CN105115924A - Method and apparatus for testing demercuration performance of carbon-based adsorbent - Google Patents
Method and apparatus for testing demercuration performance of carbon-based adsorbent Download PDFInfo
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- CN105115924A CN105115924A CN201510393354.1A CN201510393354A CN105115924A CN 105115924 A CN105115924 A CN 105115924A CN 201510393354 A CN201510393354 A CN 201510393354A CN 105115924 A CN105115924 A CN 105115924A
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Abstract
The present invention provides a method and an apparatus for testing the demercuration performance of a carbon-based adsorbent. The method specifically comprises preparing mixing gas, adsorbing, carrying out post-treatment, and detecting, wherein the mixing gas is prepared to simulate the flue gas environment in real industry, and then the experiment is performed to test the demercuration performance of the carbon-based adsorbent. According to the present invention, the method and the apparatus have characteristics of simple operation, low gas consumption, short test time, low cost, true reflection of the demercuration effect of the adsorbent, high reliability, important guiding significance, and important reference value.
Description
Technical field
The present invention relates to performance test field, be specifically related to a kind of test of carbon-supported catalyst demercuration performance.
Background technology
Coal combustion is except causing CO
2, SO
x, NO
x, beyond PM10 pollution problem, be that the detrimental trace elements pollution on the environment problem of representative is more and more outstanding with mercury.Mercury not easily removes after entering environment, and in the environment by biologic chain long term accumulation, produces long-term toxic action to biological and human body.Research shows, over nearest more than 20 years, the mercury concentration in global atmosphere is in ascendant trend year by year, and especially nearly ten years ascendant trends are more obvious.In March, 2011, U.S. EPA promulgated up-to-date power plant pollution thing emission standard, had wherein carried out strict restriction to mercury emissions in power plant soot fume.In July, 2011, up-to-date " fossil-fuel power plant atmospheric pollutant emission standard (GB13223-2011) " of Environment Protect in China cloth promulgated by the ministries or commissions of the Central Government, requires from 2015, controls mercury and mercuric compounds discharge capacity in power plant soot fume at 0.03mg/Nm
3below.Under the background of China's economic high speed development, coal-burning power plant and large and medium-sized coal-burned industrial boiler are still also being greatly developed, and the problem of preventing and treating of coal burning pollution is a problem of not allowing to avoid.Therefore, the research of the aspects such as coal-fired mercury pollution control must be strengthened, set up the scientific theory of system, develop the economy, efficient mercury pollution control technology.
Mercury in coal-fired flue-gas mainly contains three kinds of existing forms: particulate Hg (Hg
p), bivalent mercury (Hg
2+) and Elemental Mercury (Hg
0).Particle mercury can be removed by cleaner, and bivalent mercury is easily by wet flue gas desulfurizer and most of adsorbent institute absorbing and removing, and Elemental Mercury, owing to being insoluble in water and having higher volatility, is difficult to be absorbed by existing pollutant catabolic gene device.In recent years, Chinese scholar has carried out large quantity research in adsorbent mercury, and except the adsorbents such as flying dust class material, Ca-base adsorbent, noble metal adsorbent, living beings class adsorbent, ore class adsorbent, what be most widely used surely belongs to carbon-supported catalyst.By carrying out modification to activated charcoal, obtain good mercury adsorption effect.As related documents describes Nitric Acid Modified acticarbon, Preparation Method And The Use for flue gas demercuration, make it have good demercuration effect by Nitric Acid Modified activated charcoal; And for example related documents describes the iron chlorine modified activated carbon absorbent for flue gas demercuration, improves its demercuration efficiency by ferric nitrate-chloric acid mixed solution Immesion active carbon.Although Modified Activated Carbon base adsorbent has good effect in mercury removal, but directly cannot test and then evaluate its quality to its demercuration performance in actual production, therefore, be necessary that simulating actual condition in laboratory conditions carries out the performance test of adsorbent demercuration, thus it is good and bad better to evaluate its performance, reduces commerical test cost.
Summary of the invention
The object of this invention is to provide a kind of method of testing and device of carbon-supported catalyst demercuration performance.
The technical scheme adopted for realizing the object of the invention is such, and a kind of method of testing carbon-supported catalyst demercuration performance, comprises and prepare mixed gas, absorption, aftertreatment and testing process, and described method specifically comprises the following steps:
1) be that the carbon-supported catalyst sample of 2 ~ 4mm loads in adsorptive reactor by 50mg granularity.
2) by N
2, CO
2, NO, NO
2, HCl, SO
2, and O
2mixing, N
2mercuryvapour is brought into mixed gas through mercury osmos tube before mixing; Obtained mixed gas is by 20ppmNO
2, 300ppmNO, 5 ~ 10ppmHCl, 300ppmSO
2, 6%O
2, 13.5%CO
2, 15 ± 1ng/L mercury and N
2composition, wherein N
2as balanced gas.
3) obtained mixed gas is heated to 100 ~ 150 DEG C; Then pass into adsorptive reactor, the total flow of mixed gas is 1L/min, and adsorption reaction actuator temperature is 140 DEG C.
4) through step 3) process after mixed gas pass into heating cabinet, after 100 DEG C are heated to it be incubated.
5) through step 4) process after mixed gas pass into 10%SnCl successively
2solution and 10%NaOH solution.
6) to through step 5) mixed gas after process carries out detections analysis; Twin-beam cold-vapour atomic absorption method is adopted to measure and pass through the areal calculation mercury adsorbance between integration breakthrough curve and datum line; Its computing formula is
A represents the adsorbance (μ g/g) of carbon-supported catalyst to mercury.
C
0represent datum line mixed gas mercury concentration (ng/L).
C
trepresent mixed gas mercury concentration (ng/L) in test process.
M represents carbon-supported catalyst quality (g).
C represents the curve of mercury concentration changes with time in mixed gas.
Based on a kind of above-mentioned method of testing carbon-supported catalyst demercuration performance, the present invention also provides a kind of carbon-supported catalyst demercuration performance testing device, comprises gas distributing system, mercury generating means, fixed bed reactors, mercury shape conversion system and mercury analytic system.
Described gas distributing system comprises generator and the distribution branch road of above-mentioned various gas.Described mercury generating means comprises mercury osmos tube, U-tube and thermostatical oil bath.Described mercury osmos tube is positioned at U-tube, and U-tube is positioned at thermostatical oil bath.Described fixed bed reactors and adsorptive reactor.Described mercury shape conversion system comprises heating cabinet and two Drexel bottles, and two Drexel bottles are equipped with 10%SnCl respectively
2solution and 10%NaOH solution.Described mercury analytic system comprises mercury vapor analyzer and common computer.
Described mercury generating means is arranged on N
2in distribution branch road.The gas outlet of described gas distributing system is connected with the air intake opening of fixed bed reactors.The gas outlet of described fixed bed reactors is connected with the air intake opening of heating cabinet.Described heating cabinet gas outlet with 10%SnCl is housed
2the air intake opening of the Drexel bottle I of solution connects.The gas outlet of described Drexel bottle I is connected with the air intake opening of the Drexel bottle II that 10%NaOH solution is housed.The gas outlet of described Drexel bottle II is communicated with mercury analytical equipment.
Further, described fixed bed reactors can accurate temperature controlling to 0.1 DEG C, can simulate actual condition adsorbent working environment, as all kinds of gas-solid reaction proving installation.
Further, this device is from gas distributing system to mercury shape conversion system, and whole process carries out air preheat insulation by heat tape.
Technique effect of the present invention is mathematical, has following beneficial effect:
1, the present invention utilizes laboratory room small-sized simulated flue gas platform test carbon-supported catalyst demercuration performance, avoids medium-sized or large test device complicated operation, gas consumption is large, the test duration is long, high in cost of production shortcoming, has important directive significance and reference value;
2, this analog detection method and system truly can reduce actual condition adsorbent working environment, truly can reflect adsorbent demercuration effect, with a high credibility, simple to operate.
Accompanying drawing explanation
Fig. 1 is proving installation schematic diagram of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention and be only limitted to following embodiment.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, make various replacement and change, all should be included in protection scope of the present invention.
Embodiment 1:
Test a method for carbon-supported catalyst demercuration performance, comprise and prepare mixed gas, absorption, aftertreatment and testing process, described method specifically comprises the following steps:
1) be that the carbon-supported catalyst sample of 2 ~ 4mm loads in adsorptive reactor by 50mg granularity;
2) by N
2, CO
2, NO, NO
2, HCl, SO
2, and O
2mixing, N
2mercuryvapour is brought into mixed gas through mercury osmos tube before mixing; Obtained mixed gas is by 20ppmNO
2, 300ppmNO, 5 ~ 10ppmHCl, 300ppmSO
2, 6%O
2, 13.5%CO
2, 15 ± 1ng/L mercury and N
2composition; Wherein N
2as balanced gas, can ensure that total gas flow rate is certain, and by constantly regulating, ensure that other gas concentrations are in specialized range; When the amount of other gas reaches fixed value, the amount of nitrogen is also fixed thereupon; When other gas concentration changes, nitrogen then correspondingly can make change; Obtained mixed gas simulates the environment of actual industrial flue gas as far as possible really;
3) obtained mixed gas is heated to 100 ~ 150 DEG C; Then pass into adsorptive reactor, the total flow of mixed gas is 1L/min, and adsorption reaction actuator temperature is 140 DEG C;
4) through step 3) process after mixed gas pass into heating cabinet, after 100 DEG C are heated to it be incubated;
5) through step 4) process after mixed gas pass into 10%SnCl successively
2solution and 10%NaOH solution; SnCl
2solution is used for mercury all in mixed gas to be reduced into Elemental Mercury, and NaOH solution, for removing the sour gas in mixed gas, avoids the corrosion to mercury vapor analyzer; In practical operation, ventilation order can exchange;
6) to through step 5) mixed gas after process carries out detections analysis; Twin-beam cold-vapour atomic absorption method is adopted to measure and pass through the areal calculation mercury adsorbance between integration breakthrough curve and datum line; Its computing formula is
A represents the adsorbance (μ g/g) of carbon-supported catalyst to mercury;
C
0represent datum line mixed gas mercury concentration (ng/L);
C
trepresent mixed gas mercury concentration (ng/L) in test process;
M represents carbon-supported catalyst quality (g);
C represents the curve of mercury concentration changes with time in mixed gas.
Embodiment 2:
Based on method of testing carbon-supported catalyst demercuration performance a kind of in embodiment 1, the present embodiment provides a kind of carbon-supported catalyst demercuration performance testing device, comprises gas distributing system, mercury generating means, fixed bed reactors, mercury shape conversion system and mercury analytic system.
Described gas distributing system comprises generator and the distribution branch road of above-mentioned various gas.The gas of often kind of gas generator generation is converged to together by respective distribution branch road.Gas generator can be used for the flow controlling gas.Described mercury generating means comprises mercury osmos tube, U-tube and thermostatical oil bath.Described mercury osmos tube is positioned at U-tube, and U-tube is positioned at thermostatical oil bath.Described mercury generating means is for providing stable elemental mercury.Mercury is obtained by the mercury osmos tube in mercury generating means, and mercury infiltration capacity raises with oil bath temperature and increases, and namely mercury concentration is controlled by temperature.
Described fixed bed reactors and adsorptive reactor, be specially quartz glass tube, and by tubular furnace temperature control, its diameter is 8 ~ 10mm, and length is 400 ~ 500mm.Described fixed bed reactors can accurate temperature controlling to 0.1 DEG C, can simulate actual condition adsorbent working environment, as all kinds of gas-solid reaction proving installation.
Described mercury shape conversion system comprises heating cabinet and two Drexel bottles, and heating cabinet is used for mixed gas through row heating and insulation, and two Drexel bottles are equipped with 10%SnCl respectively
2solution and 10%NaOH solution.Described mercury analytic system comprises mercury vapor analyzer (Lumex) and common computer.Described mercury vapor analyzer is for detecting Elemental Mercury, and the display of actual measurement mercury concentration curve on computers.
Described mercury generating means is arranged on N
2in distribution branch road.The gas outlet of described gas distributing system is connected with the air intake opening of fixed bed reactors.The gas outlet of described fixed bed reactors is connected with the air intake opening of heating cabinet.Described heating cabinet gas outlet with 10%SnCl is housed
2the air intake opening of the Drexel bottle I of solution connects.The gas outlet of described Drexel bottle I is connected with the air intake opening of the Drexel bottle II that 10%NaOH solution is housed.The gas outlet of described Drexel bottle II is communicated with mercury analytical equipment.
Said apparatus is from gas distributing system to mercury shape conversion system, and whole process carries out air preheat insulation by heat tape, avoids temperature decrease to impact mercury concentration.
During experiment, N
2after flowing through mercury generating means, mercury vapour will be taken out of and together enter in mixed gas.Then mixed gas passes into fixed bed reactors and adsorbs.Mercury analytic system labelling experiment mercury intensity reference line in addition, device under test analog gas exit mercury concentration stabilize enters reactor again and detects after 15ng/L ± 1ng; In testing process when analog gas exit mercury concentration reaches 15ng/L ± 1ng, stop experiment.
Embodiment 3:
Adopt embodiment 1 and the method and apparatus described in embodiment 2 to test, select the carbon-supported catalyst 50mg through vulcanizing treatment, experiment test condition is as follows:
Mixed gas total flow: 1L/min; Fixed bed reaction actuator temperature: 140 DEG C; Mercury concentration: 15ng/L; Oxygen content: 6%; Carbon dioxide content: 13.5%; NO
2concentration: 20ppm; NO concentration: 300ppm; SO
2concentration: 300ppm; HCl concentration: 8ppm; N
2: carrier gas Balance Air.
The carbon-supported catalyst that processed under selecting different technology conditions in test process (all kinds of vulcanizing treatment carbon-supported catalyst preparation process is see the record of the patent document of the patent No. 200810237190.3 " sulfur loading active carbon and preparation method thereof for flue gas demercuration ") is tested, represent untreated carbon-supported catalyst with VAC, AC-x-y represents the sample of vulcanizing treatment y minute under X DEG C of condition.
Utilize this method of testing and proving installation to evaluate the demercuration performance of different carbon-supported catalyst, experimental result is in table 1.
The mercury adsorbance of the different carbon-supported catalyst of table 1
Wherein the content of unit mass adsorbent mercury is higher, illustrates that adsorbent demercuration effect is better.
Claims (4)
1. test a method for carbon-supported catalyst demercuration performance, it is characterized in that, comprise and prepare mixed gas, absorption, aftertreatment and testing process, described method specifically comprises the following steps:
1) be that the carbon-supported catalyst sample of 2 ~ 4mm loads in adsorptive reactor by 50mg granularity;
2) by N
2, CO
2, NO, NO
2, HCl, SO
2, and O
2mixing, N
2mercuryvapour is brought into mixed gas through mercury osmos tube before mixing; Obtained mixed gas is by 20ppmNO
2, 300ppmNO, 5 ~ 10ppmHCl, 300ppmSO
2, 6%O
2, 13.5%CO
2, 15 ± 1ng/L mercury and N
2composition, wherein N
2as balanced gas;
3) obtained mixed gas is heated to 100 ~ 150 DEG C; Then pass into adsorptive reactor, the total flow of mixed gas is 1L/min, and adsorption reaction actuator temperature is 140 DEG C;
4) through step 3) process after mixed gas pass into heating cabinet, after 100 DEG C are heated to it be incubated;
5) through step 4) process after mixed gas pass into 10%SnCl successively
2solution and 10%NaOH solution;
6) to through step 5) mixed gas after process carries out detections analysis; Twin-beam cold-vapour atomic absorption method is adopted to measure and pass through the areal calculation mercury adsorbance between integration breakthrough curve and datum line; Its computing formula is
A represents the adsorbance (μ g/g) of carbon-supported catalyst to mercury;
C
0represent datum line mixed gas mercury concentration (ng/L);
C
trepresent mixed gas mercury concentration (ng/L) in test process;
M represents carbon-supported catalyst quality (g);
C represents the curve of mercury concentration changes with time in mixed gas.
2. a kind of method of testing carbon-supported catalyst demercuration performance according to claim 1, a kind of carbon-supported catalyst demercuration performance testing device is provided, it is characterized in that: comprise gas distributing system, mercury generating means, fixed bed reactors, mercury shape conversion system and mercury analytic system;
Described gas distributing system comprises generator and the distribution branch road of above-mentioned various gas; Described mercury generating means comprises mercury osmos tube, U-tube and thermostatical oil bath; Described mercury osmos tube is positioned at U-tube, and U-tube is positioned at thermostatical oil bath; Described fixed bed reactors and adsorptive reactor; Described mercury shape conversion system comprises heating cabinet and two Drexel bottles, and two Drexel bottles are equipped with 10%SnCl respectively
2solution and 10%NaOH solution; Described mercury analytic system comprises mercury vapor analyzer and common computer;
Described mercury generating means is arranged on N
2in distribution branch road; The gas outlet of described gas distributing system is connected with the air intake opening of fixed bed reactors; The gas outlet of described fixed bed reactors is connected with the air intake opening of heating cabinet; Described heating cabinet gas outlet with 10%SnCl is housed
2the air intake opening of the Drexel bottle I of solution connects; The gas outlet of described Drexel bottle I is connected with the air intake opening of the Drexel bottle II that 10%NaOH solution is housed; The gas outlet of described Drexel bottle II is communicated with mercury analytical equipment.
3. a kind of carbon-supported catalyst demercuration performance testing device according to claim 2, is characterized in that: described fixed bed reactors can accurate temperature controlling to 0.1 DEG C, can simulate actual condition adsorbent working environment, as all kinds of gas-solid reaction proving installation.
4. a kind of carbon-supported catalyst demercuration performance testing device according to claim 2, is characterized in that: this device is from gas distributing system to mercury shape conversion system, and whole process carries out air preheat insulation by heat tape.
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Cited By (3)
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| CN113155695A (en) * | 2021-01-28 | 2021-07-23 | 徐州工程学院 | Device and method for testing mercury removal efficiency of adsorbent |
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