Hollow microsphere molecular sieve, preparation method thereof and application thereof to arene preparation through methyl alcohol

A molecular sieve and hollow technology, applied in molecular sieve catalysts, chemical instruments and methods, and hydrocarbon production from oxygen-containing organic compounds, etc., can solve the problems of high selectivity and long life of aromatics, so as to facilitate diffusion, increase life, and improve selectivity Effect

Active Publication Date: 2017-03-29
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
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Problems solved by technology

When the hollow microsphere molecular sieve provided by the present invention is used in the reaction

Method used

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  • Hollow microsphere molecular sieve, preparation method thereof and application thereof to arene preparation through methyl alcohol
  • Hollow microsphere molecular sieve, preparation method thereof and application thereof to arene preparation through methyl alcohol
  • Hollow microsphere molecular sieve, preparation method thereof and application thereof to arene preparation through methyl alcohol

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preparation example Construction

[0043] The present invention also provides a method for preparing the hollow microsphere molecular sieve described in the above technical solution, comprising the following steps:

[0044] (1) Mix the silicon source, aluminum source, n-butylamine, EDTA chelating agent and water, adjust the pH value to 8-10, and stir to obtain the sol;

[0045] (2) hydrothermal crystallization of the sol obtained in the step (1) to obtain the former powder of molecular sieve;

[0046] (3) Roasting the molecular sieve former powder that described step (2) obtains, obtains modified molecular sieve;

[0047] (4) performing ion exchange on the modified molecular sieve obtained in the step (3) to obtain an ammonium molecular sieve;

[0048](5) Calcining the ammonium molecular sieve obtained in the step (4) to obtain a hollow microsphere molecular sieve.

[0049] The invention mixes silicon source, aluminum source, n-butylamine, EDTA chelating agent and water, adjusts pH value to 8-10, and stirs to...

Embodiment 1

[0069] According to the molar ratio Si:Al:n-butylamine:EDTA-Na 2 : water=1:0.028:0.15:0.08:31 ratio, sodium metaaluminate is added to water, stir until clear; add n-butylamine and EDTA-Na 2 , and finally add silica sol (JN-40, 40.5wt%of SiO 2 , Qingdao Haiyang Chem.Co.).

[0070] The pH of the synthesis system was maintained at 8.5 with 5 mol / L NaOH solution, and stirred at a rate of 500 r / min for 0.5 h to form a uniform sol.

[0071] The above-mentioned sol was transferred into a synthesis kettle lined with polytetrafluoroethylene, and rotated and dynamically crystallized at a speed of 20 r / min for 38 hours in a homogeneous reactor at 170°C.

[0072] The crystallized product was fully washed, centrifuged and dried at 105°C for 12 hours to obtain the molecular sieve powder.

[0073] The original powder was calcined at 450°C for 24 hours in the air to obtain the modified molecular sieve.

[0074] The modified molecular sieve was mixed with 0.8mol / L ammonium nitrate solution...

Embodiment 2

[0078] According to the molar ratio Si:Al:n-butylamine:EDTA-Na 2 : water=1:0.02:0.15:0.08:31 ratio, sodium metaaluminate is added to water, stir until clear; add n-butylamine and EDTA-Na 2 , and finally add silica sol (JN-40, 40.5wt%of SiO 2 , Qingdao Haiyang Chem.Co.).

[0079] Use NaOH solution to maintain the pH of the synthesis system = 8.5 to form a uniform sol.

[0080] The above-mentioned sol was transferred into a synthesis kettle lined with polytetrafluoroethylene, and rotated and dynamically crystallized at a speed of 20 r / min for 38 hours in a homogeneous reactor at 170°C.

[0081] The crystallized product was fully washed, centrifuged and dried at 105°C for 12 hours to obtain the molecular sieve powder.

[0082] The original powder was calcined at 450°C for 24 hours in the air to obtain the modified molecular sieve.

[0083] Mix the modified molecular sieve with 1.2mol / L ammonium nitrate solution at 90°C, perform ion exchange twice to obtain ammonium molecular si...

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Abstract

The invention provides a hollow microsphere molecular sieve, a preparation method thereof and application thereof to arene preparation through methyl alcohol conversion. The hollow microsphere molecular sieve provided by the invention comprises a shell and a macroporous structure, wherein the shell is formed by stacking ZSM-5 crystalline grains, and the macroporous structure is formed by being wrapped with the shell. The hollow microsphere molecular sieve is of a multi-stage pore structure. Multi-stage pores comprise macropores, mesopores formed by stacking the ZSM-5 crystalline grains, and micropores of the ZSM-5 crystalline grains. The hollow microsphere molecular sieve provided by the invention is of the multi-stage pore structure, and can be used as a catalyst for reaction during arene preparation through methyl alcohol conversion; reactant molecules enter an inner space through the shell, and generated products are further diffused through the shell; compared with other molecular sieves, the reactant molecules are subjected to a larger number of multi-stage reactions on hollow microspheres, and accordingly the selectivity of arene is improved; and since the mesopores formed by stacking the ZSM-5 crystalline grains and the internally hollow macropores in the shell are beneficial to diffusion of the products, the service life of the catalyst is greatly prolonged.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a hollow microsphere molecular sieve, a preparation method thereof and an application in methanol to aromatics. Background technique [0002] Benzene, toluene and xylene in aromatic hydrocarbons are important organic chemical raw materials, which are widely used in many fields such as materials, household appliances, pesticides and daily chemicals. The traditional methods of producing aromatics mainly rely on petrochemical processes such as catalytic reforming of petroleum products and hydrogenation extraction of pyrolysis gasoline. Due to the shortage of oil resources in China, the prices of benzene, toluene and xylene continued to rise. [0003] Methanol is an important chemical organic raw material with abundant sources, such as natural gas and biomass. With the development of coal chemical industry, coal-based synthetic methanol technology is mature, but the tr...

Claims

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Application Information

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IPC IPC(8): B01J29/40C01B39/40C07C1/20C07C15/02
CPCB01J29/40B01J2229/40C01B39/40C01P2004/03C01P2004/61C07C1/20C07C15/02
Inventor 樊卫斌王凯董梅王建国秦张峰王浩李俊汾
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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