CN114272949B - M1 type molybdenum molecular sieve denitration catalyst resistant to ABS poisoning at low temperature and preparation method thereof - Google Patents
M1 type molybdenum molecular sieve denitration catalyst resistant to ABS poisoning at low temperature and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 27
- 231100000572 poisoning Toxicity 0.000 title claims abstract description 27
- 230000000607 poisoning effect Effects 0.000 title claims abstract description 27
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 14
- 239000011733 molybdenum Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 3
- 229910019614 (NH4)6 Mo7 O24.4H2 O Inorganic materials 0.000 claims 1
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 16
- 239000003546 flue gas Substances 0.000 abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052717 sulfur Inorganic materials 0.000 abstract description 8
- 239000011593 sulfur Substances 0.000 abstract description 8
- 229910001868 water Inorganic materials 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulfur dioxide Inorganic materials O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a low-temperature anti-ABS poisoning M1 type molybdenum molecular sieve denitration catalyst and a preparation method thereof, wherein the catalyst comprises a molecular sieve structure, and a molecular sieve framework is formed by MoO 6 Octahedra and AO 6 The octahedron is composed of one or more of V, nb, sb, te and the like, and AO 6 Octahedral atomic scale dispersion in MoO 6 In the octahedral molecular sieve framework, AO 6 Octahedron is a catalytic active center, moO 6 The octahedron is an ABS decomposition center, and the pore canal structure of the molecular sieve promotes the decomposition of ABS. The beneficial effects are that: the defect that the traditional SCR catalyst is easy to deactivate due to ABS deposition at low temperature is effectively overcome, the low-temperature stability of the catalyst is improved, and the energy consumption and the cost for catalyst regeneration are reduced. Under the condition of containing water and sulfur at 150-250 ℃, the denitration efficiency of the M1 type molybdenum molecular sieve catalyst can be stably maintained to be more than 80%, and N is 2 The selectivity can reach more than 95 percent, and is suitable for controlling the emission of nitrogen oxides of various industrial source flue gases.
Description
Technical Field
The invention relates to the technical field of air pollution control, in particular to an M1 type molybdenum molecular sieve denitration catalyst resistant to ABS poisoning at low temperature and a preparation method thereof.
Background
Nitrogen oxides (NOx) are the current primary atmospheric pollutants, and involve numerous environmental problems, which are important inducement of acid rain, ozone layer destruction, photochemical smog and greenhouse effect, and are also important precursors of PM2.5, thus bringing serious threat to human health and climate environment. Currently, NOx and ammonia Selective Catalytic Reduction (SCR) technology is one of the most effective, mature and most widely applied emission abatement measures for both stationary and mobile sources of NOx. According to national environmental statistics publication 2011-2015 and Chinese statistics annual authentication 2017, NOx emission in the power industry of China is effectively controlled, wherein the V2O5-WO3/TiO2 catalyst is the most commonly used SCR catalyst in coal-fired power plants. However, the NOx emission of non-electric industries (such as steel coking, glass cement, garbage incineration, etc.) is still in an increasing trend, because the flue gas temperature in the non-electric industries is lower (< 300 ℃), SO2, H2O and NH3 in the flue gas react to generate Ammonium Bisulfate (ABS), ABS is deposited and covered on the surface of the catalyst, and the active site of the catalyst is blocked to deactivate the catalyst, thereby remarkably reducing the service life of the traditional SCR catalyst.
The method for resisting ABS poisoning commonly used in industrial flue gas denitration at present utilizes additional energy to heat and decompose ABS so as to achieve the effect of catalyst regeneration, however, the method has very high energy consumption and cost. Therefore, the research and development of the novel low-temperature anti-ABS poisoning denitration catalyst has great scientific significance and practical value in the fields of environment and energy. Recent progress has been made in developing catalysts having sulfur-resistant properties, and researchers have reduced SO by reducing the redox capacity of the catalyst 2 To reduce SO at the oxidation rate of (2) 3 Thereby suppressing the generation of ABS. However, the reduction of the oxidation-reduction capability of the catalyst also leads to the reduction of the low-temperature activity, and in addition, ABS is slowly accumulated, so that the problem of ABS poisoning of the catalyst cannot be fundamentally solved. The development of high-efficiency denitration catalysts resistant to ABS poisoning at low temperatures still faces a great challenge.
For the problems in the related art, no effective solution has been proposed at present.
Disclosure of Invention
The invention aims to provide an M1 type molybdenum molecular sieve denitration catalyst capable of resisting ABS poisoning at low temperature and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the above object, the present invention provides the followingThe technical scheme is as follows: an M1 type molybdenum molecular sieve denitration catalyst resistant to ABS poisoning at low temperature comprises a molecular sieve structure, wherein a molecular sieve framework is formed by MoO 6 Octahedra and AO 6 The octahedron is composed of one or more of V, nb, sb, te and the like, and AO 6 Octahedral atomic scale dispersion in MoO 6 In the octahedral molecular sieve framework, AO 6 Octahedron is a catalytic active center, moO 6 The octahedron is an ABS decomposition center, and the pore canal structure of the molecular sieve promotes the decomposition of ABS.
Further, the content of V element in the element A is 0.5-15 atom percent relative to Mo, the content of Nb, sb, te and other elements is 0-10 atom percent, the site A is atomically dispersed in the molecular sieve framework, and the relative content of the element A does not influence the integral structure of the molecular sieve.
According to another aspect of the invention, a preparation method of an M1 type molybdenum molecular sieve denitration catalyst resistant to ABS poisoning at low temperature comprises the following steps:
(1) Will (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O is dissolved in ultrapure water to form a clear solution;
(2) Dissolving a required amount of soluble precursor salt of the element A in ultrapure water to prepare a clear solution, wherein a cosolvent (such as oxalic acid, ethanol and the like) is added into part of the precursor salt with low solubility for dissolution;
(3) Mixing the A precursor solution prepared in the step (2) with the Mo precursor solution obtained in the step (1);
(4) Taking the sample in the step (3) to perform a high-temperature hydrothermal reaction for a certain time;
(5) And centrifugally separating, washing, drying, grinding to fine powder, and calcining to obtain the low-temperature anti-ABS poisoning denitration catalyst.
Further, the hydrothermal reaction temperature in the step (4) is 150-250 ℃ and the time is 20-48h.
Further, the low-temperature drying temperature in the step (5) is 80-120 ℃ and the time is 8-12h.
Further, the specific conditions of the calcination in the step (5) are as follows: heating to 400-500 ℃ at the speed of 5-10 ℃/min, preserving heat for 2-6h, and naturally cooling to room temperature.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention makes VO 6 Octahedral atomic scale dispersion in MoO 6 The low-temperature anti-ABS poisoning denitration catalyst is prepared on the molecular sieve framework structure. Wherein the M1 type molybdenum-oxygen molecular sieve has excellent sulfur-resistant and water-resistant poisoning performance and low-temperature ABS decomposition performance, and the low-temperature denitration activity is realized by VO 6 The octahedron provides, so that the catalyst can maintain excellent stability and activity under the condition of medium-low temperature water-containing sulfur-containing flue gas;
2. the invention is compared with commercial V 2 O 5 -WO 3 /TiO 2 The denitration catalyst has better low-temperature SCR catalytic activity and more excellent sulfur and water resistance;
3. the invention adopts a hydrothermal method for preparation, and has simple operation process and high repeatability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the experimental results of the low-temperature anti-ABS poisoning denitration catalysts prepared in examples 1 and 2 of the present invention.
FIG. 2 is a graph showing the second experimental result of the low temperature anti-ABS poisoning denitration catalyst prepared in example 1 of the present invention.
FIG. 3 is a third graph showing the experimental results of the low temperature anti-ABS poisoning denitration catalyst prepared in example 2 of the present invention.
FIG. 4 is a graph showing the experimental results of the VWTi catalyst prepared in example 3 of the present invention against ammonium bisulfate poisoning.
Detailed Description
The invention is further described below with reference to the accompanying drawings and detailed description:
example 1
(1) Will be 3.6 g (NH 4 ) 6 Mo 7 O 24 ·4H 2 O was dissolved in 30mL of ultrapure water;
(2) 0.07 g NH was taken 4 VO 3 And 0.3. 0.3 g cosolvent (oxalic acid) in 30mL of ultrapure water;
(3) Mixing the materials obtained in the step (1) and the step (2), performing hydrothermal reaction at 175 ℃ for 48 hours, centrifuging and washing solid powder after the reaction is finished, and drying the solid powder in an oven overnight;
(4) Grinding the solid to fine powder, pouring the fine powder into a crucible, and putting the crucible into a muffle furnace for sealing and roasting, wherein the sealing and roasting specifically comprises the following steps: heating to 400 ℃ at a speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature to obtain a powder sample.
The SCR denitration performance of the catalyst was evaluated in a fixed bed reactor. The reaction flue gas condition is set to 600 ppm NO,600 ppm NH 3 ，3 vol% O 2 ，200 ppm SO 2 (when used), 10 vol% H 2 O (when in use), N 2 Balance gas, total gas flow is 600mL/min. And (3) introducing the simulated flue gas into a reaction furnace filled with the low-temperature anti-ABS poisoning denitration catalyst of 0.5-g, setting a temperature programming for the reactor, and monitoring the gas phase concentration of each component on line in real time by using a flue gas analyzer. The results of the denitration performance are shown in FIG. 1. As can be seen from fig. 1, the catalyst has good low-temperature denitration catalytic activity. The reactor was programmed to 210 ℃ and held steady, the change in NO concentration at the outlet was recorded, and the NO conversion was calculated. As can be seen from FIG. 2, in the stability test at 210 ℃, the NO conversion rate is stabilized at about 80%, and the high sulfur and water resistance is shown.
Example 2
(1) Will be 3.6 g (NH 4 ) 6 Mo 7 O 24 ·4H 2 O was dissolved in 30mL of ultrapure water;
(2) 0.1g VOSO was taken 4 And 0.1g C 10 H 5 NbO 20 ·xH 2 O（MW =538.04 Dissolving in 30mL ultrapure water;
(3) Mixing the materials obtained in the step (1) and the step (2), performing hydrothermal reaction at 180 ℃ for 48h, centrifugally separating and washing solid powder after the reaction is finished, and drying the solid powder in an oven overnight;
(4) Grinding the solid to fine powder, pouring the fine powder into a crucible, and putting the crucible into a muffle furnace for sealing and roasting, wherein the sealing and roasting specifically comprises the following steps: heating to 400 ℃ at a speed of 5 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature to obtain a powder sample.
The SCR denitration performance of the catalyst was evaluated in a fixed bed reactor. The reaction flue gas condition is set to 600 ppm NO,600 ppm NH 3 ，3 vol% O 2 ，200 ppm SO 2 (when used), 10 vol% H 2 O (when in use), N 2 Balance gas, total gas flow is 600mL/min. And (3) introducing the simulated flue gas into a reaction furnace filled with the low-temperature anti-ABS poisoning denitration catalyst of 0.5-g, setting a temperature programming for the reactor, and monitoring the gas phase concentration of each component on line in real time by using a flue gas analyzer. The results of the denitration performance are shown in FIG. 1. As can be seen from fig. 1, the catalyst has good low-temperature denitration catalytic activity. The reactor was programmed to 210 ℃ and held steady, the change in NO concentration at the outlet was recorded, and the NO conversion was calculated. As can be seen from FIG. 3, in the stability test at 210 ℃, the NO conversion rate is stabilized at about 88%, and the high sulfur and water resistance is shown.
Example 3
For commercial V in a fixed bed reactor 2 O 5 -WO 3 /TiO 2 The SCR denitration performance of the catalyst was evaluated. The reaction flue gas condition is set to 600 ppm NO,600 ppm NH 3 ，3 vol% O 2 ，200 ppm SO 2 (when used), 10 vol% H 2 O (when in use), N 2 Balance gas, total gas flow is 600mL/min. The simulated flue gas was charged with 0.5. 0.5 g commercial V 2 O 5 -WO 3 /TiO 2 In a reaction furnace of the catalyst, setting the temperature of the reactor to 230 ℃ and keeping the temperature stable, and monitoring the gas phase concentration of each component on line in real time by using a smoke analyzer. The results are shown in the figure4, it can be seen from FIG. 4 that NO conversion gradually decreases in the stability test at 230℃to illustrate the conventional commercial V 2 O 5 -WO 3 /TiO 2 The catalyst becomes deactivated under low temperature conditions including water and sulfur.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited to the above-described embodiment, but may be modified or substituted for some of the technical features described in the above-described embodiments by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The M1 type molybdenum molecular sieve denitration catalyst capable of resisting ABS poisoning at low temperature is characterized by comprising a molecular sieve structure, wherein a molecular sieve framework is composed of MoO6 octahedron and AO6 octahedron, wherein an element A is one or more of V, nb, sb and Te elements, the AO6 octahedron is atomically dispersed in the MoO6 octahedral molecular sieve framework, the AO6 octahedron is a catalytic active center, and the MoO6 octahedron is an ABS decomposition center.
2. The low-temperature anti-ABS poisoning M1 type molybdenum molecular sieve denitration catalyst according to claim 1, wherein the content of V element in the element A is 0.5-15 atom percent relative to Mo, the content of Nb, sb and Te elements is 0-10 atom percent, and the site A is atomically dispersed in a molecular sieve framework.
3. The preparation method of the M1 type molybdenum molecular sieve denitration catalyst resistant to ABS poisoning at low temperature is characterized by comprising the following steps:
(1) Dissolving (NH 4) 6Mo7O24.4H2O in ultrapure water to form a clear solution;
(2) Dissolving a required amount of soluble precursor salt of the element A in ultrapure water to prepare a clear solution, wherein a part of precursor salt with low solubility is dissolved by adding a cosolvent;
(3) Mixing the A precursor solution prepared in the step (2) with the Mo precursor solution obtained in the step (1);
(4) Taking the sample in the step (3) to perform a high-temperature hydrothermal reaction for a certain time;
(5) And centrifugally separating, washing, drying, grinding to fine powder, and calcining to obtain the low-temperature anti-ABS poisoning denitration catalyst.
4. The method for preparing the low-temperature anti-ABS poisoning M1 type molybdenum molecular sieve denitration catalyst according to claim 3, wherein the hydrothermal reaction temperature in the step (4) is 150-250 ℃ and the time is 20-48h.
5. The method for preparing a low-temperature anti-ABS poisoning M1 type molybdenum molecular sieve denitration catalyst according to claim 3, wherein the low-temperature drying temperature in the step (5) is 80-120 ℃ and the time is 8-12h.
6. The method for preparing the low-temperature ABS poisoning-resistant M1 type molybdenum molecular sieve denitration catalyst according to claim 3, wherein the specific conditions for calcination in the step (5) are as follows: heating to 400-500 ℃ at the speed of 5-10 ℃/min, preserving heat for 2-6h, and naturally cooling to room temperature.
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| "WO3添加方式对V2O5/TiO2催化剂性能影响";贺媛媛等;《功能材料》;第43卷(第16期);第2233页右栏第1、3段 * |
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