CN103920489A - Preparation method of denitration catalyst for effectively inhibiting SO2 oxidation - Google Patents

Preparation method of denitration catalyst for effectively inhibiting SO2 oxidation Download PDF

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CN103920489A
CN103920489A CN201410153821.9A CN201410153821A CN103920489A CN 103920489 A CN103920489 A CN 103920489A CN 201410153821 A CN201410153821 A CN 201410153821A CN 103920489 A CN103920489 A CN 103920489A
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solution
suspension
titanium dioxide
nitrate
oxalic acid
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CN103920489B (en
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李俊华
彭悦
李柯志
郝吉明
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Tsinghua University
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Priority to PCT/CN2014/092858 priority patent/WO2015158139A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B01D53/46—Removing components of defined structure
    • B01D53/54—Nitrogen compounds
    • B01D53/56—Nitrogen oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/10—Magnesium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J23/20—Vanadium, niobium or tantalum
    • B01J23/22—Vanadium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J23/24—Chromium, molybdenum or tungsten
    • B01J23/30—Tungsten

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Catalysts (AREA)

Abstract

The invention relates to a preparation method for a denitration catalyst for effectively inhibiting SO2 oxidation. The preparation method comprises the following steps: adding ammonium metavanadate and ammonium paratungstate into an oxalic acid solution, and stirring to obtain a solution; adding nitrate barium, magnesium nitrate and strontium nitrate or a solution prepared from a mixture of nitrate barium, magnesium nitrate and strontium nitrate into a mixed solution of titanium dioxide and ludox, and steeping and stirring, thus obtaining a turbid liquid; then pouring the solution into the turbid liquid of the same volume, steeping, stirring, heating, and stirring again until a mixture becomes pasty, and drying; and mashing blocks obtained through drying, and calcining in the air to obtain the catalyst. The catalyst is used for reducing the SO2 oxygenation efficiency under high-concentration SO2 smoke condition, and is widely applied to the NOx catalytic reduction of high-sulphur coal-fired power plants and industrial boilers.

Description

A kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation
Technical field
The present invention relates to the nitrogen oxide control technology field in environmental protection, be specifically related to a kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation.
Background technology
The coal of China has a big chunk to belong to sulphur coal, is mainly distributed in the provinces and regions such as Sichuan, Guizhou, Guangxi, Shandong, Shaanxi.The SO producing in this high sulfur coal combustion process 3easily form aerosol, cause fine particle PM2.5 concentration to raise, cause the regional heavily contaminated haze weather of the frequent occurrence of large-area of China in recent years, people's healthy and productive life is caused and had a strong impact on.The SO of coal fired power plant discharge 3except deriving from burning, also have most to derive from SCR denitrating catalyst to SO in flue gas 2oxidation.The active component V of industry SCR denitrating catalyst 2o 5can promote significantly SO 2change into SO 3, in flue gas, also contain in addition a large amount of steam (10%), SO 3under specific temperature and humidity condition, can form sulfuric acid droplet, when sulfuric acid droplet surpasses 30mg/m 3in time, can produce " blue smoke " and pollutes.Although denitrification apparatus General Requirements SO 2/ SO 3low conversion rate is in 1%, but for sulphur coal (SO 2concentration 2000-5000ppm), the SO of denitration outlet place 3concentration even can reach 60-150mg/m 3, even higher.
Although the flue gas polution control such as dedusting, desulfurizer facility all can be removed SO to some extent 3but removal efficiency deviation is larger.According to the data of U.S. EPA, the use bituminous coal of 75-85% and SCR denitrification apparatus is housed and the thermal power plant of wet desulphurization facility because SO 3concentration of emission is compared with high and have " blue smoke " problem, and wet desulphurization only can be removed about 50% SO 3.Yet China's thermal power generation reaches 77.5% by coal metabituminous coal ratio, and most (>97%) desulfurization facilities in coal-burning power plant all adopt wet processing.According to national environmental protection planning, to " 12 " end, a large amount of fired power generating unit will be installed SCR equipment for denitrifying flue gas, when the time comes SO 3the environmental problem that discharge brings will be more outstanding.So improve the formula of catalyst from source, be formed on and meet under high denitration activity prerequisite, effectively suppress SO 2the formula of oxidation is academic circles at present and industrial quarters problem demanding prompt solution.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation, is applicable to high concentration SO 2under flue gas condition, (2000ppm) reduces SO 2oxygenation efficiency, can be widely used in the coal-burning power plant of high-sulfur and the NO of Industrial Boiler xcatalytic reduction.
In order to achieve the above object, the technical scheme that the present invention takes is:
A kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step 1: ammonium metavanadate and ammonium paratungstate are joined in the solution being formed for 20:1 preparation in mass ratio by deionized water and oxalic acid by the mass ratio of 0.8:5 respectively, at 60 ℃, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution, become solution 1;
Step 2: the solution that respectively barium nitrate, magnesium nitrate, strontium nitrate or its mixture is configured to 1wt% joins dipping in titanium dioxide and Ludox mixed liquor and stirs 1 hour, become suspension 1, wherein the mass ratio of barium nitrate, magnesium nitrate or strontium nitrate and titanium dioxide and Ludox mixed liquor is 1:99, SiO in titanium dioxide and Ludox mixed liquor 2be respectively (5-20) with the mass ratio of titanium dioxide: (95-80);
Step 3: again solution 1 is poured in the suspension 1 of same volume into dipping and stirred after 1 hour and be heated to 80 ℃, continue to be stirred to pasty state, 120 ℃ of oven dry, wherein the mass ratio of the solid matter in ammonium metavanadate, ammonium paratungstate and suspension 1 is 0.8:5:94.2;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
Compared with prior art, tool of the present invention has the following advantages:
1. catalyst of the present invention is changed not quite the catalyst system of industrial maturation, and production technology is simple, is suitable for catalyst plant large-scale production.
2. catalyst of the present invention is at 30000h -1air speed under, the SO of 2000ppm 2under concentration conditions, the temperature range of 300-440 ℃, there is good denitration activity (more than 80%) and lower SO 2conversion ratio (0.5% left and right).
Accompanying drawing explanation
Fig. 1 is denitration efficiency and the SO of the embodiment of the present invention 1 2conversion ratio.
Fig. 2 is denitration efficiency and the SO of the embodiment of the present invention 2 2conversion ratio.
Fig. 3 is denitration efficiency and the SO of the embodiment of the present invention 3 2conversion ratio.
The specific embodiment
Embodiment mono-
A kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step 1: take respectively the ammonium metavanadate of 0.0343g, the ammonium paratungstate of 0.2814g and 1g oxalic acid are dissolved in 20mL deionized water, stir until ammonium metavanadate, ammonium paratungstate and oxalic acid are dissolved in solution at 60 ℃, become solution 1;
Step 2: 5g titanium dioxide is joined to 20mL deionized water for stirring and form suspension 1;
Step 3: pour solution 1 in 20mL suspension 1 dipping stirring and be heated to 80 ℃ after 1 hour, continue to be stirred to pasty state, 120 ℃ of oven dry;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
The appreciation condition of catalyst (lower same): catalyst is got 0.2g, and flue gas concentration is 500ppmNH 3, 500ppm NO, 3%O 2with 2000ppm SO 2, balanced gas is N 2, total tolerance is 100mL/min, air speed is about 30000h -1.The temperature spot of test is 300,320,360,400,440 ℃, each temperature spot balance 2 hours.Fig. 1 is denitration efficiency and the SO of embodiment 1 2conversion ratio, as can be seen from Figure 1, can obviously suppress SO although reduce the content of vanadium to 0.4wt% 2oxygenation efficiency, but due to the reduction of amount of active ingredients, the denitration efficiency of catalyst exists obviously and declines.So after modified catalyst in, the content of vanadium is selected 0.8wt%.
Embodiment bis-
A kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step 1: take respectively the ammonium metavanadate of 0.0343g and the ammonium paratungstate of 0.2814g, be dissolved in the oxalic acid solution 20mL of 1g, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 ℃, become solution 1;
Step 2: include in 5g titanium dioxide suspension and add respectively the magnesium nitrate of 0.0853g barium nitrate, 0.0837g and the strontium nitrate of 0.0690g to stir 1 hour at 20mL, become suspension 1;
Step 3: solution 1 being poured into becomes in suspension 1 dipping and stir after 1 hour and be heated to 80 ℃ again, continues to be stirred to pasty state, 120 ℃ of oven dry;
Step 4: the bulk of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
Fig. 2 is denitration efficiency and the SO of embodiment 2 2conversion ratio, as can be seen from Figure 2, barium monoxide, magnesia or the strontium oxide strontia that adds 1wt% all can suppress catalyst a little at the denitration efficiency of 300 ℃, simultaneously SO 2oxygenation efficiency all obviously reduce, wherein add barytic sample SO 2oxygenation efficiency is minimum.
Embodiment tri-
A kind of effective inhibition SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step 1: take respectively the ammonium metavanadate of 0.0343g, the ammonium paratungstate of 0.2814g and 1g oxalic acid are dissolved in 20mL deionized water, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 ℃, become solution 1;
Step 2: the barium nitrate of 0.0853g is joined to 4.75g titanium dioxide, 0.83g Ludox (5wt%); Or 4.5g titanium dioxide, 1.67g Ludox (10wt%); Or 4g titanium dioxide, in the mixed liquor of 3.35g Ludox (20wt%), dipping stirs 1 hour, becomes suspension 1;
Step 3: solution 1 being poured into becomes in suspension 1 dipping and stir after 1 hour and be heated to 80 ℃ again, continues to be stirred to pasty state, 120 ℃ of oven dry;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
Fig. 3 is denitration efficiency and the SO of embodiment 3 2conversion ratio, as can be seen from Figure 3, adds SiO 2although can increase a little SO 2oxygenation efficiency, but can obviously improve the denitration performance of catalyst.

Claims (4)

1. one kind is effectively suppressed SO 2the preparation method of the denitrating catalyst of oxidation, is characterized in that, step is as follows:
Step 1: ammonium metavanadate and ammonium paratungstate are joined in the solution being formed for 20:1 preparation in mass ratio by deionized water and oxalic acid by the mass ratio of 0.8:5 respectively, at 60 ℃, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution, become solution 1;
Step 2: the solution that respectively barium nitrate, magnesium nitrate, strontium nitrate or its mixture is configured to 1wt% joins dipping in titanium dioxide and Ludox mixed liquor and stirs 1 hour, become suspension 1, wherein the mass ratio of barium nitrate, magnesium nitrate or strontium nitrate and titanium dioxide and Ludox mixed liquor is 1:99, SiO in titanium dioxide and Ludox mixed liquor 2be respectively (5-20) with the mass ratio of titanium dioxide: (95-80);
Step 3: again solution 1 is poured in the suspension 1 of same volume into dipping and stirred after 1 hour and be heated to 80 ℃, continue to be stirred to pasty state, 120 ℃ of oven dry, wherein the mass ratio of the solid matter in ammonium metavanadate, ammonium paratungstate and suspension 1 is 0.8:5:94.2;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
2. a kind of effective inhibition SO according to claim 1 2the preparation method of the denitrating catalyst of oxidation, is characterized in that, step is as follows:
Step 1: take respectively the ammonium metavanadate of 0.0343g, the ammonium paratungstate of 0.2814g and 1g oxalic acid are dissolved in 20mL deionized water, stir until ammonium metavanadate, ammonium paratungstate and oxalic acid are dissolved in solution at 60 ℃, become solution 1;
Step 2: 5g titanium dioxide is joined to 20mL deionized water for stirring and form suspension 1;
Step 3: pour solution 1 in 20mL suspension 1 dipping stirring and be heated to 80 ℃ after 1 hour, continue to be stirred to pasty state, 120 ℃ of oven dry;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
3. a kind of effective inhibition SO according to claim 1 2the preparation method of the denitrating catalyst of oxidation, is characterized in that, step is as follows:
Step 1: take respectively the ammonium metavanadate of 0.0343g and the ammonium paratungstate of 0.2814g, be dissolved in the oxalic acid solution 20mL of 1g, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 ℃, become solution 1;
Step 2: include in 5g titanium dioxide suspension and add respectively the magnesium nitrate of 0.0853g barium nitrate, 0.0837g and the strontium nitrate of 0.0690g to stir 1 hour at 20mL, become suspension 1;
Step 3: solution 1 being poured into becomes in suspension 1 dipping and stir after 1 hour and be heated to 80 ℃ again, continues to be stirred to pasty state, 120 ℃ of oven dry;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
4. a kind of effective inhibition SO according to claim 1 2the preparation method of the denitrating catalyst of oxidation, is characterized in that, step is as follows:
Step 1: take respectively the ammonium metavanadate of 0.0343g, the ammonium paratungstate of 0.2814g and 1g oxalic acid are dissolved in 20mL deionized water, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 ℃, become solution 1;
Step 2: the barium nitrate of 0.0853g is joined to 4.75g titanium dioxide, 0.83g Ludox (5wt%); Or 4.5g titanium dioxide, 1.67g Ludox (10wt%); Or 4g titanium dioxide, in the mixed liquor of 3.35g Ludox (20wt%), dipping stirs 1 hour, becomes suspension 1;
Step 3: solution 1 being poured into becomes in suspension 1 dipping and stir after 1 hour and be heated to 80 ℃ again, continues to be stirred to pasty state, 120 ℃ of oven dry;
Step 4: the block of oven dry is smashed to pieces, calcined in air after 5 hours for 550 ℃ and obtain catalyst.
CN201410153821.9A 2014-04-16 2014-04-16 One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation Active CN103920489B (en)

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PCT/CN2014/092858 WO2015158139A1 (en) 2014-04-16 2014-12-03 Preparation method of denitration catalyst for effectively inhibiting oxidation of sulfur dioxide

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Cited By (5)

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CN104525216A (en) * 2014-12-11 2015-04-22 清华大学 Denitration catalyst for wide temperature window under high sulfur condition and preparation method thereof
WO2015158139A1 (en) * 2014-04-16 2015-10-22 清华大学 Preparation method of denitration catalyst for effectively inhibiting oxidation of sulfur dioxide
CN106807393A (en) * 2017-01-12 2017-06-09 中国科学院兰州化学物理研究所 A kind of low SO of low temperature2Oxygenation efficiency honeycomb type denitrification catalyst and preparation method thereof
CN106824171A (en) * 2017-01-12 2017-06-13 中国科学院兰州化学物理研究所 A kind of operating temperature sulfur resistive honeycomb type denitrification catalyst wide and preparation method thereof
CN111135820A (en) * 2019-12-30 2020-05-12 安徽元琛环保科技股份有限公司 Preparation method of barium-containing flue gas denitration catalyst and prepared denitration catalyst

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Publication number Priority date Publication date Assignee Title
WO2015158139A1 (en) * 2014-04-16 2015-10-22 清华大学 Preparation method of denitration catalyst for effectively inhibiting oxidation of sulfur dioxide
CN104525216A (en) * 2014-12-11 2015-04-22 清华大学 Denitration catalyst for wide temperature window under high sulfur condition and preparation method thereof
CN106807393A (en) * 2017-01-12 2017-06-09 中国科学院兰州化学物理研究所 A kind of low SO of low temperature2Oxygenation efficiency honeycomb type denitrification catalyst and preparation method thereof
CN106824171A (en) * 2017-01-12 2017-06-13 中国科学院兰州化学物理研究所 A kind of operating temperature sulfur resistive honeycomb type denitrification catalyst wide and preparation method thereof
CN111135820A (en) * 2019-12-30 2020-05-12 安徽元琛环保科技股份有限公司 Preparation method of barium-containing flue gas denitration catalyst and prepared denitration catalyst

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