CN102513095B - Medium temperature denitration catalyst with carbon-based material loaded with cerium tungsten and preparation method of medium temperature denitration catalyst - Google Patents
Medium temperature denitration catalyst with carbon-based material loaded with cerium tungsten and preparation method of medium temperature denitration catalyst Download PDFInfo
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- CN102513095B CN102513095B CN 201110375073 CN201110375073A CN102513095B CN 102513095 B CN102513095 B CN 102513095B CN 201110375073 CN201110375073 CN 201110375073 CN 201110375073 A CN201110375073 A CN 201110375073A CN 102513095 B CN102513095 B CN 102513095B
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Abstract
The invention discloses a medium temperature selective catalytic reduction denitration catalyst with favorable activity and selectivity. The catalyst takes a carbon-based material as a carrier, an oxide of cerium as an active material, and tungsten trioxide as a promoter, wherein the carbon-based material is one of activated carbon, activated carbon fiber or a carbon nano tube. The invention also discloses a preparation method of the catalyst, which comprises the following steps: carrying out purification and surface activation on the carbon-based material by concentrated nitric acid, and then loading the active material and the promoter by adopting an immersion method. The catalyst disclosed by the invention has favorable denitration activity and selectivity in the temperature range of 230 DEG C-420 DEG C, is a very good medium temperature denitration catalyst, and has better application prospect.
Description
Technical field
The present invention relates to the air pollution control technique field, be specifically related to a kind of denitrifying catalyst with selective catalytic reduction and preparation technology thereof, be applicable to flue-gas temperature and be the denitrating flue gas of 230~420 ℃.
Background technology
Sulfur dioxide and nitrogen oxide are the main gas pollutants that causes acid rain, and wherein nitrogen oxide also can cause the generation of photochemical fog.Along with generally applying of flue gas desulfurization technique, the discharge capacity of sulfur dioxide is effectively controlled, but the discharge capacity of nitrogen oxide but is not effectively controlled.For satisfying the needs of sustainable development and environmental protection, China had carried forward vigorously control and the improvement of nitrogen oxide in recent years, and new discharged nitrous oxides standard is also ready to appear.
Nitrogen oxide can be divided into moving source and stationary source according to the source, and stationary source is take various discharged from coal-fired boiler as main, and the denitration technology of its main flow is SCR (SCR) denitration technology.The SCR denitration technology is applied in developed countries such as Europe, the United States, days at present, is gas denitrifying technology most widely used in world wide, that occupation rate of market is the highest, operation is the most reliable and the most stable.That most SCR denitrification apparatus adopts is V
2O
5-WO
3/ TiO
2Or V
2O
5-MoO
3/ TiO
2Catalyst, this class catalytic component based on vanadium active temperature windows focuses mostly at 300~450 ℃.
The SCR denitration technology can be divided into the SCR of the high grey SCR that arranges, the low grey SCR that arranges and end layout according to the position difference.The SCR device that high ash is arranged is between economizer and air preheater, and flue-gas temperature is many at 300~400 ℃, so V
2O
5-WO
3/ TiO
2And V
2O
5-MoO
3/ TiO
2Catalyst is very applicable; After the SCR device that end is arranged was positioned at dust arrester and desulfurizer, its flue-gas temperature was too low, and the SCR device that early stage Europe and Japanese end are arranged all needs flue gas is carried out heat again, and this arrangement can cause cost to increase; After the SCR device that low ash is arranged was positioned at dust arrester, arrangement can effectively be alleviated arsenic in ash content, alkali and alkaline earth metal ions etc. to the murder by poisoning of catalyst like this, but flue-gas temperature has decline before than dedusting, and in most of situation, flue-gas temperature is not at V
2O
5-WO
3/ TiO
2And V
2O
5-MoO
3/ TiO
2In the optimum working temperature scope of catalyst, cause denitration efficiency as one wishes not to the utmost.Therefore in the situation that not to flue gas reheat, if select the catalyst (middle temperature denitrating catalyst) of optimum working temperature in the SCR device flue-gas temperature scope that low ash is arranged, effective life-span of extending catalyst, and then reduction denitration cost.
Less about the patent of middle temperature denitrating catalyst both at home and abroad at present, application number is that 200710121422.4 Chinese invention patent discloses the ferrotitanium composite oxides thing catalyst that is used for ammine selectivity catalytic reduction nitrous oxides, and this catalyst can be used for the SCR denitrification apparatus that low ash is arranged.In document, (Catalysis Communications 12 (2011) 394-398) have reported that cerium oxide loads on that to have good low-temperature denitration on NACF active.Disclosed by the invention is a kind of catalyst of carbon based material cerium-carrying tungsten, this catalyst has higher activity and selectivity between 250~400 ℃, therefore be highly suitable for the SCR denitrification apparatus that low ash is arranged, these catalyst raw material wide material sources, preparation technology are simple, are a kind of good middle temperature catalysts.
Summary of the invention
The invention provides a kind of have excellent activity and optionally in warm denitrating catalyst and preparation technology thereof, described middle temperature denitrating catalyst take carbon based material as carrier, the oxide of cerium is co-catalyst as active material, tungstic acid.
The raw material of described middle temperature denitrating catalyst consists of the soluble-salt of carbon based material, water, cerium and the soluble-salt of tungsten, and the mol ratio between each raw material is:
Carbon based material: 1
Water: 10~1000
The soluble-salt of cerium: 0.0001~0.1
The soluble-salt of tungsten: 0.0001~0.2
Described carbon based material is a kind of in active carbon, NACF or CNT.Described active carbon is a kind of in cocoanut active charcoal, active fruit shell carbon, coal mass active carbon or wood powder shaped activated carbon, and described CNT is single-walled nanotube or many walls nanotube.
The preparation technology of above-mentioned catalyst comprises the following steps:
(1) purification process of carbon based material and surface activation process: be that 60%~90% red fuming nitric acid (RFNA) soaks carbon based material with mass fraction, and stirred in the water bath with thermostatic control of 70~90 ℃ 2~10 hours, then be 6~7 with deionized water rinsing to pH, oven dry under 60~150 ℃ at last;
(2) infusion process carrying active substance and co-catalyst: first the soluble-salt of cerium and the soluble-salt decibel of tungsten are configured to cerium solution and tungsten solution; then the carrier carbon based material that step (1) is obtained joins in the mixed solution of cerium solution and tungsten solution and stirred 2~20 hours; then oven dry under 60~150 ℃; under last nitrogen protection, calcination is 2~10 hours, and calcination temperature is 300~700 ℃.
A lot of carbon based materials contain many impurity, and Fe, Co, Ni such as containing a small amount of amorphous carbon and trace in coal mass active carbon contain a small amount of amorphous carbon in CNT, and the nitric acid purification process can be got rid of these impurity to the impact of catalyst.Simultaneously the carbon based material surface after nitric acid treatment has been introduced into a large amount of oxy radicals and nitrogen-containing group, and this is conducive to the Uniform Dispersion of active component.
Cerium oxide because of environmental friendliness, have the characteristic such as oxygen storage capacity, in recent years by extensively with and catalytic field.In the catalyst take cerium oxide as active material, cerous existence has important function to the activity of catalyst, manages to improve cerous content and often can effectively improve the activity of catalyst.In the present invention, the oxide of cerium and tungstic acid all form in the calcination process, strong reciprocation can occur between both, finally cause more trivalent cerium to generate.In addition, the interpolation of tungstic acid has increased catalyst surface can be for the adsorption potential of reacting gas absorption, and this is conducive to the carrying out of catalytic reaction.Therefore, the interpolation of tungsten can effectively improve the activity of catalyst.
Catalyst preparation process disclosed by the invention is simple and practical, the denitrating catalyst of preparation has good denitration activity, selective and stable, be that 230~420 ℃, air speed are that the denitration efficiency of catalyst under the condition of 100000h-1 can be kept more than 80% in reaction temperature, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 90%.This catalyst be a kind of well in warm denitrating catalyst, have application prospect preferably.
The specific embodiment
Embodiment 1:
Catalyst raw material mol ratio is CNT, water, cerium nitrate and ammonium tungstate.CNT makes with chemical vapour deposition technique, first soaks CNT with 68% red fuming nitric acid (RFNA), and stirs 2 hours in the water bath with thermostatic control of 80 ℃, is then 6.5 with deionized water rinsing to pH, oven dry under 80 ℃ at last.Get the CNT that 2 gram nitric acid treatment are crossed, toward wherein adding 0.2 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 0.5 gram ammonium tungstate (with appropriate saturated oxalic acid solution dissolving), the rear 80 ℃ of oven dry that stir, then 350 ℃ of calcinations namely got the catalyst finished product in 3 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 85%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 95%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O
25%.
Embodiment 2:
Catalyst raw material mol ratio is active carbon, water, cerium nitrate and ammonium tungstate.Active carbon is coal mass active carbon, first soaks active carbon with 68% red fuming nitric acid (RFNA), and stirs 4 hours in the water bath with thermostatic control of 80 ℃, is then 6 with deionized water rinsing to pH, oven dry under 100 ℃ at last.Get the active carbon that 2 gram nitric acid treatment are crossed, toward wherein adding 0.05 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 0.08 gram ammonium tungstate (with appropriate saturated oxalic acid solution dissolving), the rear 80 ℃ of oven dry that stir, then 450 ℃ of calcinations namely got the catalyst finished product in 3 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 80%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 90%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O
25%.
Embodiment 3:
Catalyst raw material mol ratio is NACF, water, cerium nitrate and ammonium tungstate.First soaking NACF with 68% red fuming nitric acid (RFNA), and stirred 4 hours in the water bath with thermostatic control of 80 ℃, is then 6.5 with deionized water rinsing to pH, oven dry under 80 ℃ at last.Get the NACF that 2 gram nitric acid treatment are crossed, toward wherein adding 1 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 1.2 gram ammonium tungstates (with appropriate saturated oxalic acid solution dissolving), the rear 60 ℃ of oven dry that stir, then 550 ℃ of calcinations namely got the catalyst finished product in 3 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 80%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 90%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O
25%.
Embodiment 4:
Catalyst raw material mol ratio is active carbon, water, cerium nitrate and ammonium tungstate.Active carbon is active fruit shell carbon, first soaks active carbon with 68% red fuming nitric acid (RFNA), and stirs 5 hours in the water bath with thermostatic control of 80 ℃, is then 6.5 with deionized water rinsing to pH, oven dry under 100 ℃ at last.Get the active carbon that 2 gram nitric acid treatment are crossed, toward wherein adding 1.5 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 2 gram ammonium tungstates (with appropriate saturated oxalic acid solution dissolving), the rear 80 ℃ of oven dry that stir, then 650 ℃ of calcinations namely got the catalyst finished product in 4 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 80%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 90%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O
25%.
Embodiment 5:
Catalyst raw material mol ratio is CNT, water, cerium nitrate and ammonium tungstate.CNT makes with chemical vapour deposition technique, first soaks CNT with 68% red fuming nitric acid (RFNA), and stirs 4 hours in the water bath with thermostatic control of 80 ℃, is then 6.5 with deionized water rinsing to pH, oven dry under 150 ℃ at last.Get the CNT that 2 gram nitric acid treatment are crossed, toward wherein adding 0.2 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 0.2 gram ammonium tungstate (with appropriate saturated oxalic acid solution dissolving), the rear 80 ℃ of oven dry that stir, then 300 ℃ of calcinations namely got the catalyst finished product in 3 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 85%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 95%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O
25%.
Embodiment 6:
Catalyst raw material mol ratio is CNT, water, cerium nitrate and ammonium tungstate.CNT makes with chemical vapour deposition technique, first soaks CNT with 68% red fuming nitric acid (RFNA), and stirs 4 hours in the water bath with thermostatic control of 80 ℃, is then 6.5 with deionized water rinsing to pH, oven dry under 80 ℃ at last.Get the CNT that 2 gram nitric acid treatment are crossed, toward wherein adding 3 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 2 gram ammonium tungstates (with appropriate saturated oxalic acid solution dissolving), the rear 80 ℃ of oven dry that stir, then 350 ℃ of calcinations namely got the catalyst finished product in 3 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 85%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 95%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O2 5%.
Embodiment 7:
Catalyst raw material mol ratio is CNT, water, cerium nitrate and ammonium tungstate.CNT makes with chemical vapour deposition technique, first soaks CNT with 68% red fuming nitric acid (RFNA), and stirs 10 hours in the water bath with thermostatic control of 60 ℃, is then 6.5 with deionized water rinsing to pH, oven dry under 80 ℃ at last.Get the CNT that 2 gram nitric acid treatment are crossed, toward wherein adding 5 gram Ce (NO
3)
36H
2O (with appropriate water-soluble solution) and 3 gram ammonium tungstates (with appropriate saturated oxalic acid solution dissolving), the rear 80 ℃ of oven dry that stir, then 700 ℃ of calcinations namely got the catalyst finished product in 3 hours under nitrogen protection.
The catalyst of preparation is put into the fixed bed quartz tube reactor carry out activity and selectivity test, reaction temperature is that 230~420 ℃, air speed are 100000h
-1Condition under, denitration efficiency is stabilized in more than 85%, substantially can't detect the generation of laughing gas, in 250~400 ℃, reaction temperature interval, denitration efficiency is stabilized in more than 95%.Simulated flue gas is by N
2, O
2, NO, NH
3And SO
2Form NO 600ppm wherein, NH
3600ppm, SO
21000ppm, O
25%.
Above-described embodiment is several typical specific embodiments of the present invention, and those skilled in the art can make various modifications within the scope of the appended claims.
Claims (5)
1. the middle temperature denitrating catalyst of a carbon based material cerium-carrying tungsten is characterized in that: described middle temperature denitrating catalyst is take carbon based material as carrier, take the oxide of cerium as active material, take tungstic acid as co-catalyst;
The preparation method of described middle temperature denitrating catalyst, comprise the following steps: take the soluble-salt of the soluble-salt of carbon based material, water, cerium and tungsten as raw material, be first that 60%~90% red fuming nitric acid (RFNA) carries out purification process and surface activation process to carbon based material with mass fraction, then use infusion process carrying active substance and co-catalyst on the carbon based material carrier;
The purification process of described carbon based material and surface activation process are: be that 60%~90% red fuming nitric acid (RFNA) soaks carbon based material with mass fraction, and stirred in the water bath with thermostatic control of 70~90 ℃ 2~10 hours, then be 6~7 with deionized water rinsing to pH, oven dry under 60~150 ℃ at last;
Describedly with infusion process method of carrying active substance and co-catalyst on the carbon based material carrier be: first the soluble-salt of cerium and the soluble-salt of tungsten are configured to cerium solution and tungsten solution; then the carbon based material after purified processing and surface activation process is joined in the mixed solution of cerium solution and tungsten solution and stirred 2~20 hours; then oven dry under 60~150 ℃; under last nitrogen protection, calcination is 2~10 hours, and calcination temperature is 300~700 ℃.
2. middle temperature denitrating catalyst as claimed in claim 1 is characterized in that: described carbon based material is a kind of in active carbon, NACF or CNT.
3. middle temperature denitrating catalyst as claimed in claim 2 is characterized in that: described active carbon is a kind of in cocoanut active charcoal, active fruit shell carbon, coal mass active carbon or wood powder shaped activated carbon.
4. middle temperature denitrating catalyst as claimed in claim 2, it is characterized in that: described CNT is single-walled nanotube or many walls nanotube.
5. middle temperature denitrating catalyst as claimed in claim 1, it is characterized in that: the mol ratio of the preparation method's of described middle temperature denitrating catalyst raw material is:
Carbon based material: 1;
Water: 10~1000;
The soluble-salt of cerium: 0.0001~0.1;
The soluble-salt of tungsten: 0.0001~0.2.
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CN103785374B (en) * | 2014-02-20 | 2015-10-14 | 重庆大学 | A kind of C nano pipe demercuration catalyst and preparation method thereof |
CN104148055B (en) * | 2014-08-22 | 2016-03-02 | 北京中南亚太环境科技发展有限公司 | A kind of denitrating catalyst |
CN105921181B (en) * | 2016-04-29 | 2019-02-22 | 苏州科博思环保科技有限公司 | A kind of high-quality desulphurization denitration catalyst and its preparation method and application |
CN106345453A (en) * | 2016-08-26 | 2017-01-25 | 成都国化环保科技有限公司 | Carbon-based material low-temperature denitrification catalyst and preparation method thereof |
CN112823884A (en) * | 2019-11-21 | 2021-05-21 | 中冶京诚工程技术有限公司 | Active carbon carrier iron-based NH3-SCR catalyst, preparation method and application |
CN111686716B (en) * | 2020-07-29 | 2022-06-14 | 江西省生态环境科学研究与规划院 | WOxLow-temperature SCR (selective catalytic reduction) flue gas denitration catalyst with modified carbon nano tube loaded with metal oxide, and preparation method and application thereof |
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Application publication date: 20120627 Assignee: ZHEJIANG TIANLAN ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Assignor: ZHEJIANG University Contract record no.: X2021330000040 Denomination of invention: A carbon based material supported cerium tungsten medium temperature denitration catalyst and its preparation method Granted publication date: 20130612 License type: Common License Record date: 20210513 |