invention is placed in ice bath
The mercury of different shape in stationary source flue gas is trapped respectively, and diatom soil matrix complex solid adsorbent has biggish specific surface area
With silicone hydroxyl abundant, there is very strong chelating to act on mercury, in addition the synergistic effect of each raw material substantially increases adopting for mercury in flue gas
Collect efficiency.In addition, also having collection in worksite easy to operate, the adsorbent for having adopted sample can at least save 30 days excellent at room temperature
Point.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of stationary source mercury in flue gas sampling apparatus.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing.
Referring to Fig. 1, the present invention provides a kind of stationary source mercury in flue gas sampling apparatus, including constant temperature sampling gun 1, perseverance
Warm Rose Box 2, ice bath absorption bottle case 3, dehumidification device 4, sampling controller 5 and sampling aspiration pump 6;The constant temperature sampling gun 1
Sampling head protrudes into flue, and the outlet of the constant temperature sampling gun 1 connects with the entrance of the temperature filtration case 2, the constant temperature mistake
The outlet of filter box 2 connects with the entrance of the ice bath absorption bottle case 3, and the outlet and the dehumidifying of the ice bath absorption bottle case 3 fill
It sets 4 entrance to be connected, the outlet of the dehumidification device 4 is connected with the entrance of the sampling controller 5, described using controller
It is also connected with the sampling aspiration pump 6;In the ice bath absorption bottle case 3 be equipped with 14 absorption bottles, 7 absorption bottles be cascaded for
One group of sampling, 14 absorption bottles are for once carrying out two groups of Parallel Samplings;Series connection is numbered from left to right for one group of 7 absorption bottles
It is respectively as follows: the first absorption bottle 31, the second absorption bottle 32, third absorption bottle 33, the 4th absorption bottle 34, the 5th absorption bottle the 35, the 6th
Absorption bottle 36, the 7th absorption bottle 37, first absorption bottle 31, second absorption bottle 32, the third absorption bottle 33 are built-in
There is the diatomite base composite absorbent for trapping oxidation state mercury in flue gas, the 4th absorption bottle 34 is provided with for absorbing cigarette
The diatomite base composite absorbent of sour gas in gas;5th absorption bottle 35, the 6th absorption bottle 36, the described 7th inhale
Bottle 37 is received to be provided with for trapping the total diatomite base composite absorbent of elementary gas in flue gas.
In one embodiment of the invention, the temperature in sampling process of temperature filtration case 2 is maintained at 120 DEG C, prevents mercury cold
It is solidifying;Fiber is housed in the filter cylinder of filter in the temperature filtration case 2, is used for arrested particles state mercury.
In one embodiment of the invention, following material is can be used in the fiber in the temperature filtration case 2 in the filter cylinder of filter 21
Matter: quartz fibre, boron fibre, carbon fiber (graphite fibre), silicon carbide fibre, silicon oxide fibre, silicon nitride fiber, zirconium oxide
The inorfils such as fiber.
In one embodiment of the invention, following material manufacture can be used in the constant temperature sampling gun 1: quartz glass, polyphenyl are simultaneously
Imidazoles (PBI), liquid crystal polymer (LCP), polyetherimide (PEI), high temperature resistant nylon (PPA, PA6T), polyamidoimide
(PAI) the high temperature resistant inorganics nonmetallic materials such as.
In one embodiment of the invention, the absorption bottle that following material can be used to know for absorption bottle: glass, quartz, polytetrafluoroethyl-ne
Alkene (PTFE), polyvinyl chloride (PVC), polystyrene (PS), acrylonitrile-butadiene-styrene copolymerisation object (ABS).
In one embodiment of the invention, the preparation method of the diatomite base composite absorbent is prepared using following steps:
Step S1: by 30-45 parts of diatomite and 5-10 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S2: when preparing the diatomite base composite absorbent for trapping oxidation state mercury, the potassium chloride that 1mol/L is added is molten
6-17 parts of liquid or 10-20 parts of 8-15 parts of 1mol/L calcium chloride solution or 1mol/L potassium hydroxide solution or 1mol/L
8-22 parts of calcium hydroxide solution;
When preparing the diatomite base composite absorbent for absorbing sour gas, it is slow that 1mol/L citric acid-sodium citrate is added
10-20 parts of fliud flushing or 1.13g/ml hydrogen peroxide and 6-17 parts of 10% nitric acid mixed solution or 1mol/L hydrosulphuric acid solution
8-20 parts;
When preparation is used for the diatomite base composite absorbent of trapping gaseous element mercury, 5% liquor potassic permanganate and 18.4 is added
6-17 parts of mol/L sulfuric acid mixed solution or 5% potassium bichromate and 8-15 parts of 18.4 mol/L sulfuric acid mixed solutions or 5% potassium chlorate
Solution and 10-20 parts of 18.4 mol/L sulfuric acid mixed solutions or 5% ferrate solution and 18.4 mol/L sulfuric acid mixed solutions
8-22 parts;It carries out being heated to 120 DEG C after solution is added, and sealing stirring 1h at such a temperature;
Step S3: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, it is clear to remove upper layer
Liquid, room temperature are dried;
Step S4: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
Embodiment one
Trap the preparation of the diatomite base composite absorbent of oxidation state mercury:
Step S11: by 30 parts of diatomite and 5 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S12: 6 parts of Klorvess Liquid of 1mol/L are added;It carries out being heated to 120 DEG C, and sealing is stirred at such a temperature
Mix 1h;
Step S13: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, removes upper layer
Clear liquid, room temperature are dried;
Step S14: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
Absorb the preparation of the diatomite base composite absorbent of sour gas:
Step S21: by 30-45 parts of diatomite and 5-10 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S22: 10 parts of 1mol/l citric acid-sodium citrate buffer solution are added;It carries out being heated to 120 DEG C, and in the temperature
The lower sealing stirring 1h of degree;
Step S23: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, removes upper layer
Clear liquid, room temperature are dried;
Step S24: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
The preparation method of the diatomite base composite absorbent of trapping gaseous element mercury:
Step S31: by 30 parts of diatomite and 5 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S32: 6 parts of 5% liquor potassic permanganate and 18.4 mol/L sulfuric acid mixed solutions are added;It carries out being heated to 120
DEG C, and sealing stirring 1h at such a temperature;
Step S33: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, removes upper layer
Clear liquid, room temperature are dried;
Step S34: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
Embodiment two
Trap the preparation of the diatomite base composite absorbent of oxidation state mercury:
Step S11: by 30 parts of diatomite and 5 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S12: 12 parts of Klorvess Liquid of 1mol/L are added;It carries out being heated to 120 DEG C, and sealing is stirred at such a temperature
Mix 1h;
Step S13: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, removes upper layer
Clear liquid, room temperature are dried;
Step S14: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
Absorb the preparation method of the diatomite base composite absorbent of sour gas:
Step S21: by 40 parts of diatomite and 8 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S22: 17 parts of 1mol/l citric acid-sodium citrate buffer solution are added;It carries out being heated to 120 DEG C, and in the temperature
The lower sealing stirring 1h of degree;
Step S23: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, removes upper layer
Clear liquid, room temperature are dried;
Step S24: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
The preparation method of the diatomite base composite absorbent of trapping gaseous element mercury:
Step S31: by 40 parts of diatomite and 8 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S32: 12 parts of 5% liquor potassic permanganate and 18.4 mol/l sulfuric acid mixed solutions are added;It carries out being heated to 120
DEG C, and sealing stirring 1h at such a temperature;
Step S33: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, removes upper layer
Clear liquid, room temperature are dried;
Step S34: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
The working principle of the invention:
Flue gas is passed through from constant temperature sampling gun first, and flue gas enters heat tracing fibrous filter membrane filter, and (heat tracing is that mercury is cold in order to prevent
It is solidifying) collect particle mercury;Subsequent flue gas is passed through ice bath absorption bottle case, and flue gas passes sequentially through described first in ice bath absorption bottle case
Absorption bottle, second absorption bottle, the third absorption bottle trap oxidation state mercury in flue gas;Flue gas is passed through the described 4th again and inhales
It receives in bottle, acid gas in flue gas is absorbed;Then flue gas passes sequentially through the 5th absorption bottle, the 6th absorption bottle, institute
The 7th absorption bottle is stated, gaseous elementary mercury in flue gas is absorbed.(it is to be noted that multiple with ice water wetting diatom soil matrix when sampling
Adsorbent is closed, to improve the efficiency of trapping mercury.)
According to mercury content detection knot in three kinds of methods acquisition dust remover for coal boiler (ESP) exiting flue gas introduced in background technique
Fruit: it is 0.78 μ g/Nm that HJ 543-2009 method, which acquires total mercury content,3, it is 1.00 μ that HJ 917-2017, which acquires state total mercury content,
g/Nm3, it is 0.14 μ g/Nm that this method, which acquires particle mercury content,3, oxidation mercury content be 0.18 μ g/Nm3, element mercury content be
1.23 µg/Nm3, total mercury content be 1.55 μ g/Nm3, state total mercury content be 1.41 μ g/Nm3。
The foregoing is merely presently preferred embodiments of the present invention, should not be understood as the limitation to the application, all according to Shen of the present invention
Please the equivalent changes and modifications done of the scope of the patents, be all covered by the present invention.
Claims (3)
1. a kind of stationary source mercury in flue gas sampling apparatus, it is characterised in that: including constant temperature sampling gun, temperature filtration case, ice
Bathe absorption bottle case, dehumidification device, sampling controller and sampling aspiration pump;The sampling head of the constant temperature sampling gun protrudes into flue,
The outlet of the constant temperature sampling gun connects with the entrance of the temperature filtration case, the outlet of the temperature filtration case and the ice bath
The entrance of absorption bottle case connects, and the outlet of the ice bath absorption bottle case is connected with the entrance of the dehumidification device, the dehumidifying dress
The outlet set is connected with the entrance of the sampling controller, described to be also connected with the sampling aspiration pump using controller;It is described
14 absorption bottles are housed, 7 absorption bottles are cascaded as one group of sampling, and 14 absorption bottles are for primary in ice bath absorption bottle case
Carry out two groups of Parallel Samplings;Series connection number from left to right for one group of 7 absorption bottles is respectively as follows: the first absorption bottle, the second absorption
Bottle, third absorption bottle, the 4th absorption bottle, the 5th absorption bottle, the 6th absorption bottle, the 7th absorption bottle, it is first absorption bottle, described
Second absorption bottle, the third absorption bottle are provided with the diatomite base composite absorbent for trapping oxidation state mercury in flue gas, institute
It states the 4th absorption bottle and is provided with diatomite base composite absorbent for absorbing acid gas in flue gas;5th absorption bottle,
6th absorption bottle, the 7th absorption bottle are provided with the diatom soil matrix composite adsorption for trapping gaseous elementary mercury in flue gas
Agent.
2. a kind of stationary source mercury in flue gas sampling apparatus according to claim 1, it is characterised in that: the diatomite
The preparation method of base composite absorbent is prepared using following steps:
Step S1: by 30-45 parts of diatomite and 5-10 parts of trimethyl citrate mixed grinding, 120 meshes are crossed;
Step S2: when preparing the diatomite base composite absorbent for trapping oxidation state mercury, the potassium chloride that 1mol/L is added is molten
6-17 parts of liquid or 10-20 parts of 8-15 parts of 1mol/L calcium chloride solution or 1mol/L potassium hydroxide solution or 1mol/L
8-22 parts of calcium hydroxide solution;
When preparing the diatomite base composite absorbent for absorbing sour gas, it is slow that 1mol/L citric acid-sodium citrate is added
10-20 parts of fliud flushing or 1.13g/ml hydrogen peroxide and 6-17 parts of 10% nitric acid mixed solution or 1mol/L hydrosulphuric acid solution
8-20 parts;
When preparation is used for the diatomite base composite absorbent of trapping gaseous element mercury, 5% liquor potassic permanganate and 18.4 is added
6-17 parts of mol/L sulfuric acid mixed solution or 5% potassium bichromate and 8-15 parts of 18.4 mol/L sulfuric acid mixed solutions or 5% potassium chlorate
Solution and 10-20 parts of 18.4 mol/L sulfuric acid mixed solutions or 5% ferrate solution and 18.4 mol/L sulfuric acid mixed solutions
8-22 parts;It carries out being heated to 120 DEG C after solution is added, and sealing stirring 1h at such a temperature;
Step S3: temperature is down to 70 DEG C and carries out ultrasonic treatment 30min, and ultrasonic power 850w stands after the completion, it is clear to remove upper layer
Liquid, room temperature are dried;
Step S4: obtained solid being placed in 110 DEG C of baking oven and dried, then in 500 DEG C of temperature lower calcination 3h up to diatom
Soil matrix compound adsorbent.
3. a kind of stationary source mercury in flue gas sampling apparatus according to claim 1, it is characterised in that: the constant temperature mistake
Filter box temperature in sampling process is maintained at 120 DEG C, prevents mercury from condensing;It is equipped in the filter cylinder of filter in the temperature filtration case
Fiber is used for arrested particles state mercury.
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