CN103076215B - Bubbling type ultrasonic atomized mercury valence transformation device and method - Google Patents
Bubbling type ultrasonic atomized mercury valence transformation device and method Download PDFInfo
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- CN103076215B CN103076215B CN201210584530.6A CN201210584530A CN103076215B CN 103076215 B CN103076215 B CN 103076215B CN 201210584530 A CN201210584530 A CN 201210584530A CN 103076215 B CN103076215 B CN 103076215B
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Abstract
The invention discloses a bubbling type ultrasonic atomized mercury valence transformation device and a method, and aims to efficiently transform mercury of oxidation state, which is in coal-fired flue gas and can not be measured easily, into mercury of element state, which can be measured easily. The device provided by the invention is characterized in that flue gas extracted in the field is treated by a bubbling type reactor, so that a great amount of micron-sized bubbles are generated; meanwhile, an ultrasonic atomization technology is used to treat stannous chloride hydrochloric acid solution, so that a great amount of micron-sized fog drips are formed; after the bubbles and the fog drips are combined, the contact area of sample gas and stannous chloride hydrochloric acid solution can be improved greatly; and meanwhile, a baffle plate is arranged to prolong the interaction time of sample gas and stannous chloride hydrochloric acid solution. According to the invention, the efficiency of transforming mercury of oxidation state into mercury of element state through a stannous chloride wet chemistry method can be improved to the utmost extent, the operation of continuously transforming mercury of oxidation state into mercury of reduction state on line under the condition of a laboratory and practical flue gas can be realized, and real-time, comprehensive and accurate measurement of mercury state in an on-line mode can be implemented.
Description
Technical field
The invention belongs to the fields of measurement of heavy metal Hg, relating to a kind of is the apparatus and method of the elemental mercury easily measured by the oxidation state mercury Efficient Conversion not easily measured in coal-fired flue-gas.
Background technology
Mercury and mercuric compounds, owing to having cumulative bad and nervous lesion etc. in high volatile volatile, aerial migration, biosome, is just subject to extensive concern as a class poisonous and harmful substance.Along with the raising day by day of world's coal resources consumption, coal fired power plant has become maximum artificial mercury emissions list source, the whole world.The U.S., Canada, China etc. have formulated relevant laws and regulations or industry standard for coal fired power plant mercury emissions, the research of various control coal fired power plant mercury emissions technology, remove agent as added in coal, acticarbon back-end ductwork sprays, utilizes existing desulfuring and denitrifying dedust apparatus etc., also in mushroom development.
No matter be set up relatively accurate mercury emissions inventory, still assess the efficiency of various mercury capture technique, what realize mercury accurately measures important prerequisite and basis beyond doubt comprehensively.Mercury and mercuric compounds involved by coal fired power plant mainly comprises three kinds of forms: elementary gas state mercury, gaseous oxidation state mercury and particle mercury.Particle mercury comprises mercury in end slag and flying dust, generally can carry out lab analysis according to after strict standard method sampling.In flue gas, the measurement of gaseous mercury is then divided into two classes, one is standard method Ontario method (the Ontario-Hydro Method according to the agency recommends such as Environmental Protection Agency and Ministry of Energy, OHM) carry out on-site sampling, analysis, can effectively gather and analyze the mercury and mercuric compounds of different shape in coal-fired flue-gas; Two are based on line analysis technology, utilize the mercury concentration in the principle on-line real-time measuremen flue gas of cold vapor atomic absorption method (CVAAS) or cold vapor atomic fluorescence method (CVAFS).But current mercury concentration on-line analysis detection technique is all the method based on detection elements state mercury, namely can only detect elemental mercury and can not detect oxidation state mercury.Therefore the conversion of oxidation state mercury to elemental mercury must first be carried out for detecting oxidation state mercury.Usual way is before detecting instrument, be equipped with mercury valence transformation device, detects the total mercury content in flue gas after oxidation state mercury is converted into elemental mercury again, and the difference finally by total mercury content and elemental mercury content obtains oxidation state mercury content indirectly.
Coal-fired flue-gas mercury on-line checkingi analytical technology, due to advantageous advantages such as simple, the real-time reflected measurement results of measuring process, becomes the study hotspot in this field, countries in the world.The valence transformation device wherein possessing Efficient Conversion efficiency becomes the core component realizing elementary gas state mercury and the synchronous real time on-line monitoring of gaseous state oxidation state mercury.The valence transformation device of current mercury mainly contains two kinds, and one utilizes stannous chloride solution to carry out wet-chemical conversion, and oxidation state mercury is reduced to elemental mercury; Another kind makes all kinds of oxidation state mercury compound decomposes under the high temperature conditions, and then be converted into element state total mercury.The transformation efficiency of high-temperature heating method depends on the selection of temperature and the purging of inert gas, recently comparatively large for inversion temperature dispute, and the use of extra energy loss, inert gas also improves its complicacy used and cost.Can carry out under stannous chloride wet chemical method normal temperature, its utilize to be limited in transformation efficiency low, how in limited Time and place, to reach the transformation efficiency met the demands, become the key that the method is applied in industrialized unit.
Summary of the invention
Technical matters: the present invention is directed to oxidation state mercury in stannous chloride wet chemical method to the low present situation of the transformation efficiency of elemental mercury, provides a kind of oxidation state mercury that not only can significantly improve to elemental mercury transformation efficiency but also can the bubble type ultrasonic atomization mercury valence transformation device of synchronously detection elements state mercury and oxidation state mercury in real time.Present invention also offers a kind of method utilizing this device to carry out mercury valence state Efficient Conversion.
Technical scheme: bubble type ultrasonic atomization mercury valence transformation device of the present invention, comprise the air inlet air compartment connecting setting from bottom to up successively, air distribution plate, blistering reaction section, atomization conversion zone, cooling water jecket, extension and solution exhausting section and external gas-guide pipeline, air inlet air compartment side is provided with air inlet, embedded ultrasonic atomization sheet on air distribution plate, cooling heat transferring pipe is provided with in blistering reaction section, cooling heat transferring pipe is connected with cooling water jecket by pipeline, cooling water jecket is provided with cooling water inlet and coolant outlet, in extension and solution exhausting section, 4 ~ 6 baffles be staggeredly arranged successively are from bottom to up set, the quartz fibre drainage core of dipping sodium hydroxide solution is provided with in external gas-guide pipeline.
In apparatus of the present invention, air inlet air compartment, each conversion zone main body, cooling water jecket and external gas-guide pipeline all adopt the polytetrafluoroethylmaterial material of not Adsorption of Mercury, cooling heat transferring pipe and and cooling water jecket between connecting line adopt the high-boron-silicon glass material of not Adsorption of Mercury.
Air distribution plate in apparatus of the present invention adopts the quartz material of not Adsorption of Mercury, and densely covered pore diameter range is the aperture of 1 ~ 10 micron.A large amount of micron order apertures that it gathers can allow sample gas enter blistering reaction section smoothly from air inlet air compartment, can ensure again the unlikely seepage of held tin chloride solution simultaneously.
The present invention utilizes above-mentioned bubble type ultrasonic atomization mercury valence transformation device to carry out the method for mercury valence state conversion, comprises the steps:
1) the sample gas being mixed with elemental mercury and oxidation state mercury is passed into air inlet air compartment by air inlet, after air distribution plate, evenly enter blistering reaction section and tin chloride solution reacts;
2) shake by ultrasonic atomization sheet a large amount of stannous chloride hydrochloric acid droplets produced and be full of whole atomization conversion zone, sample gas fully contacts with stannous chloride hydrochloric acid droplet further, and reduction reaction occurs;
3) sample gas enters extension and solution exhausting section by the center pit of cooling water jecket after this two-step reaction, in extension and solution exhausting section, the passage of formation is intercepted along baffle, sample gas and stannous chloride hydrochloric acid droplet continue to interact, and stannous chloride hydrochloric acid droplet progressively condenses along sample air-flow journey simultaneously and reunites on baffle surface and fall after rise in blistering reaction section;
4) obtain fully the sample gas of reduction and the stannous chloride hydrochloric acid droplet of minute quantity to discharge and enter external gas-guide pipeline, flow through sodium hydroxide solution impregnated quartz fibre drainage core, discharged by exhausr port, enter elemental mercury analyser and carry out analyzing and measuring.
Realize oxidation state mercury to be to the principle of elemental mercury transformation efficiency: bubbling style reactor processes sample gas, produces a large amount of micron-sized bubble, drastically increases the contact area of sample gas and tin chloride solution; Ultrasonic atomization technique processes tin chloride solution, forms a large amount of micron-sized droplet, further increases the contact area of sample gas and stannous chloride hydrochloric acid droplet; In addition, the water conservancy diversion of baffle and perturbation action also can extend the interaction time of sample gas and stannous chloride hydrochloric acid droplet.Therefore oxidation state mercury is greatly improved to the transformation efficiency of elemental mercury.
Beneficial effect: a kind of bubble type ultrasonic atomization mercury valence transformation device that the present invention proposes has following characteristic and advantage:
(1) utilize bubbling style reactor principle, increase the contact area of sample gas and tin chloride solution, be conducive to improving the transformation efficiency of oxidation state mercury to elemental mercury;
(2) utilize ultrasonic atomization technique, increase the contact area of sample gas and stannous chloride hydrochloric acid droplet, be conducive to improving the transformation efficiency of oxidation state mercury to elemental mercury;
(3) baffle arrangement extends the interaction time of sample gas and tin chloride solution, reclaim the complete tin chloride solution of unreacted simultaneously, be conducive to improving oxidation state mercury to the utilization ratio also improving tin chloride solution while elemental mercury transformation efficiency;
(4) link together ingenious for above-mentioned three rightly, form the entirety of a practicality and high efficiency, under the prerequisite ensureing Efficient Conversion mercury, realize tin chloride solution use amount and minimize and minimize with plant energy consumption;
(5) bubble type ultrasonic atomization mercury valence transformation device of the present invention both can detect elemental mercury in sample gas and oxidation state mercury in laboratory conditions with all kinds of elemental mercury analyser conbined usage; Also the submodule that can be used as coal fired power plant field monitoring equipment carries out the conversion of oxidation state mercury to elemental mercury, realizes multianalysis and the measurement of mercury valence state.
Apparatus of the present invention combine principle and the ultrasonic atomization technique of bubble type chemical reactor, pre-service is carried out to the mixed gas containing elemental mercury and oxidation state mercury, the efficiency that oxidation state mercury transforms to elemental mercury can be significantly improved, for the synchronous real time on-line monitoring of elemental mercury and oxidation state mercury provides feasibility.
In apparatus of the present invention, ultrasonic atomization sheet forms the stannous chloride hydrochloric acid droplet of about 50 microns at atomization conversion zone.
Present invention incorporates bubbling bed reaction principle and ultrasonic atomization technique to realize increasing contact area and the reaction time of sample gas and reaction solution, improve the transformation efficiency of oxidation state mercury to elemental mercury.
Accompanying drawing explanation
Fig. 1 is the structural system figure of patent bubble type ultrasonic atomization mercury valence transformation device of the present invention.
Have in figure: 1 air inlet air compartment, 2 air distribution plates, 3 blistering reaction sections, 4 atomization conversion zones, 5 cooling water jeckets, 6 extensions and solution exhausting section, 7 external gas-guide pipelines, 1-1 air inlet, 2-1 ultrasonic atomization sheet, 3-1 cooling heat transferring pipe, 5-1 cooling water inlet, 5-2 coolant outlet, 6-1 baffle, 7-1 quartz fibre drainage core, 7-2 exhausr port.
Embodiment
Technical scheme of the present invention is illustrated below in conjunction with Figure of description and example.
Bubble type ultrasonic atomization mercury valence transformation device of the present invention, comprise the air inlet air compartment 1 connecting setting from bottom to up successively, air distribution plate 2, blistering reaction section 3, atomization conversion zone 4, cooling water jecket 5, extension and solution exhausting section 6 and external gas-guide pipeline 7, air inlet air compartment 1 side is provided with air inlet 1-1, embedded ultrasonic atomization sheet 2-1 on air distribution plate 2, cooling heat transferring pipe 3-1 is provided with in blistering reaction section 3, cooling heat transferring pipe 3-1 is connected with cooling water jecket 5 by pipeline, cooling water jecket 5 is provided with cooling water inlet 5-1 and coolant outlet 5-2, cooling water jecket 5 inside is two independently hollow water storage cavities, separate with dividing plate, a water storage cavity is communicated with cooling water inlet 5-1, bottom connects cooling heat transferring pipe 3-1 inlet ductwork, another water storage cavity is communicated with coolant outlet 5-2, bottom connects cooling heat transferring pipe 3-1 export pipeline, form flow of cooling water path, in extension and solution exhausting section 6,4 ~ 6 the baffle 6-1 be staggeredly arranged successively are from bottom to up set, the quartz fibre drainage core 7-1 of dipping sodium hydroxide solution is provided with in external gas-guide pipeline 7.In apparatus of the present invention, air inlet air compartment 1, each conversion zone main body, cooling water jecket 5 and external gas-guide pipeline 7 all adopt the polytetrafluoroethylmaterial material of not Adsorption of Mercury, cooling heat transferring pipe 3-1 and and cooling water jecket 5 between connecting line adopt the high-boron-silicon glass material of not Adsorption of Mercury.Air distribution plate 2 in apparatus of the present invention adopts the quartz material of not Adsorption of Mercury, and densely covered pore diameter range is the aperture of 1 ~ 10 micron.A large amount of micron order apertures that it gathers can allow sample gas enter blistering reaction section 3 smoothly from air inlet air compartment 1, can ensure again the unlikely seepage of held tin chloride solution simultaneously.
Be used alone or with elemental mercury analyser conbined usage apparatus of the present invention before, the nitric acid dousing 12 ~ 24 hours of part service property (quality) mark 10% in advance need be touched to this device sample gas, use deionized water rinse clean afterwards, to ensure in measuring process mercury without adsorption loss effect.
The tin chloride solution of preparation massfraction 10%: 100 grams of stannous chlorides are dissolved in the hydrochloric acid of volume fraction 100 milliliter 10%, and with the hydrochloric acid to 1000 milliliter of volume fraction 10%.
By in the tin chloride solution slow injection device blistering reaction section 3 for preparing, consumption is depending on estimating mercury concentration in sample gas volumetric flow and sample gas, and tin chloride solution liquid level distance air distribution plate distance is no more than 10 centimetres.Start ultrasonic atomization sheet 2-1, driven by 12 volt DC voltages, conversion zone 4 to be atomized is full of stannous chloride hydrochloric acid droplet i.e. accessible required sample gas of measuring to carry out the conversion of mercury valence state and measures.
The sample gas being mixed with elemental mercury and oxidation state mercury enters air inlet air compartment 1 by air inlet 1-1, and because air distribution plate 2 is porous plates, pressure drop is comparatively large, and sample gas is comparatively even by distribution of gas after air distribution plate 2.
Air distribution plate 2 adopts the quartz material of not Adsorption of Mercury to sinter and forms, and 1 ~ 10 micron, aperture, can make sample gas enter blistering reaction section 3 from air inlet air compartment 1.Micron-sized densely covered aperture can make sample gas by time produce a large amount of micron-sized intensive bubble, the contact area of sample gas and tin chloride solution is greatly improved, simultaneously can ensures again the unlikely seepage of held tin chloride solution.Air distribution plate 2 is looked and concrete carries the ultrasonic atomization sheet 2-1 that mercury load embeds some, because tin chloride solution has stronger corrosivity, therefore ultrasonic atomization sheet 2-1 upper surface and all scribble anticorrosion thin layer with air distribution plate 2 junction.
The mercury sample gas that carries entering blistering reaction section 3 produces a large amount of bubble through air distribution plate 2, and fully contact with tin chloride solution on air distribution plate 2, reduction reaction occurs, and the sample gas through primary transformants is overflowed by solution, enters atomization conversion zone 4.The a large amount of stannous chloride hydrochloric acid droplets produced by ultrasonic oscillation are full of whole atomization conversion zone 4, fogdrop diameter about 50 microns.Sample gas fully contacts with stannous chloride hydrochloric acid droplet further, continues reduction reaction occurs, and the sample gas through transforming further enters extension and solution exhausting section 6 by the center pit of cooling water jecket 5.
Because ultrasonic oscillation atomization can produce larger heat, therefore design the cooling that cooling water system is used for tin chloride solution, to ensure that tin chloride solution temperature maintains well-defined reaction temp.Cooling water system is made up of cooling water jecket 5, cooling water inlet 5-1, coolant outlet 5-2 and cooling heat transferring pipe 3-1 etc.Cooling water jecket 5 indoor design is two separate hollow water storage cavities, centre separates with dividing plate, the chilled water controlling certain flow enters first water storage cavity by cooling water inlet 5-1, flows through cooling heat transferring pipe 3-1 and enters another water storage cavity, finally got rid of by coolant outlet 5-2.Cooling water jecket 5 with can adopt between atomization conversion zone 4 and extension and solution exhausting section 6 be threaded or Flange joint to ensure impermeability.
The sample gas entering extension and solution exhausting section 6 continues to interact with the stannous chloride hydrochloric acid droplet risen on a small quantity, and under the water conservancy diversion and perturbation action of baffle 6-1, both continue reduction reaction occurs, stannous chloride hydrochloric acid droplet progressively condenses and reunites on baffle 6-1 surface simultaneously, fall after rise in blistering reaction section 3 along baffle 6-1 after acquiring a certain degree, so circulation repeatedly.
The stannous chloride hydrochloric acid droplet of the sample gas and minute quantity that obtain fully reduction is discharged, enter in external gas-guide pipeline 7, Partial Elements state mercury analyzer device has the requirement of water capacity to analyzed sample gas, therefore design in external gas-guide pipeline 7 and add a quartz fibre drainage core 7-1, can ensure that the condition without mercury adsorption loss is issued to the effect of dehumidifying.Quartz fibre drainage core 7-1 can flood with sodium hydroxide solution, to remove the hydrogen chloride gas that may volatilize in advance.Finally, the dry sample gas be completely reduced is discharged by exhausr port 7-2, enters elemental mercury analyser and carries out analyzing and measuring.
After each measurement uses apparatus of the present invention, all need the tin chloride solution that process is remaining in time, and with deionized water rinse air inlet 1-1, each conversion zone and external gas-guide pipeline 7.
Claims (4)
1. a bubble type ultrasonic atomization mercury valence transformation device, it is characterized in that, this device comprises the air inlet air compartment (1) connecting setting from bottom to up successively, air distribution plate (2), blistering reaction section (3), atomization conversion zone (4), cooling water jecket (5), extension and solution exhausting section (6) and external gas-guide pipeline (7), described air inlet air compartment (1) side is provided with air inlet (1-1), the upper embedded ultrasonic atomization sheet (2-1) of described air distribution plate (2), cooling heat transferring pipe (3-1) is provided with in described blistering reaction section (3), described cooling heat transferring pipe (3-1) is connected with cooling water jecket (5) by pipeline, described cooling water jecket (5) is provided with cooling water inlet (5-1) and coolant outlet (5-2), in described extension and solution exhausting section (6), 4 ~ 6 baffles (6-1) be staggeredly arranged successively are from bottom to up set, the quartz fibre drainage core (7-1) of dipping sodium hydroxide solution is provided with in described external gas-guide pipeline (7), blistering reaction section (3) is contained with tin chloride solution.
2. bubble type ultrasonic atomization mercury valence transformation device according to claim 1, it is characterized in that, described air inlet air compartment (1), each conversion zone main body, cooling water jecket (5) and external gas-guide pipeline (7) all adopt the polytetrafluoroethylmaterial material of not Adsorption of Mercury, described cooling heat transferring pipe (3-1) and and cooling water jecket (5) between connecting line adopt the high-boron-silicon glass material of not Adsorption of Mercury.
3. bubble type ultrasonic atomization mercury valence transformation device according to claim 1, is characterized in that: described air distribution plate (2) adopts the quartz material of not Adsorption of Mercury, and densely covered pore diameter range is the aperture of 1 ~ 10 micron.
4. utilize bubble type ultrasonic atomization mercury valence transformation device described in claim 1 to carry out a method for mercury valence state conversion, it is characterized in that, the method comprises the steps:
1) the sample gas being mixed with elemental mercury and oxidation state mercury is passed into air inlet air compartment (1) by air inlet (1-1), after air distribution plate (2), evenly enter blistering reaction section (3) react with tin chloride solution;
2) shake by ultrasonic atomization sheet (2-1) a large amount of stannous chloride hydrochloric acid droplets produced and be full of whole atomization conversion zone (4), sample gas fully contacts with stannous chloride hydrochloric acid droplet further, and reduction reaction occurs;
3) sample gas enters extension and solution exhausting section (6) by the center pit of cooling water jecket (5) after this two-step reaction, in extension and solution exhausting section (6), the passage formed is intercepted along baffle (6-1), sample gas and stannous chloride hydrochloric acid droplet continue to interact, and stannous chloride hydrochloric acid droplet progressively condenses along sample air-flow journey simultaneously and reunites on baffle (6-1) surface and fall after rise in blistering reaction section (3);
4) obtain fully the sample gas of reduction and the stannous chloride hydrochloric acid droplet of minute quantity to discharge and enter external gas-guide pipeline (7), flow through sodium hydroxide solution impregnated quartz fibre drainage core (7-1), discharged by exhausr port (7-2), enter elemental mercury analyser and carry out analyzing and measuring.
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| CN105067415B (en) * | 2015-08-11 | 2018-05-15 | 袁洪林 | A kind of filter that can remove the mercury in high-purity gas or aerosol |
| CN106248595B (en) * | 2016-08-04 | 2023-06-27 | 西安热工研究院有限公司 | System and method for testing bivalent mercury and zero-valent mercury in flue gas of coal-fired power plant |
| CN106568897A (en) * | 2016-10-27 | 2017-04-19 | 浙江大学宁波理工学院 | Device and measuring method used for continuous measuring of content of mercury of different valence states in flue gas |
| CN107238527A (en) * | 2017-04-28 | 2017-10-10 | 东南大学 | A kind of Pintsch process formula gas phase mercury shape reforming unit and method |
| CN109253995B (en) * | 2018-10-31 | 2021-06-01 | 中国石油天然气股份有限公司 | Mercury isotope testing method and device for natural gas |
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