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Synthesis method of MOR (Mordenite)-BEA (Beta Zeolite) core-shell zeolite

A core-shell molecular sieve and a synthesis method technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor synthesis repeatability, low yield, weak force and the like

Active Publication Date: 2014-11-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the silicalite-1 nano-crystal seeds are adsorbed on the nuclear phase molecular sieve by the polycation reagent, the force is weak, which also causes problems such as poor synthesis repeatability and low yield.

Method used

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  • Synthesis method of MOR (Mordenite)-BEA (Beta Zeolite) core-shell zeolite
  • Synthesis method of MOR (Mordenite)-BEA (Beta Zeolite) core-shell zeolite
  • Synthesis method of MOR (Mordenite)-BEA (Beta Zeolite) core-shell zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Concrete reactant proportioning and experimental method are as follows:

[0025] Ratio of reactants in nuclei seed: 7Na 2 O: 2.5NaF: 1 Al 2 o 3 : 30 SiO 2 : 360 H 2 o

[0026] The reactant ratio of β nanocrystal: 13(TEA) 2 O: 1Al 2 o 3 : 66SiO 2 : 780 H 2 o

[0027] Ratio of reactants for secondary growth of core-shell: 13(TEA) 2 O: 1 Al 2 o 3 : 71.4SiO2 2 : 2286H 2 o

[0028] Dissolve 112.5 grams of silica sol (40%wt) and 2.628 grams of NaF in 40 grams of deionized water to configure solution A; 4.1 grams of NaAlO 2 and 12.0 grams of NaOH were dissolved in 50 grams of deionized water to prepare Solution B. Slowly add solution B dropwise to solution A, stir well, and the resulting reaction mixture is crystallized at 170°C for 3 days to obtain large-grain nuclear phase MOR seed crystal I, the measured fluorine content is 614 μg / g, silicon The aluminum ratio was 20.4.

[0029] At 65°C, the MOR seed crystal I used as the nuclear phase was added to a 1% h...

Embodiment 2～6

[0036] Examples 2-6 are based on the synthesis ratio and synthesis conditions in Table 1 and Table 2, and are synthesized according to the method and steps similar to Example 1 to obtain core-shell molecular sieves CFS2-6#, see Table 2 for details.

[0037] Table 1

[0038]

[0039] Table 2

[0040]

Embodiment 7

[0042] Concrete reactant proportioning and experimental method are as follows:

[0043] Nucleus phase seed: industrial MOR (fluorine content 2 / Al 2 o 3 =22.6)

[0044] The reactant ratio of β nanocrystal: 13(TEA) 2 O: 1Al 2 o 3 : 66SiO 2 : 780 H 2 o

[0045] Ratio of reactants for secondary growth of core-shell: 13(TEA) 2 O: 1 Al 2 o 3 : 71.4SiO2 2 : 2286H 2 o

[0046] Dissolve 3 grams of PDDA (35%wt), 4.5 grams of ammonia solution (25%wt) in 142.5 grams of NaCl deionized aqueous solution (0.1mol / L) and stir evenly, and add 30 grams of industrial MOR as a nuclear phase molecular sieve to this surface modification Stir and keep at room temperature for 1 hour, filter and dry in air atmosphere at 60°C, add to zeolite beta nanocrystal suspension for pre-adhesion for 90 minutes, filter and dry in air atmosphere at 100°C The processed MOR powder is obtained. 4 grams of white carbon black, 0.765 grams of sodium aluminate, 14.137 grams of tetraethylammonium hydroxide s...

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Abstract

The invention relates to a synthesis method of an MOR (Mordenite)-BEA (Beta Zeolite) core-shell zeolite and mainly aims to solve the problem of low coverage rate of shell phase zeolites on core phase zeolites in the prior art. The problem is better solved by using the technical scheme that the synthesis method comprises the following steps of: (1) treating MOR serving as core phase zeolite by using acid, and then, filtering to obtain MOR I; (2) adding the MOR I into a modifying agent solution with the concentration of 0.1-20wt%, treating the MOR I for 0.5-24h, filtering and drying to obtain MOR II; (3) adding the MOR II into a solution containing nano BEA to obtain MOR III; and (4) adding the MOR III into a solution containing a silicon source, an aluminum source and a template R, crystallizing, and then, filtering, cleaning, carrying out ammonium exchange and drying to obtain the MOR-BEA core-shell zeolite. The synthesis method can be used for industrial production of the MOR-BEA core-shell zeolite.

Description

technical field [0001] The invention relates to a synthesis method of a MOR / BEA core-shell molecular sieve. Background technique [0002] Zeolite molecular sieve is a kind of microporous crystal material with skeleton structure. It has specific size and shape of pore structure, large specific surface area and strong adjustable acidity. It is widely used in the process of petroleum refining and processing. Such as catalytic cracking, aromatic hydrocarbon alkylation, isomerization, catalytic reforming and toluene disproportionation and other catalytic reactions. [0003] Mordenite with MOR topology and beta zeolite with BEA topology are the two most widely used zeolite molecular sieves in industry, both have twelve-membered ring channel structure. The twelve-membered ring main channel of mordenite is an elliptical channel with an orifice size of 0.65 nm×0.70 nm, and the eight-membered ring side channel communicates with it, the orifice size is 0.28 nm×0.57 nm, and the pore di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 孔德金祁晓岚戴晓群
Owner CHINA PETROLEUM & CHEM CORP
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