CN102861565A - Aluminum oxide-loaded cerium oxide catalyst and preparation method and application thereof - Google Patents
Aluminum oxide-loaded cerium oxide catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an aluminum oxide-loaded cerium oxide catalyst and a preparation method and application thereof. Calculated by mass ratio, the mass ratio of aluminum oxide to cerium oxide in the aluminum oxide-loaded cerium oxide catalyst is 85:15. The preparation method for the aluminum oxide-loaded cerium oxide catalyst is characterized in that by adopting an equivalent-volume impregnation method, a coprecipitation method or a sol-gel method, the finally obtained aluminum oxide-loaded cerium oxide catalyst is higher in denitration activity at the lower reaction temperature of 200 DEG C when being used in a selective catalytic reduction flue gas denitration process, and the denitration efficiency can reach at least 90 percent, and thereby, the abuse that the reaction temperature of a traditional catalyst is high is overcome.
Description
Technical field
The present invention relates to the catalyst for denitrating flue gas technical field, be specifically related to a kind of alumina load cerium oxide catalyst and its preparation method and application.
Background technology
Nitrogen oxide NO
xit is one of generally acknowledged Air Pollutants in countries in the world.It damages the ozone layer, and forms acid rain and photochemical fog, influence ecological environment, and harm humans health, the reduction of discharging of nitrogen oxide at present has been subject to people and has paid close attention to greatly.Fire coal be take as main developing country in China, and coal fire discharged nitrogen oxide is the main artificial source of causing the nitrogen oxide environmental pollution.Power plants discharged nitrous oxides total amounts in 2009 reach the fast development of 1,860 ten thousand tons of Chinese national economy, make China's coal fired power generation installed capacity increase sharply, scholarly forecast is arranged: if further do not take effective measures to control the discharge of nitrogen oxide, China's nitrogen oxide emission will continue to increase, and the year two thousand twenty will reach 2,900 ten thousand tons of left and right.Increasingly stringent along with the Environmental Protection in China requirement, adding of law enforcement dynamics is tight, SCR (Selective Catalytic Reduction, SCR) gas denitrifying technology becomes because of its denitration rate high (can reach more than 90%), technology maturation the first-selection that coal-fired power station boiler is controlled the NOx discharge.
Catalyst is the core of SCR gas denitrifying technology, and its formula, structure and surface area have a significant impact the effect of NO_x removal.In the process of SCR system operation, catalyst can be because various physics chemical action (poisoning, wearing and tearing, thermal sintering, obstruction/contamination etc.) and lost efficacy, and these are all closely related with the fuel characteristic of boiler.Due to the restriction that is subject to coal resources in China and fuel full-line policy, the quality of power plants fire coal is usually poor, and, in recent years due to coal in China relation between market supply and demand anxiety, the coal for power generation quality is always on a declining curve in recent years, the ash in coal and sulfur rise.China's steam coal is compared with World Developed Countries, and quality is in reduced levels, and the ash content of steam coal is less than 15% in the world, by this, weighs, and China only has 20% steam coal product quality can reach standard.Cause like this power plants complicated, various by the coal class, particularly burning inferior coal and operation coal frequent variations, make coal-fired power plant continue the off-design coal and check coal, in addition, the composition of China's fire coal is extremely complicated, and it is varied that the richness of element in coal deposited state.Therefore be badly in need of exploring the impact of thermal power plant coal qualitative change on the SCR catalyst activity, in Study on Coal different component separately and the various ingredients stack to the mechanism of action of SCR catalyst, the deactivation law of understanding catalyst, this is to reducing catalyst activity rate of decay, extending catalyst service life, reduce thermal power plant's denitration cost, promoting that applying of gas denitrifying technology has important practical significance, for the operation of SCR provides the theoretical direction foundation.Due to nano Ce O
2specific area large, chemism is high, Heat stability is good, good storage oxygen and oxygen release ability, can change the deployment conditions of active component on carrier in catalyst, obviously improve its catalytic performance, and can improve high-temperature thermal stability performance, mechanical performance and the high temperature oxidation resistance of carrier.In addition, CeO
2also in noble metal atmosphere, play stabilization, improve NO
xconversion ratio, and make catalyst keep mithridatism and higher catalytic activity preferably.And be applied to the NH of catalysis hydroxide about the load cerium oxide catalyst
3-SCR reaction has not yet to see bibliographical information.
Summary of the invention
The object of the invention is in order to improve high-temperature thermal stability performance, mechanical performance and the high temperature oxidation resistance of catalyst, make it in lower temperature range, have this technical problem of higher denitration activity and a kind of alumina load cerium oxide catalyst and preparation method thereof is provided.This alumina load cerium oxide catalyst has operation to be interrupted, and the active component depression is dispersed in carrier surface, increases surface area, can have at lower temperature window the advantage of higher denitration activity.
Technical scheme of the present invention
A kind of alumina load cerium oxide catalyst, calculate in mass ratio, i.e. aluminium oxide: cerium oxide is 85:15.
The preparation method of above-mentioned a kind of alumina load cerium oxide catalyst, can adopt conventional equi-volume impregnating, coprecipitation, sol-gal process or citric acid method etc., the present invention is only with equi-volume impregnating, and coprecipitation and sol-gal process are given an example, specific as follows:
the equi-volume impregnating preparationthe alumina load cerium oxide catalyst, step is as follows:
By the gamma aluminium oxide be dissolved in deionized water after cerous nitrate or cerous acetate are mixed, and make its thorough impregnation just saturated, adopt the polytetrafluoroethylene (PTFE) paddle under 20-100 ℃, controlling stir speed (S.S.) is that 200-600rpm stirs 0.5-3h, dry 4-12h under 80-110 ℃ then, then at the N of 300ml/min
2atmosphere, 600 ℃ are at tubular type kiln roasting 1-12h, and cerous nitrate or cerous acetate high temperature are decomposed into cerium oxide fully, and the gamma aluminium oxide is constant, then are cooled to room temperature and obtain the alumina load cerium oxide catalyst.
the coprecipitation preparationthe alumina load cerium oxide catalyst, step is as follows:
?cerous nitrate and aluminum nitrate are dissolved in deionized water, at room temperature adopt the speed stirring and dissolving of polytetrafluoroethylene (PTFE) paddle with 200-600rpm, then to the inside, add the ammoniacal liquor of 3mol/L to adjust pH to stir 1-3h after 5-11 to carry out static heavy surely, again filter after rinsing well by the sedimentation and filtration of gained and by deionized water;
After again filtering, gained is deposited in to dry 6-12h under 80-100 ℃, then at the N of 1L/min
2atmosphere, 600 ℃ are at tubular type kiln roasting 5-12h, and cerous nitrate or cerous acetate high temperature are decomposed into cerium oxide fully, and aluminum nitrate high temperature is decomposed into aluminium oxide fully, then are cooled to room temperature and obtain the alumina load cerium oxide catalyst.
the sol-gal process preparationthe alumina load cerium oxide catalyst, step is as follows:
?aluminium isopropoxide is mixed with to solution with being dissolved in deionized water after cerous nitrate or cerous acetate are mixed, at room temperature adopting polytetrafluoroethylene (PTFE) paddle mixing control stir speed (S.S.) is 100-600rpm, add wherein nitric acid, make the mol ratio 0.05-0.1 of total metal ion molar concentration and nitric acid, make colloidal sol;
Then the colloidal sol dry 12h under 80-100 ℃ made is made to xerogel, finally the N at 300ml/min by the xerogel that makes
2atmosphere, 600 ℃ are at tubular type kiln roasting 3-12h, and cerous nitrate or cerous acetate high temperature are decomposed into cerium oxide fully, and aluminium isopropoxide high temperature is decomposed into aluminium oxide fully, then are cooled to room temperature and obtain the alumina load cerium oxide catalyst.
The application of a kind of alumina load cerium oxide catalyst in denitrification process of above-mentioned gained, step is as follows:
Denitration starts frontly first with the NO in simulated flue gas, to pass into the about 1-2h of fixed bed reactors, allows alumina load cerium oxide catalyst absorption NO reach capacity, and avoids causing because of the absorption of alumina load cerium oxide catalyst the minimizing of NO; After alumina load cerium oxide catalyst absorption NO reaches capacity, the flue gas for the treatment of denitration is passed into to fixed bed reactors and control reaction temperature at 200-400 ℃, flow velocity is 500ml/min, space velocity 10000-30000h
-1, under the effect of alumina load cerium oxide catalyst, the NH in flue gas
3nO is reduced to N
2gas, reacted gaseous mixture absorbs unreacted NH through phosphoric acid solution
3enter atmosphere by blast pipe, thereby reach the purpose of denitrating flue gas;
Described simulated flue gas forms: NO200-600ppm, NH
3200
-600ppm and O
2for 0-5%, remaining gas N
2as Balance Air.
Beneficial effect of the present invention
A kind of alumina load cerium oxide catalyst of the present invention, due in porous material, the gamma aluminium oxide is one of crystalline material of the most frequently used catalytic adsorption agent carrier.Aluminium oxide is because the improvement to catalyst-sorbent of its good mechanical features and desirable pore property plays an important role.Due to nano Ce O
2specific area large, chemism is high, Heat stability is good, good storage oxygen and oxygen release ability, can change the deployment conditions of active component on carrier in catalyst, obviously improve its catalytic performance, and can improve high-temperature thermal stability performance, mechanical performance and the high temperature oxidation resistance of carrier, CeO
2also in noble metal atmosphere, play stabilization, improve CO, CH
4and NO
xconversion ratio, therefore make the final alumina load cerium oxide catalyst formed keep mithridatism and higher catalytic activity preferably.
The incipient impregnation method prepares the alumina load cerium oxide catalyst, simple to operate because of it, and the advantage that controllability is strong obtains higher denitration activity in actual denitration activity experiment, at the low temperature windows of 200 ℃, can remain on more than 88%.
Coprecipitation is the method that a kind of the most effective method prepares the alumina load cerium oxide, obtains homodisperse, nano level cerium particle, although coprecipitation is simple to operate, relatively is difficult to control.In each process of system, there is several factors to need to consider, the order of addition of the pH value of solution, ageing time, filtration washing, various precursor compounds and add difference of mode etc. during such as the degree of mixing, precipitation temperature, precipitation, all may produce impact clearly to experimental result.So the present invention has further determined above parameter, obtains optimal value, prepare efficient alumina load cerium oxide catalyst, can reach the denitration rate more than 90% equally when 200 ℃ of low temperature windows.
Sol-gal process prepares the alumina load cerium oxide catalyst, by determining experiment condition, determines cerium source and carrier, draws efficient low-temperature SCR catalyst, at 200 ℃ of low temperature window ceriums, can reach the denitration rate more than 92%.
The specific embodiment
Below by specific embodiment, the present invention is further set forth, but do not limit the present invention
.
Catalytic reactor used in embodiments of the invention adopts the fixed bed reactors that internal diameter is 14mm, and unstripped gas enters fixed bed reactors through preheating, and reaction temperature is at 200 ~ 400 ℃, and flow velocity is 500ml/min, space velocity 23000h
-1, alumina load cerium oxide catalyst 5g.
Simulated flue gas forms: NO600ppm, NH
3600ppm and O
2be 5%, remaining gas N
2as Balance Air, gas flow is controlled by mass flowmenter CS200.
The specification of the various raw materials that the present invention is used and the information of manufacturer please be supplemented.
| Reagent name | Molecular formula | CAS | Specification | Packing | Manufacturer |
| Cerous nitrate, six water | CeN 3O 9·6H 2O | 10294-41-4 | 99.5% metals basis | 100g | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
| Cerous acetate | （CH 3CO 2）3Ce·xH 2O | 206996-60-3 | 99.5% metals basis | 100g | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
| Activated alumina | Al 2O 3 | 1302-74-5 | 40-60 order GC | 100g | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
| Aluminum nitrate, nine water | Al（NO 3） 3·9H 2O | 7784-27-2 | 99.99%metals basis | 500g | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
| Aluminium isopropoxide | C 9H 21AlO 3 | 555-31-7 | 99.99%metals basis | 100g | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
| Ammoniacal liquor | H 5NO | 1336-21-6 | AR | 500ml | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
| Red fuming nitric acid (RFNA) | HNO 3 | 7697-37-2 | AR | 500ml | The brilliant pure Industrial Co., Ltd. of Aladdin reagent (Shanghai) |
embodiment 1
A kind of alumina load cerium oxide catalyst, calculate by mass percentage, i.e. aluminium oxide: cerium oxide is 85:15.
The preparation method of above-mentioned a kind of alumina load cerium oxide catalyst, be prepared by equi-volume impregnating, and step is as follows:
Two parts of 0.85g gamma aluminium oxide be impregnated in respectively in the 0.15g cerous nitrate and 0.15g cerous acetate solution prepared, under 50 ℃, adopt the polytetrafluoroethylene (PTFE) paddle to stir, it is 200rpm that whipping process is controlled stir speed (S.S.), time 1h, dry 12h under 110 ℃ respectively then, then respectively at the N of 300ml/min
2atmosphere, 600 ℃ is at tubular type kiln roasting 5h, then is cooled to respectively room temperature and obtains CeO
2load capacity be 15% alumina load cerium oxide catalyst A and B.
embodiment 2
A kind of alumina load cerium oxide catalyst, calculate by mass percentage, i.e. aluminium oxide: cerium oxide is 85:15.
The preparation method of above-mentioned a kind of alumina load cerium oxide catalyst, be prepared by coprecipitation, and step is as follows:
0.15g cerous nitrate and 0.15g cerous acetate are dissolved in deionized water with the 6.255g aluminum nitrate respectively, at room temperature adopt the polytetrafluoroethylene (PTFE) paddle, speed stirring and dissolving with 200rpm, then adding respectively the ammoniacal liquor tune pH of 3mol/L is 11, after stirring 3h, by sedimentation and filtration and by deionized water, rinse well;
Then by gained precipitation dry 12h under 100 ℃ respectively, then respectively at the N of 1L/min
2atmosphere, 600 ℃ is at tubular type kiln roasting 5h, then is cooled to respectively room temperature and obtains CeO
2load capacity be 15% alumina load cerium oxide catalyst C and D.
embodiment 3
A kind of alumina load cerium oxide catalyst, calculate by mass percentage, i.e. aluminium oxide: cerium oxide is 85:15.
The preparation method of above-mentioned a kind of alumina load cerium oxide catalyst, be prepared by sol-gal process, and step is as follows:
Claim the 3.405g aluminium isopropoxide to be dissolved in and to be mixed with solution with 0.15g cerous nitrate and 0.15g cerous acetate respectively, at room temperature adopt the polytetrafluoroethylene (PTFE) paddle, the control stir speed (S.S.) is 200rpm, and the nitric acid of 0.1mol/L that adds respectively wherein 1.2ml makes colloidal sol as peptizing agent;
Then by the colloidal sol that makes respectively under 80 ℃ dry 12h make xerogel, finally by the xerogel that makes respectively at the N of 300ml/min
2atmosphere, 600 ℃ is at tubular type kiln roasting 5h, then is cooled to respectively room temperature and obtains CeO
2load capacity be 15% alumina load cerium oxide catalyst E and F.
application Example 1
Utilize the load capacity of the cerium base of embodiment 1, embodiment 2 and embodiment 3 gained to be respectively 15% alumina load cerium oxide catalyst A, B, C, D, E, F and typical catalyst (the titania based SCR catalyst of the Cormetech of the U.S.) and carry out respectively the denitration activity experiment
Experiment test starts frontly first with the NO in simulated flue gas, to pass into the about 1h of fixed bed reactors, makes alumina load cerium oxide catalyst absorption NO saturated, is mainly to cause the minimizing of NO for fear of the absorption because of the alumina load cerium oxide catalyst;
After each component of simulated flue gas is mixed in gas mixed box, then pass into fixed bed reactors under the effect of alumina load cerium oxide catalyst, NH
3nO is reduced to N
2, reacted gaseous mixture absorbs unreacted NH through phosphoric acid solution
3enter atmosphere by blast pipe, NO concentration adopts the Model60I flue gas analyzer of U.S.'s thermoelectricity to detect, its denitration the results are shown in following table:
| ? | Raw material | The preparation method | Reaction temperature (℃) | Conversion ratio (%) |
| Typical catalyst | ? | ? | 200 | 35 |
| Catalyst A | Gamma aluminium oxide, cerous nitrate | Equi-volume impregnating | 200 | 87.13 |
| Catalyst B | Gamma aluminium oxide, cerous acetate | Equi-volume impregnating | 200 | 88.91 |
| Catalyst C | Aluminum nitrate, cerous nitrate | Coprecipitation | 200 | 93.2 |
| Catalyst D | Aluminum nitrate, cerous acetate | Coprecipitation | 200 | 92.17 |
| Catalyst E | Aluminium isopropoxide, cerous nitrate | Sol-gal process | 200 | 96.71 |
| Catalyst F | Aluminium isopropoxide, cerous acetate | Sol-gal process | 200 | 95.91 |
As can be seen from the above table, alumina load cerium oxide denitrating catalyst described in the present invention is than typical catalyst of the prior art (the titania based SCR catalyst of the Cormetech of the U.S.), there is higher denitration activity at low-temperature region, after alumina load cerium oxide catalyst application in the present invention simultaneously, its denitration rate is minimum all is greater than 87%, the highlyest all reach more than 96%, visible alumina load cerium oxide catalyst of the present invention has very high catalytic oxidative, for nitrogen oxide, very high removal activity is arranged.And manufacture craft is simple, handled easily, Modulatory character can be strong, can change load capacity and respective carrier is adjusted activity.
Above said content is the basic explanation under conceiving for the present invention only, and any equivalent transformation that technical scheme according to the present invention is done all belongs to the scope of protection of the invention.
Claims (5)
1. an alumina load cerium oxide catalyst, it is characterized in that described alumina load cerium oxide catalyst calculates by mass percentage, i.e. aluminium oxide: cerium oxide is 85:15.
2. the preparation method of a kind of alumina load cerium oxide catalyst as claimed in claim 1 is characterized in that step is as follows:
At first the gamma aluminium oxide is mixed and is dissolved in deionized water with cerous nitrate or cerous acetate, make its thorough impregnation just saturated, controlling stir speed (S.S.) under 20-100 ℃ is that 200-600rpm stirs 0.5-3h, and dry 4-12h under 80-110 ℃ then, then at the N of 300ml/min
2atmosphere, 600 ℃ are cooled to room temperature and obtain the alumina load cerium oxide catalyst after tubular type kiln roasting 1-12h.
3. the preparation method of a kind of alumina load cerium oxide catalyst as claimed in claim 1 is characterized in that step is as follows:
Cerous nitrate and aluminum nitrate are dissolved in deionized water, at room temperature controlling speed of agitator is that 200-600rpm is dissolved, then to the inside, add the ammoniacal liquor of 3mol/L to adjust pH to stir 1-3h after 5-11 to carry out static heavy surely, by the sedimentation and filtration of gained and by deionized water, rinse well again and filter;
After again filtering, gained is deposited in to dry 6-12h under 80-100 ℃, then at the N of 1L/min
2atmosphere, 600 ℃ are cooled to room temperature and obtain the alumina load cerium oxide catalyst after tubular type kiln roasting 5-12h.
4. the preparation method of a kind of alumina load cerium oxide catalyst as claimed in claim 1 is characterized in that step is as follows:
Aluminium isopropoxide and cerous nitrate or cerous acetate are dissolved in deionized water and are mixed with solution, at room temperature controlling stir speed (S.S.) is that 100-600rpm stirs, add wherein nitric acid, making the molar concentration of total metallic aluminium and cerium ion and the mol ratio of nitric acid is 0.05-0.1:1, makes colloidal sol;
Then the colloidal sol dry 12h under 80-100 ℃ made is made to xerogel;
The last N at 300ml/min by the xerogel that makes
2atmosphere, 600 ℃ are cooled to room temperature and obtain the alumina load cerium oxide catalyst after tubular type kiln roasting 3-12h.
5. the application of a kind of alumina load cerium oxide catalyst as claimed in claim 1 in denitrification process is characterized in that step is as follows:
Denitration starts frontly first with the NO in simulated flue gas, to pass into the about 1-2h of fixed bed reactors, allow alumina load cerium oxide catalyst absorption NO reach capacity, after alumina load cerium oxide catalyst absorption NO reaches capacity, the flue gas for the treatment of denitration is passed into to fixed bed reactors and control reaction temperature at 200-400 ℃, flow velocity is 500ml/min, space velocity 10000-30000h
-1, under the effect of alumina load cerium oxide catalyst, the NH in flue gas
3nO is reduced to N
2gas, reacted gaseous mixture absorbs unreacted NH through phosphoric acid solution
3enter atmosphere by blast pipe, thereby reach the purpose of denitrating flue gas;
Described simulated flue gas forms: NO200-600ppm, NH
3200
-600ppm and O
2for 0-5%, remaining gas N
2as Balance Air.
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| CN104190394A (en) * | 2014-09-19 | 2014-12-10 | 西南化工研究设计院有限公司 | Honeycombed denitration catalyst taking titanium aluminum composite oxide as carrier and preparation method thereof |
| CN105498474A (en) * | 2015-11-28 | 2016-04-20 | 成都德善能科技有限公司 | Air purification method |
| CN105797577A (en) * | 2016-04-27 | 2016-07-27 | 华北电力大学 | Process and catalyst for catalytically reducing NOX by using methane |
| CN106693954A (en) * | 2016-11-22 | 2017-05-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Manganese oxide loaded cerium oxide catalyst, preparation and application |
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| CN104190394A (en) * | 2014-09-19 | 2014-12-10 | 西南化工研究设计院有限公司 | Honeycombed denitration catalyst taking titanium aluminum composite oxide as carrier and preparation method thereof |
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Application publication date: 20130109 |