CN111921523B - Medium-low temperature SCO denitration catalyst and preparation method thereof - Google Patents
Medium-low temperature SCO denitration catalyst and preparation method 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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- 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
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- 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
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Abstract
The invention discloses a medium-low temperature SCO denitration catalyst and a preparation method thereof, and relates to a two-step method and a three-step method. The catalyst material is solid powder, and the ratio of each substance is as follows: 40-60% of manganese oxide, 40-60% of iron oxide and 0.0003-0.005% of graphene. Wherein the two-step process comprises: (1) Potassium permanganate, concentrated hydrochloric acid and ultrapure water are subjected to reduction graphene oxide mixed reaction to obtain an intermediate product; (2) And (3) filtering, washing and drying the product obtained in the previous step after hydrothermal reaction with manganese acetate, ferric nitrate, polyethylene glycol 1000 and potassium permanganate to obtain the catalyst. The three-step method is that on the basis of the two-step method, the product of the former step is hydrothermally reacted with manganese acetate, ferric nitrate, polyethylene glycol 1000 and potassium permanganate, and the product is filtered, washed and dried. The catalytic oxidation efficiency of the two-step catalyst to NO at 200 ℃ reaches 50%, and the three-step method can reach more than 80%. Compared with the existing manganese-iron catalyst, the low-temperature catalyst has higher low-temperature catalytic efficiency, can better meet the industrial requirements, and has great potential application prospect in the field of low-temperature denitration.
Description
The technical field is as follows:
the invention belongs to the technical field of NOx removal, and relates to two SCO denitration catalysts at medium and low temperature and preparation methods thereof.
Background art:
nitrogen oxides, in which NO and NO are important substances causing air pollution 2 Mainly, the large amount of emission of the compounds can not only cause a series of environmental problems such as haze, acid rain, ozone destruction of near-stratum atmosphere, eutrophication of surface water, photochemical smog and the like, but also stimulate the central nervous system and respiratory system of a human body, and seriously threaten the health of the human body. The existing nitrogen oxide treatment technology mainly adopts flue gas denitration technology, and the method thereof is divided into a dry method and a wet method: the dry method mainly includes a Selective Catalytic Reduction (SCR) method, a selective non-catalytic reduction (SNCR) method, an adsorption method, etc., and the wet method mainly includes a liquid absorption method and a Selective Catalytic Oxidation (SCO) absorption method.
Currently, the mainstream technology for treating flue gas is selective non-catalytic reduction (SNCR) and Selective Catalytic Reduction (SCR), both of which can use NH 3 By using NO as a reducing agent X The reaction temperature of the SNCR method and the SCR method is high (300-1100 ℃), the flue temperature of other enterprises is mostly less than 200 ℃ except that the flue gas temperature of the coal-fired power plant can reach, and a heating device needs to be additionally arranged in practical application, so that the operation cost is increased; in addition, ammonia used as a reducing agent has problems of leakage and escape; the adsorption capacity of the adsorbent is limited by an adsorption method, the input amount is large, and continuous regeneration is needed; in the liquid absorption method, most of nitrogen oxides in the flue gas exist in the form of NO, and the NO is not easy to dissolve in the absorption liquid, so that the absorption efficiency is not high.
The selective catalytic oxidation absorption method is characterized in that under the medium-low temperature environment of 120-300 ℃, the SCO catalyst firstly utilizes oxygen in flue gas to partially oxidize NO into NO 2 To make it oxidized (NO) 2 /NO X ) 50-60% (the absorption efficiency is highest at this moment), and then the oxidized flue gas is introduced into an absorbent to be absorbed, so that the wet-process simultaneous desulfurization and denitrification is realized, and valuable byproducts such as ammonium sulfate and the like can be generated by utilizing the auto-redox action of nitrogen oxide and sulfur oxide; the method has low requirement on reaction temperature, low investment cost and low operation cost, is matched with a downstream wet absorption process, has the treatment efficiency of over 99 percent, and can simultaneously perform desulfurization and desorptionNitre, and can produce economic benefits, reduce purification flow and cost, and is the most valuable flue gas purification technology.
The key of the selective catalytic oxidation absorption method is the catalyst, and the catalytic oxidation effect of the catalyst determines the denitration efficiency of the flue gas. The catalyst for NO catalytic oxidation reaction at present mainly comprises molecular sieve, active carbon, supported noble metal catalyst, transition metal oxide catalyst and the like. The molecular sieve has large specific surface area and unique pore channel structure, but the NO catalytic oxidation activity of the molecular sieve catalyst is not high at low temperature, only shows high-temperature activity, but is limited by thermodynamic balance, and the NO catalytic activity is not high at high temperature, and meanwhile, the preparation cost of the molecular sieve is high, so the industrial application of the molecular sieve is not realized. The activated carbon catalyst can also catalyze and oxidize NO, but under the low temperature condition, the reaction process of catalyzing and oxidizing NO by the activated carbon requires longer stable time, the reaction rate is slow, the water resistance of the activated carbon catalyst is poor, and the dosage of the catalyst is extremely large. Noble metal catalysts have relatively high activity, but are expensive and costly to apply industrially.
The transition metal oxide catalyst has wide source, low price, simple preparation process, good thermal stability and rich reaction sites and high activity, and is an ideal NO catalytic oxidation catalyst. The multi-valence transition metal elements (Mn, fe, co and Cu) have an oxygen storage function, the catalysis principle is that lattice oxygen oxidizes NO under the condition of micro oxygen, transition metal oxides change from high valence to low valence, and the transition metal elements change from low valence to high valence under the condition of oxygen enrichment, so that a catalysis cycle is formed. The low-temperature catalytic oxidation effect of the ferromanganese oxide in the multivalent transition metal is outstanding.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provide two SCO denitration catalysts for flue gas denitration. The SCO catalyst has good activity in a medium-low temperature environment, the denitration rate of the first catalyst can reach 55 percent at most and the denitration rate of the second catalyst can reach 80 percent at the reaction temperature of 200 ℃; importantly, the catalyst has higher catalytic activity in the low temperature range of 150-200 ℃, thereby greatly reducing the requirements on equipment; the preparation method of the catalyst is simple, the raw materials are cheap and easy to obtain, the product is environment-friendly, the overall cost is low, and the catalyst has a wide industrial application prospect.
The first preparation method of the medium-low temperature SCO denitration catalyst is realized by the following technical scheme:
(1) Weighing a certain amount of potassium permanganate, reducing graphene oxide powder and concentrated hydrochloric acid, adding pure water, continuously stirring until the mixture is completely mixed, reacting, cooling, washing, filtering and drying;
(2) Weighing a certain amount of manganese acetate and ferric nitrate, adding into pure water, and stirring until the manganese acetate and the ferric nitrate are completely dissolved, wherein the solution is a solution I; dissolving polyethylene glycol 1000 in pure water to obtain solution II; dissolving potassium permanganate in water to obtain a solution III; adding the product obtained in the step one into pure water, and uniformly mixing to obtain a solution IV; sequentially adding the solution II, the solution III and the solution IV into the solution I, continuously stirring for reaction, cooling, washing, filtering and drying; obtaining the medium-low temperature SCO denitration catalyst.
The second preparation method of the medium-low temperature SCO denitration catalyst is realized by the following technical scheme:
weighing a certain amount of manganese acetate and ferric nitrate, adding into pure water, and stirring until completely dissolving to obtain a solution (1); dissolving polyethylene glycol 1000 in pure water to obtain a solution (2); dissolving potassium permanganate in water to obtain a solution (3); adding the former catalyst into pure water, and uniformly mixing to obtain a solution (4); sequentially adding the solution (2), the solution (3) and the solution (4) into the solution (1), continuously stirring for reaction, cooling, washing, filtering and drying; preparing another medium-low temperature SCO denitration catalyst.
Further, in the step (1), the mass ratio of potassium permanganate to reduced graphene oxide is 15: 1-5: 1, preferably 10: 1, and the volume ratio of concentrated hydrochloric acid to pure water is 1: 50-1: 70, preferably 1: 60; 1 ml-2 ml of concentrated hydrochloric acid is prepared for each 0.675g of potassium permanganate, and 1ml of concentrated hydrochloric acid is preferably prepared for each 0.675g of potassium permanganate;
further, in the step (1), the continuous mixing and stirring time is 0.5 to 1.5 hours, preferably 1 hour; the reaction condition is that the reaction is carried out in a hydrothermal reaction kettle for 10 to 15 hours, preferably 12 hours at the temperature of 100 ℃; the cooling condition is natural cooling to room temperature; washing the precipitate in the kettle with deionized water until the pH of the filtrate is = 5-6, preferably pH =6, and then washing with ethanol twice; the drying condition is that the mixture is put into an oven to be dried for 10 to 15 hours at 70 to 100 ℃, and the drying condition is preferably that the mixture is dried for 12 hours at 80 ℃.
In the step (2), the ion molar ratio in each raw material is preferably (Mn) 7+ +Mn 2+ )∶Fe 3+ ＝1∶1，Mn 7+ ∶Mn 2+ = 4: 1, the ratio comprising the Mn used in step (1) 7+ Namely potassium permanganate; the addition amount of the polyethylene glycol 1000 is 1 to 2 percent, preferably 1.7 percent of the total mass of all other solid raw materials.
Further, in the step (2), the water bath temperature is 70-100 ℃, the reaction time is 3-5 hours, and the reaction is preferably carried out in a water bath at 90 ℃ for 4 hours; the cooling condition is natural cooling to room temperature; the washing standard is to wash and filter with clear water until the pH = 5-6, and more preferably, the pH =6; the drying condition is vacuum drying at 100 ℃ for 10 to 15 hours, preferably vacuum drying for 15 hours.
In the second catalyst preparation step, the molar ratio of the source ions in the solutions (1) and (3) is preferably (Mn) 7+ +Mn 2+ )∶Fe 3+ ＝1∶1，Mn 7+ ∶Mn 2+ = 4: 1, this ratio not comprising the raw materials used in steps (1) (2); the amount used in solution (4) is the previous catalyst yield; the amount of polyethylene glycol 1000 added in the solution (2) is preferably 1.5% of the total mass of all solid raw materials in the solutions (1), (3) and (4).
Further, in the preparation step of the second catalyst, the water bath temperature is 70-100 ℃, the reaction time is 3-5 hours, and the reaction is preferably carried out in a water bath at 90 ℃ for 4 hours; the cooling condition is natural cooling to room temperature; the washing standard is to wash and filter with clear water until the pH = 5-6, and more preferably, the pH =6; the drying condition is vacuum drying at 100 ℃ for 10 to 15 hours, preferably vacuum drying for 15 hours.
Compared with the prior art, the invention has the main advantages that:
(1) Compared with the traditional ferromanganese series denitration catalyst, the preparation method of the invention greatly improves the specific surface area of the catalyst due to the optimization of the preparation method, correspondingly increases the catalytic sites, greatly improves the catalytic efficiency, and can reach 80 percent of conversion rate at 200 ℃;
(2) Compared with the vanadium-titanium catalyst used in industry, the raw material of the invention is low in price, easy to obtain, free from environmental toxicity, green and environment-friendly;
(3) The preparation method is simple, easy to realize automatic control, low in production cost and beneficial to industrial production and use.
The specific implementation mode is as follows:
the technical solution of the present invention is further explained below with reference to examples, but the scope and the embodiments of the present invention are not limited thereto.
Example 1
The method comprises the following steps: weighing 2.70g of potassium permanganate and 0.27g of reduced graphene oxide powder, weighing 4ml of concentrated hydrochloric acid and 240ml of pure water, mixing, continuously stirring for 1 hour, transferring to a hydrothermal reaction kettle, reacting for 12 hours at 100 ℃, naturally cooling, washing precipitates in the kettle with deionized water until the pH value is equal to 6, washing with ethanol twice, and then drying in an oven at 80 ℃ for 12 hours;
step two: weighing 1.23g of manganese acetate and 10.10g of ferric nitrate, adding the manganese acetate and the ferric nitrate into 100ml of pure water, stirring until the manganese acetate and the ferric nitrate are completely dissolved, wherein the solution is solution I, weighing 0.25g of polyethylene glycol 1000, dissolving the manganese acetate and the ferric nitrate in 20ml of pure water, wherein the solution is solution II, weighing 0.46g of potassium permanganate, adding the potassium permanganate into 200ml of pure water, stirring until the potassium permanganate is completely dissolved, wherein the solution is solution III, adding the product obtained in the step one into 100ml of pure water, and uniformly mixing, wherein the solution IV is solution; placing the solution I in a water bath at 90 ℃ for continuous stirring, then sequentially adding the solution II, the solution III and the solution IV, heating in the water bath for continuous stirring and reacting for 4 hours, naturally cooling to room temperature, washing and filtering the reacted mixed solution by pure water until the pH of the filtrate is =6, collecting solid substances, and placing in an oven for drying for 15 hours at 100 ℃; obtaining the low-temperature SCO denitration catalyst.
Example 2
The method comprises the following steps: weighing 2.70g of potassium permanganate and 0.27g of graphene powder, weighing 4ml of concentrated hydrochloric acid and 240ml of pure water, mixing, continuously stirring for 1 hour, transferring to a hydrothermal reaction kettle, reacting for 12 hours at 100 ℃, naturally cooling, washing precipitates in the kettle with deionized water until the pH value is equal to 6, washing with ethanol twice, and then drying in an oven at 80 ℃ for 12 hours;
step two: weighing 1.23g of manganese acetate and 10.10g of ferric nitrate, adding the manganese acetate and the ferric nitrate into 100ml of pure water, stirring until the manganese acetate and the ferric nitrate are completely dissolved, wherein the solution is solution I, weighing 0.25g of polyethylene glycol 1000, dissolving the manganese acetate and the ferric nitrate in 20ml of pure water, wherein the solution is solution II, weighing 0.46g of potassium permanganate, adding the potassium permanganate into 200ml of pure water, stirring until the potassium permanganate is completely dissolved, wherein the solution is solution III, adding the product obtained in the step one into 100ml of pure water, and uniformly mixing, wherein the solution IV is solution; placing the solution I in a water bath at 90 ℃ for continuous stirring, then sequentially adding the solution II, the solution III and the solution IV, heating in the water bath for continuous stirring and reacting for 4 hours, naturally cooling to room temperature, washing and filtering the reacted mixed solution by pure water until the pH of the filtrate is =6, collecting solid substances, and placing in an oven for drying for 15 hours at 100 ℃;
step three: weighing 1.23g of manganese acetate and 10.10g of ferric nitrate, adding the weighed manganese acetate and the weighed ferric nitrate into 100ml of pure water, stirring the mixture until the manganese acetate and the ferric nitrate are completely dissolved to obtain a solution (1), weighing 0.25g of polyethylene glycol 1000, dissolving the weighed mixture into 20ml of pure water to obtain a solution (2), weighing 3.16g of potassium permanganate, adding the weighed mixture into 200ml of pure water, stirring the mixture until the potassium permanganate is completely dissolved to obtain a solution (3), adding the product obtained in the step two into 100ml of pure water, and uniformly mixing the solution to obtain a solution (4); and (3) placing the solution (1) in a water bath at 90 ℃ for continuous stirring, then sequentially adding the solution (2), the solution (3) and the solution (4), heating in the water bath for continuous stirring and reacting for 4 hours, naturally cooling to room temperature, washing and filtering the reacted mixed solution by pure water until the pH of the filtrate is =6, collecting solid substances, and placing the solid substances in an oven for vacuum drying at 100 ℃ for 15 hours to obtain the medium-low temperature SCO denitration catalyst.
Catalytic Oxidation Performance test
The catalyst prepared in example 1 had an initial concentration of 500ppm NO in laboratory simulated flue gas conditions 2 Is 5% of the initial concentration of N 2 As balance gas, the volume space velocity is 144000h -1 The reaction temperature is increased from 25 ℃ to 200 ℃ in a step way, and the NO conversion rate reaches 55% at 200 ℃.
Example 2 the catalyst had an initial NO concentration of 500ppm under laboratory simulated flue gas conditions，O 2 Is 5% of the initial concentration of N 2 As balance gas, the volume space velocity is 144000h -1 The reaction temperature is increased from 25 ℃ to 200 ℃ in a step mode, and the NO conversion rate reaches more than 80% at 200 ℃.
Claims (3)
1. A preparation method of a medium-low temperature SCO denitration catalyst is characterized by comprising the following specific steps: the method comprises the following steps: weighing a certain amount of potassium permanganate, reducing graphene oxide powder and concentrated hydrochloric acid, adding pure water, continuously stirring until the mixture is completely mixed, reacting, cooling, washing, filtering and drying;
step two: weighing a certain amount of manganese acetate and ferric nitrate, adding into pure water, and stirring until completely dissolving to obtain a solution I; dissolving polyethylene glycol 1000 in pure water to obtain solution II; dissolving potassium permanganate in water to obtain a solution III; adding the product obtained in the step one into pure water, and uniformly mixing to obtain a solution IV; sequentially adding the solution II, the solution III and the solution IV into the solution I, continuously stirring for reaction, cooling, washing, filtering and drying;
after the first step, the second step is carried out, and the specific process of the third step is as follows: weighing a certain amount of manganese acetate and ferric nitrate, adding into pure water, and stirring until completely dissolving to obtain a solution (1); dissolving polyethylene glycol 1000 in pure water, which is solution (2); dissolving potassium permanganate in pure water to obtain a solution (3); adding the product obtained in the step two into pure water, and uniformly mixing to obtain a solution (4); sequentially adding the solution (2), the solution (3) and the solution (4) into the solution (1), continuously stirring for reaction, cooling, washing, filtering and drying; preparing a medium-low temperature SCO denitration catalyst;
in the first step, the mass ratio of potassium permanganate to reduced graphene oxide is 15: 1-5: 1, and the volume ratio of concentrated hydrochloric acid to pure water is 1: 70-1: 50; 1 mL-2 mL concentrated hydrochloric acid is prepared by every 0.675g of potassium permanganate; in the second step, the molar ratio of ions in each raw material is (Mn) 7+ +Mn 2+ )∶Fe 3+ ＝2∶1～1∶2，Mn 7+ ∶Mn 2+ = 4: 1, the ratio including Mn used in the first step 7+ Namely potassium permanganate; the addition amount of the polyethylene glycol 1000 is that of all other solids1-2% of the total mass of the raw materials;
the medium and low temperature refers to 200 ℃;
in the first step, the continuous mixing and stirring time is 0.5 to 1.5 hours; the reaction condition is that the reaction is carried out for 10 to 15 hours in a hydrothermal reaction kettle at the temperature of 100 ℃; the cooling condition is natural cooling to room temperature; washing the precipitate in the kettle with deionized water, filtering to obtain filtrate with pH of 5-7, and washing with ethanol for two to three times; the drying condition is that the mixture is put into a drying oven to be dried for 10 to 15 hours at the temperature of between 70 and 100 ℃;
in the second step, the reaction condition is that the reaction is carried out in a water bath at the temperature of 70-100 ℃ for 3-5 hours; naturally cooling to room temperature under the cooling condition, washing with deionized water until the pH value of the filtrate is between 5 and 7, and drying under the vacuum drying condition of 100 ℃ for 10 to 15 hours;
in the third step, the molar ratio of the raw material ions in the solutions (1) and (3) is (Mn) 7+ +Mn 2+ )∶Fe 3+ ＝2∶1～1∶2，Mn 7+ ∶Mn 2+ = 4: 1, the ratio does not include the raw materials used in the first and second steps; the amount of the solution (4) is the total amount of the reaction product in the step two; the addition amount of the polyethylene glycol 1000 in the solution (2) is 1 to 2 percent of the total mass of the solid raw materials in the solutions (1), (3) and (4);
in the third step, the reaction condition is that the reaction is carried out in water bath at the temperature of 70-100 ℃ for 3-5 hours; the cooling condition is natural cooling to room temperature, the washing standard is washing and filtering with deionized water until the pH = 5-6 of the filtrate, and the drying condition is vacuum drying for 10-15 hours at 100 ℃.
2. The medium and low temperature SCO denitration catalyst prepared by the preparation method of claim 1 is characterized in that the content of manganese oxide in the catalyst is 40-60%, the content of iron oxide is 40-60%, and the content of graphene is 0.0003-0.005%; at 200 ℃, the catalytic conversion rate of NO reaches 80%;
the medium-low temperature refers to 200 ℃.
3. Use of the catalyst of claim 2 in flue gas denitration reactions.
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