CN104190464B - A kind of Sn bases micro porous molecular sieve NOx SCR catalyst preparation methods - Google Patents
A kind of Sn bases micro porous molecular sieve NOx SCR catalyst preparation methods Download PDFInfo
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Abstract
A kind of Sn bases micro porous molecular sieve NOx SCR catalyst preparation methods, are by in-situ synthesis or ion-exchange, with Sn to commercial molecular sieve ZSM 5, modenite（MOR）, Beta molecular sieves and other micro porous molecular sieves carry out modification, component Sn is introduced in framework of molecular sieve, so as to prepare Sn base micro porous molecular sieves.SCR catalyst prepared by the present invention at utmost realizes NOxSelective reduction is N2, and after 60 h reactions, the catalytic activity of catalyst does not have any decline, is a kind of NO of high efficiency high stablexRemoval of catalyst.Still there is higher catalytic activity in the presence of water or steam, excellent water resistant inactivation performance is shown.The present invention is with low cost, and simple production process is easy, and service life is long.
Description
Technical field
The present invention relates to a kind of Sn bases micro porous molecular sieve NOx-SCR method for preparing catalyst, it is mainly used in vehicle exhaust
Or NO in factory smokexPurified treatment, belongs to environmental protection and air contaminant treatment field.
Technical background
The world today, the fast development of the extensive chemical industry of the transportation and oil etc. such as automobile, promotes science
Technology is maked rapid progress, while also bringing serious harm to environment for the survival of mankind.Nearly ten years, Chinese each big city
Atmosphere pollution is serious.The composition of atmosphere pollution is very complicated, nitrogen oxides（NOx）It is exactly one of main component. NOxSource can
It is divided into static father and dynamic source, Typical Representative therein is factory smoke and motor-vehicle tail-gas.NOxHave to human environment very big
Harmfulness.Damage the ozone layer first, cause Ozone hole；Next to that and SOxDeng sour gas by being acted on and shape with water
Into acid rain, impoverish the soil, be unfavorable for the growth of crops；In addition, NOxPhotochemical fog can also be produced, is given birth in the present context
People living easily suffer from breathing problem.As can be seen here, NOxIt is an important killer of environment, eliminates NOxDischarge
An importance as prevention and control of air pollution.
So far, SCR（SCR）NOxIt is by the more generally acknowledged removal methods of scientific circles.Its principle
It is to utilize organic matter in vehicle exhaust or factory smoke to be reducing agent or add reducing agent in addition, in O2Under existence condition, selection
Property preferentially NOxIt is reduced to N2.Its catalytic process generally uses NH3, HC, CO and PM etc. as reducing agent, in oxidizing atmosphere
It is catalyzed NOxReduction reaction high is required to the selectivity of catalyst, for the technology research than wide.Wherein, HC-
SCR main chemical reactions equation is as follows：NO+HC+O2 → CO2 + H2O+N2, HC+O2 → H2O + CO2。
SNCR（SNCR）It is also that people were once used for removing NOxOne of means, it be using ammonia or
Urea is as reducing agent, by NO under conditions of catalyst is not added withxIt is converted into N2, SNCR shortcoming is that transformation efficiency is relatively low, it is impossible to
Emission request of the environmental regulation to nitrogen oxides is met, thus people seldom apply such a method now.
With the development of science and technology, people also begin to explore other eliminations NOxThe new method and new approaches of discharge, this its
Middle photocatalysis is also applied to catalytic removal NOx.Light-catalysed general principle is by photocatalysis reagent（Such as TiO2Deng）, in purple
Under outside-visible ray existence condition, photodissociation NOx, so as to reach elimination NOxThe purpose of discharge.This is a new cross discipline,
The interest of many scientists is aroused.But unfortunately, this method not yet obtain at present it is actual large-scale develop and utilize, and only
Stay in theoretical research stage.
Carried noble metal is conventional SCR catalyst, but such a catalyst is expensive, and easily because in CO, sulphur
Poison and inactivate.Molecular sieve is that a class is directed to the good catalyst that SCR reacts, and it has very high specific surface area, is easy to modulation
The features such as duct, high heat and hydrothermal stability, this makes it have the performances such as good adsorbing separation, catalysis, ion exchange.It is many
Well known, the hetero-atom molecular-sieve such as Cu bases and Fe bases is to NOxElimination reaction have higher catalytic activity（Such as patent
CN102029178A and CN101711991A）.And Sn bases zeolite molecular sieve then has no document or patent for removal of nitrogen oxide
Report.
The content of the invention
The purpose of the present invention is to be used for NO in vehicle exhaust or factory smoke there is provided one kind in view of the shortcomings of the prior artx
The Sn base micro porous molecular sieve SCR catalyst preparation methods of purified treatment, it in vehicle exhaust or factory smoke for largely existing
NOxCatalytic purification field, prepares the Sn based molecular sieve SCR catalysts with high activity and high stability.
It is provided by the present invention to be used for NOxThe Sn based molecular sieve SCR catalysts of purified treatment are to commercial molecular sieve with Sn
ZSM-5, MOR, Beta, SSZ-13, MWW molecular sieve carry out modification, prepare different Sn contents zeolite molecular sieve catalysts.
Preparation of the present invention for vehicle exhaust or the Sn based molecular sieve SCR catalysts of factory smoke purified treatment
Method has two kinds：
Method one prepares Sn based molecular sieve catalyst using in-situ synthesis：
(1) preparation of Sn-MFI molecular sieves:Using tetraethyl orthosilicate, sodium aluminate, butter of tin as presoma, 4 third
Base ammonium hydroxide is template, in 150-180oCrystallization 24-72 h, filtration washing, 60-120 under CoC dries 4-12 h, 500-
600 o4-12 h are calcined under C in-situ synthesis Sn-MFI catalyst is made；
(2) preparation of Sn-ZSM-5 molecular sieves：The preparation of Sn-ZSM-5 molecular sieves is similar with Sn-MFI, in building-up process
In need to add silicon source, silicon source is one kind in aluminum nitrate, aluminum sulfate, sodium metaaluminate, sial atomic molar ratio 15-1000 it
Between, silicon tin atom mol ratio is between 15-1000；
(3) Sn-Beta, Sn-SSZ-13, Sn-MOR, Sn-MWW molecular sieve preparation process are similar with Sn-ZSM-5, are closing
Need to add silicon source during, silicon source is one kind in aluminum nitrate, aluminum sulfate, sodium metaaluminate, and sial atomic molar ratio is in 5-
Between 1000；Template used dose of Sn-Beta, Sn-SSZ-13, Sn-MWW is respectively tetraethyl ammonium hydroxide, N, N, the trimethyls of N mono-
Golden steel alkane ammonium hydroxide, hexamethylene imine, and Sn-MOR is not required to template and can successfully synthesized；Silicon tin atom mol ratio exists
Between 15-1000；
The ion-exchange of method two synthesizes Sn base zeolite molecular sieves
（1）By Hydrogen Si-Al zeolite molecular sieve ZSM-5, Beta, SSZ-13, MOR, MWW and SnCl4Solution is well mixed,
80oBe stirred at reflux 24 h under C, repeated exchanged twice, filtration washing, 60-120o4-12 h, 500-600 are dried in C baking ovenso4-12 h are calcined under C ion-exchange Sn based molecular sieve catalyst is made, molecular sieve silica alumina ratio is controlled between 5-1000, silicon
Tin atom mol ratio is controlled between 15-1000；
Evaluation method of the Sn base zeolite molecular sieve SCR catalysts that the present invention is provided in tail gas in NOx catalytic purifications be
Using fixed bed reactors, reaction condition：Sn based molecular sieves catalyst is first subjected to pretreatment operation, room temperature is then down to, then
Temperature programming is carried out, reaction gas is passed through, total air speed is 60,000 ml/（gcat.h）, reaction temperature：200-600oC。
Beneficial effects of the present invention：Sn base microporous molecular sieve catalysts are prepared using in-situ synthesis or ion-exchange,
The a large amount of NO contained in vehicle exhaust or factory smoke can effectively be removedxToxic gas, shows that superior catalysis is stable
Property and excellent catalytic activity.
Brief description of the drawings
Fig. 1 is the in-situ synthesis Sn-ZSM-5 catalyst XRD test results of embodiment 1；
Fig. 2 is the in-situ synthesis Sn-ZSM-5 catalyst of embodiment 1 to NOxCatalytic purification curve.
Embodiment
For the clearer explanation present invention, following examples are enumerated, but it is without any restrictions to the scope of the present invention.
Embodiment 1
Using tetraethyl orthosilicate, sodium aluminate and butter of tin as presoma, TPAOH is template, according to
Sn/Al mol ratios are 2:1 is reacted, filtration washing, is dried, with 2oC/min heating rate, 550o6 h are calcined under C
Obtain the in-situ synthesis Sn based molecular sieve catalyst samples of embodiment 1.By the obtained g of catalyst 0.1 550oCarried out under C pre-
Processing 30 min of operation, are then cooled to room temperature, then with 10oC/min rate programs heat up, and are passed through total flow for 100 ml/
Min hybrid reaction gas, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oNO in C temperature rangesxConversion
Rate.
Embodiment 2
Using tetraethyl orthosilicate, sodium aluminate and butter of tin as presoma, TPAOH is template, according to
Sn/Al mol ratios are 1:1 is reacted, filtration washing, is dried, with 2oC/min heating rate, 550o6h is calcined under C to obtain
Obtain the in-situ synthesis Sn based molecular sieve catalyst samples of embodiment 2.By the obtained g of catalyst 0.1 550oLocated in advance under C
Reason 30 min of operation, are then cooled to room temperature, then with 10oC/min rate programs heat up, and are passed through total flow for 100 ml/min
Hybrid reaction gas, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oNO in C temperature rangesxConversion ratio.
Embodiment 3
Using tetraethyl orthosilicate, sodium aluminate and butter of tin as presoma, TPAOH is template, according to
Sn/Al mol ratios are 1:2 are reacted, filtration washing, are dried, with 2oC/min heating rate, 550o6 h are calcined under C
Obtain the in-situ synthesis Sn based molecular sieve catalyst samples of embodiment 3.By the obtained g of catalyst 0.1 550oCarried out under C pre-
Processing 30 min of operation, are then cooled to room temperature, then with 10oC/min rate programs heat up, and are passed through total flow for 100 ml/
Min hybrid reaction gas, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oNO in C temperature rangesxConversion
Rate.
Embodiment 4
1.0 g sodium form molecular sieves NaZSM-5 of commercialization original powder and 10 ml27%NH4NO3Solution is uniformly mixed, 80oStirred under C
24 h are mixed, repeated exchanged twice, dry, 550 by filtration washingo6h is calcined under C and obtains hydrogen type molecular sieve HZSM-5.1.0 g
HZSM-5 and 15 ml 0.1M SnCl4Solution is mixed, 80o24 h are stirred under C, repeated exchanged twice, do by filtration washing
It is dry, 550o6 h are calcined under C and obtain the ion-exchange Sn based molecular sieve catalyst samples of embodiment 4.By obtained catalyst 0.1
G is 550oThe min of pretreatment operation 30 is carried out under C, room temperature is then cooled to, then with 10oC/min rate programs heat up, and are passed through
Total flow is 100 ml/min hybrid reaction gas, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oC temperature
In the range of NOxConversion ratio.
Embodiment 5
Commercial 1.0g sodium form molecular sieve NaMOR（Mercerising molecular sieve）Former powder and 10 ml27%NH4NO3Solution is uniformly mixed,
80 o24h is stirred under C, repeated exchanged twice, dry, 550 by filtration washingo6 h are calcined under C and obtain hydrogen type molecular sieve HMOR.
1.0g HMOR and 15 ml 0.1M SnCl4Solution is mixed, 80oStir 24 h under C, repeated exchanged twice, filtration washing,
Dry, 550o6 h are calcined under C and obtain the ion-exchange Sn based molecular sieve catalyst samples of embodiment 5.By obtained catalyst
0.1 g is 550oThe min of pretreatment operation 30 is carried out under C, room temperature is then cooled to, then with 10oC/min rate programs heat up,
The hybrid reaction gas that total flow is 100 ml/min is passed through, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oNO in C temperature rangesxConversion ratio.
Embodiment 6
1.0 g sodium form molecular sieves NaMOR of commercialization（Mercerising molecular sieve）Former powder and 10 ml 27%NH4NO3Solution is uniformly mixed,
80o24 h are stirred under C, repeated exchanged twice, dry, 550 by filtration washingo6 h are calcined under C and obtain hydrogen type molecular sieve
HMOR.1.0 g HMOR and concentrated nitric acid react obtaining dealuminzation type HMOR molecular sieves, then by 1.0 g dealuminzation type HMOR molecules
The SnCl of sieve and 15 ml 0.1M4Solution is mixed, 80o24 h are stirred under C, repeated exchanged twice, dry, 550 by filtration washingo6 h are calcined under C and obtain the ion-exchange Sn based molecular sieve catalyst samples of embodiment 6.By the obtained g of catalyst 0.1 550oThe min of pretreatment operation 30 is carried out under C, room temperature is then cooled to, then with 10oC/min rate programs heat up, and being passed through total flow is
100 ml/min hybrid reaction gas, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oIn C temperature ranges
NOxConversion ratio.
Embodiment 7
1.0 g sodium form molecular sieves NaBeta of commercialization（Beta-molecular sieve）Former powder and 10 ml 27%NH4NO3Solution is uniformly mixed,
80o24 h are stirred under C, repeated exchanged twice, dry, 550 by filtration washingo6h is calcined under C and obtains hydrogen type molecular sieve HBeta.1.0
G Hbeta and 15ml0.1M SnCl4Solution is mixed, 80o24 h are stirred under C, repeated exchanged twice, dry by filtration washing,
550 o6 h are calcined under C and obtain the ion-exchange Sn based molecular sieve catalyst samples of embodiment 7.By the obtained g of catalyst 0.1
550oThe min of pretreatment operation 30 is carried out under C, room temperature is then cooled to, then with 10oC/min rate programs heat up, and are passed through total
Flow is 100 ml/min hybrid reaction gas, wherein containing 0.4%CH4, 0.6%NO, 6%O2, detection 300-600oC temperature
In the range of NOxConversion ratio.
Claims (3)
1. a kind of method that fabricated in situ prepares Sn base micro porous molecular sieves NOx-SCR, it is characterized in that：
The preparation of Sn-MFI molecular sieves:Using tetraethyl orthosilicate, sodium aluminate, butter of tin as presoma, TPAOH
For template, the crystallization 24-72h at 150-180 DEG C, filtration washing, 60-120 DEG C of dry 4-12h is calcined 4- at 500-600 DEG C
In-situ synthesis Sn-MFI catalyst is made in 12h；
Wherein, MFI molecular sieves can be substituted with ZSM-5, Beta, SSZ-13, MOR, MWW molecular sieve, and Sn-ZSM-5 molecular sieves exist
Addition silicon source and butter of tin are needed in building-up process, sial atomic molar ratio is between 15-1000, and silicon tin atom mol ratio exists
Between 15-1000；
Sn-Beta, Sn-SSZ-13, Sn-MOR, Sn-MWW molecular sieve need addition silicon source and butter of tin in building-up process,
Silica alumina ratio is between 5-1000；Sn-Beta, Sn-SSZ-13, Sn-MWW molecular sieve template used in building-up process
Respectively tetraethyl ammonium hydroxide, N, N, N- trimethyl adamantane ammonium hydroxide, hexamethylene imine, and Sn-MOR molecular sieves
Synthesis does not need template；Silicon tin atom mol ratio is between 15-1000.
2. a kind of fabricated in situ according to claim 1 prepares Sn base micro porous molecular sieves NOx-SCR method, its feature
It is：Source of aluminium is one kind in aluminum nitrate, aluminum sulfate, sodium metaaluminate.
3. a kind of Sn bases micro porous molecular sieve NOx-SCR method for preparing catalyst, it is characterized in that：By Hydrogen Si-Al zeolite molecular sieve
ZSM-5, Beta, SSZ-13, MOR, MWW and SnCl4Solution is well mixed, and 24h, repeated exchanged two are stirred at reflux at 80 DEG C
Secondary, filtration washing dries roasting 4-12h at 4-12h, 500-600 DEG C in 60-120 DEG C of baking oven and ion-exchange Sn bases point is made
Sub- sieve catalyst, molecular sieve silica alumina ratio is controlled between 5-1000, and silicon tin atom mol ratio is controlled between 15-1000.
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| CN107570205B (en) * | 2017-10-23 | 2020-07-28 | 上海歌通实业有限公司 | Preparation method of modified Beta molecular sieve catalyst |
| CN108479845B (en) * | 2018-03-22 | 2021-01-15 | 浙江致远环境科技有限公司 | Denitration catalyst and preparation method thereof |
| CN112717996B (en) * | 2021-04-02 | 2021-07-16 | 山东国瓷功能材料股份有限公司 | Composite catalyst and preparation method and application thereof |
| CN115814845B (en) * | 2022-11-10 | 2023-11-28 | 广东联南环保科技有限公司 | Preparation method of copper-tin molecular sieve HC-SCR catalyst |
| CN115814844B (en) * | 2022-11-10 | 2023-11-28 | 广东联南环保科技有限公司 | Preparation method of copper molecular sieve HC-SCR catalyst |
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