Scm-53 molecular sieve, method of making and use thereof
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHINA PETROLEUM & CHEMICAL CORP
- Filing Date
- 2024-01-24
- Publication Date
- 2026-05-29
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Figure CN118084010B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of molecular sieves, specifically to an SCM-53 molecular sieve, its preparation method, and its applications. Background Technology
[0002] Zeolite molecular sieves are a class of inorganic crystalline microporous materials with a three-dimensional four-linked framework structure formed by primary structural units TO4 ([SiO4], [AlO4], or [PO4], etc.) tetrahedra sharing vertices. The TO4 tetrahedra are connected by oxygen bridges to form various secondary structures. These secondary structures form chain structures and structural building units according to different linking methods, ultimately constructing different zeolite molecular sieve topologies.
[0003] The specific structure of zeolite molecular sieve materials results in specific powder X-ray diffraction (XRD) patterns. The position, relative intensity, and width of peaks in the powder XRD pattern are related to the chemical composition, grain size, and shape of the material. Different zeolite molecular sieves with the same topology may have different cell parameters, and their powder XRD patterns may differ slightly.
[0004] Meanwhile, zeolite molecular sieves with the same topology generally exhibit the same powder XRD pattern characteristics, but due to differences in chemical composition, they can be classified and named as different zeolite molecular sieve materials. A typical example is the zeolite molecular sieve materials ZSM-5 and TS-1, which have the same MFI topology. Both materials possess the same powder XRD spectroscopic characteristics, but their framework chemical compositions differ, making them two distinct zeolite molecular sieve materials. The framework structure of ZSM-5 zeolite molecular sieve material is composed of Si, Al, and O, and it is primarily used in acid catalysis. In contrast, the framework structure of TS-1 zeolite molecular sieve material is composed of Si, Ti, and O, and it is primarily used in catalytic oxidation processes.
[0005] Zeolite molecular sieves possess excellent hydrothermal stability, tunable pore diameter and shape, and variable pore chemical composition. These properties enable zeolite molecular sieve materials to be widely used in adsorption, separation, catalysis, microelectronics, and medical diagnostics. Therefore, the synthesis of molecular sieves with special framework structures has always been one of the most important research directions in the field of molecular sieves. Summary of the Invention
[0006] This invention provides a novel aluminosilicate molecular sieve, SCM-53, which is a germanium-free, high-silicon molecular sieve material with significant application value.
[0007] In a first aspect, the present invention provides an X-ray diffraction pattern of SCM-53 molecular sieve including one or more diffraction peaks with 2θ of 4.363°±0.30°, 8.940°±0.30°, 12.08°±0.30° and 26.09°±0.30°.
[0008] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes diffraction peaks with 2θ values of 4.363°±0.03°, 4.363°±0.05°, 4.363°±0.07°, 4.363°±0.1°, 4.363°±0.13°, 4.363°±0.15°, 4.363°±0.17°, 4.363°±0.2°, 4.363°±0.23°, 4.363°±0.25°, or 4.363°±0.27°.
[0009] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes diffraction peaks with 2θ values of 8.940°±0.03°, 8.940°±0.05°, 8.940°±0.07°, 8.940°±0.1°, 8.940°±0.13°, 8.940°±0.15°, 8.940°±0.17°, 8.940°±0.2°, 8.940°±0.23°, 8.940°±0.25°, or 8.940°±0.27°.
[0010] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes diffraction peaks with 2θ values of 12.08°±0.03°, 12.08°±0.05°, 12.08°±0.07°, 12.08°±0.1°, 12.08°±0.13°, 12.08°±0.15°, 12.08°±0.17°, 12.08°±0.2°, 12.08°±0.23°, 12.08°±0.25°, or 12.08°±0.27°.
[0011] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes diffraction peaks with 2θ values of 26.09°±0.03°, 26.09°±0.05°, 26.09°±0.07°, 26.09°±0.1°, 26.09°±0.13°, 26.09°±0.15°, 26.09°±0.17°, 26.09°±0.2°, 26.09°±0.23°, 26.09°±0.25°, or 26.09°±0.27°.
[0012] In some embodiments, the diffraction peak intensity at 4.363°±0.30° and / or 26.09°±0.30° is greater than the diffraction peak intensity at 8.940°±0.30° and / or 12.08°±0.30°.
[0013] In some implementations, the intensity of the diffraction peak at 4.363°±0.30° is greater than that at 26.09°±0.30°.
[0014] In some implementations, the intensity of the diffraction peak at 4.363°±0.30° is less than the intensity of the diffraction peak at 26.09°±0.30°.
[0015] In some embodiments, the strongest diffraction peak in the X-ray diffraction pattern of SCM-53 molecular sieve is the one with 2θ of 4.363° ± 0.30°.
[0016] In some embodiments, the strongest diffraction peak in the X-ray diffraction pattern of SCM-53 molecular sieve is the one with 2θ of 26.09° ± 0.30°.
[0017] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve also includes one or more diffraction peaks with 2θ values of 14.48°±0.30°, 18.42°±0.50°, and 23.05°±0.30°.
[0018] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve also includes diffraction peaks with 2θ values of 14.48°±0.03°, 14.48°±0.05°, 14.48°±0.07°, 14.48°±0.1°, 14.48°±0.13°, 14.48°±0.15°, 14.48°±0.17°, 14.48°±0.2°, 14.48°±0.23°, 14.48°±0.25°, or 14.48°±0.27°.
[0019] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve further includes 2θ values of 18.42°±0.03°, 18.42°±0.05°, 18.42°±0.07°, 18.42°±0.1°, 18.42°±0.13°, 18.42°±0.15°, 18.42°±0.17°, 18.42°±0.2°, and 18.4°. Diffraction peaks at 2°±0.23°, 18.42°±0.25°, 18.42°±0.27°, 18.42°±0.3°, 18.42°±0.33°, 18.42°±0.35°, 18.42°±0.37°, 18.42°±0.4°, 18.42°±0.43°, 18.42°±0.45°, or 18.42°±0.47°.
[0020] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve also includes diffraction peaks with 2θ values of 23.05°±0.03°, 23.05°±0.05°, 23.05°±0.07°, 23.05°±0.1°, 23.05°±0.13°, 23.05°±0.15°, 23.05°±0.17°, 23.05°±0.2°, 23.05°±0.23°, 23.05°±0.25°, or 23.05°±0.27°.
[0021] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table A:
[0022] Table A
[0023] 2θ <![CDATA[Relative intensity (I / I0×100)]]> 4.363°±0.30° s-vs 8.940°±0.30° ms 12.08°±0.30° ms 26.09°±0.30° vs .
[0024] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table A-1:
[0025] Table A-1
[0026] 2θ <![CDATA[Relative intensity (I / I0×100)]]> 4.363°±0.30° vs 8.940°±0.30° ms 12.08°±0.30° ms 26.09°±0.30° s-vs .
[0027] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table A-2:
[0028] Table A-2
[0029] 2θ <![CDATA[Relative intensity (I / I0×100)]]> 4.363°±0.30° 95-100 8.940°±0.30° 35-55 12.08°±0.30° 35-50 26.09°±0.30° 90-100 .
[0030] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table B:
[0031] Table B
[0032] 2θ <![CDATA[Relative intensity (I / I0×100)]]> 4.363°±0.30° s-vs 8.940°±0.30° ms 12.08°±0.30° ms 14.48°±0.30° ms 18.42°±0.50° wm 23.05°±0.30° wm 26.09°±0.30° vs .
[0033] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table B-1:
[0034] Table B-1
[0035] 2θ <![CDATA[Relative intensity (I / I0×100)]]> 4.363°±0.30° vs 8.940°±0.30° ms 12.08°±0.30° ms 14.48°±0.30° ms 18.42°±0.50° wm 23.05°±0.30° wm 26.09°±0.30° s-vs .
[0036] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table B-2:
[0037] Table B-2
[0038] 2θ <![CDATA[Relative intensity (I / I0×100)]]> 4.363°±0.30° 95-100 8.940°±0.30° 35-55 12.08°±0.30° 35-50 14.48°±0.30° 30-45 18.42°±0.50° 20-35 23.05°±0.30° 20-35 26.09°±0.30° 90-100 .
[0039] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table C:
[0040] Table C
[0041]
[0042] Where b: varies with 2θ.
[0043] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table C-1:
[0044] Table C-1
[0045]
[0046] Where b: varies with 2θ.
[0047] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table C-2:
[0048] Table C-2
[0049]
[0050] Where b: varies with 2θ.
[0051] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table D:
[0052] Table D
[0053]
[0054] Where b: varies with 2θ.
[0055] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table D-1:
[0056] Table D-1
[0057]
[0058] Where b: varies with 2θ.
[0059] In some embodiments, the X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table D-2:
[0060] Table D-2
[0061]
[0062] Where b: varies with 2θ.
[0063] In some embodiments, the framework topology of the SCM-53 molecular sieve includes [4] 2 ·5 4 ·10 4 ]、[5 2 ·6·10 2 ]、[4·5 4 ·6 5 ·7 4 ]、[6·7 2 The natural splicing structure of ].
[0064] In some embodiments, the framework topological minimal repeating unit of the SCM-53 molecular sieve consists of 1 [4] 2 ·5 4 ·10 4 ], 2 [5 2 ·6·10 2 ], 2 [4.5] 4 ·6 5 ·7 4 ] and 4 [6·7 2 Composed of naturally spliced structures.
[0065] In some embodiments, the SCM-53 molecular sieve includes a 10×10-membered ring channel structure.
[0066] In some embodiments, the SCM-53 molecular sieve contains one or more of 4-membered rings, 5-membered rings, 6-membered rings, 7-membered rings, and 10-membered rings.
[0067] In some embodiments, the SCM-53 molecular sieve belongs to the monoclinic crystal system.
[0068] In some embodiments, the cell parameters of the SCM-53 molecular sieve include Preferred More
[0069] In some embodiments, the cell parameters of the SCM-53 molecular sieve include Preferred More
[0070] In some embodiments, the cell parameters of the SCM-53 molecular sieve include Preferred More
[0071] In some embodiments, the cell parameters of the SCM-53 molecular sieve include α = 90° and γ = 90°.
[0072] In some embodiments, the cell parameters of the SCM-53 molecular sieve are β = 100°-125°, preferably β = 105°-115°.
[0073] In some embodiments, the SCM-53 molecular sieve comprises silicon, aluminum, and oxygen.
[0074] In some embodiments, the molar ratio (i.e., silicon-to-alumina ratio) of silica to alumina in the SCM-53 molecular sieve is 10-400, for example, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 105, 110, 115, 120, 125, 130, 135, 140, 145, 150, 155, 16 0, 165, 170, 175, 180, 185, 190, 195, 200, 205, 210, 215, 220, 225, 230, 235, 240, 245, 250, 255, 260, 265, 270, 275, 280, 285, 290, 300, 310, 320, 330, 340, 350, 360, 370, 380, 390, or any value between them. In some embodiments, the molar ratio of silicon dioxide to aluminum oxide is 15-350.
[0075] In some embodiments, the SCM-53 molecular sieve has a chemical composition of mSiO2·Al2O3 with the following molar ratios, where 10 ≤ m ≤ 400, for example, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, 90, 95, 100, 105, 110, 115, 120, 125, 130, 135, 140, 145, 150, 155, 160, 165, 170, 175, 180, 185, 190, 195, 200, 205, 210, 215, 220, 225, 230, 235, 240, 245, 250, 255, 260, 265, 270, 275, 280, 285, 290, 300, 310, 320, 330, 340, 350, 360, 370, 380, 390, or any value between them.
[0076] In some implementations, 15 ≤ m ≤ 350. In some implementations, 20 ≤ m ≤ 300.
[0077] In some embodiments, the SCM-53 molecular sieve crystals have a nanosheet morphology. In some embodiments, the average thickness of the crystals is less than or equal to 19 nm.
[0078] In some embodiments, the average thickness of the crystal is 3nm-18nm, for example, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, 10nm, 11nm, 12nm, 13nm, 14nm, 15nm, 16nm, 17nm, or any value between them. In some embodiments, the average thickness of the crystal is 5nm-16nm.
[0079] In some embodiments, in the SCM-53 molecular sieve, crystals with a thickness of less than or equal to 16 nm account for at least 70% of the total number of crystals, for example, at least 75%, at least 77%, at least 80%, at least 82%, at least 84%, at least 86%, at least 90%, at least 93%, or at least 95%.
[0080] In some embodiments, the specific surface area of the SCM-53 molecular sieve is 100 m². 2 / g-500m 2 / g, for example, 150m 2 / g、200m 2 / g、210m 2 / g、220m 2 / g、230m 2 / g、240m 2 / g、250m 2 / g、260m 2 / g、270m 2 / g、280m 2 / g、290m 2 / g、300m 2 / g、310m 2 / g、320m 2 / g、330m 2 / g、340m 2 / g, 350m 2 / g、360m 2 / g、370m 2 / g、380m 2 / g、390m 2 / g、400m 2 / g、430m 2 / g、450m 2 / g、470m 2 / g or any value between them. In some embodiments, the specific surface area of the SCM-53 molecular sieve is 200m². 2 / g-400m 2 / g.
[0081] In some embodiments, the pore volume of the SCM-53 molecular sieve is 0.015 cm³. 3 / g-1.0cm 3 / g, for example, 0.07cm 3 / g, 0.1cm 3 / g, 0.13cm 3 / g, 0.15cm 3 / g, 0.17cm 3 / g, 0.2cm 3 / g, 0.23cm 3 / g, 0.25cm 3 / g, 0.27cm 3 / g, 0.3cm 3 / g, 0.33cm 3 / g, 0.35cm 3 / g, 0.37cm 3 / g, 0.4cm 3 / g, 0.43cm 3 / g, 0.45cm 3 / g, 0.47cm 3 / g, 0.5cm 3 / g, 0.55cm 3 / g, 0.6cm 3 / g, 0.65cm 3 / g, 0.7cm 3 / g, 0.75cm3 / g, 0.8cm 3 / g, 0.85cm 3 / g, 0.9cm 3 / g, 0.95cm 3 / g or any value between them. In some embodiments, the pore volume of the SCM-53 molecular sieve is 0.05 cm³. 3 / g-0.75cm 3 / g.
[0082] In some embodiments, the SCM-53 molecular sieve further includes non-silicon and non-aluminum elements, preferably selected from one or more of sodium, potassium, germanium, titanium, boron, zirconium, tin, and iron.
[0083] In some embodiments, the SCM-53 molecular sieve further includes one or more elements selected from sodium, potassium, germanium, titanium, boron, zirconium, tin, and iron.
[0084] Secondly, the present invention provides a method for preparing SCM-53 molecular sieve, which includes the following steps:
[0085] S1: A mixture containing a silicon source, an aluminum source, an organic structure directing agent, and a solvent is subjected to crystallization treatment to obtain a crystallized product;
[0086] S2: Under acidic conditions, the crystallized product is mixed with a silanizing agent and then subjected to hydrothermal treatment to obtain the hydrothermally treated product;
[0087] S3: The hydrothermal treatment product is dried and calcined;
[0088] Preferably, the organic structure directing agent comprises a compound represented by Formula I.
[0089]
[0090] In Equation I, R1 and R2 may be the same or different, and are each independently selected from C. 1-8 Alkyl, X - Selected from OH - Halogen anions, nitrate ions, or monovalent organic acid anions; R3, R4, R5, and R6 may be the same or different, and each is independently selected from hydrogen, halogens, C 1-4 alkyl.
[0091] In some implementations, in Formula I, R1 and R2 may be the same or different, and each is independently selected from C. 1-4 Alkyl groups, such as methyl, ethyl, or propyl.
[0092] In some implementations, X - Selected from OH -Bromine ions, chloride ions, iodide ions, nitrate ions, or acetate ions.
[0093] In some embodiments, R3, R4, R5, and R6 may be the same or different, and each may be independently selected from hydrogen, fluorine, chlorine, bromine, methyl, ethyl, or propyl.
[0094] In some embodiments, at least one of R3, R4, R5, and R6 is hydrogen. In some embodiments, at least two of R3, R4, R5, and R6 are hydrogen. In some embodiments, all of R3, R4, R5, and R6 are hydrogen.
[0095] In some embodiments, the organic structure directing agent is selected from one or more of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide, 2,2-dimethyl-1,3-dihydroisoindole ammonium bromide, and 2,2-dimethyl-1,3-dihydroisoindole ammonium chloride.
[0096] In some embodiments, the silicon source is SiO2 and the aluminum source is Al2O3, and the molar ratio of the silicon source to the aluminum source is 1:(0.0025-0.1), for example 1:0.003, 1:0.004, 1:0.005, 1:0.006, 1:0.007, 1:0.008, 1:0.009, 1:0.0095, 1:0.01, 1:0.013, 1:0.015, 1:0.017, 1:0.02, 1:0.023, 1:0.025, 1:0.027, 1:0.03, 1:0.033, 1:0.004, 1:0.005 ... 0.035, 1:0.037, 1:0.04, 1:0.043, 1:0.045, 1:0.047, 1:0.05, 1:0.053, 1:0.055, 1:0.057, 1:0.06, 1:0.063, 1:0.065, 1:0.067, 1:0.07, 1:0.073, 1:0.075, 1:0.077, 1:0.08, 1:0.083, 1:0.085, 1:0.047, 1:0.09, 1:0.093, 1:0.095, 1:0.097, or any value between them.
[0097] In some embodiments, the molar ratio of the silicon source to the aluminum source is 1:(0.0025-0.08). In some embodiments, the molar ratio of the silicon source to the aluminum source is 1:(0.005-0.05).
[0098] In some embodiments, the silicon source is SiO2, and the molar ratio of the silicon source to the organic structure directing agent is 1:(0.10-0.50), for example, 1:0.13, 1:0.15, 1:0.17, 1:0.20, 1:0.23, 1:0.25, 1:0.27, 1:0.30, 1:0.33, 1:0.35, 1:0.37, 1:0.40, 1:0.43, 1:0.45, 1:0.47 or any value between them.
[0099] In some embodiments, the molar ratio of the silicon source to the organic structure directing agent is 1:(0.20-0.50). In some embodiments, the molar ratio of the silicon source to the organic structure directing agent is 1:(0.30-0.50).
[0100] In some embodiments, the silicon source is SiO2, and the molar ratio of the silicon source to the solvent is 1:(8-100), for example, 1:10, 1:15, 1:20, 1:25, 1:30, 1:35, 1:40, 1:45, 1:50, 1:55, 1:60, 1:65, 1:70, 1:75, 1:80, 1:85, 1:90, 1:95, or any value between them.
[0101] In some embodiments, the molar ratio of the silicon source to the solvent is 1:(15-100). In some embodiments, the molar ratio of the silicon source to the solvent is 1:(15-50).
[0102] In some embodiments, the acidic conditions are provided by an acid solution. In some embodiments, the concentration of the acid solution is 0.5 mol / L to 6 mol / L, for example, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L, 3 mol / L, 3.5 mol / L, 4 mol / L, 4.5 mol / L, 5 mol / L, 5.5 mol / L, or any value between them. In some embodiments, the concentration of the acid solution is 1 mol / L to 5 mol / L. In some embodiments, the concentration of the acid solution is 1.5 mol / L to 4.5 mol / L.
[0103] In some embodiments, the liquid-to-solid ratio of the acid solution to the crystallized product is (10-100) mL:1g, for example, 20 mL:1g, 30 mL:1g, 40 mL:1g, 50 mL:1g, 60 mL:1g, 70 mL:1g, 80 mL:1g, or 90 mL:1g. In some embodiments, the liquid-to-solid ratio of the acid solution to the crystallized product is (20-80) mL:1g. In some embodiments, the liquid-to-solid ratio of the acid solution to the crystallized product is (40-60) mL:1g.
[0104] In some embodiments, the mass ratio of the silanizing agent to the crystallized product is (0.1-4):1, for example, 0.2:1, 0.3:1, 0.4:1, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1.0:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1, 1.8:1, 1.9:1, 2.0:1, 2.3:1, 2.5:1, 2.7:1, 3.0:1, 3.3:1, 3.5:1, or 3.7:1. In some embodiments, the mass ratio of the silanizing agent to the crystallized product is (0.2-2):1.
[0105] In some embodiments, the acid solution is selected from aqueous hydrochloric acid solution, aqueous acetic acid solution, aqueous nitric acid solution, hydrochloric acid ethanol solution, acetic acid ethanol solution, or nitric acid ethanol solution.
[0106] In some embodiments, the silanizing agent comprises a compound represented by Formula II.
[0107]
[0108] In Equation II, R7, R8, R9 and R 10 Whether the elements are the same or different, they are each independently selected from hydrogen, halogens, and carbon. 1-6 Alkyl, C 1-6 Alkyl group.
[0109] In some implementations, R7, R8, R9 and R 10 They may be the same or different, each independently selected from hydrogen, fluorine, chlorine, bromine, methyl, ethyl, propyl, methoxy, ethoxy, and propoxy.
[0110] In some embodiments, the silanizing agent is selected from one or more of monomethylchlorosilane, dimethylchlorosilane, monomethylmethoxysilane, dimethylmethoxysilane, monomethylethoxysilane, and dimethylethoxysilane.
[0111] In this invention, silanizing agents are used to directionally modify the pore walls of molecular sieve precursors under acidic conditions.
[0112] In some embodiments, the silicon source is selected from one or more of silica sol, silica gel, tetraethyl orthosilicate, and silicic acid.
[0113] In some embodiments, the aluminum source is selected from one or more of aluminum hydroxide, aluminum isopropoxide, aluminum nitrate, and aluminum oxide.
[0114] In some embodiments, the solvent is selected from water.
[0115] In some embodiments, the mixture does not contain alkali metals or alkaline earth metals.
[0116] According to one embodiment of the present invention, in the method for synthesizing the molecular sieve, from the perspective of more advantageously obtaining the SCM-53 molecular sieve of the present invention, the mixture does not contain an alkaline source. Examples of alkaline sources include, for example, alkaline substances other than silicon sources, aluminum sources, and organic structure directing agents; specifically, any alkaline source conventionally used in the art for the purpose of making the system alkaline; more specifically, inorganic bases with alkali metal or alkaline earth metal cations, particularly sodium hydroxide and potassium hydroxide, etc. Here, "does not contain an alkaline source" means that no alkaline source is intentionally or actively introduced into the mixture.
[0117] In some embodiments, the crystallization process of the mixture is a rotating dynamic crystallization. In some embodiments, the rotation speed is 10 rpm to 60 rpm, for example, 20 rpm, 30 rpm, or 40 rpm.
[0118] In some embodiments, the crystallization process of the mixture is dynamic crystallization with stirring. In some embodiments, the stirring speed is 30 rpm to 400 rpm, for example, 50 rpm, 100 rpm, 150 rpm, 200 rpm, 250 rpm, 300 rpm, or 350 rpm.
[0119] In some embodiments, the crystallization conditions of the mixture are 130°C-180°C, for example, 135°C, 140°C, 145°C, 150°C, 155°C, 160°C, 165°C, 170°C, or 175°C, for 1-12 days, for example, 2 days, 3 days, 4 days, 5 days, 6 days, 7 days, 8 days, 9 days, 10 days, or 11 days. In some embodiments, the crystallization conditions of the mixture are 135°C-175°C, for 2-11 days. In some embodiments, the crystallization conditions of the mixture are 140°C-170°C, for 3-10 days.
[0120] In some embodiments, the temperature of the hydrothermal treatment is 80°C-190°C, for example, 90°C, 100°C, 110°C, 120°C, 130°C, 140°C, 150°C, 160°C, 170°C or 180°C.
[0121] In some embodiments, the hydrothermal treatment time is 5h-48h, for example 8h, 10h, 12h, 15h, 20h, 24h, 28h, 30h, 32h, 36h, 40h, 44h or 46h.
[0122] In some embodiments, the calcination temperature is 400°C-800°C, for example, 450°C, 500°C, 550°C, 600°C, 650°C, 700°C, or 750°C. In some embodiments, the calcination temperature is 500°C-700°C.
[0123] In some embodiments, the roasting time is 2h-10h, for example 3h, 4h, 5h, 6h, 7h, 8h or 9h. In some embodiments, the roasting time is 3h-9h.
[0124] In some embodiments, the calcination is carried out in an oxygen-containing atmosphere.
[0125] In some embodiments, the calcination conditions for the hydrothermal treatment product are calcination at 400℃-800℃ in an oxygen-containing atmosphere for 2 to 10 hours, preferably calcination at 500℃-700℃ in an oxygen-containing atmosphere for 3 to 9 hours.
[0126] According to the present invention, the various SCM-53 molecular sieves obtained above can be used in any physical form, such as powder, granules, or molded products (e.g., strips, clover shapes, etc.). These physical forms can be obtained in any manner conventionally known in the art, without particular limitation.
[0127] Thirdly, the present invention provides a molecular sieve composition comprising the SCM-53 molecular sieve described in the first aspect or the SCM-53 molecular sieve prepared by the preparation method described in the second aspect, and an optional binder.
[0128] According to the present invention, the SCM-53 molecular sieve can be used in combination with other materials to obtain an SCM-53 molecular sieve composition. Examples of these other materials include active and inactive materials. Examples of active materials include synthetic zeolites, natural zeolites, or other types of molecular sieves, while examples of inactive materials (generally referred to as binders) include clay, kaolin, silica gel, and alumina. These other materials can be used individually or in combination in any proportion. The amount of these other materials used can be directly referenced from conventional amounts used in the art and is not particularly limited.
[0129] Fourthly, the present invention provides the application of the SCM-53 molecular sieve described in the first aspect, the SCM-53 molecular sieve prepared by the preparation method described in the second aspect, or the molecular sieve composition described in the third aspect in adsorption separation, ion exchange, or catalytic conversion of organic compounds.
[0130] In some embodiments, the SCM-53 molecular sieve or molecular sieve composition is used to separate at least one component from a mixture of multiple components in a gaseous or liquid phase. Accordingly, the at least one component can be partially or substantially completely separated from the mixture of various components, for example by contacting the mixture with the SCM-53 molecular sieve or the molecular sieve composition to selectively adsorb the component.
[0131] The SCM-53 molecular sieve involved in this invention has a novel framework structure and / or chemical composition, and has very important application value. Attached Figure Description
[0132] Figure 1 The X-ray diffraction (XRD) pattern of the sample in Example 1;
[0133] Figure 2 This is a schematic diagram of the crystal structure (2×2×2 unit cells) of the sample in Example 1 projected along the directions a)
[100] , b)
[010] , c)
[110] and d)
[010] .
[0134] Figure 3 a) Naturally collaged composition and b) Naturally collaged blocks contained in the crystal topology of the sample in Example 1;
[0135] Figure 4 The image shown is a scanning electron microscope (SEM) image of the sample in Example 1.
[0136] Figure 5 This is the N2 adsorption-desorption curve of the sample in Example 1;
[0137] Figure 6 The X-ray diffraction (XRD) pattern of the sample in Example 2;
[0138] Figure 7 This is a scanning electron microscope (SEM) image of the sample in Example 2. Detailed Implementation
[0139] The specific embodiments of the present invention will be described in detail below. However, it should be noted that the scope of protection of the present invention is not limited to these specific embodiments, but is determined by the claims in the appendix.
[0140] All publications, patent applications, patents, and other references mentioned in this specification are incorporated herein by reference. Unless otherwise defined, all technical and scientific terms used in this specification have the meanings commonly understood by those skilled in the art. In case of conflict, the definitions in this specification shall prevail.
[0141] When this specification uses the prefixes “known to those skilled in the art,” “prior art,” or similar terms to derive materials, substances, methods, steps, apparatus, or components, the objects derived from such prefixes cover those commonly used in the art at the time of this application, but also include those that are not currently commonly used but will become generally recognized in the art as suitable for similar purposes.
[0142] In the context of this specification, except where expressly stated, any matters or issues not mentioned herein shall apply directly to those known in the art without any modification. Furthermore, any implementation described herein may be freely combined with one or more other implementations described herein, and any resulting technical solutions or concepts shall be considered part of the original disclosure or original record of this invention, and should not be regarded as new content not disclosed or anticipated herein, unless those skilled in the art consider such combination to be clearly unreasonable.
[0143] In the context of this specification, in XRD data of molecular sieve precursors, w, m, s, and vs represent diffraction peak intensities, where w is weak, m is moderate, s is strong, and vs is very strong, as is well known to those skilled in the art. Generally, w is less than 20, for example, 5, 7, 10, 11, 12, 13, 14, 15, 16, 17, 18, or 19; m is 20–40, for example, 21, 23, 25, 27, 29, 30, 31, 33, 35, 37, or 39; s is 40–70, for example, 41, 43, 45, 47, 49, 50, 51, 53, 55, 57, 59, 60, 61, 63, 65, 67, or 69; and vs is greater than 70, for example, 75, 80, 85, 90, 95, or 100.
[0144] In the context of this specification, the structure of the molecular sieve is determined by X-ray diffraction (XRD), which is measured using an X-ray powder diffractometer with a Cu-Kα ray source and a nickel filter. Before sample testing, the crystallization of the molecular sieve precursor sample is observed using a scanning electron microscope (SEM) to confirm that the sample contains only one type of crystal, i.e., the molecular sieve sample is a pure phase. XRD testing is then performed to ensure that there are no interfering peaks from other crystals in the diffraction pattern.
[0145] In the context of this specification, including in the following examples and comparative examples, the X-ray powder diffractometer used for the molecular sieves is a Panalytical X-PERPRO type X-ray powder diffractometer, used to analyze the phase composition of the samples, and a CuKα ray source. Nickel filter, 2θ scanning range 2°-50°, operating voltage 40KV, current 40mA, scanning rate 10° / min.
[0146] In some embodiments, the SCM-53 molecular sieve of the present invention has Figure 1 or Figure 6 The X-ray diffraction pattern shown.
[0147] In some embodiments, the framework topology of the SCM-53 molecular sieve of the present invention includes, for example: Figure 3 The natural splicing structure shown in b.
[0148] In some embodiments, the framework topology of the SCM-53 molecular sieve of the present invention has the following characteristics: Figure 3 The repeating unit shown in a.
[0149] In the context of this specification, including in the following examples and comparative examples, the scanning electron microscope (SEM) used for the molecular sieves is an S-4800II field emission scanning electron microscope. The molecular sieves were observed using this SEM at a magnification of 40,000x. A randomly selected field of view was used to calculate the average sum of the thicknesses of all crystals within that field of view, and this operation was repeated 10 times. The average sum of the 10 measurements was taken as the crystal thickness, and the size of all aggregates within that field of view was measured using the same method.
[0150] In the context of this specification, including in the following examples and comparative examples, the molecular sieve was analyzed using an inductively coupled plasma atomic emission spectrometer (ICP) model Varian 725-ES, and the elemental content, in molar terms, was determined by dissolving the analytical sample in hydrofluoric acid.
[0151] In the context of this specification, specific surface area refers to the total surface area per unit mass of a sample, including internal and external surface areas. Non-porous samples only have external surface area, such as silicate cement and some clay mineral powders; porous and multi-porous samples have both external and internal surface areas, such as asbestos fibers, diatomaceous earth, and molecular sieves. In porous and multi-porous samples, the surface area of pores with a diameter less than 2 nanometers is the internal surface area; the surface area after deducting the internal surface area is called the external surface area. The external surface area per unit mass of a sample is called the external specific surface area.
[0152] In the context of this specification, pore volume refers to the volume of pores per unit mass of porous material. Total pore volume refers to the volume of all pores per unit mass of molecular sieve (generally only pores with a channel diameter less than 50 nanometers are included). Micropore volume refers to the volume of all micropores per unit mass of molecular sieve (generally referring to pores with a channel diameter less than 2 nanometers). The pore structure parameters of the molecular sieve, such as total pore volume, micropore volume, total specific surface area, and external specific surface area, are obtained by measuring the nitrogen physical adsorption-desorption isotherm of the molecular sieve using a physical adsorption instrument (such as the TriStar 3000 physical adsorption instrument from Micron Instruments, Inc.), and then calculating them using the BET method and t-plot method. The experimental conditions for nitrogen physical adsorption-desorption are: measurement temperature -169℃, and the molecular sieve is pretreated in vacuum at 300℃ for 10 hours before measurement.
[0153] The technical solution of the present invention will be further described in detail below through embodiments, but the scope of protection of the present invention is not limited to these embodiments.
[0154] The 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution in this invention is prepared by the following method:
[0155] 6.7336 g of 1,2-di(bromomethyl)benzene, 3.4551 g of anhydrous potassium carbonate (acid-binding agent), and 100 mL of N,N-dimethylformamide were mixed and stirred at 1000 rpm until homogeneous. Under reflux, the mixture was heated to 60 °C while stirring. Then, 12.5 mL of dimethylamine (a tetrahydrofuran solution of dimethylamine, 2 M solution in THF) was added dropwise to the system at a constant pressure, controlling the dropping rate at 3-4 seconds per drop. The final molar ratio of the reactants in the reaction system was: anhydrous potassium carbonate / 1,2-di(bromomethyl)benzene = 1, dimethylamine / 1,2-di(bromomethyl)benzene = 1, and N,N-dimethylformamide / 1,2-di(bromomethyl)benzene = 51.7.
[0156] After the addition was complete, reflux was continued for 8 hours, and the mixture was allowed to stand at room temperature to obtain the reaction mixture. The reaction mixture was filtered to remove the solid-phase acid-binding agent and some byproducts. The liquid phase was subjected to vacuum distillation to recover most of the N,N-dimethylformamide and reused. The remaining mother liquor was recrystallized multiple times with tetrahydrofuran solution and dried to obtain a nitrogen-containing heterocyclic quaternary ammonium salt based on 1,2-di(bromomethyl)benzene.
[0157] 0.1 mol of a nitrogen-containing heterocyclic quaternary ammonium salt, an appropriate amount of deionized water, and 100 g of anion exchange resin were stirred at room temperature for 12 h, and then filtered to obtain 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide. Solution.
[0158] Example 1
[0159] 35.17 g of deionized water, 155.1 g of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution (containing 17 wt% OSDA 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide), 75.11 g of silica sol (containing 40 wt% SiO2), and 1.758 g of aluminum hydroxide were mixed evenly and stirred at room temperature for 10 hours to obtain a mixture. The final material ratio (molar ratio) was: Al2O3 / SiO2 = 0.02, OSDA / SiO2 = 0.32, H2O / SiO2 = 40.
[0160] The mixture prepared above was placed in a stainless steel reactor and crystallized for 3 days at 160°C and 30 rpm. After crystallization, the mixture was centrifuged and washed until the pH value was near neutral (pH = 7-8), and then dried in an oven at 110°C to obtain the precursor.
[0161] The precursor prepared above was subjected to silanization treatment. 10 g of precursor, 400 mL of 2 mol / L nitric acid solution and 3 g of dimethylethoxysilane were mixed and stirred at room temperature for 0.5 h. The mixed solution was then hydrothermally treated at 170 °C for 24 h and finally calcined at 550 °C in an oxygen-containing atmosphere for 6 h to obtain 16.5 g of sample.
[0162] The XRD pattern of the sample is as follows Figure 1 As shown in Table 1, the yield of SCM-53 molecular sieve is 55 wt%.
[0163] Synchrotron radiation XRD determines the structural information of the sample, such as Figure 2 As shown in Tables 2 and 3, information on hydrogen atoms is omitted from the sample structure information tables. The natural composition of the samples is as follows: Figure 3 As shown.
[0164] from Figure 2 As can be seen, the sample is a two-dimensional 10×10 membered ring pore structure molecular sieve, and the sample structure contains 4-membered rings, 5-membered rings, 6-membered rings, 7-membered rings and 10-membered rings.
[0165] from Figure 3 As can be seen from b: the skeleton topology of the sample includes [4] 2 ·5 4 ·10 4 ]、[5 2 ·6·10 2 ]、[4·5 4 ·6 5 ·7 4 ]、[6·7 2 The natural splicing structure of ].
[0166] from Figure 3 As can be seen from a: the minimum repeating unit of the sample's skeleton topology consists of 1 [4] 2·5 4 ·10 4 ], 2 [5 2 ·6·10 2 ], 2 [4.5] 4 ·6 5 ·7 4 ] and 4 [6·7 2 Composed of naturally spliced structures.
[0167] SEM images of the samples are as follows Figure 4 As shown, it has a nanosheet-like morphology.
[0168] The N2 adsorption-desorption curves of the obtained samples are shown below. Figure 5 As shown, the specific surface area of the sample is 170 m². 2 / gram, total pore volume is 0.17 cm³ 3 / gram.
[0169] The silicon-aluminum molar ratio of the sample was determined to be 76.89SiO2·Al2O3 using inductively coupled plasma atomic emission spectrometry (ICP).
[0170] Table 1
[0171]
[0172] Table 2
[0173]
[0174]
[0175] Table 3
[0176]
[0177] Example 2
[0178] 22.1 g of deionized water, 242.5 g of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution (containing 33 wt% OSDA2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide), 75.11 g of silica sol (containing 40 wt% SiO2), and 4.393 g of aluminum hydroxide were mixed evenly and stirred at room temperature for 5 hours to obtain a mixture. The final material ratio (molar ratio) was: Al2O3 / SiO2 = 0.05, OSDA / SiO2 = 0.5, H2O / SiO2 = 30.
[0179] The mixture prepared above was placed in a stainless steel reactor and crystallized for 4 days at 150°C and 30 rpm. After crystallization, the mixture was centrifuged and washed until the pH value was near neutral (pH = 7-8), and then dried in an oven at 110°C to obtain the precursor.
[0180] The precursor prepared above was subjected to silanization treatment. 10 g of precursor, 500 mL of 2 mol / L nitric acid solution and 3 g of dimethylethoxysilane were mixed and stirred at room temperature for 0.5 h. The mixed solution was then hydrothermally treated at 160 °C for 28 h. Finally, it was calcined at 550 °C in an oxygen-containing atmosphere for 5 h to obtain 18.0 g of sample.
[0181] The XRD pattern of the sample is as follows Figure 6 As shown in Table 4, the yield of SCM-53 molecular sieve is 60 wt%.
[0182] SEM images of the samples are as follows Figure 7 As shown, it has a nanosheet-like morphology.
[0183] Table 4
[0184]
[0185] The specific surface area of the obtained sample was 308 m². 2 / gram, total pore volume is 0.22 cm³. 3 / gram.
[0186] The silicon-aluminum molar ratio of the sample was determined to be 43.21SiO2·Al2O3 using inductively coupled plasma atomic emission spectrometry (ICP).
[0187] Example 3
[0188] 12.9 g of deionized water, 145.5 g of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution (containing 17 wt% OSDA2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide), 75.11 g of silica sol (containing 40 wt% SiO2), and 3.516 g of aluminum hydroxide were mixed evenly and stirred at room temperature for 4 hours to obtain a mixture. The final material ratio (molar ratio) was: Al2O3 / SiO2 = 0.02, OSDA / SiO2 = 0.3, H2O / SiO2 = 20.
[0189] The mixture prepared above was placed in a stainless steel reactor and crystallized for 3 days at 170°C and 30 rpm. After crystallization, the mixture was centrifuged and washed until the pH value was near neutral (pH = 7-8), and then dried in an oven at 110°C to obtain the precursor.
[0190] The precursor prepared above was subjected to silanization treatment. 10 g of precursor, 500 mL of 2 mol / L nitric acid solution and 3.375 g of dimethylethoxysilane were mixed and stirred at room temperature for 0.5 h. The mixed solution was then hydrothermally treated at 150 °C for 24 h and finally calcined at 550 °C in an oxygen-containing atmosphere for 5 h to obtain 17.4 g of sample.
[0191] The XRD patterns of the samples are shown in Table 5. The samples are SCM-53 molecular sieves, and the yield of the molecular sieves is 58 wt%.
[0192] SEM images of the samples and Figure 4 Similarly, it has a nanosheet-like morphology.
[0193] Table 5
[0194]
[0195] The specific surface area of the obtained sample was 328 m². 2 / gram, total pore volume is 0.25 cm³ 3 / gram.
[0196] The silicon-aluminum molar ratio of the sample was determined to be 75.01SiO2·Al2O3 using inductively coupled plasma atomic emission spectrometry (ICP).
[0197] Example 4
[0198] 16.8 g of deionized water, 15.00 g of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution (containing 17 wt% OSDA 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide), 15.02 g of silica sol (containing 40 wt% SiO2), and 0.352 g of aluminum hydroxide were mixed evenly and stirred at room temperature for 6 hours to obtain a mixture. The final material ratio (molar ratio) was: Al2O3 / SiO2 = 0.01, OSDA / SiO2 = 0.4, H2O / SiO2 = 30.
[0199] The mixture prepared above was placed in a stainless steel reactor and crystallized for 5 days at 140°C and 30 rpm. After crystallization, the mixture was centrifuged and washed until the pH value was near neutral (pH = 7-8), and then dried in an oven at 110°C to obtain the precursor.
[0200] The precursor prepared above was subjected to silanization treatment. 10 g of precursor, 400 mL of 2.5 mol / L nitric acid solution and 2.275 g of dimethylethoxysilane were mixed and stirred at room temperature for 0.5 h. The mixed solution was then hydrothermally treated at 190 °C for 5 h and finally calcined at 600 °C in an oxygen-containing atmosphere for 6 h to obtain 3.2 g of sample.
[0201] The XRD pattern of the sample is similar to that in Table 6, indicating that it is an SCM-53 molecular sieve with a yield of 54 wt%.
[0202] SEM images of the samples and Figure 4 Similarly, it has a nanosheet-like morphology.
[0203] Table 6
[0204]
[0205] The specific surface area of the obtained sample was 288 m². 2 / gram, total pore volume is 0.21 cm³ 3 / gram.
[0206] The silicon-aluminum molar ratio of the sample was determined to be 105.21SiO2·Al2O3 using inductively coupled plasma atomic emission spectrometry (ICP).
[0207] Example 5
[0208] 5.1 g of deionized water, 58.196 g of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution (containing 17 wt% OSDA 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide), 30.045 g of silica sol (containing 40 wt% SiO2), and 1.5 g of aluminum nitrate were mixed evenly and stirred at room temperature for 10 hours to obtain a mixture. The final material ratio (molar ratio) was: Al2O3 / SiO2 = 0.01, OSDA / SiO2 = 0.3, H2O / SiO2 = 20.
[0209] The mixture prepared above was placed in a stainless steel reactor and crystallized for 3 days at 160°C and 30 rpm. After crystallization, the mixture was centrifuged and washed until the pH value was near neutral (pH = 7-8), and then dried in an oven at 110°C to obtain the precursor.
[0210] The precursor prepared above was subjected to silanization treatment. 10 g of precursor, 400 mL of 2 mol / L nitric acid solution and 3 g of dimethylethoxysilane were mixed and stirred at room temperature for 0.5 h. The mixed solution was then hydrothermally treated at 170 °C for 24 h. Finally, it was calcined at 550 °C in an oxygen-containing atmosphere for 6 h to obtain 8.4 g of sample.
[0211] The XRD patterns of the samples are shown in Table 7. The samples are SCM-53 molecular sieves, and the yield of the molecular sieves is 70 wt%.
[0212] SEM images of the samples and Figure 4 Similarly, it has a nanosheet-like morphology.
[0213] Table 7
[0214]
[0215]
[0216] The specific surface area of the obtained sample was 301 m². 2 / gram, total pore volume is 0.22 cm³. 3 / gram.
[0217] The silicon-aluminum molar ratio of the sample was determined to be 101.89SiO2·Al2O3 using inductively coupled plasma atomic emission spectrometry (ICP).
[0218] Example 6
[0219] 35.17 g of deionized water, 58.196 g of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide solution (containing 17 wt% OSDA 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide), 41.67 g of tetraethyl orthosilicate (containing 28.8 wt% SiO2), and 0.409 g of aluminum isopropoxide were mixed evenly and stirred at room temperature for 10 hours to obtain a mixture. The final material ratio (molar ratio) was: Al2O3 / SiO2 = 0.01, OSDA / SiO2 = 0.3, H2O / SiO2 = 20.
[0220] The mixture prepared above was placed in a stainless steel reactor and crystallized for 3 days at 160°C and 30 rpm. After crystallization, the mixture was centrifuged and washed until the pH value was near neutral (pH = 7-8), and then dried in an oven at 110°C to obtain the precursor.
[0221] The precursor prepared above was subjected to silanization treatment. 10 g of precursor, 400 mL of 2 mol / L nitric acid solution and 3 g of dimethylethoxysilane were mixed and stirred at room temperature for 0.5 h. The mixed solution was then hydrothermally treated at 170 °C for 24 h and finally calcined at 550 °C in an oxygen-containing atmosphere for 6 h to obtain 8.64 g of sample.
[0222] The XRD patterns of the samples are shown in Table 8. The samples are SCM-53 molecular sieves, and the yield of the molecular sieves is 72 wt%.
[0223] SEM images of the samples and Figure 4 Similarly, it has a nanosheet-like morphology.
[0224] Table 8
[0225]
[0226] The specific surface area of the obtained sample was 288 m². 2 / gram, total pore volume is 0.20 cm³ 3 / gram.
[0227] The silicon-aluminum molar ratio of the sample was determined to be 103.8SiO2·Al2O3 using inductively coupled plasma atomic emission spectrometry (ICP).
[0228] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.
Claims
1. An SCM-53 molecular sieve, characterized in that, The X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table A: Table A 。 2. The SCM-53 molecular sieve according to claim 1, characterized in that, The X-ray diffraction pattern of the SCM-53 molecular sieve also includes one or more diffraction peaks with 2θ values of 14.48°±0.30°, 18.42°±0.50°, and 23.05°±0.30°.
3. The SCM-53 molecular sieve according to claim 1, characterized in that, The X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table B: Table B 。 4. The SCM-53 molecular sieve according to claim 1, characterized in that, The X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table C: Table C Where b: varies with 2θ.
5. The SCM-53 molecular sieve according to claim 1, characterized in that, The X-ray diffraction pattern of the SCM-53 molecular sieve includes the diffraction peaks shown in Table D: Table D Where b: varies with 2θ.
6. The SCM-53 molecular sieve according to claim 1, characterized in that, The SCM-53 molecular sieve comprises silicon, aluminum, and oxygen; and / or The SCM-53 molecular sieve crystals have a nanosheet morphology, and the average thickness of the crystals is less than or equal to 19 nm; and / or The specific surface area of the SCM-53 molecular sieve is 100 m². 2 / g-500m 2 / g; and / or The SCM-53 molecular sieve has a pore volume of 0.015 cm³. 3 / g-1.0cm 3 / g.
7. The SCM-53 molecular sieve according to claim 1, characterized in that, In the SCM-53 molecular sieve, the molar ratio of silicon dioxide to aluminum oxide is 10-400.
8. The SCM-53 molecular sieve according to claim 1, characterized in that, In the SCM-53 molecular sieve, the molar ratio of silicon dioxide to aluminum oxide is 15-350.
9. The SCM-53 molecular sieve according to claim 1, characterized in that, The SCM-53 molecular sieve has a chemical composition with the following molar ratio: mSiO2·Al2O3, where 10≤m≤400.
10. The SCM-53 molecular sieve according to claim 9, characterized in that, 15≤m≤350。 11. The SCM-53 molecular sieve according to claim 9, characterized in that, 20≤m≤300。 12. The SCM-53 molecular sieve according to claim 1, characterized in that, The SCM-53 molecular sieve crystals have a nanosheet morphology, and the average thickness of the crystals is 3nm-18nm.
13. The SCM-53 molecular sieve according to claim 1, characterized in that, The SCM-53 molecular sieve crystals have a nanosheet morphology, and the average thickness of the crystals is 5nm-16nm.
14. The SCM-53 molecular sieve according to claim 1, characterized in that, In the SCM-53 molecular sieve, crystals with a thickness of 16 nm or less account for at least 70% of the total number of crystals.
15. The SCM-53 molecular sieve according to claim 1, characterized in that, The specific surface area of the SCM-53 molecular sieve is 200 m². 2 / g-400m 2 / g.
16. The SCM-53 molecular sieve according to claim 1, characterized in that, The SCM-53 molecular sieve has a pore volume of 0.05 cm³. 3 / g-0.75cm 3 / g.
17. The SCM-53 molecular sieve according to claim 1, characterized in that, The SCM-53 molecular sieve further includes one or more elements selected from sodium, potassium, titanium, boron, zirconium, tin, and iron; and / or The framework topology of the SCM-53 molecular sieve includes [4] 2 5 4 10 4 ]、[5 2 6 10 2 ]、[4 5 4 6 5 7 4 ]、[6 7 2 The natural splicing structure of ]; and / or The minimum repeating unit of the SCM-53 molecular sieve framework topology consists of 1 [4] 2 5 4 10 4 ], 2 [5 2 6 10 2 ], 2 [4 5 4 6 5 7 4 ] and 4 [6 7 2 Composed of naturally joined structural elements; and / or The SCM-53 molecular sieve comprises a 10×10 member ring channel structure; and / or The SCM-53 molecular sieve contains one or more of the following: 4-membered rings, 5-membered rings, 6-membered rings, 7-membered rings, and 10-membered rings; and / or The SCM-53 molecular sieve belongs to the monoclinic crystal system.
18. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include a = 8.0 Å-11.5 Å.
19. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include a = 8.5 Å-11.0 Å.
20. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include a = 9.0 Å - 10.5 Å.
21. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include b = 8.0 Å - 11.5 Å.
22. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include b = 8.5 Å - 11.0 Å.
23. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include b = 9.0 Å - 11.0 Å.
24. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include c = 18.0 Å - 22.0 Å.
25. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include c = 18.5Å-21.5Å.
26. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include c = 19.0 Å - 21.0 Å.
27. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve include α = 90 ° and γ = 90 °.
28. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve are β = 100°-125°.
29. The SCM-53 molecular sieve according to claim 1, characterized in that, The cell parameters of the SCM-53 molecular sieve are β = 105°-115°.
30. A method for preparing SCM-53 molecular sieve, comprising the following steps: S1: A mixture containing a silicon source, an aluminum source, an organic structure directing agent, and a solvent is subjected to crystallization treatment to obtain a crystallized product; S2: Under acidic conditions, the crystallized product is mixed with a silanizing agent and then subjected to hydrothermal treatment to obtain the hydrothermally treated product; S3: The hydrothermal treatment product is dried and calcined; The organic structure directing agent includes compounds represented by Formula I. Equation I In Equation I, R1 and R2 may be the same or different, and are each independently selected from C. 1-8 Alkyl; X - Selected from OH - Halogen anions, nitrate ions, or monovalent organic acid anions; R3, R4, R5, and R6 may be the same or different, and each is independently selected from hydrogen, halogens, C 1-4 alkyl; The silicon source is calculated as SiO2 and the aluminum source is calculated as Al2O3, and the molar ratio of the silicon source to the aluminum source is 1:(0.0025-0.1). The molar ratio of the silicon source to the organic structure directing agent is 1:(0.10-0.50); The molar ratio of the silicon source to the solvent is 1:(8-100); The acidic conditions are provided by an acid solution; The mass ratio of the silanizing agent to the crystallization product is (0.1-4):1; The concentration of the acid solution is 0.5 mol / L-6 mol / L; The liquid-to-solid ratio of the acid solution to the crystallized product is (10-100) mL:1 g; The silanizing agent includes compounds represented by Formula II. Formula II In Equation II, R7, R8, R9 and R 10 Whether the elements are the same or different, they are each independently selected from hydrogen, halogens, and carbon. 1-6 Alkyl, C 1-6 Alkoxy; The crystallization process of the mixture is dynamic crystallization by rotation or stirring, with a rotation speed of 10 rpm-60 rpm and a stirring speed of 30 rpm-400 rpm; the crystallization conditions of the mixture are crystallization at 130℃-180℃ for 1-12 days. The temperature of the hydrothermal treatment is 80℃-190℃; The hydrothermal treatment time is 5h-48h; The roasting temperature is 400℃-800℃; The roasting time is 2h-10h.
31. The preparation method according to claim 30, characterized in that, In Equation I, R1 and R2 may be the same or different, and are each independently selected from C. 1-4 alkyl.
32. The preparation method according to claim 30, characterized in that, In Formula I, R1 and R2 may be the same or different, and each is independently selected from methyl, ethyl or propyl.
33. The preparation method according to claim 30, characterized in that, R3, R4, R5, and R6 may be the same or different, and each is independently selected from hydrogen, fluorine, chlorine, bromine, methyl, ethyl, or propyl.
34. The preparation method according to claim 30, characterized in that, The organic structure directing agent is selected from one or more of 2,2-dimethyl-1,3-dihydroisoindole ammonium hydroxide, 2,2-dimethyl-1,3-dihydroisoindole ammonium bromide, and 2,2-dimethyl-1,3-dihydroisoindole ammonium chloride.
35. The preparation method according to claim 30, characterized in that, The silicon source is calculated as SiO2 and the aluminum source is calculated as Al2O3, and the molar ratio of the silicon source to the aluminum source is 1:(0.0025-0.08).
36. The preparation method according to claim 30, characterized in that, The silicon source is SiO2 and the aluminum source is Al2O3, and the molar ratio of the silicon source to the aluminum source is 1:(0.005-0.05).
37. The preparation method according to claim 30, characterized in that, The molar ratio of the silicon source to the organic structure directing agent is 1:(0.20-0.50).
38. The preparation method according to claim 30, characterized in that, The molar ratio of the silicon source to the organic structure directing agent is 1:(0.30-0.50).
39. The preparation method according to claim 30, characterized in that, The molar ratio of the silicon source to the solvent is 1:(15-100).
40. The preparation method according to claim 30, characterized in that, The molar ratio of the silicon source to the solvent is 1:(15-50).
41. The preparation method according to claim 30, characterized in that, The concentration of the acid solution is 1 mol / L to 5 mol / L.
42. The preparation method according to claim 30, characterized in that, The concentration of the acid solution is 1.5 mol / L to 4.5 mol / L.
43. The preparation method according to claim 30, characterized in that, The liquid-to-solid ratio of the acid solution to the crystallized product is (20-80) mL:1 g.
44. The preparation method according to claim 30, characterized in that, The liquid-to-solid ratio of the acid solution to the crystallized product is (40-60) mL:1 g.
45. The preparation method according to claim 30, characterized in that, The mass ratio of the silanizing agent to the crystallized product is (0.2-2):
1.
46. The preparation method according to claim 30, characterized in that, The acid solution is selected from hydrochloric acid, acetic acid, or a solution of nitric acid in water or ethanol.
47. The preparation method according to claim 30, characterized in that, The silicon source is selected from one or more of silica sol, silica gel, tetraethyl orthosilicate, and silicic acid; and / or The aluminum source is selected from one or more of aluminum hydroxide, aluminum isopropoxide, aluminum nitrate, and aluminum oxide; and / or The solvent is selected from water; and / or The mixture does not contain alkali metals or alkaline earth metals.
48. The preparation method according to claim 30, characterized in that, In Equation II, R7, R8, R9 and R 10 They may be the same or different, each independently selected from hydrogen, fluorine, chlorine, bromine, methyl, ethyl, propyl, methoxy, ethoxy, and propoxy.
49. The preparation method according to claim 30, characterized in that, The silanizing agent is selected from one or more of monomethylchlorosilane, dimethylchlorosilane, monomethylmethoxysilane, dimethylmethoxysilane, monomethylethoxysilane, and dimethylethoxysilane.
50. The preparation method according to claim 30, characterized in that, The crystallization conditions for the mixture are 135℃-175℃ for 2-11 days.
51. The preparation method according to claim 30, characterized in that, The crystallization conditions for the mixture are 140℃-170℃ for 3-10 days.
52. The preparation method according to claim 30, characterized in that, The roasting temperature is 500℃-700℃.
53. The preparation method according to claim 30, characterized in that, The roasting time is 3-9 hours.
54. A molecular sieve composition comprising the SCM-53 molecular sieve according to any one of claims 1-29 or the SCM-53 molecular sieve prepared by the preparation method according to any one of claims 30-53, and optionally a binder.
55. The use of the SCM-53 molecular sieve according to any one of claims 1-29, or the SCM-53 molecular sieve prepared by the preparation method according to any one of claims 30-53, or the molecular sieve composition according to claim 54, in adsorption separation, ion exchange, or catalytic conversion of organic compounds.