CN115304077A - Molecular sieve for selective catalytic reduction of nitrogen oxides and preparation method and application thereof - Google Patents
Molecular sieve for selective catalytic reduction of nitrogen oxides and preparation method and application thereof Download PDFInfo
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- 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
- C01B39/20—Faujasite type, e.g. type X or Y
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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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- 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
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
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- 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
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/10—After treatment, characterised by the effect to be obtained
- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
- B01J2229/186—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself not in framework positions
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention relates to a molecular sieve for selective catalytic reduction of nitrogen oxides, a preparation method and application thereof, wherein the preparation method comprises the following steps: so as to contain Cu salt and NH 4 And (3) mechanically ball-milling the mixture of the-SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve at room temperature to prepare the molecular sieve for selectively catalytically reducing the nitrogen oxide. The beneficial effects of the invention are: the molecular sieve for selective catalytic reduction of nitrogen oxides prepared by the invention has excellent activity of selective catalytic reduction of nitrogen oxides, and is suitable for purification of tail gas of diesel vehicles, power plants and the like.
Description
Technical Field
The invention relates to the technical field of molecular sieves, in particular to a molecular sieve for selective catalytic reduction of nitrogen oxides, and a preparation method and application thereof.
Background
After extensive research and experimentation, researchers have found that Cu-exchanged CHA-type molecular sieves, such as Cu-SAPO-34 and Cu-SSZ-13, can selectively catalyze the reduction of nitrogen oxides with high efficiency. The use temperature window is 200-500 ℃. Among them, the Cu-SSZ-13 molecular sieve has much attention from both academic and industrial fields because it is excellent in hydrothermal stability and is an ideal catalyst for the denitration of diesel vehicle exhaust.
Cu-SSZ-13 is H in SSZ-13 molecular sieve + Ion is by Cu 2+ Substituted molecular sieves. Notably, researchers have found that Cu-SSZ-13 has superior hydrothermal stability to SSZ-13, i.e., cu 2+ The skeleton structure can be stabilized. The main preparation method of Cu-SSZ-13 is an ion exchange method, i.e. by reacting NH 4 -placing the SSZ-13 or H-SSZ-13 molecular sieve in a Cu source solution, and performing ion exchange under the conditions of stirring and heating; there are also reports of one-step synthesis of Cu-SSZ-13 molecular sieve, but the Cu content in the one-step synthesized Cu-SSZ-13 is very high, and a large amount of Cu is contained 2+ The ions remain in the channels and the product is impure.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a molecular sieve for selective catalytic reduction of nitrogen oxides, and a preparation method and application thereof.
In a first aspect, there is provided a method for preparing a molecular sieve for selective catalytic reduction of nitrogen oxides, comprising: so as to contain Cu salt and NH 4 Mechanical ball milling treatment of the mixture of-SSZ-13 molecular sieve and/or H-SSZ-13 molecular sieve at room temperature to produce the molecular sieve for selective catalytic reduction of nitrogen oxides.
Preferably, the method specifically comprises the following steps:
s1, mixingDissolving Cu salt in water to form Cu salt solution, and adding NH 4 -the SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve are thoroughly mixed to form the mixture;
s2, placing the mixture in a ball milling device for mechanical ball milling treatment, and then carrying out centrifugal washing, drying and calcining treatment to obtain the molecular sieve for selective catalytic reduction of nitrogen oxides.
Preferably, in S1, the Cu salt is reacted with NH 4 -the mass ratio of the SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve is between 0.05 and 1.25; in S2, the ball milling device comprises a vibration ball mill or a planetary ball mill, the calcining temperature is 500-600 ℃, and the calcining time is 2-6 h.
Preferably, in S1, the Cu salt includes any one or a combination of two or more of copper sulfate, copper sulfate hydrate, copper acetate hydrate, copper chloride, and copper chloride hydrate.
Preferably, before S1, the method further comprises:
contacting SSZ-13 molecular sieve with NH 4 + Exchanging for 6-24 h at 60-80 ℃ to obtain the NH 4 -SSZ-13 molecular sieves.
Preferably, the SSZ-13 molecular sieve has a Si/Al atomic ratio of 6 to 30.
Preferably, before S1, the method further comprises:
reacting the NH with 4 Calcining the SSZ-13 molecular sieve at 500-600 ℃ for 2-6H to prepare the H-SSZ-13 molecular sieve.
Preferably, the structure of the SSZ-13 molecular sieve is CHA type, and the SSZ-13 molecular sieve is made of AlO 4 And SiO 4 The tetrahedrons are connected end to end through oxygen atoms and are orderly arranged into an ellipsoidal cage with an eight-membered ring structure.
Preferably, cu in the molecular sieve for selective catalytic reduction of nitrogen oxide 2+ Uniformly dispersing the active carbon on an octagon ring and a hexatomic ring of a SSZ-13 molecular sieve with a negative charge framework structure; these active sites are capable of selectively donating NO under a reducing atmosphere x Is converted into N 2 And H 2 O。
In a second aspect, there is provided a use of the molecular sieve for selective catalytic reduction of nitrogen oxide according to the first aspect in purification of diesel exhaust or power plant exhaust, the molecular sieve for selective catalytic reduction of nitrogen oxide selectively catalytic reduces nitrogen oxide over a wide temperature range.
The invention has the beneficial effects that:
1. the method provided by the invention can be carried out at room temperature, and compared with the traditional ion exchange method which needs to be carried out under heating and stirring, the method provided by the invention is simpler and more convenient to operate.
2. The molecular sieve (Cu-SSZ-13 molecular sieve) for selective catalytic reduction of nitrogen oxides prepared by the invention has more excellent SCR catalytic performance, and the NO conversion efficiency is more than 85% in a temperature window of 100-550 ℃.
3. The method provided by the invention can more efficiently crush the Cu by virtue of the local crushing of the molecular sieve particles and the violent collision action of the ions and the molecular sieve particles in the ball milling process compared with the traditional ion exchange method 2+ Is introduced into the SSZ-13 structure.
Drawings
FIG. 1 is an XRD pattern of Cu-SSZ-13 molecular sieves in examples 1-3 of the present invention and comparative example 1;
FIG. 2 is an SEM picture of a Cu-SSZ-13 molecular sieve in example 1 of the invention;
FIG. 3 is an SEM picture of the Cu-SSZ-13 molecular sieve in example 2 of the invention;
FIG. 4 is an SEM picture of a Cu-SSZ-13 molecular sieve in example 3 of the invention;
FIG. 5 is an SEM picture of a Cu-SSZ-13 molecular sieve in example 4 of the invention;
FIG. 6 is an SEM picture of a Cu-SSZ-13 molecular sieve in comparative example 1 of the present invention;
FIG. 7 is an element distribution diagram of a Cu-SSZ-13 molecular sieve in example 1 of the present invention;
FIG. 8 is a test chart of the SCR performance of Cu-SSZ-13 molecular sieves in example 1, example 3 and comparative example 1 of the present invention;
fig. 9 is a schematic diagram of a ball milling process in an exemplary embodiment of the 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.
The invention provides a preparation method of a molecular sieve for selective catalytic reduction of nitrogen oxides, which is used for efficiently carrying out Cu ball milling at room temperature by a mechanical ball milling method 2+ Exchange into the framework structure of SSZ-13, comprising: the mixture containing the Cu salt, NH4-SSZ-13 molecular sieve and/or H-SSZ-13 molecular sieve is subjected to mechanical ball milling at room temperature to produce a molecular sieve for selective catalytic reduction of nitrogen oxides (also referred to as Cu-SSZ-13 molecular sieve).
The method specifically comprises the following steps:
s1, dissolving Cu salt in water to form a Cu salt solution, and adding NH 4 -the SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve are thoroughly mixed to form a mixture.
In S1, the mass ratio of the Cu salt to the NH4-SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve is 0.05-1.25. The Cu salt comprises one or more of copper sulfate, copper sulfate hydrate, copper acetate hydrate, copper chloride and copper chloride hydrate.
And S2, placing the mixture in a ball milling device for mechanical ball milling treatment, and then performing centrifugal washing, drying and calcining treatment to obtain the molecular sieve for selective catalytic reduction of nitrogen oxides.
In S2, mechanical ball milling means that the materials are crushed and mixed by using the impact action of the falling milling bodies (steel balls or ceramic balls) and the milling action of the milling bodies and the inner wall of the ball mill. The mechanical ball milling treatment is used for physically impacting the material through a medium, and a schematic diagram of the ball milling process is shown in fig. 9. The ball milling device comprises a vibration ball mill or a planetary ball mill, the calcining temperature is 500-600 ℃, and the calcining time is 2-6 h.
Before S1, further comprising:
contacting SSZ-13 molecular sieve with NH 4 + Exchange for 6-24 h at 60-80 ℃ to prepare NH 4 -SSZ-13 molecular sieves.
The SSZ-13 molecular sieve has an Si/Al atomic ratio of 6 to 30, preferably 9 to 12.
Before S1, further comprising:
reacting NH 4 Calcining the-SSZ-13 molecular sieve at 500-600 ℃ for 2-6H to prepare the H-SSZ-13 molecular sieve.
The structure of the SSZ-13 molecular sieve is CHA type, and the SSZ-13 molecular sieve is an ellipsoid cage with eight-membered ring structure formed by orderly arranging AlO4 and SiO4 tetrahedrons end to end through oxygen atoms.
Cu in molecular sieve (Cu-SSZ-13 molecular sieve) for selective catalytic reduction of nitrogen oxides 2+ Uniformly dispersing the active carbon on an octagon ring and a hexatomic ring of a SSZ-13 molecular sieve with a negative charge framework structure; in a reducing atmosphere (NH) 3 Or urea) are capable of selectively converting NOx to N 2 And H 2 And (O). Illustratively, cu in the above Cu-SSZ-13 molecular sieve 2+ The content of (B) is 0.5-4 wt%.
In addition, the invention also provides application of the molecular sieve for selectively catalytically reducing nitrogen oxides in purification of diesel vehicle tail gas or power plant tail gas, in particular application of the Cu-SSZ-13 molecular sieve in selectively catalytically reducing nitrogen oxides in a wide temperature range. Furthermore, the Cu-SSZ-13 molecular sieve has the NO conversion efficiency of more than 85 percent in a temperature window of 100-550 ℃.
The technical solutions of the present invention are further described in detail below with reference to several preferred embodiments and the accompanying drawings, which are implemented on the premise of the technical solutions of the present invention, and a detailed implementation manner and a specific operation process are provided, but the scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples below were obtained from conventional biochemicals unless otherwise specified.
Example 1:
(1) Weighing 0.1g of copper acetate to dissolve in 2mL of water;
(2) Weighing 1g of H-SSZ-13 molecular sieve, adding the H-SSZ-13 molecular sieve into the copper acetate solution obtained in the step 1), and uniformly stirring;
(3) Transferring the mixed solution in the step (2) into a ball milling tank with the volume of 20mL, and putting matched ceramic spheres with different diameters;
(4) And (4) placing the ball milling tank in the step (3) in a planetary ball milling instrument for mechanical ball milling at the rotating speed of 350 r/min for 3h.
(5) Washing the product in the step (4) by deionized water, centrifuging and drying at 80 ℃;
(6) And (3) placing the molecular sieve powder in the step (5) in a muffle furnace, calcining at 560 ℃ for 2h, and naturally cooling to obtain the Cu-SSZ-13 molecular sieve.
The XRD pattern, the SEM pattern, the element distribution pattern and the SCR performance test of the Cu-SSZ-13 molecular sieve prepared in this example are shown in fig. 1, fig. 2, fig. 7 and fig. 8, respectively.
Example 2:
replacement of H-SSZ-13 in step (2) in example 1 with NH 4 SSZ-13, the other steps being identical to those of example 1.
The XRD pattern and SEM pattern of the Cu-SSZ-13 molecular sieve prepared in the example are shown in figure 1 and figure 3 respectively.
Example 3:
(1) Weighing 1.0g of blue vitriol and dissolving in 20mL of water;
(2) Weighing 1g of H-SSZ-13 molecular sieve, adding the H-SSZ-13 molecular sieve into the copper sulfate solution obtained in the step (1), and uniformly stirring;
(3) Transferring the mixed solution in the step (2) into a ball milling tank with the volume of 100mL, and putting matched ceramic spheres with different diameters;
(4) And (4) placing the ball milling tank in the step (3) in a planetary ball milling instrument for mechanical ball milling at the rotating speed of 350 r/min for 3h.
(5) Washing the product in the step (4) by deionized water, centrifuging and drying at 80 ℃;
(6) And (3) placing the molecular sieve powder in the step (5) in a muffle furnace, calcining at 560 ℃ for 4h, and naturally cooling to obtain the Cu-SSZ-13 molecular sieve.
The XRD pattern, SEM pattern and SCR performance test of the Cu-SSZ-13 molecular sieve prepared in the embodiment are shown in figures 1, 4 and 8 respectively.
Example 4:
the H-SSZ-13 in step (2) in example 3 was replaced with NH 4 SSZ-13, the other steps being identical to those of example 3.
The SEM image of the Cu-SSZ-13 molecular sieve prepared in this example is shown in FIG. 5.
Comparative example 1:
using a conventional ion exchange process comprising:
(1) Weighing 1.0g of blue vitriol and dissolving in 20mL of water;
(2) Weighing 1g of H-SSZ-13 molecular sieve, adding the H-SSZ-13 molecular sieve into the copper sulfate solution obtained in the step 1), and stirring the mixture at the temperature of 80 ℃ for reaction for 3 hours;
(3) Washing the product in the step 2) by using deionized water, centrifuging and drying at 80 ℃;
(4) And (3) placing the molecular sieve powder in the step 3) into a muffle furnace, calcining at 560 ℃ for 4h, and naturally cooling to obtain the Cu-SSZ-13 molecular sieve.
The XRD pattern, SEM pattern and SCR performance test of the Cu-SSZ-13 molecular sieve prepared by the comparative example are shown in figures 1, 6 and 8 respectively.
The elemental analysis results of the Cu-SSZ-13 molecular sieves prepared in example 1, example 3 and comparative example 1 are shown in Table 1.
TABLE 1ICP elemental analysis results
| Sample numbering | Si(mg/kg) | Al(mg/kg) | Cu(mg/kg) |
| Cu-SSZ-13 (example 1) | 360734 | 35938 | 23597 |
| Cu-SSZ-13 (example 3) | 370335 | 36015 | 20631 |
| Cu-SSZ-13 (comparative example 1) | 367912 | 35129 | 17826 |
The products of examples 1 and 3 and comparative example 1 were subjected to SCR tests under the following conditions: [ NO ]]＝[NH 3 ]＝500ppm；[O 2 ]＝10％，[H 2 O]＝5％，N 2 Balancing; airspeed 350000h -1 。
As shown in FIG. 8, cu-SSZ-13 (example 1) and Cu-SSZ-13 (example 3) prepared by the ball milling method have excellent SCR performance, the NO conversion rate at 150 ℃ reaches 85%, the NO conversion efficiency in the range of 200-400 ℃ reaches 100%, and the conversion rate at 600 ℃ is still higher than 70%, which is obviously better than that of Cu-SSZ-13 prepared by the conventional ion exchange method in comparative example 1.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
Claims (10)
1. A method of making a molecular sieve for selective catalytic reduction of nitrogen oxides, comprising: and (2) performing mechanical ball milling treatment on the mixture containing the Cu salt, the NH4-SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve at room temperature to prepare the molecular sieve for selectively catalyzing and reducing the nitrogen oxide.
2. The method of claim 1, comprising the steps of:
s1, dissolving Cu salt in water to form a Cu salt solution, and adding NH 4 -the SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve are intimately mixed to form said mixture;
s2, placing the mixture in a ball milling device for mechanical ball milling treatment, and then carrying out centrifugal washing, drying and calcining treatment to obtain the molecular sieve for selective catalytic reduction of nitrogen oxides.
3. The method of claim 2, wherein in S1, the Cu salt is reacted with NH 4 -the mass ratio of the SSZ-13 molecular sieve and/or the H-SSZ-13 molecular sieve is between 0.05 and 1.25; in S2, the ball milling device comprises a vibration ball mill or a planetary ball mill, the calcining temperature is 500-600 ℃, and the calcining time is 2-6 h.
4. The method of claim 2, wherein in S1, the Cu salt comprises any one or a combination of two or more of copper sulfate, copper sulfate hydrate, copper acetate hydrate, copper chloride and copper chloride hydrate.
5. The method of claim 2, further comprising, prior to S1:
contacting SSZ-13 molecular sieve with NH 4 + Exchanging for 6-24 h at 60-80 ℃ to obtain the NH 4 -SSZ-13 molecular sieves.
6. The method of claim 5, wherein the SSZ-13 molecular sieve has an Si/Al atomic ratio of 6 to 30.
7. The method of claim 5, further comprising, prior to S1:
reacting the NH with 4 Calcining the SSZ-13 molecular sieve at 500-600 ℃ for 2-6H to prepare the H-SSZ-13 molecular sieve.
8. The method of claim 5, wherein the SSZ-13 molecular sieve has a CHA-type structure, and the SSZ-13 molecular sieve is made of AlO 4 And SiO 4 The tetrahedrons are connected end to end through oxygen atoms and are orderly arranged to form an ellipsoidal cage with an eight-membered ring structure.
9. The method of any one of claims 1 to 8, wherein Cu is contained in the molecular sieve for selective catalytic reduction of nitrogen oxide 2+ Uniformly dispersing on eight-sided rings and six-membered rings of the SSZ-13 molecular sieve with a negative charge framework structure; these active sites are capable of selectively donating NO under a reducing atmosphere x Is converted into N 2 And H 2 O。
10. Use of the molecular sieve for selective catalytic reduction of nitrogen oxides according to claim 9 in the purification of diesel exhaust or power plant exhaust, wherein the molecular sieve for selective catalytic reduction of nitrogen oxides selectively catalytically reduces nitrogen oxides over a wide temperature range.
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| CN113694962A (en) * | 2021-09-30 | 2021-11-26 | 中化泉州石化有限公司 | Isomerization dewaxing catalyst for hydrocracking tail oil and preparation method thereof |
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