CN103920489B - One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation - Google Patents

One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation Download PDF

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CN103920489B
CN103920489B CN201410153821.9A CN201410153821A CN103920489B CN 103920489 B CN103920489 B CN 103920489B CN 201410153821 A CN201410153821 A CN 201410153821A CN 103920489 B CN103920489 B CN 103920489B
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solution
catalyst
nitrate
suspension
titanium dioxide
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CN103920489A (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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    • 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)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Biomedical Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation, joins in oxalic acid solution by ammonium metavanadate and ammonium paratungstate, stirs and becomes solution; Again the solution that barium nitrate, magnesium nitrate, strontium nitrate or its mixture configure is joined dipping in titanium dioxide and Ludox mixed liquor to stir, become suspension; Then solution is poured into after dipping in the suspension of same volume stirs and heat, continue to be stirred to pasty state, dry; Finally smashed to pieces by the block of oven dry, obtain catalyst after calcining in atmosphere, this catalyst is applicable to high concentration SO 2sO is reduced under flue gas condition 2oxygenation efficiency, can be widely used in the coal-burning power plant of high-sulfur and the NO of Industrial Boiler xcatalytic reduction.

Description

One effectively suppresses 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 one and effectively suppress 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 produced in this high sulfur coal combustion process 3easy formation aerosol, causes fine particle PM2.5 concentration to raise, and causes the regional heavily contaminated haze weather of the frequent occurrence of large-area of China in recent years, causes have a strong impact on the healthy of people and productive life.The SO of coal fired power plant discharge 3except deriving from burning, most is also had to derive from SCR denitration to SO in flue gas 2oxidation.The active component V of industry SCR denitration 2o 5sO can be promoted significantly 2change into SO 3, also contain a large amount of steam (10%) in flue gas in addition, SO 3sulfuric acid droplet can be formed at specific temperature and humidity conditions, when sulfuric acid droplet is more than 30mg/m 3time can produce " blue smoke " pollute.Although denitrification apparatus General Requirements SO 2/ SO 3low conversion rate in 1%, but for sulphur coal (SO 2concentration 2000-5000ppm), denitration outlet place SO 3concentration even can reach 60-150mg/m 3, even higher.
Although the flue gas polution control such as dedusting, desulfurizer facility all can remove 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 the thermal power plant of SCR denitration device and wet desulphurization facility is housed because SO 3concentration of emission is higher and there is " blue smoke " problem, and wet desulphurization only can remove the SO of about 50% 3.But China's thermal power generation coal metabituminous coal ratio reaches 77.5%, and the coal-burning power plant overwhelming majority (>97%) desulfurization equipment all adopts wet processing.According to national environmental protection planning, to " 12 " end, a large amount of fired power generating unit will install SCR equipment for denitrifying flue gas, when the time comes SO 3discharging the environmental problem brought will be more outstanding.So improve the formula of catalyst from source, be formed under meeting 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, one is the object of the present invention is to provide effectively to suppress 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:
One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step one: ammonium metavanadate and ammonium paratungstate are joined by deionized water and oxalic acid in mass ratio for 20:1 prepares in the solution formed by the mass ratio of 0.8:5 respectively, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 DEG C, become solution 1;
Step 2: the solution respectively barium nitrate, magnesium nitrate, strontium nitrate or its mixture being configured to 1wt% joins in titanium dioxide and Ludox mixed liquor and floods stirring 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: poured into by solution 1 and flood stirring in the suspension 1 of same volume and be heated to 80 DEG C after 1 hour, continue to be stirred to pasty state, 120 DEG C of oven dry, the mass ratio of the solid matter wherein in ammonium metavanadate, ammonium paratungstate and suspension 1 is 0.8:5:94.2;
Step 4: smashed to pieces by the block of oven dry, calcines in atmosphere after 5 hours for 550 DEG C and obtains catalyst.
Compared with prior art, tool of the present invention has the following advantages:
1. catalyst of the present invention is changed little to industrial ripe catalyst system, 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 DEG C, there is good denitration activity (more than 80%) and lower SO 2conversion ratio (about 0.5%).
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.
Detailed description of the invention
Embodiment one
One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step one: take the ammonium metavanadate of 0.0343g, the ammonium paratungstate of 0.2814g and 1g oxalic acid respectively and be dissolved in 20mL deionized water, stirs until ammonium metavanadate, ammonium paratungstate and dissolving oxalic acid are in solution at 60 DEG C, becomes solution 1;
Step 2: 5g titanium dioxide is joined 20mL deionized water for stirring and form suspension 1;
Step 3: solution 1 is poured in 20mL suspension 1 and flood stirring and be heated to 80 DEG C after 1 hour, continue to be stirred to pasty state, 120 DEG C of oven dry;
Step 4: smashed to pieces by the block of oven dry, calcines in atmosphere after 5 hours for 550 DEG C and obtains catalyst.
The appreciation condition (lower same) of catalyst: 0.2g got by catalyst, and flue gas concentration is 500ppmNH 3, 500ppmNO, 3%O 2and 2000ppmSO 2, balanced gas is N 2, total tolerance is 100mL/min, and air speed is about 30000h -1.The temperature spot of test is 300,320,360,400,440 DEG C, and each temperature spot balances 2 hours.Fig. 1 is denitration efficiency and the SO of embodiment 1 2conversion ratio, as can be seen from Figure 1, although the content reducing vanadium obviously can suppress SO to 0.4wt% 2oxygenation efficiency, but due to the reduction of amount of active ingredients, the denitration efficiency of catalyst exists and obviously declines.So in modified catalyst afterwards, the content of vanadium selects 0.8wt%.
Embodiment two
One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step one: take the ammonium metavanadate of 0.0343g and the ammonium paratungstate of 0.2814g respectively, is dissolved in the oxalic acid solution 20mL of 1g, stirs until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution, become solution 1 at 60 DEG C;
Step 2: include in 5g titanium dioxide suspension at 20mL and add 0.0853g barium nitrate, the magnesium nitrate of 0.0837g and the strontium nitrate of 0.0690g respectively and stir 1 hour, become suspension 1;
Step 3: solution 1 is poured into become in suspension 1 again and flood stirring and be heated to 80 DEG C after 1 hour, continue to be stirred to pasty state, 120 DEG C of oven dry;
Step 4: the bulk of oven dry smashed to pieces, calcines in atmosphere after 5 hours for 550 DEG C and obtains catalyst.
Fig. 2 is denitration efficiency and the SO of embodiment 2 2conversion ratio, as can be seen from Figure 2, adds the barium monoxide of 1wt%, magnesia or strontium oxide strontia and catalyst all can be suppressed a little at the denitration efficiency of 300 DEG C, SO simultaneously 2oxygenation efficiency all obviously reduce, wherein add barytic sample SO 2oxygenation efficiency is minimum.
Embodiment three
One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation, step is as follows:
Step one: take the ammonium metavanadate of 0.0343g, the ammonium paratungstate of 0.2814g and 1g oxalic acid respectively and be dissolved in 20mL deionized water, stirs until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 DEG C, becomes solution 1;
Step 2: the barium nitrate of 0.0853g is joined 4.75g titanium dioxide, 0.83g Ludox (5wt%); Or 4.5g titanium dioxide, 1.67g Ludox (10wt%); Or 4g titanium dioxide, flood stirring 1 hour in the mixed liquor of 3.35g Ludox (20wt%), become suspension 1;
Step 3: solution 1 is poured into become in suspension 1 again and flood stirring and be heated to 80 DEG C after 1 hour, continue to be stirred to pasty state, 120 DEG C of oven dry;
Step 4: smashed to pieces by the block of oven dry, calcines in atmosphere after 5 hours for 550 DEG C and obtains catalyst.
Fig. 3 is denitration efficiency and the SO of embodiment 3 2conversion ratio, as can be seen from Figure 3, adds SiO 2although SO can be increased a little 2oxygenation efficiency, but the denitration performance of catalyst can be significantly improved.

Claims (1)

1. one kind is effectively suppressed SO 2the preparation method of the denitrating catalyst of oxidation, it is characterized in that, step is as follows:
Step one: ammonium metavanadate and ammonium paratungstate are joined by deionized water and oxalic acid in mass ratio for 20:1 prepares in the solution formed by the mass ratio of 0.8:5 respectively, stir until ammonium metavanadate and ammonium paratungstate are dissolved in oxalic acid solution at 60 DEG C, become solution 1;
Step 2: the solution respectively barium nitrate, magnesium nitrate, strontium nitrate or its mixture being configured to 1wt% joins in titanium dioxide and Ludox mixed liquor and floods stirring 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 (5-20) with the mass ratio of titanium dioxide: (95-80);
Step 3: poured into by solution 1 and flood stirring in the suspension 1 of same volume and be heated to 80 DEG C after 1 hour, continue to be stirred to pasty state, 120 DEG C of oven dry, the mass ratio of the solid matter wherein in ammonium metavanadate, ammonium paratungstate and suspension 1 is 0.8:5:94.2;
Step 4: smashed to pieces by the block of oven dry, calcines in atmosphere after 5 hours for 550 DEG C and obtains 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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CN103920489B (en) * 2014-04-16 2016-04-13 清华大学 One effectively suppresses SO 2the preparation method of the denitrating catalyst of oxidation
CN104525216B (en) * 2014-12-11 2017-01-04 清华大学 Denitrating catalyst under the conditions of wide temperature window high-sulfur 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
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
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
CN111330609B (en) * 2020-02-21 2023-02-24 大唐南京环保科技有限责任公司 Denitration catalyst resistant to alkali metal poisoning and preparation method thereof
CN113413742A (en) * 2021-07-15 2021-09-21 山东国舜建设集团有限公司 Flue gas magnesium desulfurization treatment method
CN114433083B (en) * 2021-12-29 2023-06-16 深圳华明环保科技有限公司 Preparation method of catalyst for denitration and degradation of dioxin
CN115501872B (en) * 2022-09-19 2024-03-15 山西格盟普丽环境股份有限公司 High Wen Tuoxiao catalyst for flue gas of gas generator set and preparation method thereof

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