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A kind of hollow microsphere molecular sieve and its preparation method and its application in methanol to aromatics

A molecular sieve and ammonium molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, hydrocarbon production from oxygen-containing organic compounds, etc., can solve the problems of high selectivity of aromatic hydrocarbons and long life, and achieve the benefits of diffusion, increased life, and improved selective effect

Active Publication Date: 2020-01-03
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the hollow microsphere molecular sieve provided by the present invention is used in the reaction of methanol conversion to aromatics, the selectivity of aromatics is high and the service life is long

Method used

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  • A kind of hollow microsphere molecular sieve and its preparation method and its application in methanol to aromatics
  • A kind of hollow microsphere molecular sieve and its preparation method and its application in methanol to aromatics
  • A kind of hollow microsphere molecular sieve and its preparation method and its application in methanol to aromatics

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preparation example Construction

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

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

[0045] (2) Hydrothermally crystallize the sol obtained in step (1) to obtain the original molecular sieve powder;

[0046] (3) Roasting the original molecular sieve powder obtained in the step (2) to obtain a modified molecular sieve;

[0047] (4) Perform ion exchange on the modified molecular sieve obtained in 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] In the invention, a silicon source, an aluminum source, n-butylamine, an EDTA chelating agent and water are mixed, the pH value is adjusted to 8-10, and the sol is obtained by stirri...

Embodiment 1

[0069] According to the molar ratio Si: Al: n-butylamine: EDTA-Na 2 : Water=1:0.028:0.15:0.08:31, add sodium metaaluminate to water, stir until clear; add n-butylamine and EDTA-Na in turn 2 , And finally add silica sol (JN-40, 40.5wt% of SiO) dropwise at a rate of 0.3mL / s 2 , Qingdao Haiyang Chem. Co.).

[0070] A 5mol / L NaOH solution was used to maintain the pH of the synthesis system at 8.5, and stirring was carried out at a rate of 500r / min for 0.5h to form a uniform sol.

[0071] The above-mentioned sol was transferred to a synthesis kettle with polytetrafluoroethylene lining, and it was rotated and dynamically crystallized at a rate of 20r / min for 38h in a homogeneous reactor at 170°C.

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

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

[0074] The modified molecular sieve ...

Embodiment 2

[0078] According to the molar ratio Si: Al: n-butylamine: EDTA-Na 2 : Water = 1:0.02:0.15:0.08:31, add sodium metaaluminate to water, stir until clear; add n-butylamine and EDTA-Na in turn 2 , And finally add silica sol (JN-40, 40.5wt% of SiO) dropwise at a rate of 0.3mL / s 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 to a synthesis kettle with polytetrafluoroethylene lining, and it was rotated and dynamically crystallized at a rate of 20r / min for 38h in a homogeneous reactor at 170°C.

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

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

[0083] The modified molecular sieve was mixed with 1.2 mol / L ammonium nitrate solution at 90°C, ion exchanged t...

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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 the preparation of aromatic hydrocarbons from methanol. Background technique [0002] Benzene, toluene and xylene in aromatics 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 the catalytic reforming of petroleum products and the hydro-extraction of pyrolysis gasoline. Due to the shortage of oil resources in China, the prices of benzene, toluene and xylene continue 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 has mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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