CN108333290A - A kind of test device and test method of cement kiln low-temperature denitration of flue gas catalyst sulfur resistive water resistance - Google Patents
A kind of test device and test method of cement kiln low-temperature denitration of flue gas catalyst sulfur resistive water resistance Download PDFInfo
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- CN108333290A CN108333290A CN201810342215.XA CN201810342215A CN108333290A CN 108333290 A CN108333290 A CN 108333290A CN 201810342215 A CN201810342215 A CN 201810342215A CN 108333290 A CN108333290 A CN 108333290A
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- catalyst
- air admission
- gas
- admission unit
- flue gas
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- 239000003054 catalyst Substances 0.000 title claims abstract description 206
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000003546 flue gas Substances 0.000 title claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000012360 testing method Methods 0.000 title claims abstract description 34
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000004568 cement Substances 0.000 title claims abstract description 25
- 239000011593 sulfur Substances 0.000 title claims abstract description 24
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 24
- 238000010998 test method Methods 0.000 title abstract description 9
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000007789 gas Substances 0.000 claims abstract description 117
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 101
- 238000006243 chemical reaction Methods 0.000 claims abstract description 77
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 71
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 71
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 52
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 34
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 30
- 239000001301 oxygen Substances 0.000 claims abstract description 30
- 238000004868 gas analysis Methods 0.000 claims abstract description 8
- 239000000428 dust Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 14
- 238000010521 absorption reaction Methods 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 229910052593 corundum Inorganic materials 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 229910052682 stishovite Inorganic materials 0.000 claims description 9
- 229910052905 tridymite Inorganic materials 0.000 claims description 9
- 238000010926 purge Methods 0.000 claims description 7
- 238000006555 catalytic reaction Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000000443 aerosol Substances 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 2
- 239000010935 stainless steel Substances 0.000 abstract description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 22
- 208000005374 Poisoning Diseases 0.000 description 18
- 231100000572 poisoning Toxicity 0.000 description 18
- 230000000607 poisoning effect Effects 0.000 description 18
- 239000002131 composite material Substances 0.000 description 13
- 229910000616 Ferromanganese Inorganic materials 0.000 description 11
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 9
- 238000000605 extraction Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 7
- 239000011572 manganese Substances 0.000 description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000004088 foaming agent Substances 0.000 description 3
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 208000005735 Water intoxication Diseases 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- HNBFUFIYQWYCDM-UHFFFAOYSA-N oxygen(2-) sulfane titanium(4+) Chemical compound [O--].[O--].S.[Ti+4] HNBFUFIYQWYCDM-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
Abstract
The present invention relates to a kind of cement kiln test devices and test method of low-temperature denitration of flue gas catalyst sulfur resistive water resistance.The test device, including air distribution system, catalyst reaction system, flue gas analysis and exhaust treatment system；The nitrogen air admission unit, oxygen air admission unit, nitric oxide air admission unit, sulfur dioxide air admission unit are respectively connected with gas mixer；Gas mixer is connected with hydrogen-catalyst reactor；Ammonia air admission unit is connect with hydrogen-catalyst reactor；Nitrogen air admission unit is also connected with water vapor generation device, and water vapor generation device with hydrogen-catalyst reactor by connecting；The catalyst reaction system includes hydrogen-catalyst reactor, temperature control equipment and tubular heater.The present invention can effectively prevent the catalytic of stainless steel tube to error caused by experiment, improve the accuracy of test result.
Description
Technical field
The present invention relates to the test devices and test method of a kind of sulfur resistive of catalyst and water intoxication performance, specially a kind of
The test device and test method of the sulfur resistive water resistance of cement kiln low-temperature denitration of flue gas catalyst.
Background technology
Nitrogen oxides (NOx) it is one of major pollutants in air, with NO and NO2Proportion is maximum.Nitrogen oxides meeting
Huge harm is generated to human body and environment.Selective catalytic reduction (SCR) technique is current control stationary source nitrogen oxides row
The major technique put, at present, industrially most widely used is with medium temperature (300 DEG C -400 DEG C) active V2O5-WO3/
TiO2Catalyst, in order to utilize flue-gas temperature, V2O5-WO3/TiO2Catalyst is usually arranged in before dedusting and desulfurizer, and
Low-temperature SCR reactor uses tail portion arrangement form, flue gas by eliminated after desulfurization and dust-extraction unit most dust and
SO2, avoid erosion of the high concentrate dust to catalyst.But can also there are certain density dust and low concentration SO in flue gas2,
Can still catalyst poisoning be made to inactivate, it is difficult to realize industrial applications.Currently, the test device of denitrating catalyst is mostly active testing
Device, Chinese invention patent CN105628858A discloses a kind of catalyst test system, but the system passes through simultaneously to catalysis
Be passed through in agent reaction system the denitration efficiency of the method evaluation power plant denitrating catalyst of all reaction gas, the escaping of ammonia rate and
SO2/SO3Conversion ratio does not control SO2The break-make of gas and vapor in catalytic reaction process to resist tested catalyst
The poisoning performance of sulphur and water is evaluated.It is different from power-plant flue gas feature simultaneously, cement kiln flue gas feature big, dust for exhaust gas volumn
Concentration height, dust particles carefully glue, dust main component is CaO, SiO2And Al2O3The features such as, there is presently no simulate practical water
The device and method that stall smoke characteristic can test cement kiln with low-temperature denitration catalyst anti-toxicity.
Invention content
The purpose of the present invention is to provide a kind of cement kiln low-temperature denitration catalyst for deficiency present in current techniques
The test device and test method of sulfur resistive water resistance.The thin and viscous feature of, particle high for dust concentration in cement kiln flue gas,
It, can essence after catalyst for denitrating flue gas is arranged in desulfation dust-extraction device by the present invention, and using 150 DEG C or so of operating temperature
Really cement kiln practical flue gas environment of the simulation after dust-extraction unit.And it is controlled with mass flowmenter using gas circulation control valve
SO processed2Gas and vapor break-make and uninterrupted in catalytic reaction process, and pass through various concentration at a constant temperature
SO2The situation of change that catalyst denitration efficiency is tested after being passed through of gas and vapor is come effectively, accurately to low-temperature denitration
The sulfur resistive water resistant poisoning performance of catalyst is evaluated.
The present invention adopts the following technical scheme that：
A kind of test device of cement kiln low-temperature denitration of flue gas catalyst sulfur resistive water resistance, including air distribution system, urge
Agent reaction system, flue gas analysis and exhaust treatment system；
The air distribution system includes nitrogen air admission unit, oxygen air admission unit, nitric oxide air admission unit, sulfur dioxide
Air admission unit, ammonia air admission unit, water vapor generation device, gas mixer and dust generator；
The nitrogen air admission unit is nitrogen cylinder；The oxygen air admission unit is oxygen bottle；One oxygen
Change nitrogen air admission unit is nitric oxide gas steel cylinder；Sulfur dioxide air admission unit is sulfur dioxide gas steel cylinder；Ammonia air inlet list
Member is ammonia steel cylinder；
The dust generator is dust aerosol generator；
The nitrogen air admission unit, oxygen air admission unit, nitric oxide air admission unit, sulfur dioxide air admission unit are divided equally
It is not connected with gas mixer；Gas mixer is connected with hydrogen-catalyst reactor；Ammonia air admission unit and catalyst reaction
Device connects；Nitrogen air admission unit is also connected with water vapor generation device, and water vapor generation device with hydrogen-catalyst reactor by connecting
It connects；
The catalyst reaction system includes hydrogen-catalyst reactor, temperature control equipment and tubular heater；Described
Hydrogen-catalyst reactor is crystal reaction tube, and is positioned in the through-hole of tubular heater；Tubular heater is connected with temperature control device,
The temperature control device is temperature controller；Hydrogen-catalyst reactor is for placing tested catalyst；
The flue gas analysis and exhaust treatment system includes ammonia absorption device, flue gas analyzer and tail gas absorption dress
It sets；The hydrogen-catalyst reactor is connected by ammonia absorption device with flue gas analyzer, and the ammonia absorption device is acid
Liquid bottle；
The device for absorbing tail gas is lye pond.
The nitrogen air admission unit is also aoxidized with oxygen air admission unit, one by respective gas circulation control valve respectively
The pipeline that nitrogen air admission unit, sulfur dioxide air admission unit lead to gas mixer is connected.
The test method of the cement kiln test device of low-temperature denitration of flue gas catalyst sulfur resistive water resistance, including
Following steps：
Tested catalyst is positioned in hydrogen-catalyst reactor, nitrogen air admission unit is opened, into catalyst reaction system
It is passed through nitrogen, by pressure stability in 0.3-0.4MPa, stablizes and keeps 5-15min；Then oxygen air admission unit, an oxidation are opened again
Nitrogen air admission unit makes oxygen and nitric oxide gas are passed into hydrogen-catalyst reactor after gas mixer；Ammonia is opened again
Gas air admission unit, ammonia is passed into hydrogen-catalyst reactor, and gas group becomes 800ppmNO, 800ppmNH3, 5% (volume hundred
Divide ratio) O2, N2As Balance Air, total gas flow rate 1000mL/min, gas space velocity ratio is 30000h-1；Open dust
Device is passed through a concentration of 60mg/m into catalyst reaction system3, granular size be 5~20 microns, main component CaO, SiO2
And Al2O3Dust, stablize keep 0.5 hour；Hydrogen-catalyst reactor 17 is heated to 150 DEG C followed by temperature control equipment,
10 DEG C/min of heating rate stablizes after being kept for 0.5-1.0 hours, is carried out to tested catalyst NOx conversion rate with flue gas analyzer
It measures and records；After 1h, opens sulfur dioxide air admission unit and be passed through 200ppmSO into the hydrogen-catalyst reactor2, every
30min flue gas analyzers acquire a data and record, and stop being passed through SO after reacting 7-8h2, flue gas analyzer is used after 30min
Data of acquisition simultaneously record；Curve is drawn according to the data of acquisition.
After the test, the pipeline of nitric oxide and sulfur dioxide is purged with nitrogen.
Mass percentage composition is 55%CaO+25%SiO in the dust2+ 20%Al2O3。
The present invention substantive distinguishing features be：
Denitrating catalyst patent is all thermoelectricity station-service denitrating catalyst at present, and catalyst for denitrating flue gas used is mostly VWTi systems
Catalyst, this kind of catalyst activity temperature range are 320~450 DEG C, are usually arranged to meet this active temperature section
Between economizer and air preheater；But this region flue-gas temperature is high, and the SO containing a large amount of flying dust and high concentration2, from
And lead to the easy poisoning and deactivation of SCR catalyst, seriously affect its service life.The present invention according to the practical smoke characteristic of cement kiln with
The difference of power-plant flue gas feature after catalyst for denitrating flue gas is arranged in desulfation dust-extraction device, can make catalyst from height
The SO of concentration2Murder by poisoning；Also, compared with power plant's denitrating catalyst, cement kiln with catalyst for denitrating flue gas operating temperature compared with
It is low, usually (80-180 DEG C).For this feature, the difference of operating steps of the present invention is mainly reflected in lower
Under steady temperature (150 DEG C), by being passed through SO into reaction system2And H2The variation of nitric oxide conversion ratio comes to catalyst after O
Anti-toxicity can be evaluated.
Advantageous effect of the present invention：
Can still exist although low-temperature denitration catalyst is arranged in after dedusting and desulfurizer, in flue gas certain density
Dust and low concentration SO2, can still make denitrating catalyst poisoning and deactivation, therefore to the denitrating catalyst sulfur resistive in practical flue gas environment
Water resistant poisoning performance, which carries out effectively evaluating, has great importance to its practical application in industry.The present invention provides a kind of cement kiln
With the anti-SO of low-temperature denitration catalyst2And H2The test device and test method of O poisoning performances.It is dense for dust in cement kiln flue gas
Degree is high, particle is thin and viscous feature, the present invention can generate a concentration of 60mg/m using dust generator3, granular size 10
Microns, main component CaO, SiO2And Al2O3Dust, can accurately simulate the practical cigarette of the cement kiln after dust-extraction unit
Compression ring border.And control valve is circulated with mass flowmenter to control SO by gas2Gas and vapor are in catalytic reaction process
Middle break-make and uninterrupted, and pass through the SO of various concentration at a constant temperature2Gas and being passed through for vapor are catalyzed to tested
The influence situation of agent denitration efficiency is next effectively, accurately evaluates the sulfur resistive water resistant poisoning performance of low-temperature denitration catalyst.
After reacting 1h i.e. at 150 DEG C, if being individually passed through 200ppm SO to catalyst reaction system2Afterwards, tested catalyst remains to keep
85% or more conversion rate of NOx；After being individually passed through 10% vapor, tested catalyst remains to keep 90% or more NOx conversion
Rate；It is passed through 200ppm SO simultaneously2After 10% vapor, tested catalyst remains to the conversion rate of NOx of 80% or more holding then
The denitrating catalyst has excellent sulfur resistive water resistant poisoning performance.And hydrogen-catalyst reactor uses crystal reaction tube, Ke Yiyou
Effect prevents the catalytic of stainless steel tube to error caused by experiment, improves the accuracy of test result.After reaction, nitrogen is utilized
Gas purges reaction gas pipeline, and nitrogen oxides and sulfur dioxide is effectively prevent to cause to corrode to pipeline.
Description of the drawings
Fig. 1 is denitrating catalyst sulfur resistive water repelling property evaluating apparatus figure.
Fig. 2 is gas mixer figure；
Fig. 3 is to be passed through 200ppmSO in embodiment 12It is tested the conversion rate of NOx of catalyst afterwards
Fig. 4 is to be passed through 10%H in embodiment 22The conversion rate of NOx of catalyst is tested after O；
Fig. 5 is to be passed through 10%H in embodiment 32O+200ppmSO2It is tested the conversion rate of NOx of catalyst afterwards.
Fig. 6 is to be passed through 200ppmSO in embodiment 42It is tested the conversion rate of NOx of catalyst afterwards；
Fig. 7 is to be passed through 10%H in embodiment 52The conversion rate of NOx of catalyst is tested after O；
Fig. 8 is to be passed through 10%H in embodiment 62O+200ppmSO2It is tested the conversion rate of NOx of catalyst afterwards.
Fig. 9 is to be passed through 200ppmSO in embodiment 72It is tested the conversion rate of NOx of catalyst afterwards；
Figure 10 is to be passed through 10%H in embodiment 82The conversion rate of NOx of catalyst is tested after O；
Figure 11 is to be passed through 10%H in embodiment 92O+200ppmSO2It is tested the conversion rate of NOx of catalyst afterwards.
Specific implementation mode
As shown in Figure 1, a kind of test device of cement kiln with low-temperature denitration of flue gas catalyst sulfur resistive water resistance, including match
Gas system, catalyst reaction system, flue gas analysis and exhaust treatment system.
The air distribution system includes nitrogen air admission unit 1, oxygen air admission unit 2, nitric oxide air admission unit 3, dioxy
Change sulphur air admission unit 4, ammonia air admission unit 5, water vapor generation device 6, gas mixer 7 and dust generator 23；
The nitrogen air admission unit is nitrogen cylinder；The oxygen air admission unit is oxygen bottle；One oxygen
Change nitrogen air admission unit is nitric oxide gas steel cylinder；Sulfur dioxide air admission unit is sulfur dioxide gas steel cylinder；Ammonia air inlet list
Member is ammonia steel cylinder；
The dust generator is DG-100 type dust aerosol generators, which can generate a concentration of
60mg/m3, granular size be 10 microns dust, can accurately simulate the practical flue gas ring of the cement kiln after dust-extraction unit
Border.
The nitrogen air admission unit 1, oxygen air admission unit 2, nitric oxide air admission unit 3, sulfur dioxide air admission unit 4
Respectively pass through gas circulation control valve 7-1,7-2,7-3,7-4, pressure reducing valve 8,9,10,11 and the gas mixing on respective pipeline
Device 7 is connected.Above-mentioned four kinds of gas is passed into through gas mixer 7 in hydrogen-catalyst reactor 17 after mixing.Gas is mixed
The flow quantity control valve and mass flowmenter set and include above-mentioned four kinds of gas in 7 are attached together, is controlled by gas mixer above-mentioned several
The uninterrupted and break-make of kind gas.Ammonia air admission unit 5 is by pipeline successively through pressure reducing valve 12, gas circulation control valve
13, gas mass flow gauge 14 is connect with hydrogen-catalyst reactor 17；Nitrogen air admission unit 1 is also filled by pipeline and vapor
Set 6 be connected, water vapor generation device 6 by pipeline successively through gas circulate control valve 15, gas mass flow gauge 16 with
Hydrogen-catalyst reactor 17 connects.
As shown in Fig. 2, the nitrogen air admission unit 1, oxygen air admission unit 2, nitric oxide air admission unit 3, titanium dioxide
Sulphur air admission unit 4 respectively by gas circulation control valve 7-1,7-2 on respective pipeline, 7-3,7-4, pressure reducing valve 8,9,10,
11 are connected with gas mixer 7.The nitrogen air admission unit 1 also passes through gas circulation control valve 7-9,7-10,7-11 points
The pipeline of gas mixer 7 is not led to oxygen air admission unit 2, nitric oxide air admission unit 3, sulfur dioxide air admission unit 4
It is connected.The gas mixer 7 include gas circulation control valve 7-1,7-2,7-3,7-4 and mass flowmenter 7-5,7-6,
7-7,7-8 control the break-make and uninterrupted of nitrogen, oxygen, nitric oxide and sulfur dioxide gas respectively.After reaction,
It opens gas circulation control valve 7-9,7-10,7-11 to purge other three kinds of gas pipings using nitrogen, prevents nitrogen oxygen
Compound and sulfur dioxide cause to corrode to pipeline.
Catalyst reaction system includes hydrogen-catalyst reactor 17, temperature control equipment 18 and tubular heater 19；Described
Hydrogen-catalyst reactor 17 is the crystal reaction tube of a diameter of 2.8cm, and is positioned in the through-hole of tubular heater 19, and catalyst is anti-
Answer device 17 for placing tested catalyst.Tubular heater 19 is connected by conducting wire with temperature control device 18, the temperature control device
18 be WP-80 temperature controllers.And control flue gas temperature and heating rate using temperature control device 18.
The flue gas analysis and exhaust treatment system includes ammonia absorption device 20, flue gas analyzer 21 and tail gas absorption
Device 22；
The hydrogen-catalyst reactor 17 is connected by pipeline with flue gas analyzer 21, and the flue gas analyzer 21 is
KM940 formula flue gas analyzers.And it is equipped with ammonia absorption device 20 among hydrogen-catalyst reactor 17 and flue gas analyzer 21, is used for
Prevent corrosion of the remaining ammonia to flue gas analyzer after reacting.The ammonia absorption device 20 is acid solution bottle (phosphoric acid, concentration
For 2mol/L).NOx concentration after being reacted catalysis using flue gas analyzer 21 is recorded and analyzed.And by steady temperature
Under, SO is passed through into catalytic reactor2Come with the situation of change for being tested catalyst NOx conversion rate before and after vapor anti-to its sulfur resistive
It is aqueous to be evaluated.Simulated flue gas is passed into after the analysis record of flue gas analyzer 21 in device for absorbing tail gas 22, and reduction is urged
Change remaining NO and NH after reacting3The pollution caused by air.
The device for absorbing tail gas 22 is lye pond (sodium hydroxide, a concentration of 2mol/L).
Present invention catalyst group to be measured becomes mn-ni compound oxide catalyst, ferromanganese composite oxide catalysts and pure
Manganese oxide catalyst, catalyst to be measured are prepared by coprecipitation, manganese acetate (Mn (CH3COO)2·4H2O), nickel nitrate
(Ni(NO3)2·6H2) and ferric nitrate (Fe (NO O3)3·9H2O) it is precursor salt, precipitating reagent is ammonium hydroxide, Mn/Ni and Mn/Fe's
Molar ratio is 4:1, Mn2+A concentration of 0.5mol/L.
Mn-ni compound oxide catalyst specific make step is as follows：
1) by 12.25g manganese acetates (Mn (CH3COO)2·4H2) and 3.625g nickel nitrates (Ni (NO O3)2·6H2O it) is dissolved in
In 100ml deionized waters, magnetic agitation 20min, wiring solution-forming A.
2) ammonium hydroxide of a concentration of 2mol/L is added dropwise in solution A, until PH=8-9, continues to stir 30min.
3) it filters, wash after aging 1h, manganese nickel is made and answers through 80 DEG C of dryings, 450 DEG C of roasting 5h (2 DEG C/min of heating rate)
Close oxide catalyst.
Ferromanganese composite oxide catalysts specific make step is as follows：
Preparation process is identical as mn-ni compound oxide catalyst preparation step, and difference is by 12.25g manganese acetates
(Mn(CH3COO)2·4H2) and 5.05g ferric nitrates (Fe (NO O3)3·9H2O it) is dissolved in 100ml deionized waters, magnetic agitation
20min, wiring solution-forming A.
Pure manganese oxide catalyst specific make step is as follows：
Preparation process is identical as mn-ni compound oxide catalyst preparation step, and difference is by 12.25g manganese acetates
(Mn(CH3COO)2·4H2O it) is dissolved in 100ml deionized waters, magnetic agitation 20min, wiring solution-forming A.
For the thin and viscous feature of dust concentration height, particle in cement kiln flue gas, having newly increased dust generator can be accurate
The practical flue gas environment of cement kiln after dust-extraction unit is simulated, is the innovative point on device.The difference of operating procedure is exactly mainly
By controlling SO in reaction process at a constant temperature2And H2The break-make of O, then by the variation of conversion of nitric oxide gas rate come pair
Catalyst anti-toxicity can be evaluated.
The test method of the device, includes the following steps：
Tested catalyst is positioned in hydrogen-catalyst reactor 17, nitrogen air admission unit 1 is opened, and opens gas circulation control
Valve 7-1 processed is passed through nitrogen into catalyst reaction system, and utilizes nitrogen pressure reducing valve 8 by pressure stability in 0.4MPa (0.3-
0.4MPa provides range) stablize holding 5-15min；Open oxygen air admission unit 2, nitric oxide air admission unit 3, make oxygen and
Nitric oxide gas is passed into after gas mixer 7 in hydrogen-catalyst reactor 17；Ammonia air admission unit 5 is opened again, by ammonia
Gas is passed into hydrogen-catalyst reactor 17, and gas group becomes 800ppm NO, 800ppm NH3, 5% (percent by volume) O2, N2Make
For Balance Air, total gas flow rate 1000mL/min, gas space velocity ratio is 30000h-1；Dust generator 23 is opened, to catalyst
A concentration of 60mg/m is passed through in reaction system3, granular size be 10 microns, main component CaO, SiO2And Al2O3Powder
Dirt (55%CaO+25%SiO2+ 20%Al2O3It is mass percent), stablize and is kept for 1 hour.It controls and fills followed by temperature
It sets 18 and hydrogen-catalyst reactor 17 is heated to 150 DEG C, 10 DEG C/min of heating rate, stablize after being kept for half an hour, use flue gas analysis
Instrument 21 is measured and records to tested catalyst NOx conversion rate.After 1h, opens sulfur dioxide air admission unit 4 and urged to described
It is passed through 200ppmSO in agent reactor 172, acquire a data every 30min flue gas analyzers 21 and record, react
Stop being passed through SO after 7.5h2, a data are acquired with KM940 type flue gas analyzers after 30min and are recorded.According to the data of acquisition
Draw curve；
After test, purging 10min is carried out to the pipeline of nitric oxide and sulfur dioxide with nitrogen.
Embodiment 1
2ml is tested catalyst to be positioned in hydrogen-catalyst reactor 17, opens nitrogen air admission unit 1, and open gas stream
Logical control valve 7-1 is slowly introducing nitrogen into catalyst reaction system, and pressure stability is existed using nitrogen pressure reducing valve 8
0.4MPa or so stablizes after keeping 10min, is hunted leak to all seal points with the method for brushing neutral foaming agent, leak test closes
After lattice, next step experiment can be carried out.
Oxygen air admission unit 2, nitric oxide air admission unit 3 are opened, and opens gas circulation control valve 7-2,7-3, makes oxygen
Gas and nitric oxide gas are passed into after pressure reducing valve 9,10 and gas mixer 7 in hydrogen-catalyst reactor 17, open ammonia
Air admission unit 5 is passed into after pressure reducing valve 12, gas circulation control valve 13, mass flowmenter 14 in hydrogen-catalyst reactor 17,
Gas group becomes 800ppmNO, 800ppm NH3, 5% (percent by volume) O2, N2As Balance Air, total gas flow rate is
1000mL/min, gas space velocity ratio are 30000h-1.Dust generator 23 is opened, is passed through into catalyst reaction system a concentration of
60mg/m3, granular size be 10 microns, main component CaO, SiO2And Al2O3Dust, stablize keep 1 hour.With
Hydrogen-catalyst reactor 17 is heated to 150 DEG C, 10 DEG C/min of heating rate using temperature control equipment 18 afterwards, it is small to stablize holding half
Shi Hou is measured and is recorded to tested catalyst NOx conversion rate with KM940 types flue gas analyzer 21.After 1h, titanium dioxide is opened
Sulphur air admission unit 4 and gas circulation control valve 7-4, through pressure reducing valve 11, gas mixer 7 to the hydrogen-catalyst reactor 17
In be passed through 200ppmSO2, acquire a data every 30min KM940 types flue gas analyzers 21 and record, closed after reacting 7.5h
Hold one's breath body circulation control valve 7-4, and stopping is passed through SO2, a data are acquired with KM940 type flue gas analyzers after 30min and are recorded.
Curve is drawn according to the data of acquisition, as shown in figure 3, being passed through 200ppmSO into catalyst reaction system2Afterwards, manganese nickel composite oxygen
The conversion rate of NOx of compound catalyst remains to maintain 87% or so, is higher than 85%.So mn-ni compound oxide catalyst has
Excellent anti-SO2Poisoning capability.It can be by being passed through 200ppmSO into catalyst reaction system2The NOx of front and back tested catalyst
The variation of conversion ratio comes to its anti-SO2Poisoning performance is evaluated.After test, gas circulation control valve 7-10,7- are opened
11, purging 10min is carried out to the pipeline of nitric oxide and sulfur dioxide using nitrogen.
Embodiment 2
2ml is tested catalyst to be positioned in hydrogen-catalyst reactor 17, opens nitrogen air admission unit 1, and open gas stream
Logical control valve 7-1 is slowly introducing nitrogen into catalyst reaction system, and pressure stability is existed using nitrogen pressure reducing valve 8
0.4MPa or so stablizes after keeping 10min, is hunted leak to all seal points with the method for brushing neutral foaming agent, leak test closes
After lattice, next step experiment can be carried out.
Oxygen air admission unit 2, nitric oxide air admission unit 3 are opened, and opens gas circulation control valve 7-2,7-3, makes oxygen
Gas and nitric oxide gas are passed into after pressure reducing valve 9,10 and gas mixer 7 in hydrogen-catalyst reactor 17, open ammonia
Air admission unit 5 is passed into after pressure reducing valve 12, gas circulation control valve 13, mass flowmenter 14 in hydrogen-catalyst reactor 17,
Ammonia air admission unit 5 is opened, it is anti-to be passed into catalyst after pressure reducing valve 12, gas circulation control valve 13, mass flowmenter 14
It answers in device 17, gas group becomes 800ppmNO, 800ppmNH3, 5% (percent by volume) O2, N2As Balance Air, gas always flows
Amount is 1000mL/min, and gas space velocity ratio is 30000h-1.Dust generator 23 is opened, is passed through into catalyst reaction system dense
Degree is 60mg/m3, granular size be 10 microns, main component CaO, SiO2And Al2O3Dust, stablize and keep 1 small
When.Hydrogen-catalyst reactor 17 is heated to 150 DEG C, 10 DEG C/min of heating rate followed by temperature control equipment 18, stablizes and protects
After holding half an hour, with KM940 types flue gas analyzer 21 to being tested catalyst n OxConversion ratio is measured and records.After 1h, open
Gas circulation control valve 15 is taken the vapor that water vapor generation device 6 generates out of by nitrogen, it is controlled through mass flowmenter 16
It is passed into after actual flow velocity in hydrogen-catalyst reactor 17, a data is acquired simultaneously every 30min KM940 types flue gas analyzers 21
Record closes gas circulation control valve 15 after reacting 7.5h, and stopping is passed through water vapour, KM940 type flue gas analyzers are used after 30min
21 data of acquisition simultaneously record.Curve is drawn according to the data of acquisition, as shown in figure 4, being passed through into catalyst reaction system
10%H2After O, the conversion rate of NOx of mn-ni compound oxide catalyst remains to maintain 92% or so, is higher than 90%.So manganese nickel
Composite oxide catalysts have excellent water resistant poisoning capability.It can be by being passed through 10%H into catalyst reaction system2O
The NO of front and back tested catalystxIts water resistant poisoning performance is evaluated in the variation of conversion ratio.After test, gas is opened
Circulation control valve 7-10,7-11 carry out purging 10min using nitrogen to the pipeline of nitric oxide and sulfur dioxide.
Embodiment 3
2ml is tested catalyst to be positioned in hydrogen-catalyst reactor 17, opens nitrogen air admission unit 1, and open gas stream
Logical control valve 7-1 is slowly introducing nitrogen into catalyst reaction system, and pressure stability is existed using nitrogen pressure reducing valve 8
0.4MPa or so stablizes after keeping 10min, is hunted leak to all seal points with the method for brushing neutral foaming agent, leak test closes
After lattice, next step experiment can be carried out.
Oxygen air admission unit 2, nitric oxide air admission unit 3 are opened, and opens gas circulation control valve 7-2,7-3, makes oxygen
Gas and nitric oxide gas are passed into after pressure reducing valve 9,10 and gas mixer 7 in hydrogen-catalyst reactor 17, open ammonia
Air admission unit 5 is passed into after pressure reducing valve 12, gas circulation control valve 13, mass flowmenter 14 in hydrogen-catalyst reactor 17,
Ammonia air admission unit 5 is opened, it is anti-to be passed into catalyst after pressure reducing valve 12, gas circulation control valve 13, mass flowmenter 14
It answers in device 17, gas group becomes 800ppmNO, 800ppmNH3, 5% (percent by volume) O2, N2As Balance Air, gas always flows
Amount is 1000mL/min, and gas space velocity ratio is 30000h-1.Dust generator 23 is opened, is passed through into catalyst reaction system dense
Degree is 60mg/m3, granular size be 10 microns, main component CaO, SiO2And Al2O3Dust, stablize and keep 1 small
When.Hydrogen-catalyst reactor 17 is heated to 150 DEG C, 10 DEG C/min of heating rate followed by temperature control equipment 18, stablizes and protects
After holding half an hour, with KM940 types flue gas analyzer 21 to being tested catalyst n OxConversion ratio is measured and records.After 1h, open
Sulfur dioxide air admission unit 4 and gas circulation control valve 7-4 are anti-to the catalyst through pressure reducing valve 11, gas mixer 7
It answers in device 17 and is passed through 200ppmSO2, and open gas circulation control valve 15, the vapor that water vapor generation device 6 is generated by
Nitrogen is taken out of, is passed into hydrogen-catalyst reactor 17 after mass flowmenter 16 controls its actual flow velocity, is used every 30min
KM940 types flue gas analyzer 21 acquires a data and records, and gas circulation control valve 7-4 and gas are closed after reacting 7.5h
Body circulation control valve 15, stopping are passed through SO2+ 10%H2A data are acquired with KM940 type flue gas analyzers and remember after O, 30min
Record.Curve is drawn according to the data of acquisition, as shown in figure 5, being passed through 200ppmSO into catalyst reaction system2+ 10%H2After O,
The NO of mn-ni compound oxide catalystxConversion ratio remains to maintain 81% or so, is higher than 80%.So mn-ni compound oxide
Catalyst has excellent sulfur resistive water resistant poisoning capability.By being passed through 200ppmSO into catalyst reaction system2+ 10%H2Before O
It is tested the variation of the conversion rate of NOx of catalyst afterwards to evaluate its sulfur resistive and water resistant poisoning performance.After test, open
Gas circulation control valve 7-10,7-11 carry out purging 10min using nitrogen to the pipeline of nitric oxide and sulfur dioxide.
Embodiment 4
Other steps are changed to ferromanganese composite oxide catalysts with embodiment 1, difference for catalyst, as shown in fig. 6,
It is passed through 200ppmSO into catalyst reaction system2Afterwards, the NO of ferromanganese composite oxide catalystsxConversion ratio remains to maintain
86% or so, it is higher than 85%.So ferromanganese composite oxide catalysts have excellent anti-SO2Poisoning capability.
Embodiment 5
Other steps are changed to ferromanganese composite oxide catalysts with embodiment 2, difference for catalyst, as shown in fig. 7,
It is passed through 10%H into catalyst reaction system2After O, the NO of ferromanganese composite oxide catalystsxConversion ratio remains to maintain 93%
Left and right is higher than 90%.So ferromanganese composite oxide catalysts have excellent water resistant poisoning capability.
Embodiment 6
Other steps are changed to ferromanganese composite oxide catalysts with embodiment 3, difference for catalyst, as shown in figure 8,
It is passed through 200ppmSO into catalyst reaction system2+ 10%H2After O, the conversion rate of NOx of ferromanganese composite oxide catalysts remains to
82% or so is maintained, is higher than 80%.So ferromanganese composite oxide catalysts have excellent sulfur resistive water resistant poisoning capability.
Embodiment 7
Other steps are with embodiment 1, and difference is that catalyst is changed to pure manganese oxide catalyst, as shown in figure 9, to urging
It is passed through 200ppmSO in agent reaction system2Afterwards, the NO of pure manganese oxide catalystxConversion ratio drops to 63% or so, significantly low
In 85%.So the anti-SO of pure manganese oxide catalyst2Poisoning capability is weaker.
Embodiment 8
For other steps with embodiment 2, difference is that catalyst is changed to pure manganese oxide catalyst, as shown in Figure 10, to
It is passed through 10%H in catalyst reaction system2After O, the NO of pure manganese oxide catalystxConversion ratio drops to 78% or so, is less than
90%.So the water resistant poisoning capability of pure manganese oxide catalyst is weaker.
Embodiment 9
For other steps with embodiment 3, difference is that catalyst is changed to pure manganese oxide catalyst, as shown in figure 11, to
It is passed through 200ppmSO in catalyst reaction system2+ 10%H2After O, the conversion rate of NOx of pure manganese oxide catalyst drops to 55%
Left and right, hence it is evident that be less than 80%.So the sulfur resistive water resistant poisoning capability of pure manganese oxide catalyst is weaker.
Unaccomplished matter of the present invention is known technology.
Claims (5)
1. a kind of cement kiln test device of low-temperature denitration of flue gas catalyst sulfur resistive water resistance, it is characterized in that the device includes
Air distribution system, catalyst reaction system, flue gas analysis and exhaust treatment system；
The air distribution system includes nitrogen air admission unit, oxygen air admission unit, nitric oxide air admission unit, sulfur dioxide air inlet
Unit, ammonia air admission unit, water vapor generation device, gas mixer and dust generator；
The nitrogen air admission unit is nitrogen cylinder；The oxygen air admission unit is oxygen bottle；The nitric oxide
Air admission unit is nitric oxide gas steel cylinder；Sulfur dioxide air admission unit is sulfur dioxide gas steel cylinder；Ammonia air admission unit is
Ammonia steel cylinder；The dust generator is dust aerosol generator；
The nitrogen air admission unit, oxygen air admission unit, nitric oxide air admission unit, sulfur dioxide air admission unit respectively with
Gas mixer is connected；Gas mixer is connected with hydrogen-catalyst reactor；Ammonia air admission unit connects with hydrogen-catalyst reactor
It connects；Nitrogen air admission unit is also connected with water vapor generation device, and water vapor generation device with hydrogen-catalyst reactor by connecting；
The catalyst reaction system includes hydrogen-catalyst reactor, temperature control equipment and tubular heater；The catalysis
Agent reactor is crystal reaction tube, and is positioned in the through-hole of tubular heater；Tubular heater is connected with temperature control device, described
Temperature control device be temperature controller；Hydrogen-catalyst reactor is for placing tested catalyst；
The flue gas analysis and exhaust treatment system includes ammonia absorption device, flue gas analyzer and device for absorbing tail gas；Institute
The hydrogen-catalyst reactor stated is connected by ammonia absorption device with flue gas analyzer, and the ammonia absorption device is acid solution bottle；
The device for absorbing tail gas is lye pond.
2. the cement kiln as described in claim 1 test device of low-temperature denitration of flue gas catalyst sulfur resistive water resistance, special
Sign be the nitrogen air admission unit also by respective gas circulation control valve respectively with oxygen air admission unit, nitric oxide into
The pipeline that gas unit, sulfur dioxide air admission unit lead to gas mixer is connected.
3. the cement kiln as described in claim 1 test of the test device of low-temperature denitration of flue gas catalyst sulfur resistive water resistance
Method, it is characterized in that including the following steps：
Tested catalyst is positioned in hydrogen-catalyst reactor, nitrogen air admission unit is opened, is passed through into catalyst reaction system
Nitrogen is stablized by pressure stability in 0.3-0.4MPa and keeps 5-15min；Then open again oxygen air admission unit, nitric oxide into
Gas unit makes oxygen and nitric oxide gas are passed into hydrogen-catalyst reactor after gas mixer；Open again ammonia into
Gas unit, ammonia is passed into hydrogen-catalyst reactor, and gas group becomes 800 ppm NO, 800 ppm NH3、5%（Volume hundred
Divide ratio）O2, N2As Balance Air, total gas flow rate 1000mL/min, gas space velocity ratio is 30000 h-1；Open dust
Device is passed through a concentration of 60mg/m into catalyst reaction system3, granular size be 5 ~ 20 microns, main component CaO, SiO2With
Al2O3Dust, stablize keep 0.5 hour；Hydrogen-catalyst reactor 17 is heated to 150 DEG C followed by temperature control equipment, is risen
10 DEG C/min of warm rate stablizes after being kept for 0.5-1.0 hours, is surveyed to tested catalyst NOx conversion rate with flue gas analyzer
Determine and records；After 1h, opens sulfur dioxide air admission unit and be passed through 200ppmSO into the hydrogen-catalyst reactor2, every
30min flue gas analyzers acquire a data and record, and stop being passed through SO after reacting 7-8h2, flue gas analyzer is used after 30min
Data of acquisition simultaneously record；Curve is drawn according to the data of acquisition.
4. the cement kiln as claimed in claim 3 test of the test device of low-temperature denitration of flue gas catalyst sulfur resistive water resistance
Method purges the pipeline of nitric oxide and sulfur dioxide with nitrogen it is characterized in that after the test.
5. the cement kiln as described in claim 1 test of the test device of low-temperature denitration of flue gas catalyst sulfur resistive water resistance
Method, it is characterized in that mass percentage composition is 55%CaO+25%SiO in the dust2+20%Al2O3。
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