CN108435159B - Denitration catalyst for improving arsenic poisoning resistance and preparation method and application thereof - Google Patents
Denitration catalyst for improving arsenic poisoning resistance and preparation method and application thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/30—Tungsten
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
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- B01D53/8628—Processes characterised by a specific catalyst
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
Abstract
The invention discloses a denitration catalyst for improving arsenic poisoning resistance and a preparation method thereof, and belongs to the technical field of environmental protection and catalysts. According to the invention, the novel denitration catalyst is obtained by introducing the arsenic-resistant auxiliary agent in the preparation process of the denitration catalyst, so that the chemical stability of the existing vanadium-based and cerium-based catalysts is effectively improved, and the catalyst is used for fixed source denitration. Tests show that after anti-poisoning elements are added, compared with a fresh catalyst, the denitration activity of the simulated poisoning catalyst under the arsenic-containing condition is remarkably improved, the NO conversion rate can be increased to more than 78% from 35% at 300 ℃, and the optimal NO conversion rate can be as high as 88%; and with increasing temperature to 400 c the NO conversion is further mentioned to reach 90%. The optimal arsenic-resistant additive is a magnesium salt, the arsenic poisoning resistance of the catalyst is well improved through the synergistic effect of Mg and As, and the influence of component addition on a temperature window and activity is greatly avoided.
Description
Technical Field
The invention relates to the technical field of environmental protection and catalysts, in particular to a denitration catalyst for improving arsenic poisoning resistance, a preparation method thereof and application of the denitration catalyst in the field of nitrogen oxide purification.
Background
Nitrogen Oxides (NO)xMainly comprising NO and NO2) Not only are important precursors constituting Secondary Organic Aerosols (SOA) in PM2.5, but also Secondary pollutants such as O3 can be generated through a series of photochemical reactions, resulting in occurrence of photochemical smog events. Therefore, the emission of nitrogen oxides is greatly reduced, and the method has important significance for improving the air quality of China. In 1851.9 ten thousand tons (2015) of total nitrogen oxide emission in China, the emission amount of fixed source NOx represented by the power industry, industrial boilers and the like accounts for about 63.8 percent, and the emission amount is NOxThe main source of emissions. Among the fixed source nitrogen oxide control technologies, the Selective Catalytic Reduction (SCR) technology is the most effective and widely applicable denitration technology. And the catalyst is the core of the whole technology.
The fly ash of the flue gas of the coal combustion contains a large amount of alkali metals (such As potassium, sodium and the like), alkaline earth metal elements (such As calcium and magnesium), phosphorus (P) and arsenic (As), so that the chemical poisoning phenomenon of the denitration catalyst frequently occurs during the treatment of boiler flue gas of coal combustion, biomass and the like. Wherein, arsenic existing in the fly ash of the fire coal is used as an inorganic highly toxic substance, which can cause the SCR denitration catalyst to generate strong deactivation effect. Research shows that As in smoke2O3Molecules not only can block the catalyst pore channels, but also are often adsorbed on the carrier and react with the catalystThe reactive sites react to form a stable compound without catalytic effect to inert the active center, which hinders the continuous progress of the catalytic reaction and leads the chemical inactivation of the catalyst. In the prior art, the arsenic poisoning resistance of the catalyst is improved by adding a molybdenum oxide component, but after the molybdenum oxide component is added, the activity, the selectivity and the temperature window of the catalyst are obviously influenced. Therefore, the proper additive is selected, the arsenic poisoning resistance is improved on the premise of less influence on the denitration performance, and the denitration catalyst has a wider denitration application prospect.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a denitration catalyst for improving the arsenic poisoning resistance and a preparation method thereof.
The preparation method of the denitration catalyst for improving the arsenic poisoning resistance comprises the preparation of an arsenic-vanadium-based denitration catalyst and an arsenic-cerium-based denitration catalyst, and specifically comprises the following steps:
preparing an arsenic-vanadium-resistant denitration catalyst:
step one, uniformly mixing ammonium metavanadate, oxalic acid, ammonium metatungstate and an arsenic-resistant auxiliary agent, adding deionized water, and stirring to obtain a precursor solution; the arsenic-resistant auxiliary agent can be any one of magnesium salt, barium salt, cobalt salt or iron salt. And adding titanium dioxide as a carrier into the precursor solution, continuously stirring to obtain slurry, and heating the slurry to 100 ℃ under the condition of continuous stirring until the water is completely volatilized to obtain a solid substance.
The mass ratio (calculated by oxide) of the addition amount of each element is as follows: tungsten oxide: titanium oxide: and (3) an anti-arsenic auxiliary agent (0.1-0.8): (4.5-8.5): (85-93): (1.5-5). The molar ratio of the oxalic acid to the metal precursor salt A is 0.5-5, and the metal precursor salt A is the sum of ammonium metavanadate, ammonium metatungstate, an arsenic-resistant auxiliary agent and titanium dioxide.
Secondly, washing the solid substance obtained in the first step for multiple times by using deionized water to remove impurities and residues on the surface, and then drying the washed solid substance in an oven at the temperature of 80-110 ℃; and roasting the dried solid to obtain the arsenic poisoning resistant vanadium-based denitration catalyst. The roasting conditions are as follows: heating to 400-600 ℃ at a heating rate of 1-20 ℃/min in an air atmosphere, and keeping calcining for 2-5 hours.
Preparation of the arsenic-resistant cerium-based denitration catalyst:
uniformly mixing cerium salt, oxalic acid, ammonium tungstate and an arsenic-resistant auxiliary agent, adding deionized water, and stirring to obtain a mixed solution; the arsenic-resistant auxiliary agent is also magnesium salt, barium salt, cobalt salt or iron salt. And adding a precipitant into the mixed solution, and precipitating under the condition of regulating and controlling the pH value to be 11 until the precipitate is fully precipitated to obtain a precipitate. The mass ratio (in terms of oxide) of the addition amounts of the elements is as follows, cerium oxide: tungsten oxide: 20-40% of an arsenic-resistant auxiliary agent: 50-80: 2 to 20.
Step two, carrying out suction filtration on the precipitate obtained in the step one, washing with deionized water, and then drying in an oven at 80-110 ℃ to obtain a semi-finished product; and putting the obtained semi-finished product into a muffle furnace for calcining to obtain the arsenic poisoning resistant cerium-based denitration catalyst. The calcination conditions are as follows: heating to 400-600 ℃ at a heating rate of 1-20 ℃/min in an air atmosphere, and keeping calcining for 2-5 hours.
The cerium salt is trivalent or quadrivalent cerium salt containing crystal water, and can be cerium chloride, cerium nitrate, ammonium cerium nitrate and cerium sulfate, preferably cerium nitrate; the magnesium salt is a divalent magnesium salt containing crystal water, and comprises magnesium nitrate, magnesium sulfate and magnesium chloride, and preferably magnesium nitrate; the barium salt is barium nitrate and barium chloride, preferably barium nitrate; the cobalt salt can be cobalt sulfate, cobalt nitrate, cobalt chloride and cobalt acetylacetonate, and cobalt nitrate is preferred; the ferric salt is ferric iron salt such as ferric chloride, ferric nitrate, ferric acetate and the like, and ferrous iron salt such as ferrous nitrate, ferrous chloride and the like, preferably ferrous nitrate; the precipitant may be ammonia water, ammonium carbonate or ammonium bicarbonate, preferably ammonia water.
The molar ratio of the oxalic acid to the metal precursor salt B is 0.5-5, and the metal precursor salt B is the sum of cerium salt, ammonium tungstate and an arsenic-resistant auxiliary agent.
The vanadium-based and cerium-based denitration catalyst with arsenic poisoning resistance prepared by the method can be applied to denitration of fixed source nitrogen oxides, and specifically comprises the following steps:
(1) and (3) soaking the prepared fresh catalyst in an arsenic oxide solution, then evaporating to dryness, and roasting at 400 ℃ for 3h to obtain the poisoned simulated poisoning catalyst. Wherein the loading content of the arsenic oxide on the simulated poisoned catalyst is controlled to be 3 wt%.
(2) Placing the simulated poisoning catalyst in a miniature fixed bed reactor for activity test, and controlling the reaction temperature to be between 150 and 500 ℃;
(3) controlling the flow of gas at 200mL/min, the volume content of oxygen at 3%, the content of ammonia gas and nitric oxide at 500ppm, the volume content of water vapor at 2%, balancing gas at nitrogen, and controlling the space velocity at 120000mL g-1h-1. Activity tests show that: when the arsenic-resistant assistant is not added, the denitration activity of the cerium-based and vanadium-based catalysts poisoned by arsenic at 300 ℃ and 400 ℃ is less than 50%, and when the arsenic-resistant assistant is added, the denitration activity of the cerium-based and vanadium-based catalysts poisoned by arsenic at 300 ℃ and 400 ℃ can be improved to more than 76%, and the highest denitration activity can reach 90%.
Compared with the conventional catalyst, the invention can improve the arsenic poisoning resistance of the catalyst on the premise of ensuring a wide temperature denitration window. The catalyst mainly adds an arsenic poisoning resistant element which has small influence on denitration performance, can form a stable arsenate structure with arsenic oxide in fly ash at high temperature, reduces the influence of arsenic on active components vanadium, tungsten and cerium of the catalyst, and has the advantages of low cost, high stability and the like. Through tests, the optimal arsenic-resistant additive is a magnesium salt, the arsenic poisoning resistance of the catalyst is well improved through the synergistic effect of Mg and As, and the influence of component addition on a temperature window and activity is greatly avoided.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1And (3) preparing a VWMgTi catalyst.
(1) Dissolving 0.13g of ammonium metavanadate, 0.86g of ammonium metatungstate, 2g of oxalic acid and 1.1g of magnesium nitrate in 100mL of deionized water, and stirring and mixing to obtain a precursor solution;
(2) adding 9g of titanium dioxide into the precursor solution in the step (1), and stirring at room temperature for 120min to obtain slurry;
(3) heating and stirring the serous fluid at 100 ℃, and gradually evaporating the water in the serous fluid to dryness to obtain a solid substance;
(4) washing and filtering the solid substance prepared in the step (3) for multiple times by using deionized water, and then drying the solid substance overnight at the temperature of 110 ℃ to obtain a semi-finished product;
(5) and (4) placing the semi-finished product obtained in the step (4) into a muffle furnace for roasting. The roasting conditions are as follows: under the air atmosphere, the temperature is raised from room temperature to 500 ℃ at the speed of 2 ℃/min and kept for 4h, and the vanadium-tungsten-magnesium-titanium catalyst with arsenic poisoning resistance is prepared.
Example 2And preparing a VWBaTi catalyst.
(1) Dissolving 0.13g of ammonium metavanadate, 0.86g of ammonium metatungstate, 2g of oxalic acid and 0.34g of barium nitrate in 100mL of deionized water, and stirring and mixing to obtain a precursor solution;
(2) adding 9g of titanium dioxide into the precursor solution in the step (1), and stirring at room temperature for 120min to obtain slurry;
(3) heating and stirring the serous fluid at 100 ℃, and gradually evaporating the water in the serous fluid to dryness to obtain a solid substance;
(4) washing and filtering the solid substance prepared in the step (3) for multiple times by using deionized water, and then drying the solid substance overnight at the temperature of 110 ℃ to obtain a semi-finished product;
(5) and (4) putting the semi-finished product obtained in the step (4) into a muffle furnace for roasting to obtain the arsenic poisoning resistant vanadium-tungsten-barium-titanium catalyst.
The roasting conditions are as follows: under air atmosphere, the temperature was raised from room temperature to 500 ℃ at a rate of 2 ℃/min and maintained for 4 hours.
Example 3Preparation of CeWMg catalyst.
(1) Dissolving 8.68g of cerium nitrate, 7.605g of ammonium tungstate, 2g of oxalic acid and 4.6g of magnesium nitrate in 100mL of deionized water solution, and stirring and mixing;
(2) dropwise adding 25 wt% ammonia water into the solution obtained in the step (1), controlling the pH value to be 11, stirring at room temperature for 120min, and fully precipitating;
(3) carrying out suction filtration on the precipitate obtained in the step (2), washing the precipitate for multiple times by using deionized water, and drying the precipitate overnight at the temperature of 110 ℃ after washing to obtain a semi-finished product;
(4) and (4) putting the semi-finished product obtained in the step (3) into a muffle furnace, and heating the semi-finished product from room temperature to 500 ℃ at the speed of 2 ℃/min in the air atmosphere and keeping the temperature for 4 hours to obtain the arsenic poisoning resistant cerium-tungsten-magnesium catalyst.
Example 4Preparation of CeWBa catalyst.
(1) Dissolving 8.68g of cerium nitrate, 7.605g of ammonium tungstate, 2g of oxalic acid and 3.2g of barium nitrate in 100mL of deionized water solution, and stirring and mixing;
(2) dropwise adding 25 wt% ammonia water into the solution obtained in the step (1), controlling the pH value to be 11, stirring at room temperature for 120min, and fully precipitating;
(3) carrying out suction filtration on the precipitate obtained in the step (2), washing the precipitate for multiple times by using deionized water, and drying the precipitate overnight at the temperature of 110 ℃ after washing to obtain a semi-finished product;
(4) and (4) putting the semi-finished product obtained in the step (3) into a muffle furnace, and heating the semi-finished product from room temperature to 500 ℃ at the speed of 2 ℃/min in the air atmosphere and keeping the temperature for 4 hours to obtain the arsenic poisoning resistant cerium-tungsten-barium catalyst.
Example 5Preparation of CeWCo catalyst.
(1) Dissolving 8.68g of cerium nitrate, 7.605g of ammonium tungstate, 2g of oxalic acid and 2.91g of cobalt nitrate in 100mL of deionized water solution, and stirring and mixing;
(2) dropwise adding 25 wt% ammonia water into the solution obtained in the step (1), controlling the pH value to be 11, stirring at room temperature for 120min, and fully precipitating;
(3) carrying out suction filtration on the precipitate obtained in the step (2), washing the precipitate for multiple times by using deionized water, and drying the precipitate overnight at the temperature of 110 ℃ after washing to obtain a semi-finished product;
(4) and (4) putting the semi-finished product obtained in the step (3) into a muffle furnace, and heating the semi-finished product from room temperature to 500 ℃ at the speed of 2 ℃/min in the air atmosphere and keeping the temperature for 4 hours to obtain the arsenic poisoning resistant cerium-tungsten-cobalt catalyst.
Application example 1:
simulating a poisoned catalyst: and respectively soaking the prepared fresh catalysts in a certain amount of arsenic oxide solution, then evaporating to dryness, and roasting at 400 ℃ for 3h to obtain the simulated poisoning catalyst. The loading content of the arsenic oxide on the simulated poisoned catalyst is controlled to be 3 wt%. The activity of the catalyst was evaluated in a quartz tube reactor having an inner diameter of 6mm and a length of 300 mm. The catalyst contained 500ppm of ammonia and 500ppm of nitric oxide, 3% by volume of O22% by volume of H2O, the residual gas is N2Under the reaction conditions of (1), the amount of the catalyst is 0.1g, and the reaction space velocity is 120000ml g-1h-1. The results of the catalytic performance tests are shown in table 1.
TABLE 1 NO conversion of arsenic poisoning resistant denitration catalyst
Table 1 shows that, among various types of modifying elements, the addition of Mg (examples 1 and 3) can minimize the influence on the catalytic activity and has the most excellent arsenic poisoning resistance; the table shows that after the anti-poisoning element is added, compared with a fresh catalyst, the denitration activity of the simulated poisoning catalyst under the arsenic-containing condition is remarkably improved, the NO conversion rate can be increased to more than 78% from 35% at 300 ℃, and the optimal NO conversion rate can be as high as 88%; and with increasing temperature to 400 c the NO conversion is further mentioned to reach 90%. By comprehensively considering the anti-poisoning performance of each catalyst at 300 ℃ and 400 ℃, the cerium-based catalyst without the anti-poisoning element can be obtained, wherein the denitration activity of the cerium-based catalyst is as large as VWMgTi approximately equal to CeWMg > CeWBa > VWBaTi > CeWCo > without the anti-poisoning element, and the denitration activity of the cerium-based catalyst is as small as VWMgTi approximately equal to CeWMg > CeWBa > VWBaTi > CeWCo > without the anti-poisoning element.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (2)
1. A preparation method of a denitration catalyst applied to denitration of fixed source nitrogen oxides and capable of improving arsenic poisoning resistance is characterized by comprising the following steps:
adding an arsenic-resistant auxiliary agent in the preparation process of the denitration catalyst with arsenic poisoning resistance to form an arsenic-resistant denitration catalyst;
the arsenic-resistant auxiliary agent is magnesium nitrate;
the arsenic-resistant denitration catalyst is an arsenic-resistant vanadium-based denitration catalyst, and the preparation method comprises the following specific steps:
step one, after 0.13g of ammonium metavanadate, 2g of oxalic acid, 0.86g of ammonium metatungstate and 1.1g of magnesium nitrate are uniformly mixed, 100mL of deionized water is added and stirred to obtain a precursor solution; adding 9g of carrier titanium dioxide into the precursor solution, continuously stirring for 120min to obtain slurry, heating the slurry to 100 ℃ under the condition of continuous stirring until the water is completely volatilized to obtain a solid substance;
secondly, washing the solid substance obtained in the first step by using deionized water, and then drying the washed solid substance in a drying oven at 110 ℃; roasting the dried solid in a muffle furnace to obtain an arsenic-vanadium-resistant denitration catalyst;
the roasting conditions are as follows: heating to 500 ℃ at a heating rate of 2 ℃/min under an air atmosphere, and keeping the calcination for 4 hours.
2. A preparation method of a denitration catalyst applied to denitration of fixed source nitrogen oxides and capable of improving arsenic poisoning resistance is characterized by comprising the following steps:
adding an arsenic-resistant auxiliary agent in the preparation process of the denitration catalyst with arsenic poisoning resistance to form an arsenic-resistant denitration catalyst;
the arsenic-resistant auxiliary agent is magnesium nitrate;
the arsenic-resistant denitration catalyst is an arsenic-resistant cerium-based denitration catalyst, and the preparation method comprises the following specific steps:
step one, uniformly mixing 8.68g of cerium nitrate, 2g of oxalic acid, 7.605g of ammonium tungstate and 4.6g of magnesium nitrate, adding 100mL of deionized water, and stirring to obtain a mixed solution; adding a precipitator into the mixed solution to precipitate under the condition of regulating and controlling the pH =11 until the precipitate is sufficient, so as to obtain a precipitate;
the precipitator is ammonia water;
step two, carrying out suction filtration on the precipitate obtained in the step one, washing with deionized water, and then drying in a drying oven at 110 ℃ to obtain a semi-finished product; putting the obtained semi-finished product into a muffle furnace for calcining to obtain an arsenic-resistant cerium-based denitration catalyst;
the calcination conditions are as follows: heating to 500 ℃ at a heating rate of 2 ℃/min under an air atmosphere, and keeping the calcination for 4 hours.
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