CN104741143A - Preparation method and application of Cu-ZSM-5 doped Zr and Sr composite catalyst - Google Patents
Preparation method and application of Cu-ZSM-5 doped Zr and Sr composite catalyst Download PDFInfo
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Abstract
The invention provides a preparation method and an application of a Cu-ZSM-5 doped Zr and Sr composite catalyst. The composite Zr-Sr/Cu-ZSM-5 catalyst which is high in specific surface area (350-400m2/g) is prepared by the following steps: exchanging a Na-ZSM-5 molecular sieve with NH4Cl to prepare an amino type NH4-ZSM-5 molecular sieve; then, adding a copper acetate solution to the NH4-ZSM-5 molecular sieve, preparing a Cu-ZSM-5 molecular sieve by virtue of an ion exchange method, and doping little Zr and Sr by virtue of an impregnation method. Within a relatively wide temperature range, the catalyst has a high catalytic elimination effect (NO conversion rate is 50-97%) for pollutants which are high in space velocity (120,000-360,000mL.(g.h)-1), high in O2 concentration (10-20vl%), high in H2O content (5-10wt%) and low in NO concentration (300-1000ppm). By adding a hydrocarbon compound (100-300ppm propylene) to a reaction system, the catalyst is high in anti-carbon-deposition performance.
Description
Technical field
The present invention relates to the preparation method of a kind of Cu-ZSM-5 for catalytic removal NO doping Zr and Sr composite catalyst and the application of selective catalysis elimination NO thereof.
Background technology
Nitrogen oxide (NO
x) be a kind of main pollutant in air, it has huge harm to ecological environment and health, it not only causes acid rain, also be form surface layer ozone pollution, secondary subparticle pollutes and the presoma of surface water eutrophication, the environmental problem caused thus has become atmospheric environment hot issue the most outstanding together with depletion of the ozone layer, Global climate change.Cause NO
xproducing reason can be divided into two aspects: naturally-occurring source and artificial occurring source.The NOx that the coal-burning boiler (stationary source) in vehicle exhaust (moving source) and power plant discharges accounts for more than 90% of anthropogenic discharge's total amount.According to estimates, NOx discharge annual growth is 5.0%-8.0%; 3,540 ten thousand tons will be reached to the year two thousand thirty China's nitrogen oxide emission, so, current NO in the urgent need to address
xpollution problem.
Owing to administering NO
xdifficulty is large, controls and administers NO
xpollute and become one of most active problem in current environmental protection research.There is multiple elimination NO both at home and abroad at present
xmethod, wherein NH
3selective Catalytic Reduction of NO
xmeasures compare ripe, be applied to vehicle exhaust (stationary source) and thermal power plant (moving source) NO
xthe improvement of polluting.NH
3-SCR catalysis material mainly contains noble metal catalyst, metal oxide catalyst, molecular sieve catalyst and other catalysis materials 4 kinds of systems, wherein, and V
2o
5-WO
3-TiO
2system is most widely used, this system commercialization at present, but exhaust temperature scope when diesel vehicle actual load runs is 150 ~ 700 DEG C, V
2o
5-WO
3-TiO
2there is low temperature active deficiency, high high-temp stability difference and high temperature V (vanadium) volatilization and produce secondary pollution problems in catalyst system and catalyzing.
ZSM race zeolite is developed by Mobil oil company of the U.S., and wherein ZSM-5 is one of most important member, has two-dimentional ten-ring duct.Become the object of falling over each other to develop of catalysis circle due to the structure of its uniqueness and physicochemical properties, be widely used in the catalytic fields such as Coal Chemical Industry, PETROLEUM PROCESSING and fine chemistry industry at present.The ZSM-5 molecular sieve that this patent selects heat endurance higher is carrier, is prepared into Cu-ZSM-5 by ion-exchange, then Zr and the Sr composite catalyst that adulterates, and obtains the catalytic removal NO in good wide temperature range (150 DEG C ~ 650 DEG C)
xhigh activity and high anti-carbon performance.With regard to the document of current all reports, although Cu-ZSM-5 also has good activity, but great majority use independent copper supported catalyst, reaction temperature is narrower, anti-carbon poor performance, and the Zr-Sr/Cu-ZSM-5 catalyst prepared by this patent has preferably active and anti-carbon performance, and adulterate the again research of Zr and Sr loaded catalyst of use Cu-ZSM-5 is simultaneously less both at home and abroad at present.
This project implementation obtains: project of national nature science fund project (numbering: 21277008; 20777005); Beijing institution of higher education directly under the jurisdiction of a municipal government Construction of Creativity Team promotes the subsidy of planning item (KM2013100050010) and Education Commission of Beijing development in science and technology plan general project (KM2013100050010), is also the research contents of these projects.
Summary of the invention
The object of this invention is to provide a kind of ZSM-5 load Zr-Sr-Cu composite catalyst preparation and for catalytic removal NO pollutant.The catalyst provided under wide reaction temperature (150 DEG C ~ 650 DEG C), can efficiently eliminate NO (the NO conversion ratio of 50% ~ 98%).And add hydrocarbon after, this catalyst has higher anti-carbon performance.And this catalyst preparation process is simple.
The invention provides the preparation method of a kind of Cu-ZSM-5 for catalytic removal NO doping Zr and Sr composite catalyst.
(1) by silica alumina ratio be Na-ZSM-5 molecular sieve and the 0.1mol.L of (20mol ~ 25mol): 1mol
-1~ 0.5mol.L
-1nH
4cl solution is at 60 ~ 80 DEG C of ion-exchange 2 ~ 5h, wherein Na-ZSM-5 molecular sieve and NH
4the ratio of Cl is 100g:(0.6mol ~ 3.0mol), said process repeats 1 ~ 3 time, and filtration, washing 3 ~ 5 times, 120 ~ 140 DEG C drying 18 ~ 24h obtain NH
4-ZSM-5 molecular sieve; By gained NH
4-ZSM-5 molecular sieve joins 0.01mol.L
-1~ 0.024mol.L
-1cu (OAc)
2in, 60 ~ 80 DEG C of ion-exchange 2 ~ 5h, wherein NH
4-ZSM-5 molecular sieve and Cu (OAc)
2ratio is 100g:(0.03mol ~ 0.072mol), according to said process, repeat 1 ~ 3 time, filter, wash 3 ~ 5 times, 120 ~ 140 DEG C drying 18 ~ 24h, obtain Cu-ZSM-5 presoma.Homogeneous phase mixing 0.001mol.L subsequently
-1~ 0.003mol.L
-1zr (NO
3)
4solution and 0.001mol.L
-1~ 0.003mol.L
-1sr (NO
3)
2solution, wherein Zr (NO
3)
4with Sr (NO
3)
2ratio is 1:1, adds in above-mentioned mixed liquor by the Cu-ZSM-5 presoma prepared above, uses impregnation 24 ~ 48h, wherein, and Cu-ZSM-5 presoma and Zr (NO
3)
4ratio be 100g:(0.003mol ~ 0.009mol), 120 ~ 140 DEG C of drying 18 ~ 24h subsequently, 450 ~ 550 DEG C of roasting 4 ~ 6h, obtained support type compound Zr-Sr/Cu-ZSM-5 catalyst.
The application of prepared catalyst, is characterized in that: be placed in continuous-flow fixed bed device by above-mentioned catalyst and pass into containing 300ppm ~ 1000ppm NH
3, 300ppm ~ 1000ppm NO, 10vl.% ~ 20vl.%O
2with 5wt% ~ 10wt%H
2react in the gaseous mixture of O, its concentration is except H
2o is that outside weight percentage, all the other are all volumn concentration, wherein NO and NH
3concentration equal; The remaining gas of above gaseous mixture is inert gas, and reaction pressure is normal pressure 1atm, and reaction velocity is 120,000mL. (g.h)
-1~ 360,000mL. (g.h)
-1, reaction temperature is 150 DEG C ~ 650 DEG C.
Further, in reacting gas, inert gas is He or N
2.
Add 100ppm ~ 300ppm propylene again in further gaseous mixture, in 150 DEG C ~ 650 DEG C temperature ranges, reaction pressure is normal pressure 1atm, and reaction velocity is 120,000mL. (g.h)
-1~ 360,000mL. (g.h)
-1, test load type compound Zr-Sr/Cu-ZSM-5 catalyst anti-carbon performance.
Catalyst of the present invention, (120,000mL. (g.h) under high-speed
-1~ 360,000mL. (g.h)
-1), high O
2concentration (10vl.% ~ 20vl.%), high H
2o content (5wt% ~ 10wt%) and NO (300ppm ~ 1000ppm), NH
3under (300ppm ~ 1000ppm) condition.In wide temperature range (150 DEG C ~ 650 DEG C), there is high catalytic removal low concentration of NO (300ppm ~ 1000ppm) active (NO conversion ratio=50% ~ 97%); Under above reaction condition, hydrocarbon (100ppm ~ 300ppm propylene) is added again in reaction system, for support type compound Zr-Sr/Cu-ZSM-5 catalyst, slightly reduce in low-temperature zone and middle-temperature section (150 DEG C ~ 350 DEG C) reactivity, in the not change of high temperature section (400 DEG C ~ 650 DEG C) activity, show certain anti-carbon performance.
Accompanying drawing explanation
Fig. 1 is that Na-ZSM-5 and comparative example of the present invention, Cu-ZSM-5, the support type compound Zr-Sr/Cu-ZSM-5-I of embodiment 1,2,3 preparation, the XRD of Zr-Sr/Cu-ZSM-5-II, Zr-Sr/Cu-ZSM-5-III catalyst scheme.
Fig. 2 is Cu-ZSM-5, the support type compound Zr-Sr/Cu-ZSM-5-I of comparative example of the present invention and embodiment 1,2,3 preparation, the N of Zr-Sr/Cu-ZSM-5-II, Zr-Sr/Cu-ZSM-5-III catalyst
2-absorption/desorption figure.
Fig. 3 is NH on the support type Cu-ZSM-5 catalyst prepared of comparative example of the present invention
3selective Catalytic Reduction of NO activity and anti-carbon performance.
Fig. 4 be the embodiment of the present invention 1 prepare support type compound Zr-Sr/Cu-ZSM-5-I catalyst on NH
3selective Catalytic Reduction of NO activity and anti-carbon performance.
Fig. 5 be the embodiment of the present invention 2 prepare support type compound Zr-Sr/Cu-ZSM-5-II catalyst on NH
3selective Catalytic Reduction of NO activity and anti-carbon performance.
Fig. 6 be the embodiment of the present invention 3 prepare support type compound Zr-Sr/Cu-ZSM-5-III catalyst on NH
3selective Catalytic Reduction of NO activity and anti-carbon performance.
Detailed description of the invention
Comparative example
(1) by silica alumina ratio be Na-ZSM-5 molecular sieve and the 0.3mol.L of 23mol:1mol
-1solution is at 70 DEG C of ion-exchange 2h, wherein Na-ZSM-5 molecular sieve and NH
4the ratio of Cl is 100g:1.5mol, and said process repeats 2 times, and filtration, washing 4 times, 130 DEG C dry 20h obtain NH
4-ZSM-5 molecular sieve; By gained NH
4-ZSM-5 molecular sieve joins 0.02mol.L
-1cu (OAc)
2in, 70 DEG C of ion-exchange 3h, wherein NH
4-ZSM-5 molecular sieve and Cu (OAc)
2ratio is 100g:0.05mol, according to said process, repeats 2 times, and filter, wash 4 times, 130 DEG C dry 20h, 450 DEG C of roasting 4h, obtain Cu-ZSM-5.
(2) catalyst 240,000mL. (g.h) under high-speed
-1, 15vl.% height O
2concentration, 7wt% height H
2o content and 700ppm NO, 700ppm NH
3under condition, in wide temperature range (150 DEG C ~ 650 DEG C), there is high catalytic removal low concentration 700ppm NO activity (NO conversion ratio=45% ~ 95%); Under above reaction condition, 200ppm propylene hydrocarbon is added again in reaction system, for Cu-ZSM-5 catalyst, slightly reduce in low-temperature zone and middle-temperature section (150 DEG C ~ 350 DEG C) reactivity, in the not change of high temperature section (400 DEG C ~ 650 DEG C) activity, show certain anti-carbon performance.
Embodiment 1
(1) by silica alumina ratio be Na-ZSM-5 molecular sieve and the 0.1mol.L of 20mol:1mol
-1nH
4cl solution is at 60 DEG C of ion-exchange 2h, wherein Na-ZSM-5 molecular sieve and NH
4the ratio of Cl is 100g:0.6mol, and said process repeats 1 time, and filtration, washing 3 times, 120 DEG C dry 18h obtain NH
4-ZSM-5 molecular sieve; By gained NH
4-ZSM-5 molecular sieve joins 0.01mol.L
-1cu (OAc)
2in, 60 DEG C of ion-exchange 2h, wherein NH
4-ZSM-5 molecular sieve and Cu (OAc)
2ratio is 100g:0.03mol, according to said process, repeats 1 time, filters, washs 3 times, 120 DEG C dry 18h, obtain Cu-ZSM-5 presoma.Homogeneous phase mixing 0.001mol.L subsequently
-1zr (NO
3)
4solution and 0.001mol.L
-1sr (NO
3)
2solution, wherein Zr (NO
3)
4with Sr (NO
3)
2ratio is 1:1, adds in above-mentioned mixed liquor by the Cu-ZSM-5 presoma prepared above, uses impregnation 24h, wherein, and Cu-ZSM-5 presoma and Zr (NO
3)
4ratio be 100g:0.003mol, 120 DEG C of dry 18h subsequently, 450 DEG C of roasting 4h, obtained support type compound Zr-Sr/Cu-ZSM-5-I catalyst.
(2) catalyst is at 120,000mL. (g.h)
-1under air speed, 10vl.%O
2concentration, 5wt%H
2o concentration and 300ppmNO, 300ppm NH
3under condition, in wide temperature range (150 DEG C ~ 550 DEG C), to 300ppm NO, there is high catalytic removal activity (NO conversion ratio=51% ~ 97%); Under above reaction condition, 100ppm propylene hydrocarbon is added again in reaction system, support type compound Zr-Sr/Cu-ZSM-5-I catalyst, slightly reduce in low-temperature zone and middle-temperature section (150 DEG C ~ 350 DEG C) reactivity, in the not change of high temperature section (400 DEG C ~ 650 DEG C) activity, show certain anti-carbon performance.
Embodiment 2
(1) by silica alumina ratio be Na-ZSM-5 molecular sieve and the 0.3mol.L of 23mol:1mol
-1nH
4cl solution is at 70 DEG C of ion-exchange 3h, wherein Na-ZSM-5 molecular sieve and NH
4the ratio of Cl is 100g:2.0mol, and said process repeats 2 times, and filtration, washing 4 times, 130 DEG C dry 20h obtain NH
4-ZSM-5 molecular sieve; By gained NH
4-ZSM-5 molecular sieve joins 0.015mol.L
-1cu (OAc)
2in, 780 DEG C of ion-exchange 3h, wherein NH
4-ZSM-5 molecular sieve and Cu (OAc)
2ratio is 100g:0.05mol, according to said process, repeats 2 times, filters, washs 4 times, 130 DEG C dry 20h, obtain Cu-ZSM-5 presoma.Homogeneous phase mixing 0.002mol.L subsequently
-1zr (NO
3)
4solution and 0.002mol.L
-1sr (NO
3)
2solution, wherein Zr (NO
3)
4with Sr (NO
3)
2ratio is 1:1, adds in above-mentioned mixed liquor by the Cu-ZSM-5 presoma prepared above, uses impregnation 36h, wherein, and Cu-ZSM-5 presoma and Zr (NO
3)
4ratio be 100g:0.006mol, 130 DEG C of dry 20h subsequently, 500 DEG C of roasting 5h, obtained support type compound Zr-Sr/Cu-ZSM-5-II catalyst.
(2) catalyst is at 200,000mL. (g.h)
-1under air speed, 15vl.%O
2concentration, 8wt%H
2o content and 500ppm NO, 500ppm NH
3under condition, in wide temperature range (150 DEG C ~ 650 DEG C), there is high catalytic removal low concentration 500ppm NO activity (NO conversion ratio=50% ~ 98%); Under above reaction condition, 200ppm propylene hydrocarbon is added again in reaction system, support type compound Zr-Sr/Cu-ZSM-5-II catalyst, slightly reduce in low-temperature zone and middle-temperature section (150 DEG C ~ 350 DEG C) reactivity, in the not change of high temperature section (400 DEG C ~ 650 DEG C) activity, show certain anti-carbon performance.
Embodiment 3
(1) by silica alumina ratio be Na-ZSM-5 molecular sieve and the 0.5mol.L of 25mol:1mol
-1nH
4cl solution is at 80 DEG C of ion-exchange 5h, wherein Na-ZSM-5 molecular sieve and NH
4the ratio of Cl is 100g:3.0mol, and said process repeats 3 times, and filtration, washing 5 times, 40 DEG C dry 24h obtain NH
4-ZSM-5 molecular sieve; By gained NH
4-ZSM-5 molecular sieve joins 0.024mol.L
-1cu (OAc)
2in, 80 DEG C of ion-exchange 5h, wherein NH
4-ZSM-5 molecular sieve and Cu (OAc)
2ratio is 100g:0.072mol, according to said process, repeats 3 times, filters, washs 5 times, 140 DEG C dry 24h, obtain Cu-ZSM-5 presoma.Homogeneous phase mixing 0.003mol.L subsequently
-1zr (NO
3)
4solution and 0.003mol.L
-1sr (NO
3)
2solution, wherein Zr (NO
3)
4with Sr (NO
3)
2ratio is 1:1, adds in above-mentioned mixed liquor by the Cu-ZSM-5 presoma prepared above, uses impregnation 48h, wherein, and Cu-ZSM-5 presoma and Zr (NO
3)
4ratio be 100g:0.009mol, 140 DEG C of dry 24h subsequently, 550 DEG C of roasting 6h, obtained support type compound Zr-Sr/Cu-ZSM-5-III catalyst.
(2) catalyst is at 360,000mL. (g.h)
-1under air speed, 20vl.%O
2concentration, 10wt%H
2o content and 1000ppm NO, 1000ppm NH
3under condition, in wide temperature range (150 DEG C ~ 650 DEG C), there is high catalytic removal low concentration 1000ppm NO activity (NO conversion ratio=53% ~ 98%); Under above reaction condition, 300ppm propylene hydrocarbon is added again in reaction system, support type compound Zr-Sr/Cu-ZSM-5-III catalyst, slightly reducing in low-temperature zone and middle-temperature section (150 DEG C ~ 350 DEG C) reactivity, in the not change of high temperature section (400 DEG C ~ 650 DEG C) activity, show certain anti-carbon performance.
Claims (4)
- The preparation method of 1.Cu-ZSM-5 doping Zr and Sr composite catalyst, is characterized in that:By Na-ZSM-5 molecular sieve and 0.1 ~ 0.5mol.L -1nH 4cl solution is at 60 ~ 80 DEG C of ion-exchange 2 ~ 5h, and wherein the silica alumina ratio of Na-ZSM-5 molecular sieve is (20mol ~ 25mol): 1mol; Wherein Na-ZSM-5 molecular sieve and NH 4the ratio of Cl is 100g:(0.6mol ~ 3.0mol), said process repeats 1 ~ 3 time, and filtration, washing 3 ~ 5 times, 120 ~ 140 DEG C drying 18 ~ 24h obtain NH 4-ZSM-5 molecular sieve; By gained NH 4-ZSM-5 molecular sieve joins 0.01mol.L -1~ 0.024mol.L -1cu (OAc) 2in, 60 ~ 80 DEG C of ion-exchange 2 ~ 5h, wherein NH 4-ZSM-5 molecular sieve and Cu (OAc) 2ratio is 100g:(0.03mol ~ 0.072mol), according to said process, repeat 1 ~ 3 time, filter, wash 3 ~ 5 times, 120 ~ 140 DEG C drying 18 ~ 24h, obtain Cu-ZSM-5 presoma; Homogeneous phase mixing 0.001mol.L subsequently -1~ 0.003mol.L -1zr (NO 3) 4solution and 0.001mol.L -1~ 0.003mol.L -1sr (NO 3) 2solution, wherein Zr (NO 3) 4with Sr (NO 3) 2molar ratio is 1:1, adds in above-mentioned mixed liquor by the Cu-ZSM-5 presoma prepared above, uses impregnation 24 ~ 48h, wherein, and Cu-ZSM-5 presoma and Zr (NO 3) 4ratio be 100g:(0.003mol ~ 0.009mol), 120 ~ 140 DEG C of drying 18 ~ 24h subsequently, 450 ~ 550 DEG C of roasting 4 ~ 6h, obtained support type compound Zr-Sr/Cu-ZSM-5 catalyst.
- 2. the application of the catalyst according to claim 1 prepared by method, is characterized in that: be placed in continuous-flow fixed bed device by above-mentioned catalyst and pass into containing 300ppm ~ 1000ppm NH 3, 300ppm ~ 1000ppm NO, 10vl.% ~ 20vl.%O 2with 5wt% ~ 10wt%H 2react in the gaseous mixture of O, its concentration is except H 2o is that outside weight percentage, all the other are all volumn concentration, wherein NO and NH 3concentration equal; The remaining gas of above gaseous mixture is inert gas, and reaction pressure is normal pressure 1atm, and reaction velocity is 120,000mL. (g.h) -1~ 360,000mL. (g.h) -1, reaction temperature is 150 DEG C ~ 650 DEG C.
- 3. application according to claim 2, is characterized in that: in reacting gas, inert gas is He or N 2.
- 4. application according to claim 2, is characterized in that: add 100ppm ~ 300ppm propylene again in gaseous mixture, and in 150 DEG C ~ 650 DEG C temperature ranges, reaction pressure is normal pressure 1atm, and reaction velocity is 120,000mL. (g.h) -1~ 360,000mL. (g.h) -1, test load type compound Zr-Sr/Cu-ZSM-5 catalyst anti-carbon performance.
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| CN105413652A (en) * | 2015-11-06 | 2016-03-23 | 中国第一汽车股份有限公司 | Preparation method of particle filter carrier material mixture containing diatom ooze |
| JP2017140614A (en) * | 2016-02-12 | 2017-08-17 | 現代自動車株式会社Ｈｙｕｎｄａｉ Ｍｏｔｏｒ Ｃｏｍｐａｎｙ | Catalyst and method for producing catalyst |
| CN109046439A (en) * | 2018-08-27 | 2018-12-21 | 宝鸡文理学院 | A kind of synthetic method of highly doped amount peracidity position mesopore silicon oxide solid acid catalyst |
| CN111250150A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Preparation method and application of modified ZSM-5 molecular sieve catalyst, and method for preparing ethylene from coal-based ethanol |
| CN114146724A (en) * | 2021-12-01 | 2022-03-08 | 南宁师范大学 | Preparation method of modified ZSM-5 molecular sieve |
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Cited By (11)
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| CN105413652A (en) * | 2015-11-06 | 2016-03-23 | 中国第一汽车股份有限公司 | Preparation method of particle filter carrier material mixture containing diatom ooze |
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| CN109046439A (en) * | 2018-08-27 | 2018-12-21 | 宝鸡文理学院 | A kind of synthetic method of highly doped amount peracidity position mesopore silicon oxide solid acid catalyst |
| CN109046439B (en) * | 2018-08-27 | 2021-05-07 | 宝鸡文理学院 | Synthesis method of high-doping high-acidity mesoporous silica solid acid catalyst |
| CN111250150A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Preparation method and application of modified ZSM-5 molecular sieve catalyst, and method for preparing ethylene from coal-based ethanol |
| CN111250150B (en) * | 2018-11-30 | 2023-06-20 | 中国科学院大连化学物理研究所 | Preparation method and application of modified ZSM-5 molecular sieve catalyst and method for preparing ethylene from coal-based ethanol |
| CN114146724A (en) * | 2021-12-01 | 2022-03-08 | 南宁师范大学 | Preparation method of modified ZSM-5 molecular sieve |
| CN114146724B (en) * | 2021-12-01 | 2024-01-30 | 南宁师范大学 | Preparation method of modified ZSM-5 molecular sieve |
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Application publication date: 20150701 |