CN102814191A - Low-temperature denitrated CeO2-NaX molecular sieve catalyst and preparation method thereof - Google Patents

Low-temperature denitrated CeO2-NaX molecular sieve catalyst and preparation method thereof Download PDF

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CN102814191A
CN102814191A CN2012103190564A CN201210319056A CN102814191A CN 102814191 A CN102814191 A CN 102814191A CN 2012103190564 A CN2012103190564 A CN 2012103190564A CN 201210319056 A CN201210319056 A CN 201210319056A CN 102814191 A CN102814191 A CN 102814191A
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molecular sieve
low
ceo
temperature
nax molecular
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郭瑞堂
周曰
潘卫国
徐宏建
于月良
何明福
闻雪平
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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Abstract

The invention discloses a low-temperature denitrated CeO2-NaX molecular sieve catalyst and a preparation method thereof. The low-temperature denitrated CeO2-NaX molecular sieve catalyst takes a NaX molecular sieve to load CeO2; and the mass ratio of the CeO2 to the NaX molecular sieve is (1-15):100. The preparation method comprises the following steps of: utilizing an equal volume immersing method to immerse the NaX molecular sieve into a soluble cerium salt solution and agitating and heating at 20-80 DEG C for 1-2 hours; then drying at 80-110 DEG C for 6-12 hours; roasting in an N2 atmosphere by controlling the temperature at 600 DEG C for 3-12 hours; and then cooling to a room temperature to obtain the low-temperature denitrated CeO2-NaX molecular sieve catalyst. The low-temperature denitrated CeO2-NaX molecular sieve catalyst disclosed by the invention has the advantages of higher catalytic performance, high-temperature heat stability, mechanism strength and high-temperature oxidization performance, and has the characteristics of simple preparation process, low production cost and suitableness for industrial production.

Description

A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst and preparation method thereof
Technical field
The present invention relates to the low-temperature denitration of flue gas field, be specifically related to a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst and preparation method thereof.
Background technology
SCR method (selective catalytic reduction) is that at present both at home and abroad the coal-burning power plant uses at most and the technology of the most ripe effective removal nitrogen oxide, and denitration efficiency can reach more than 90%, and it generally makes reducing agent with ammonia, injects at the upper reaches of air preheater to contain NO xFlue gas, NO under the effect of catalyst xBe reduced to N 2And water, wherein catalyst is the key factor of decision denitration efficiency, its operating temperature is 300～400 ℃.After the SCR reactor is arranged on electric cleaner, before the wet desulphurization device; Catalyst receives flying dust and impurity effect less; But the exhaust temperature of coal-fired flue-gas is generally at 150～220 ℃; Need flue gas is heated again, consumes energy, exploring the economic denitrating catalyst of low temperature becomes nitrogen oxide control technology development in future direction and key.The also just positive exploration of foreign scholar at present has the denitrating catalyst of low temperature active.
(selective catalytic reduction, SCR) owing to the ripe and efficient denitration technology that becomes stationary source main flows such as thermal power plant, its core mainly is (to comprise CO and H with NH3 or other hydro carbons to selective catalytic reduction 2Deng) as reducing agent, under the effect of catalyst, NO etc. is reduced into N 2And water.Wherein, with NH 3For the SCR technology of reducing agent has obtained extensive use because of its efficient is high.But traditional catalysts selective requires temperature at 300～400 ℃, for station boiler, must be placed on before the deduster, has shortened the service life of catalyst, has increased the difficulty that existing boiler denitration is transformed.Therefore, the SCR catalyst that research and development can cold operation can be arranged in after dedusting and the desulfurizer catalytic reactor, and is significant.The SCR catalysis technique enjoys favor because of characteristics such as its conversion ratio are high, selectivity is good, practical.The low-temperature SCR catalyst system and catalyzing of broad research is mainly with NH at present 3Be reducing agent, catalyst can be divided into 4 types: noble metal catalyst, molecular sieve catalyst, metal oxide catalyst and carbonaceous material catalyst.People such as Krishnan utilize artificial synthetic flue gas, to a kind of business level SCR Reduction of NO that contains precious metals pt xThe cryogenic property of CAT920LTTM is tested.Test result shows: at medium air speed (24000/ h), and when temperature is 150 ℃～200 ℃, NO xClearance is the highest to be merely 35%.This shows that existing commercial catalysts can't reach the desirable NO that removes at low temperatures xEffect must be developed novel low-temperature SCR catalyst.
At present, the development of low temperature catalyst mainly concentrates on following 2 aspects: (1) is to different carriers, like material with carbon element, metal oxide catalyst Al 2O 3, TiO 2Develop low-temperature SCR catalyst efficiently with metal ion exchanged molecular sieve catalyst ZSM-5 etc.; (2) cooperating the different activity material on the carrier efficiently,, make catalyst have high anti-SO like metal oxides such as V, W, Mn, Cu, Ni and Pt 2Active with steam.Discover that Cu oxide has good low-temperature catalysis characteristics, CuO/Al 2O 3With NH 3For reducing agent can reach the denitration rate more than 90%, but Cu oxide is to the SO in the flue gas 2Relatively more responsive.
To the development and application situation of present low-temperature SCR catalyst, should aspect following, do further research, in the hope of developing the low temperature catalyst that is fit to commercial Application.
(1), improve activity of such catalysts and selectivity, make it lower temperature (<200 ℃) and the temperature window of broad in have higher NO xConversion ratio;
(2), make catalyst have good anti-SO at low temperatures 2Character with materials such as water poison prolongs its service life;
(3), improve the mechanical strength and the heat endurance of catalyst, reduce the pressure loss, reduce cost, make it to have suitable commodity.
Summary of the invention
The objective of the invention is for solve have higher denitration rate in the temperature window that above-mentioned raising activity of such catalysts and selectivity make it to have low and broad and improve catalyst mechanical strength and heat endurance technical problem and a kind of low-temperature denitration CeO is provided 2-NaX molecular sieve catalyst and preparation method thereof.
Technical scheme of the present invention
A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 1-15:100.
Above-mentioned a kind of low-temperature denitration CeO 2The preparation method of-NaX molecular sieve catalyst, step is following:
Promptly adopt equi-volume impregnating; The NaX molecular sieve impregnated in the solubility cerium solution; 20-80 ℃ of following agitating heating 1-2h, preferably controlling stir speed (S.S.) is 200-600rpm, adopts the polytetrafluoroethylene (PTFE) paddle; Then dry 6-12h under 80-110 ℃ is the N of 300ml/min at preferred flow velocity then 2Atmosphere, control temperature are 600 ℃ of roasting 3-12h, are cooled to room temperature again and promptly obtain a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst.
Described solubility cerium salt is CeN 3O 96H 2O or (CH 3CO 2) 3CexH 2O;
Described NaX molecular sieve is Na 86[(AlO 2) 86(SiO 2) 106] xH 2O.
Above-mentioned a kind of low-temperature denitration CeO 2The application of-NaX molecular sieve catalyst in denitrification process, step is following:
Before beginning, denitration, lets low-temperature denitration CeO earlier with the about 1-2h of the feeding fixed bed reactors of the NO gas in the simulated flue gas component 2-NaX molecular sieve catalyst absorption NO reaches capacity, and can avoid because of low-temperature denitration CeO like this 2The absorption of-NaX molecular sieve catalyst causes the minimizing of NO; Treat low-temperature denitration CeO 2After-NaX molecular sieve catalyst absorption NO reaches capacity, the flue gas of treating denitration is got into fixed bed reactors control reaction temperature at 200-400 ℃, flow velocity is 1000ml/min, space velocity 20000-30000h -1, at low-temperature denitration CeO 2Under the effect of-NaX molecular sieve catalyst, the NH in the flue gas 3NO is reduced to N 2Gas, reacted gaseous mixture absorbs unreacted NH through phosphoric acid solution 3After blast pipe enters atmosphere, thereby reach the purpose of denitrating flue gas.
Described simulated flue gas is formed: NO200-600ppm, NH 3200-600ppm and O 2Be 0-5%, remaining gas N 2As balance gas.
Beneficial effect of the present invention
A kind of low-temperature denitration CeO of the present invention 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of X type 2, since load specific area big, chemism is high, Heat stability is good, good storage oxygen and the nano Ce O of oxygen release ability 2, therefore can obviously improve catalytic performance, and can improve high-temperature thermal stability performance, mechanical performance and the high temperature oxidation resistance of NaX molecular sieve.
Further, a kind of low-temperature denitration CeO of the present invention 2-NaX molecular sieve catalyst is because used CeO 2Cheap and easy to get, and whole low-temperature denitration CeO 2Therefore the preparation technology of-NaX molecular sieve catalyst is simple, and it is low to have a production cost, is suitable for the characteristics of suitability for industrialized production.
Further, the low-temperature denitration CeO of final gained 2-NaX molecular sieve catalyst Modulatory character is more intense, can be through changing molecular sieve carried CeO 2Measure or introduce other suitable cerium source and improve CeO 2The catalytic performance of-NaX molecular sieve catalyst.
In addition, a kind of low-temperature denitration CeO of the present invention 2-NaX molecular sieve catalyst is because CeO 2In noble metal atmosphere, play stabilization, therefore have raising NO xConversion ratio, and make catalyst keep anti-preferably sulphur property and advantages of high catalytic activity.
The specific embodiment
Through concrete embodiment the present invention is further set forth below, but do not limit the present invention.
It is the fixed bed reactors of 14mm that used catalytic reactor in the embodiments of the invention adopts internal diameter, and unstripped gas gets into reactor through preheating, and reaction temperature is at 200 ℃, and flow velocity is 1000ml/min, space velocity 23000h -1
The composition of the used simulated flue gas in the embodiments of the invention: NO600ppm, NH 3600ppm and O 2Be 5%, remaining gas N 2As balance gas, 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 replenished.
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. in Shanghai
Cerous acetate （CH 3CO 2）3Ce·xH 2O 206996-60-3 99.5% metals basis 100g The brilliant pure Industrial Co., Ltd. in Shanghai
The NaX molecular sieve Na 86[(AlO 2) 86(SiO 2) 106]xH 2O 63231-69-6 The 60-80 order 500g The brilliant pure Industrial Co., Ltd. in Shanghai
 
Embodiment 1
A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 1:100.
Above-mentioned a kind of low-temperature denitration CeO 2The preparation method of-NaX molecular sieve catalyst, step is following:
Na with 100g 86[(AlO 2) 86(SiO 2) 106] xH 2O molecular sieve and 1gCeN 3O 96H 2O mixing incipient impregnation in deionized water, 50 ℃ of following agitating heating 1h, stir speed (S.S.) is 200rpm (adopts polytetrafluoroethylene (PTFE) paddle), then at 110 ℃ of dry 12h down, then at the N of 300ml/min 2Atmosphere, control temperature be 600 ℃ at tubular type kiln roasting 5h, be cooled to room temperature again and obtain a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst A.
Embodiment 2
A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 2:100.
Above-mentioned a kind of low-temperature denitration CeO 2The preparation method of-NaX molecular sieve catalyst, step is following:
Na with 100g 86[(AlO 2) 86(SiO 2) 106] xH 2O molecular sieve and 2gCeN 3O 96H 2O mixing incipient impregnation in deionized water, 50 ℃ of following agitating heating 1h, stir speed (S.S.) is 200rpm (adopts polytetrafluoroethylene (PTFE) paddle), then at 110 ℃ of dry 12h down, then at the N of 300ml/min 2Atmosphere, control temperature be 600 ℃ at tubular type kiln roasting 5h, be cooled to room temperature again and obtain a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst B.
Embodiment 3
A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 5:100.
Above-mentioned a kind of low-temperature denitration CeO 2The preparation method of-NaX molecular sieve catalyst, step is following:
Na with 100g 86[(AlO 2) 86(SiO 2) 106] xH 2O molecular sieve and 5gCeN 3O 96H 2O mixing incipient impregnation in deionized water, 50 ℃ of following agitating heating 1h, stir speed (S.S.) is 200rpm (adopts polytetrafluoroethylene (PTFE) paddle), then at 110 ℃ of dry 12h down, then at the N of 300ml/min 2Atmosphere, control temperature be 600 ℃ at tubular type kiln roasting 5h, be cooled to room temperature again and obtain a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst C.
Embodiment 4
A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 10:100.
Above-mentioned a kind of low-temperature denitration CeO 2The preparation method of-NaX molecular sieve catalyst, step is following:
Na with 100g 86[(AlO 2) 86(SiO 2) 106] xH 2O molecular sieve and 10gCeN 3O 96H 2O mixing incipient impregnation in deionized water, 50 ℃ of following agitating heating 1h, stir speed (S.S.) is 200rpm (adopts polytetrafluoroethylene (PTFE) paddle), then at 110 ℃ of dry 12h down, then at the N of 300ml/min 2Atmosphere, control temperature be 600 ℃ at tubular type kiln roasting 5h, be cooled to room temperature again and obtain a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst D.
Embodiment 5
A kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst is promptly with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 15:100.
Above-mentioned a kind of low-temperature denitration CeO 2The preparation method of-NaX molecular sieve catalyst, step is following:
Na with 100g 86[(AlO 2) 86(SiO 2) 106] xH 2O molecular sieve and 15gCeN 3O 96H 2O mixing incipient impregnation in deionized water, 50 ℃ of following agitating heating 1h, stir speed (S.S.) is 200rpm (adopts polytetrafluoroethylene (PTFE) paddle), then at 110 ℃ of dry 12h down, then at the N of 300ml/min 2Atmosphere, control temperature be 600 ℃ at tubular type kiln roasting 5h, be cooled to room temperature again and obtain a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst E.
Application implementation example 1-5
Utilize the low-temperature denitration CeO of embodiment 1-5 gained 2-NaX molecular sieve catalyst A, B, C, D, E and typical catalyst are that the titania based SCR catalyst of the Cormetech of the U.S. carries out the denitration activity experiment respectively, and be specific as follows:
Before beginning, experiment test, lets CeO earlier with the about 1h of the feeding fixed bed reactors of the NO gas in the simulated flue gas 2NO is saturated for the absorption of-NaX molecular sieve catalyst, avoids because of CeO 2The absorption of-NaX molecular sieve catalyst causes the minimizing of NO;
Then after mixing, gas is passed into fixed bed reactors respectively forming of simulated flue gas in gas mixed box, at CeO 2Under the effect of-NaX molecular sieve catalyst, NH 3NO is reduced to N 2, reacted gaseous mixture absorbs unreacted NH through phosphoric acid solution 3After blast pipe enters atmosphere, NO concentration adopts the thermoelectric model60i flue gas analyzer of the U.S. to detect, and the result of its denitration activity sees the following form:
Catalyst sample Reaction temperature (℃) Denitration activity (%)
Typical catalyst 200 35
CeO 2-NaX molecular sieve catalyst A 200 70
CeO 2-NaX molecular sieve catalyst B 200 70.5
CeO 2-NaX molecular sieve catalyst C 200 71.5
CeO 2-NaX molecular sieve catalyst D 200 83
CeO 2-NaX molecular sieve catalyst E 200 74.5
Denitration activity in the table is expressed as: NO Denitration activity(%)=
Figure 457363DEST_PATH_IMAGE002
* 100%
Where
Figure 2012103190564100002DEST_PATH_IMAGE004
and?
Figure 2012103190564100002DEST_PATH_IMAGE006
Export fixed bed reactor were NO concentration.
From last table, can find out, adopt low-temperature denitration CeO of the present invention 2The denitration activity of-NaX molecular sieve catalyst all has higher denitration activity than typical catalyst (the titania based SCR catalyst of the Cormetech of the U.S.) under cryogenic conditions; Make it wider active window; Be beneficial to and make the SCR denitrification apparatus be arranged in thermal power plant's back-end ductwork; Reduce the waste heat loss, improve thermal power plant's performance driving economy.And low-temperature denitration CeO of the present invention 2The preparation technology of-NaX molecular sieve catalyst is simple, the low-temperature denitration CeO of the present invention that makes 2-NaX molecular sieve catalyst Modulatory character is more intense, can be through changing the molecular sieve carried CeO of NaX 2Amount or introduce other suitable cerium source or catalytic performance that metal improves catalyst.
The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all belongs to the scope of the present invention's protection.

Claims (7)

1. low-temperature denitration CeO 2-NaX molecular sieve catalyst is characterized in that described low-temperature denitration CeO 2-NaX molecular sieve catalyst is with the molecular sieve carried CeO of NaX 2, press mass ratio and calculate CeO 2: the NaX molecular sieve is 1-15:100.
2. a kind of low-temperature denitration CeO as claimed in claim 1 2The preparation method of-NaX molecular sieve catalyst is characterized in that step is following:
Adopt equi-volume impregnating, the NaX molecular sieve impregnated in the solubility cerium solution, 20-80 ℃, the following heating of stirring condition 1-2h are then at 80-110 ℃ of following dry 6-12h, then at N 2The control temperature is 600 ℃ of roasting 3-12h under the atmosphere, is cooled to room temperature again and promptly obtains a kind of low-temperature denitration CeO 2-NaX molecular sieve catalyst.
3. a kind of low-temperature denitration CeO as claimed in claim 2 2The preparation method of-NaX molecular sieve catalyst is characterized in that described solubility cerium salt is CeN 3O 96H 2O or (CH 3CO 2) 3CexH 2O, described NaX molecular sieve is Na 86[(AlO 2) 86(SiO 2) 106] xH 2O.
4. a kind of low-temperature denitration CeO as claimed in claim 2 2The preparation method of-NaX molecular sieve catalyst is characterized in that heating under the described stirring condition, and promptly controlling stir speed (S.S.) is 200-600rpm, adopts the polytetrafluoroethylene (PTFE) paddle to stir.
5. a kind of low-temperature denitration CeO as claimed in claim 2 2The preparation method of-NaX molecular sieve catalyst is characterized in that described N 2Atmosphere is promptly controlled N 2Flow is the N of 300ml/min 2Under the environment.
6. a kind of low-temperature denitration CeO as claimed in claim 2 2The preparation method of-NaX molecular sieve catalyst is characterized in that described roasting carries out in tube furnace.
7. a kind of low-temperature denitration CeO as claimed in claim 1 2The application of-NaX molecular sieve catalyst in denitrification process is characterized in that step is following:
Before beginning, denitration, lets low-temperature denitration CeO earlier with the about 1-2h of the feeding fixed bed reactors of the NO gas in the simulated flue gas component 2After-NaX molecular sieve catalyst absorption NO reaches capacity, the flue gas of treating denitration is got into fixed bed reactors control reaction temperature at 200-400 ℃, flow velocity is 1000ml/min, space velocity 20000-30000h -1, at low-temperature denitration CeO 2Under the effect of-NaX molecular sieve catalyst, the NH in the flue gas 3NO is reduced to N 2Gas, reacted gaseous mixture absorbs unreacted NH through phosphoric acid solution 3After blast pipe enters atmosphere;
Described simulated flue gas is formed: NO200-600ppm, NH 3200-600ppm and O 2Be 0-5%, remaining gas N 2As balance gas.
CN2012103190564A 2012-09-03 2012-09-03 Low-temperature denitrated CeO2-NaX molecular sieve catalyst and preparation method thereof Pending CN102814191A (en)

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Application publication date: 20121212