CN111592008A - Method for in-situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve - Google Patents
Method for in-situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve Download PDFInfo
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- CN111592008A CN111592008A CN202010532865.8A CN202010532865A CN111592008A CN 111592008 A CN111592008 A CN 111592008A CN 202010532865 A CN202010532865 A CN 202010532865A CN 111592008 A CN111592008 A CN 111592008A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/04—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/763—CHA-type, e.g. Chabazite, LZ-218
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention relates to a method for in-situ hydrothermal synthesis of a Fe-SSZ-13 molecular sieve, which comprises the following steps: step 1, preparation of a complex of Fe: adding divalent Fe metal salt into organic amine to perform a complex reaction for 2-6 h to form a Fe complex; step 2, preparing a reaction mixture; and 3, heating the aged reaction mixture obtained in the step 2.2 at 180-220 ℃ for 12-72 h under the crystallization condition until a crude product of Fe-SSZ-13 is formed. The invention has the beneficial effects that: the invention is a one-step method for preparing Fe-SSZ-13, compared with the traditional method for preparing Fe-SSZ-13 by ion exchange through a two-step method, the preparation process is simple; because a large amount of waste water is not generated, the cost is lower, and the method is simpler and more efficient; the obtained Fe-SSZ-13 molecular sieve catalyst has excellent hydrothermal stability and acid and alkali resistance after acid washing treatment; Fe-SSZ-13 molecular sieve can be appliedIn selective catalytic reduction (NH)3SCR) of nitrogen oxides in exhaust gases of engines, chemical plants, etc.
Description
Technical Field
The invention relates to a preparation method for synthesizing a Fe-SSZ-13 molecular sieve in situ by one step. The Fe-SSZ-13 molecular sieve can be applied to selective catalytic reduction (NH)3SCR) of nitrogen oxides in exhaust gases of engines, chemical plants, etc.
Background
The molecular sieve material is a crystalline porous material with regular pore channels and a high specific surface, the framework structure mainly comprises aggregates of silicon-aluminum oxide which are connected through oxygen bridges to form a regular pore structure and a cavity system, and the pore size is mainly 0.3-2.0 nm. Molecular sieve materials have wide industrial application in the fields of ion exchange, adsorption separation, catalysis and the like due to unique physical and chemical properties, and become indispensable important materials in the chemical field. For convenience of research and exchange, The International Zeolite Association (IZA) classifies molecular sieves according to their framework topologies, such as CHA, MFI, FAU, VFI, and The like. For example, the current hot spot molecular sieve material SSZ-13 has the CHA topology, which is formed by AlO4And SiO4The tetrahedron are connected end to end through oxygen atoms and are orderly arranged into an ellipsoidal cage (0.73nm × 1.2.2 nm) with an eight-membered ring structure and a three-dimensional cross pore channel structure, the pore channel size is 0.37nm × 0.42.42 nm SSZ-13 has the characteristics of ordered pore channel, good hydrothermal stability, more surface proton acid centers, exchangeable cations and the like, and the SSZ-13 molecular sieve after divalent Fe ions or divalent Cu ions are exchanged is an excellent Selective Catalytic Reduction (SCR) catalyst, and NO is not contained in the catalystxThe removal rate can reach 80-90%. The current research result shows that the work of the Cu-SSZ-13 molecular sieve catalystThe temperature window is generally 200-400 ℃, and the working temperature window of the Fe-SSZ-13 molecular sieve catalyst is generally 300-550 ℃. Compared with the Cu-SSZ-13 molecular sieve, the Fe-SSZ-13 molecular sieve has better SCR performance at high temperature.
The synthesis method of SSZ-13 is disclosed in the US patent document US 4544538 of 1982 for the first time, and the method needs to use expensive N, N, N-trimethyl-1-amantadine cation template agent, thus increasing the synthesis cost of the SSZ-13 molecular sieve and greatly limiting the popularization and application of the SSZ-13 molecular sieve. And the preparation of the SSZ-13 molecular sieve with the SCR activity also needs ion exchange, thereby further increasing the working procedure and the cost.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for synthesizing a Fe-SSZ-13 molecular sieve by in-situ hydrothermal synthesis.
The method for in-situ hydrothermal synthesis of the Fe-SSZ-13 molecular sieve comprises the following steps:
step 1, preparation of a complex of Fe: adding divalent Fe metal salt into organic amine to perform a complex reaction for 2-6 h to form a Fe complex;
step 2, preparing a reaction mixture:
step 2.1, adding an inorganic base and a trivalent aluminum source into the Fe complex, adding N, N, N-trimethyl-1-amantadine after completely dissolving, uniformly stirring, and finally dropwise adding a tetravalent silicon source to obtain a reaction mixture;
step 2.2, aging the mixture obtained in the step 2.1 for a certain time under the condition of stirring;
step 3, heating the aged reaction mixture obtained in the step 2.2 at 180-220 ℃ for 12-72 h under the crystallization condition until a crude product of Fe-SSZ-13 is formed;
step 4, placing the Fe-SSZ-13 crude product prepared in the step 3 in a specific atmosphere, and roasting at 500-700 ℃ for 6-12 h to remove a template agent, so as to obtain a Fe-SSZ-13 molecular sieve; the temperature rise rate of the roasting is 1-5 ℃/min.
Preferably, in the step 1, the divalent Fe metal salt is ferrous nitrate and its hydrate, ferrous acetate and its hydrate, ferrous sulfate and its hydrate or ferrous chloride and its hydrate (ferrous sulfate and its hydrate have better performance); the organic amine is triethylene diamine or tetraethylene pentamine (the performance of the tetraethylene pentamine is better).
Preferably, the time for the complexing reaction of the divalent Fe metal salt and the organic amine in the step 1 is 2 hours.
Preferably, the trivalent aluminum source in the step 2.1 is at least one of aluminum hydroxide, aluminum oxide, aluminum isopropoxide and sodium metaaluminate; preferably aluminum isopropoxide and sodium metaaluminate, more preferably sodium metaaluminate; the inorganic base is sodium hydroxide.
Preferably, the aging time in the step 2.2 is 5-20 h.
Preferably, the temperature of the reaction mixture after heat aging in the step 3 is 200 ℃, and the heating time is 72 h.
Preferably, in the step 4, the roasting temperature is 550 ℃, the roasting time is 6 hours, and the heating rate of the roasting is 5 ℃/m in.
Preferably, the specific atmosphere in step 4 is air.
Preferably, the molar ratio of the trivalent aluminum source to the tetravalent silicon source in the step 2.1 is in a range of 0.01 to 0.10; the molar ratio of the hydroxyl ions to the tetravalent silicon source is 0.2-0.6; the molar ratio of the organic base to the tetravalent silicon source is 0.05-0.2; the molar ratio of the N, N, N-trimethyl-1-amantadine cation to the tetravalent silicon source is 0.08-0.2.
Preferably, the Fe complex and the N, N, N-trimethyl-1-amantadine in the step 2.1 both serve as template agents, and the Fe complex simultaneously serves as an Fe source for synthesizing the Fe-SSZ-13 molecular sieve.
The invention has the beneficial effects that: the invention is a one-step method for preparing Fe-SSZ-13, compared with the traditional method for preparing Fe-SSZ-13 by ion exchange through a two-step method, the preparation process is simple; because a large amount of waste water is not generated, the cost is lower, and the method is simpler and more efficient; the obtained Fe-SSZ-13 molecular sieve catalyst has excellent hydrothermal stability and acid and alkali resistance after acid washing treatment; f e-SSZ-13 molecular sieve can be applied to selective catalytic reduction (NH)3SCR) of nitrogen oxides in exhaust gases of engines, chemical plants, etcA compound (I) is provided.
Drawings
FIG. 1 is a powder XRD pattern of Fe-SSZ-13 molecular sieves prepared in examples 1 to 3 of the present invention;
FIG. 2 is an SEM picture of a Fe-SSZ-13 molecular sieve prepared in example 1 of the present invention;
FIG. 3 is a diagram showing the denitration performance test results of the Fe-SSZ-13 molecular sieve prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
Example 1
Weighing 2.78 parts of ferrous sulfate heptahydrate in a beaker, adding 20g of deionized water, stirring until the ferrous sulfate heptahydrate is dissolved, adding 4.2g of tetraethylenepentamine into the ferrous sulfate solution, reacting for 2 hours, adding 1.6g of sodium hydroxide and 0.82g of sodium metaaluminate, completely dissolving, adding 20g of 25 mass percent N, N, N-trimethyl-1-adamantanamine template agent, stirring uniformly, finally dropwise adding 40g of 30 mass percent silica sol, aging the reaction mixture in a mechanical stirring manner for 10 hours, and placing the mixture in a 200-DEG oven for reacting for 1 day. And after the reaction is finished, performing suction filtration and washing with water, and placing the powder into a 100-DEG oven for drying and then placing the powder into a muffle furnace for calcining for 6 hours at 500-600 ℃. The sample number is S1, and the powder XRD pattern of the prepared Fe-SSZ-13 molecular sieve is shown in figure 1. The IC P analysis showed a Fe content of 2.5 wt%.
Example 2
Weighing 2.5g of ferrous nitrate into a beaker, adding 20g of deionized water, stirring until the ferrous nitrate is dissolved, adding 2.1g of triethylene diamine into a ferrous sulfate solution, reacting for 2 hours, adding 1.6g of sodium hydroxide and 0.82g of sodium metaaluminate, completely dissolving, adding 20g of 25 mass percent N, N, N-trimethyl-1-adamantanamine template agent, uniformly stirring, finally dropwise adding 40g of 30 mass percent silica sol, aging the reaction mixture in a mechanical stirring process for 10 hours, and placing the mixture in a 200-DEG oven for reaction for 1 day. And after the reaction is finished, performing suction filtration and washing with water, and placing the powder into a 100-DEG oven for drying and then calcining the powder in a muffle furnace at 500-600 ℃ for 6 hours. The sample number is S2, and the powder XRD pattern of the prepared Fe-SSZ-13 molecular sieve is shown in figure 1. The content of Fe was 1.9 wt% as a result of ICP analysis.
Example 3
Weighing 1.72g of ferrous sulfate heptahydrate in a beaker, adding 20g of deionized water, stirring until the ferrous sulfate heptahydrate is dissolved, adding 4.2g of tetraethylenepentamine into the ferrous sulfate solution, reacting for 2 hours, adding 1.6g of sodium hydroxide and 0.82g of sodium metaaluminate, completely dissolving, adding 20g of 25 mass percent N, N, N-trimethyl-1-adamantanamine template agent, stirring uniformly, finally dropwise adding 40g of 30 mass percent silica sol, aging the reaction mixture in a mechanical stirring manner for 20 hours, and placing the mixture in a 200-DEG oven for reaction for 3 days. And after the reaction is finished, performing suction filtration and washing with water, and placing the powder into a 100-DEG oven for drying and then calcining the powder in a muffle furnace at 500-600 ℃ for 6 hours. The sample number is S3, and the powder XRD pattern of the prepared Fe-SSZ-13 molecular sieve is shown in figure 1. The content of Fe was 1.2 wt% as a result of ICP analysis.
Example 4
The denitration performance test of example 1 was carried out under the following test conditions: [ NO ]]＝[NH3]＝500ppm；[O2]＝10％；[H2O]＝10％；N2Balancing; space velocity of 100000h-1The water vapor content was 10%. The test results are shown in FIG. 3, and the results show that the S1 sample has better NO reduction performance and good N2And (4) selectivity.
Claims (10)
1. The method for in-situ hydrothermal synthesis of the Fe-SSZ-13 molecular sieve is characterized by comprising the following steps:
step 1, preparation of a complex of Fe: adding divalent Fe metal salt into organic amine to perform a complex reaction for 2-6 h to form a Fe complex;
step 2, preparing a reaction mixture:
step 2.1, adding an inorganic base and a trivalent aluminum source into the Fe complex, adding N, N, N-trimethyl-1-amantadine after completely dissolving, uniformly stirring, and finally dropwise adding a tetravalent silicon source to obtain a reaction mixture;
step 2.2, aging the mixture obtained in the step 2.1 for a certain time under the condition of stirring;
step 3, heating the aged reaction mixture obtained in the step 2.2 at 180-220 ℃ for 12-72 h under the crystallization condition until a crude product of Fe-SSZ-13 is formed;
step 4, placing the Fe-SSZ-13 crude product prepared in the step 3 in a specific atmosphere, and roasting at 500-700 ℃ for 6-12 h to remove a template agent, so as to obtain a Fe-SSZ-13 molecular sieve; the temperature rise rate of the roasting is 1-5 ℃/min.
2. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: in the step 1, the divalent Fe metal salt is ferrous nitrate and hydrate thereof, ferrous acetate and hydrate thereof, ferrous sulfate and hydrate thereof or ferrous chloride and hydrate thereof; the organic amine is triethylene diamine or tetraethylenepentamine.
3. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: in the step 1, the time for carrying out the complex reaction of the divalent Fe metal salt and the organic amine is 2 hours.
4. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: the trivalent aluminum source in the step 2.1 is at least one of aluminum hydroxide, aluminum oxide, aluminum isopropoxide and sodium metaaluminate; the inorganic base is sodium hydroxide.
5. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: the aging time in the step 2.2 is 5-20 h.
6. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: the temperature of the reaction mixture after heating and aging in the step 3 is 200 ℃, and the heating time is 72 h.
7. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: in the step 4, the roasting temperature is 550 ℃, the roasting time is 6h, and the heating rate of roasting is 5 ℃/min.
8. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: the specific atmosphere in step 4 is air.
9. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: the molar ratio of the trivalent aluminum source to the tetravalent silicon source in the step 2.1 is 0.01-0.10; the molar ratio of the hydroxyl ions to the tetravalent silicon source is 0.2-0.6; the molar ratio of the organic base to the tetravalent silicon source is 0.05-0.2; the molar ratio of the N, N, N-trimethyl-1-amantadine cation to the tetravalent silicon source is 0.08-0.2.
10. The method for in situ hydrothermal synthesis of Fe-SSZ-13 molecular sieve according to claim 1, characterized in that: and 2.1, both the complex of Fe and the N, N, N-trimethyl-1-amantadine are used as template agents, and the Fe complex is simultaneously used as an Fe source for synthesizing the Fe-SSZ-13 molecular sieve.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112295594A (en) * | 2020-11-11 | 2021-02-02 | 中国科学院宁波材料技术与工程研究所 | Packaging type molecular sieve metal catalyst and preparation method and application thereof |
| CN113104858A (en) * | 2021-04-29 | 2021-07-13 | 钛纶新材料(昆山)有限公司 | Preparation method of Fe-SSZ-13 molecular sieve with heat conductivity |
| CN113277927A (en) * | 2021-05-28 | 2021-08-20 | 中国科学院宁波材料技术与工程研究所 | Application of microporous molecular sieve in adsorption and separation of n-butane and isobutane |
| CN114130404A (en) * | 2021-12-07 | 2022-03-04 | 浙江浙能技术研究院有限公司 | Preparation method of ultralow-temperature SCR denitration catalyst |
| CN114345396A (en) * | 2021-11-30 | 2022-04-15 | 西安交通大学 | Molecular sieve in-situ packaging active component type oxygen carrier and preparation method and application thereof |
| CN116393164A (en) * | 2023-03-30 | 2023-07-07 | 华中科技大学 | Auxiliary metal modified Fe-SSZ-13 molecular sieve, preparation and application as denitration catalyst |
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| CN113277927A (en) * | 2021-05-28 | 2021-08-20 | 中国科学院宁波材料技术与工程研究所 | Application of microporous molecular sieve in adsorption and separation of n-butane and isobutane |
| CN114345396A (en) * | 2021-11-30 | 2022-04-15 | 西安交通大学 | Molecular sieve in-situ packaging active component type oxygen carrier and preparation method and application thereof |
| CN114130404A (en) * | 2021-12-07 | 2022-03-04 | 浙江浙能技术研究院有限公司 | Preparation method of ultralow-temperature SCR denitration catalyst |
| CN116393164A (en) * | 2023-03-30 | 2023-07-07 | 华中科技大学 | Auxiliary metal modified Fe-SSZ-13 molecular sieve, preparation and application as denitration catalyst |
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