Preparation method of core-shell molecular sieve MOR/BEA (mordenite/bromoethylamine)

A core-shell molecular sieve and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of high product shell coverage, low core-shell molecular sieve shell coverage, and low synthesis cost

Active Publication Date: 2014-12-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is the problem of low shell coverage of core-shell molecular sieves in the prior art, and a new preparation method for MOR / BEA core-shell molecular sieves is provided; the second technical problem to be solved by the present invention is to provide a MOR / BEA core-shell molecular sieve synthesis method, which has the advantages of low synthesis cost and high product shell coverage

Method used

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  • Preparation method of core-shell molecular sieve MOR/BEA (mordenite/bromoethylamine)
  • Preparation method of core-shell molecular sieve MOR/BEA (mordenite/bromoethylamine)
  • Preparation method of core-shell molecular sieve MOR/BEA (mordenite/bromoethylamine)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Concrete reactant proportioning and experimental method are as follows:

[0023] Ratio of reactants in nuclei seed: 7Na 2 O: 2.5NaF: 1Al 2 o 3 : 30SiO 2 : 360H 2 o

[0024] The reactant ratio of β nanocrystal: 13(TEA) 2 O: 1Al 2 o 3 : 66SiO 2 : 780H 2 o

[0025] Ratio of reactants for secondary growth of core-shell: 13(TEA) 2 O: 1Al 2 o 3 : 71.4SiO2 2 : 2286H 2 o

[0026] 112.5 grams of silica sol (40%wt) and 2.628 grams of NaF were dissolved 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 crystallize the formed reaction mixture at 170°C for 3 days to obtain large-grain nuclei-phase mordenite I, with a measured fluorine content of 614 μg / g, silicon-alumina The ratio is 20.4.

[0027] 30 grams of white carbon black and 110 grams of tetraethylammonium hydroxide solution (mas...

Embodiment 2～6

[0033] Examples 2-6 are based on the synthesis ratio and synthesis conditions in Table 1, and are synthesized according to the method and steps similar to Example 1 to obtain core-shell molecular sieves CFS2-6#, see Table 1 for details.

Embodiment 7

[0035] Concrete reactant proportioning and experimental method are as follows:

[0036] Nucleus phase seed: industrial MOR (fluorine content 2 / Al 2 o 3 =22.6)

[0037] The reactant ratio of β nanocrystal: 13(TEA) 2 O: 1Al 2 o 3 : 66SiO 2 : 780H 2 o

[0038] Ratio of reactants for secondary growth of core-shell: 13(TEA) 2 O: 1Al 2 o 3 : 71.4SiO2 2 : 2286H 2 O Dissolve 3 g of PDDA (35% wt), 4.5 g of ammonia solution (25% wt) in 142.5 g of NaCl deionized water (0.1 mol / L) and stir evenly, 30 g of industrial MOR is added to this surface as a nuclear phase molecular sieve In the modifier solution, stir and keep at room temperature for 1 hour, filter and dry in an air atmosphere at 60°C, add to the beta zeolite nanocrystal suspension for pre-adhesion for 90 minutes, filter and dry in an air atmosphere at 100°C That is, the processed MOR powder is obtained. 4 grams of white carbon black, 0.765 grams of sodium aluminate, 14.137 grams of tetraethylammonium hydroxide solu...

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Abstract

The invention relates to a preparation method of core-shell molecular sieve MOR / BEA (mordenite / bromoethylamine) and mainly solves the problem that a core-shell molecular sieve layer is low in coverage in the prior art. The preparation method includes: firstly, pre-processing mordenite to obtain mordenite I; secondly, adding the mordenite I into solution of nano beta-zeolite, and adhering nano beta-zeolite seed crystal to the surface of the mordenite I to obtain mordenite II; and thirdly, adding the mordenite II to solution containing silicon source, aluminum source and template R to allow for crystallization, and performing filtration, washing, ammonium exchange and drying after crystallization to obtain core-shell molecular sieve MOR / BEA. The problem is solved well by the application of the technical scheme. The preparation method is applicable to industrial production of core-shell molecular sieve MOR / BEA.

Description

technical field [0001] The invention relates to a preparation 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 0.65nm×0.70nm, and the eight-membered ring side channel communicates with it, the orifice size is 0.28nm×0.57nm, and the pore diam...

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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