CN101980013B - System for detecting activity of adsorbent - Google Patents
System for detecting activity of adsorbent Download PDFInfo
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- CN101980013B CN101980013B CN201010507622.5A CN201010507622A CN101980013B CN 101980013 B CN101980013 B CN 101980013B CN 201010507622 A CN201010507622 A CN 201010507622A CN 101980013 B CN101980013 B CN 101980013B
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Abstract
The invention discloses a system for detecting the activity of an adsorbent and relates to the adsorbent. The system is provided with a stimulation fire coal flue gas phase mercury generation unit, a reaction unit, and a detection unit, wherein the stimulation fire coal flue gas phase mercury generation unit is provided with a N2 gas cylinder, a CO2 gas cylinder, a SO2 gas cylinder, an O2 gas cylinder, a NO2 gas cylinder, a HCl gas cylinder, a NO gas cylinder, a mass flow controller, an HgO permeability tube, an Hg<2+> permeability tube, and a constant temperature water bath kettle; the reaction unit is provided with a drying oven, a mixing preheater and an adsorption reactor; and the detection unit is provided with a gas-washing bottle with solution of SnCl2 and NaOH, a gas-washing bottle with solution of KCl and NaOH, an ice-bath condenser, and a mercury vapourmeter for continuously measuring the mercury-vapor content. The system can conveniently, quickly and stably generates a full composition stimulation fire coal flue gas at certain gaseous mercury concentration, and can provide stable reaction temperature and monitor the total mercury or elemental mercury content in real time by matching with the mercury vapourmeter through a rotation valve.
Description
Technical field
The present invention relates to a kind of adsorbent, especially relate to a kind of activity monitor system of adsorbent that be used for studying the adsorbent of the absorption of coal-fired flue-gas gas phase mercury.
Background technology
On March 15th, 2005, Environmental Protection Agency has issued the clean air mercury bill.This bill regulation, by 2018, the emission level of mercury will reduce by 70% on basis in 1999.
The sorbent injection technology is the removal of mercury technology that is used for coal-fired plant flue gas of tool market outlook.This technology is gone into sorbent injection in the flue gas stream between air preheater and the cleaner (electrostatic precipitator, sack cleaner etc.), makes adsorbent finish absorption to mercury in flue gas, and is captured by follow-up cleaner with flying dust.Sorbent injection removal of mercury technology has been successfully applied to a plurality of case histories, yet, before this technology commercialization and being widely used, also need it is much studied and develops.Because this Technology Need uses a large amount of adsorbents, thus the particle that will increase fly-ash separator load and then may influence the normal operation of power plant, and will increase the processing of flying dust and the operating cost of disposal and other aspect.Therefore, efficient, the low-cost adsorbent of development of new is a hot research in recent years.
Influencing adsorbent comprises the factor of the adsorption efficiency of mercury: the physics of adsorbent, chemical property, flue gas condition (temperature, halogen and SO
3Content etc.) and the configuration of power plant's Air Pollution Control Board control equipment etc.Present stage, the scientific research personnel mainly carries out at the ADSORPTION IN A FIXED BED reactive system of bench scale the research of the adsorbent that is used for mercury pollution control.Yet the ADSORPTION IN A FIXED BED reactive system majority that uses in the bibliographical information is only used N
2Or N
2With other a few flue gas composition, or can not detect total mercury and element mercury content in the adsorptive reactor outlet simulated flue gas simultaneously, or only relate to Hg
0, and lack Hg as mercury important morphological in the coal-fired flue-gas
2+Deng ([4] Stuart JL.DEVELOPMENT OF AN EXPERIMENTAL SYSTEM TO STUDYMERCURY UPTAKE BY ACTIVATED CARBONS UNDER SIMULATED FLUE GASCONDITIONS.Pittsburgh:University of Pittsburgh; 2002; [5] Diamantopoulou I, Skodras G, Sakellaropoulos GP.Sorption of mercury by activated carbon in the presence of flue gascomponents.Fuel Processing Technology, 2010,91 (2): 158-163; [6] Lee J-Y, Ju Y, Lee S-S, et al.Novel Mercury Oxidant and Sorbent for Mercury Emissions Control from Coal-fired Power Plants.Water, Air, ﹠ Soil Pollution:Focus, 2008,8 (3): 333-341).Therefore, set up one reliable and stable, can be used for studying fully compositional simulation flue gas (N
2, CO
2, O
2, SO
2, NO
2, HCl, NO, moisture and Hg
0Or Hg
2+) different adsorbents are very necessary to the experimental system of the absorption property of mercury under the condition.
Summary of the invention
The object of the present invention is to provide a kind of activity monitor system of adsorbent.
The present invention is provided with simulation coal-fired flue-gas gas phase mercury generating unit, reaction member and detecting unit.
Described simulation coal-fired flue-gas gas phase mercury generating unit is provided with N
2Gas cylinder, CO
2Gas cylinder, SO
2Gas cylinder, O
2Gas cylinder, NO
2Gas cylinder, HCl gas cylinder, NO gas cylinder, mass flow controller, Hg
0Osmos tube, Hg
2+Osmos tube and thermostat water bath.In thermostat water bath, be provided with the Drexel bottle that produces moisture and produce gas phase mercury (Hg
0Or HgCl
2) the mercury osmos tube, be connected with the stripping carrier gas N of constant rate in the Drexel bottle
2, the mercury osmos tube is located in the U type pipe, and U type pipe is furnished with pipe close, and U type tube inlet one side fills beaded glass, and the mercury osmos tube is located at U type pipe and is exported a side; N
2Gas cylinder, CO
2Gas cylinder, SO
2Gas cylinder, O
2Gas cylinder, NO
2The flow of gas cylinder, HCl gas cylinder and NO gas cylinder is controlled by mass flow controller, and the pipeline of all mercury vapour and water vapour process all is wound with the heating tape;
Described reaction member is provided with baking oven, mix primary heater and adsorptive reactor, the baking oven top has 2 circular holes that are used for conveniently being connected with the pipeline turnover of simulating coal-fired flue-gas, the mercurous air-flow that flows out through U type pipe and other each flue gas composition air communication are crossed a Y-type three way type and are integrated with a pipeline, be split as three pipelines by two Y-type three way types afterwards, can select to make air-flow from then on to pass through among any in 3 pipelines by changeover valve, article 3, the whereabouts of pipeline is respectively: feed baking oven (route I), feed exhaust gas processing device, and directly lead to detecting unit in order to assaying reaction device inlet mercury concentration (route II); The pipeline that feeds permanent sound of a roaring fire case is connected with adsorptive reactor with the mixing primary heater, stretches out from baking oven afterwards; The pipeline that stretches out from baking oven is split as parallel two-way by a Y-type three way type and two valves with it, is connected with total mercury route, element mercury route in the detecting unit respectively;
Described detecting unit is provided with and contains SnCl
2Mercury vapor analyzer with the Drexel bottle of NaOH solution, the Drexel bottle that contains KCl and NaOH solution, ice bath condenser and METHOD FOR CONTINUOUS DETERMINATION bicycle pump content; Can select total mercury content or the element mercury content in the simulation coal-fired flue-gas behind the assaying reaction by changeover valve, the ice bath condenser is made of the Drexel bottle that is immersed in the sky in the ice cube.
Described pipe close can adopt the hollow quartz glass tube plug with holes of frosted.
The described SnCl that contains
2With the Drexel bottle of NaOH solution, can adopt to contain 200mL 2%SnCl
2With the Drexel bottle of 20%NaOH solution, form the total mercury route; Described KCl can adopt 200mL 1mol/L KCl.
The described Drexel bottle that contains KCl and NaOH solution can be adopted the Drexel bottle that contains 200mL 1mol/L KCl and 20%NaOH solution, component mercury route.
Described mercury vapor analyzer can adopt the Jerome mercury vapor analyzer.
The invention has the beneficial effects as follows: can easily and fast, stably produce the fully compositional simulation coal-fired flue-gas that contains certain gas phase mercury concentration, stable temperature of reaction can be provided, can cooperate with mercury vapor analyzer by changeover valve, with real-time monitoring total mercury or element mercury content.Circuit design is convenient and practical, acidproof, high temperature resistant (＜200 ℃).Through experimental verification, in pipeline, be connected with 1L/minN
2With 10～50 μ g/m
3Hg
0Or Hg
2+The time, the mercury concentration before and after the reaction member is identical, that is: this experimental system is reliable and stable, can be used for the absorption research of adsorbent to gas phase mercury in the coal-fired flue-gas.
The present invention adopts reliable and stable, convenient and practical equipment and material to set up the generation of a fully compositional simulation coal-fired flue-gas gas phase mercury, reaction and detection system, and is applied under the test simulation flue gas condition different adsorbents to the absorption property of mercury.Studies show that, this system can produce the fully compositional simulation flue gas that contains constant mercury concentration, suitable adsorption reaction condition (flue gas composition concentration, temperature etc.) can be provided, the total mercury and the element mercury concentration of monitoring reaction device import and export in real time, thus can be used for studying single fully and effectively or the polycomponent flue gas to adsorbents adsorb Hg
0Or Hg
2+Research.
Description of drawings
Fig. 1 is the U type pipe unit synoptic diagram that holds the mercury osmos tube.
Fig. 2 is that the structure of the embodiment of the invention is formed synoptic diagram.
Embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
The present invention is provided with simulation coal-fired flue-gas gas phase mercury generating unit, reaction member and detecting unit.
Described simulation coal-fired flue-gas gas phase mercury generating unit is provided with N
2Gas cylinder, CO
2Gas cylinder, SO
2Gas cylinder, O
2Gas cylinder, NO
2Gas cylinder, HCl gas cylinder, NO gas cylinder, mass flow controller, Hg
0Osmos tube, Hg
2+Osmos tube and thermostat water bath.In thermostat water bath, be provided with the Drexel bottle that produces moisture and produce gas phase mercury (Hg
0Or HgCl
2) the mercury osmos tube, be connected with the stripping carrier gas N of constant rate in the Drexel bottle
2, the mercury osmos tube is located in the quartzy U type pipe, and U type pipe is furnished with the hollow quartz glass tube plug with holes of frosted, and U type tube inlet one side fills beaded glass, and U type pipe exports a side mounting and places the mercury osmos tube; N
2Gas cylinder, CO
2Gas cylinder, SO
2Gas cylinder, O
2Gas cylinder, NO
2The flow of gas cylinder, HCl gas cylinder and NO gas cylinder is controlled by mass flow controller, and the pipeline of all mercury vapour and water vapour process all is wound with the heating tape.
Described reaction member is provided with baking oven, mix primary heater and adsorptive reactor, the baking oven top has 2 circular holes that are used for conveniently being connected with the pipeline turnover of simulating coal-fired flue-gas, the mercurous air-flow that flows out through U type pipe and other each flue gas composition air communication are crossed a Y-type three way type and are integrated with a pipeline, be split as three pipelines by two Y-type three way types afterwards, can select to make air-flow from then on to pass through among any in 3 pipelines by changeover valve, article 3, the whereabouts of pipeline is respectively: feed baking oven (route I), feed exhaust gas processing device, and directly lead to detecting unit in order to assaying reaction device inlet mercury concentration (route II); The pipeline that feeds permanent sound of a roaring fire case is connected with adsorptive reactor with the mixing primary heater, stretches out from baking oven afterwards; The pipeline that stretches out from baking oven is split as parallel two-way by a Y-type three way type and two valves with it, is connected with total mercury route, element mercury route in the detecting unit respectively.
Described detecting unit is provided with and contains 200mL 2%SnCl
2With the Drexel bottle (total mercury route) of 20%NaOH solution, contain the Jerome mercury vapor analyzer of Drexel bottle (element mercury route), ice bath condenser and the METHOD FOR CONTINUOUS DETERMINATION bicycle pump content of 200mL 1mol/LKCl and 20%NaOH solution; Can select total mercury content or the element mercury content in the simulation coal-fired flue-gas behind the assaying reaction by changeover valve, the ice bath condenser is made of the Drexel bottle that is immersed in the sky in the ice cube.
Referring to Fig. 1, in Fig. 1, the acting as preheating, stablize the stripping carrier gas of beaded glass 12; The position that act as fixing glass pearl 12 of silica wool 13; Mercury osmos tube 14 is suspended in the U type pipe 11 by diagramatic way by a polytetrafluoroethylraw raw material band 15.U type pipe is partially immersed in the water-bath below the interface for 11 liang.
1, set up the U type pipe unit that holds the mercury osmos tube by Fig. 1, the pipeline main body all adopts the D8*6 polyfluortetraethylene pipe 16 of ultralow adsorbability.Each component-assembled is become the activity monitor system of complete adsorbent by Fig. 2.Can connect with a bit of D6*9 silicone tube neatly between any two interfaces.Exhaust gas processing device is the Powdered Activated Carbon adsorption column, and its effect is the micro-gas phase mercury that exists in the adsorption gas flow.The solution of using in this system is matching while using.
2, simulation coal-fired flue-gas (the 15 μ g/m under 140 ℃ that contain the typical concentration component with generation
3Hg
0, 13%CO
2, 9% moisture, 300ppm NO, 6%O
2, 300ppm SO
2, 20ppm HCl, and 20ppm NO
2) be example, operate as follows:
2.1 with mass flow controller A shown in Figure 2
nFlow be set to (unit: mL/min) N respectively
21#800, CO
2130, O
260, SO
260, NO
240, HCl 40, NO 60, N
22# (moisture) 90, and N
23#200.
2.2 open line II.Open water-bath, open N
23# (that is: opens, opens N among Fig. 2
2The gas cylinder of 3# correspondence, mass flow controller A
nAnd valve B
n), make the mercury osmos tube be in the down stable about 2h of state of 39.6 ℃ of constant water bath temperatures (every mercury osmos tube all will be determined its suitable bath temperature through testing, and this sentences used mercury osmos tube is example), the carrier gas of constant rate 0.2L/min stripping to obtain constant mercury release rate.Open source of water vapor (can adopt steam generator) 21, make it produce the moisture N of steady concentration
2 Open baking oven 22, its temperature is set is 140.0 ℃ and make it stable.
2.3 open N
21#.Total flow is 1L/min among the route II at this moment, can use mercury vapor analyzer (can adopt Jerome 431X type mercury vapor analyzer) 23 to measure the mercury concentration of air-flows, is reactor inlet mercury concentration and (is called for short C
In).If the concentration of surveying is 15 μ g/m
3, then can carry out next step.Otherwise, then continue 2.2 described steps.
2.4 after the inlet mercury concentration stabilize, with N
21# corresponding mass flow controller A
nFlow set be 320mL/min.Open all flue gas compositions, make each flue gas composition stability of flow.Can open baking oven 22 this moment, by need to fill adsorbent separately, install the adsorption reaction post and wait for so that in the baking oven 22 temperature reach stable again.
2.5 open line I and total mercury route (2%SnCl
2aqWith 20%NaOH
Aq) 24 and close closed edge train II.Promptly obtain to contain the simulation coal-fired flue-gas of typical concentration component this moment, the adsorbent in the adsorptive reactor begins and the reaction of simulation coal-fired flue-gas.But use mercury vapor analyzer 23 assaying reaction devices outlet total mercury concentration (to be called for short C
Out, T).By changeover valve B
nAir-flow can be switched to element mercury route (200mL 1mol/LKCl
AqWith 20%NaOH
Aq) 25, but use mercury vapor analyzer 23 assaying reaction devices outlet element mercury concentration (to be called for short C
Out, E).Pass through C
In, C
Out, T, and C
Out, ENumerical value can analyze the Adsorption law (for example curve of adsorption kinetics etc.) of adsorbent to gas phase mercury in the simulation coal-fired flue-gas.
In Fig. 2, mark C
nW type threeway for each road; D
nHeating tape for each road; M is an adsorptive reactor for mixing primary heater: R; 26 is the ice bath condenser; 27 is the gaseous mercury generator; PC is a computing machine.
The present invention is provided with simulation coal-fired flue-gas gas phase mercury generating unit, reaction member and detecting unit.The pipeline main body of each unit adopts the D 8*6 teflon hose or the D 9*6 silicone tube of acid resistance gas, low absorbability; The valve of pipeline junction adopting quartz glass or acrylic plastering material and Y-type three way type joint.The total flow of simulation coal-fired flue-gas is 1L/min.
Simulation coal-fired flue-gas gas phase mercury generating unit is mainly by N
2(99.999%), CO
2(99.99%), SO
2(5000ppm), O
2(99.99%), NO
2(500ppm), HCl (500ppm), NO (5000ppm) gas cylinder, mass flow controller (100mL/min, 200mL/min, 500mL/min or 1000mL/min), Hg
0Osmos tube (HE-SR 2.4cm, VICI) and Hg
2+Osmos tube (HE-SR 1.0cm, VICI) and composition such as thermostat water bath.Moisture produces ([7] Bhardwaj R.IMPACT OF TEMPERATURE AND FLUEGAS COMPONENTS ON MERCURY SPECIATION AND UPTAKE BY ACTIVATED CARBONSORBENTS:UNIVERSITY OF PITTSBURGH by the Drexel bottle that certain mass water is housed that is positioned in the thermostat water bath; 2007), be connected with the stripping carrier gas N of constant rate in the Drexel bottle
2Gas phase mercury (Hg
0Or HgCl
2) by the internal diameter 15mm that is positioned in the thermostat water bath, the mercury osmos tube that always is about in the quartzy U type pipe of 380mm produces.U type pipe is furnished with the hollow quartz glass plug with holes of frosted.U type tube inlet one side fills about 25g soaks 4h through 10% salpeter solution D 6 beaded glasses.The effect of beaded glass is preheating, stablize the stripping carrier gas; U type pipe exports a side mounting and places the mercury osmos tube.All the other flue gas composition gases are flowed out by each gas cylinder.The flow of all gas is accurately controlled by mass flow controller.The pipeline of all mercury vapour and water vapour process all has been wound the heating tape, and pipe surface temperature is remained on about 140 ℃; The heating tape is by electroheat pair (± 1 ℃) temperature control.When the constant flow of each component gas and bath temperature were constant, this unit can produce the simulation coal-fired flue-gas that contains constant mercury concentration.Determine that the principle that each flue gas composition enters the order of pipeline is: the flue gas composition that character is stable more, flow is big more at first enters pipeline (that is: enter before the reaction member pipeline of process shorter).The order of determining by this principle is followed successively by: N
2, CO
2, O
2, SO
2, NO
2, HCl, NO, moisture, and Hg
0Or Hg
2+
Reaction member mainly is made up of baking oven (± 0.1 ℃), mixing primary heater (can dispose as required), adsorptive reactor (can dispose as required).The baking oven top has the circular hole of two diameter 2cm, conveniently to be connected with the pipeline turnover of simulation coal-fired flue-gas.The mercurous air-flow that flows out through U type pipe and other each flue gas composition air communication are crossed a Y-type three way type and are integrated with a pipeline, are split as three pipelines by two Y-type three way types afterwards.Can select to make air-flow from then on to pass through among any in three pipelines by changeover valve.Article three, the whereabouts of pipeline is respectively: feed baking oven (route I), feed exhaust gas processing device, and directly lead to detecting unit in order to assaying reaction device inlet mercury concentration (route II).The pipeline that feeds baking oven is connected with mixing primary heater, adsorptive reactor, stretches out from baking oven afterwards.The pipeline that stretches out from baking oven is split as parallel two-way by a Y-type three way type and two valves with it, is connected with total mercury route, element mercury route in the detecting unit respectively.
Detecting unit mainly contains 200mL 2%SnCl by a 250mL
2With the Drexel bottle that contains 200mL 1mol/L KCl and 20%NaOH solution (element mercury route) of the Drexel bottle (total mercury route) of 20%NaOH solution, a 250mL, an ice bath condenser, and the Jerome mercury vapor analyzer composition that can measure bicycle pump content rapidly, continuously.SnCl
2The effect of solution is with the Hg in the simulation coal-fired flue-gas
2+Be reduced to Hg
0Thereby, obtain reacted total mercury concentration; The effect of KCl solution is with the Hg in the simulation coal-fired flue-gas
2+Trap in the solution, thereby obtain reacted Hg
0Concentration; The effect of NaOH in two Drexel bottles is absorption can influence the sour gas of mercury vapor analyzer reading ([8] Mibeck BAF, Olson ES, Miller SJ.HgCl2 sorption onlignite activated carbon:Analysis of fixed-bed results.Fuel Processing Technology, 2009,90 (11): 1364-1371).Can select total mercury content or the element mercury content in the simulation coal-fired flue-gas behind the assaying reaction by changeover valve.The ice bath condenser is made of the Drexel bottle of the 250mL that is immersed in the sky in the ice cube, its effect be in the condensing gas stream moisture with the protection mercury vapor analyzer.
Claims (6)
1. the activity monitor system of an adsorbent is characterized in that being provided with simulation coal-fired flue-gas gas phase mercury generating unit, reaction member and detecting unit;
Described simulation coal-fired flue-gas gas phase mercury generating unit is provided with N
2Gas cylinder, CO
2Gas cylinder, SO
2Gas cylinder, O
2Gas cylinder, NO
2Gas cylinder, HCl gas cylinder, NO gas cylinder, mass flow controller, Hg
0Osmos tube, Hg
2+Osmos tube and thermostat water bath; In thermostat water bath, be provided with Drexel bottle that produces moisture and the mercury osmos tube that produces gas phase mercury, be connected with the stripping carrier gas N of constant rate in the Drexel bottle
2, the mercury osmos tube is located in the U type pipe, and U type pipe is furnished with pipe close, and U type tube inlet one side fills beaded glass, and the mercury osmos tube is located at U type pipe and is exported a side; N
2Gas cylinder, CO
2Gas cylinder, SO
2Gas cylinder, O
2Gas cylinder, NO
2The flow of gas cylinder, HCl gas cylinder and NO gas cylinder is controlled by mass flow controller, and the pipeline of all mercury vapour and water vapour process all is wound with the heating tape;
Described reaction member is provided with baking oven, mix primary heater and adsorptive reactor, the baking oven top has 2 circular holes that are used for conveniently being connected with the pipeline turnover of simulating coal-fired flue-gas, the mercurous air-flow that flows out through U type pipe and other each flue gas composition air communication are crossed a Y-type three way type and are integrated with a pipeline, be split as three pipelines by two Y-type three way types afterwards, select to make air-flow from then on to pass through among any in 3 pipelines by changeover valve, article 3, the whereabouts of pipeline is respectively: feed baking oven, feed exhaust gas processing device, and directly lead to detecting unit in order to assaying reaction device inlet mercury concentration; The pipeline that feeds baking oven is connected with adsorptive reactor with the mixing primary heater, stretches out from baking oven afterwards; The pipeline that stretches out from baking oven is split as parallel two-way by a Y-type three way type and two valves with it, is connected with total mercury route, element mercury route in the detecting unit respectively;
Described detecting unit is provided with and contains SnCl
2Mercury vapor analyzer with the Drexel bottle of NaOH solution, the Drexel bottle that contains KCl and NaOH solution, ice bath condenser and METHOD FOR CONTINUOUS DETERMINATION bicycle pump content; Can select total mercury content or the element mercury content in the simulation coal-fired flue-gas behind the assaying reaction by changeover valve, the ice bath condenser is made of the Drexel bottle that is immersed in the sky in the ice cube.
2. the activity monitor system of a kind of adsorbent as claimed in claim 1 is characterized in that described pipe close is the hollow quartz glass tube plug with holes of frosted.
3. the activity monitor system of a kind of adsorbent as claimed in claim 1 is characterized in that the described SnCl of containing
2With the Drexel bottle of NaOH solution, adopt to contain 200mL2%SnCl
2With the Drexel bottle of 20%NaOH solution, form the total mercury route.
4. the activity monitor system of a kind of adsorbent as claimed in claim 1 is characterized in that described KCl adopts 200mL1mol/L KCl.
5. the activity monitor system of a kind of adsorbent as claimed in claim 1 is characterized in that the Drexel bottle of described KCl of containing and NaOH solution, adopts the Drexel bottle that contains 200mL1mol/L KCl and 20%NaOH solution, component mercury route.
6. the activity monitor system of a kind of adsorbent as claimed in claim 1 is characterized in that described mercury vapor analyzer is the Jerome mercury vapor analyzer.
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|---|---|---|---|
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|---|---|---|---|
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