Hollow microsphere molecular sieve and preparation method thereof

A technology of molecular sieves and microspheres, applied in the direction of molecular sieve catalysts, molecular sieve characteristic polycrystalline silicon, chemical instruments and methods, etc., can solve the problems of complex steps, time-consuming and labor-consuming, etc., and achieve the effect of easy separation and simple and fast synthesis process

Active Publication Date: 2017-03-22
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing preparation method of hollow microsphere molecular sieve is complicated, time-consuming and labor-intensive

Method used

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  • Hollow microsphere molecular sieve and preparation method thereof
  • Hollow microsphere molecular sieve and preparation method thereof
  • Hollow microsphere molecular sieve and preparation method thereof

Examples

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preparation example Construction

[0040] The invention provides a kind of preparation method of hollow microsphere molecular sieve, comprises the following steps:

[0041] adjusting the pH value of the mixture comprising silicon source, templating agent, EDTA chelating agent and water to 8-11 to obtain a sol;

[0042] Carrying out hydrothermal crystallization to the sol to obtain molecular sieve powder;

[0043] The molecular sieve raw powder is calcined to obtain a hollow microsphere molecular sieve.

[0044] In the present invention, the silicon source, template agent, EDTA chelating agent and water are preferably mixed first to obtain a mixed solution; then the pH value of the mixed solution is adjusted to 8-11 to obtain a sol. In the present invention, the molar ratio of the silicon source, template agent, EDTA chelating agent and water is preferably 1:0.05~0.2:0.06~0.12:21~41, more preferably 1:0.08~0.18:0.08~0.11 :25~35, most preferably 1:0.1~0.15:0.09~0.1:28~32.

[0045] In the present invention, the...

Embodiment 1

[0062] According to the molar ratio Si: n-butylamine: EDTA-Na 2 : The ratio of water=1:0.15:0.08:31, water, n-butylamine and EDTA-Na 2 Mix, and finally add silica sol (JN-40, 40.5wt%of SiO 2 , Qingdao Haiyang Chem. Co.).

[0063] 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.

[0064] 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.

[0065] The crystallized product was fully washed, centrifuged and dried at 105°C for 12 hours to obtain the molecular sieve powder.

[0066] The original powder was calcined at 450° C. for 24 hours in the air to obtain the hollow microsphere molecular sieve silicalite-1.

[0067] According to XRD analysis, the hollow microsphere molecular sieve prepared in this example has an MFI st...

Embodiment 2

[0070] According to the ratio of molar ratio Si:Ti:n-butylamine:EDTA:water=1:0.02:0.15:0.08:31, EDTA and n-butylamine are added into water successively, after stirring until clarification, tetrabutyl titanate is added, and finally to the above Ethyl orthosilicate was added dropwise to the sol.

[0071] Use 5 mol / L NaOH solution to maintain the pH of the synthesis system = 11, and stir at 500 r / min for 0.5 h to form a uniform sol.

[0072] The above sol was transferred into a synthesis kettle with a polytetrafluoroethylene liner, and in a homogeneous reactor at 170°C, it was rotated and dynamically crystallized at a speed of 20r / min for 150h.

[0073] The crystallized product was fully washed, centrifuged and dried at 105°C for 12 hours to obtain the molecular sieve powder.

[0074] The original powder was calcined at 450°C for 24 hours in air to obtain hollow microsphere titanium silicon molecular sieve TS-1.

[0075] According to XRD analysis, the hollow microsphere molecul...

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Abstract

The invention provides a hollow microsphere molecular sieve. The hollow microsphere molecular sieve comprises a shell formed by stacking MFI molecular sieve grains, and a macroporous structure wrapped by the shell. The hollow microsphere molecular sieve has a hierarchical pore structure, and hierarchical pores include macropores, mesopores formed by stacking MFI molecular sieve grains, and micropores of MFI molecular sieve grains. Silicon and oxygen serve as framework elements of the molecular sieve. The invention further provides a preparation method of the hollow microsphere molecular sieve. According to the preparation method, a templating agent is used in cooperation with an EDTA chelating agent, the pH value of the system is maintained at 8-11, hollow microspheres are formed through the electrostatic interaction between EDTA4- and positive ions of the templating agent, gel is wrapped in the hollow microspheres, and hierarchical pore hollow microspheres are obtained through hydrothermal crystallization and modification. The synthesis process is simple and fast, it is not needed to prepare seed crystals in advance, product separation is easy, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a hollow microsphere molecular sieve and a preparation method thereof. Background technique [0002] Inorganic hollow capsule materials have a shell and a large internal core space. Because of its large internal space, it can store various materials, and has been widely used as controlled release capsules, main materials, coatings, confined space catalysts, and bioreactors. and other functional materials. Hollow microsphere molecular sieve is a special inorganic hollow capsule material with high thermal and chemical stability. Molecular sieve materials are considered to be an ideal building block for forming hollow structural shells due to their high thermal stability, regular micropores, unique shape selectivity, and intrinsic chemical activity. [0003] So far, there are three methods for synthesizing hollow microsphere molecular sieves in the prior art: hard tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/02C01B39/08B01J29/89B01J29/40C07D223/10C07C37/60C07C39/08
CPCB01J29/40B01J29/89C01B37/02C01B39/08C01P2004/03C01P2004/61C07C37/60C07D223/10C07C39/08
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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