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Preparation method for hollow ZSM-5 zeolite microspheres

A technology of ZSM-5 and zeolite, which is applied in the field of preparation of ZSM-5 zeolite, can solve the problems of limited application range, large internal hollow structure size, high manufacturing cost, etc., and achieves the reduction of production cost, high mechanical strength, and avoiding operation steps Effect

Inactive Publication Date: 2016-12-07
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is simple to operate, the added suspending agent or emulsifier is generally a surfactant with a special structure, which is often expensive to manufacture, and the internal hollow structure synthesized by this method is relatively large in size, with a diameter of up to Tens of microns or even tens of microns limit its practical application range

Method used

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  • Preparation method for hollow ZSM-5 zeolite microspheres
  • Preparation method for hollow ZSM-5 zeolite microspheres
  • Preparation method for hollow ZSM-5 zeolite microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] At room temperature, 0.13g of sodium aluminate (41%Al 2 o 3 , 35%Na 2 O), 1.2g of sodium hydroxide and 2g of ethylenediamine were dissolved in 86g of distilled water. After stirring and clarification, 20g of 40% silica sol was slowly added dropwise, mixed evenly, moved into a stainless steel reaction kettle, and crystallized at 180°C for 3 days. The obtained solid product was washed with distilled water to neutrality, filtered, dried, and then calcined in a muffle furnace at 550° C. for 6 hours with air to obtain hollow ZSM-5 zeolite microspheres.

[0022] figure 1 The XRD diffraction pattern of the obtained sample shows that the obtained sample is a ZSM-5 zeolite crystal phase, and no other miscellaneous crystals are formed; the scanning electron microscope characterization shows that the obtained ZSM-5 zeolite is spherical, and the sphere is formed by the interlaced growth of about 200nm×100nm crystals. In order to facilitate the observation of the internal struct...

Embodiment 2

[0024] At room temperature, 0.73g of sodium aluminate (41%Al 2 o 3 , 35%Na 2 O), 0.3g of sodium hydroxide, 5g of ethylenediamine were dissolved in 86g of distilled water, stirred and clarified, slowly added dropwise 12g of 40% silica sol, mixed evenly, moved into a stainless steel reaction kettle, and crystallized at 140°C for 6 days, The obtained solid product was washed with distilled water to neutrality, filtered, dried, and then calcined in a muffle furnace at 550° C. for 4 hours with air to obtain hollow ZSM-5 zeolite microspheres.

[0025] The XRD diffraction pattern shows that the obtained sample is a ZSM-5 zeolite crystal phase, and no other miscellaneous crystals are generated; figure 2 The scanning electron microscope characterization shows that the obtained ZSM-5 zeolite is spherical, and the sphere is formed by the interlaced growth of about 200nm×100nm crystals. The scanning electron microscope after the sample is squeezed with a pressure of 20MPa is as follow...

Embodiment 3

[0027] At room temperature, dissolve 1.65g of aluminum hydroxide, 1.12g of sodium hydroxide, and 6g of ethylenediamine in 86g of distilled water. After stirring and clarification, slowly add 10g of fumed silica, mix well, and transfer to a stainless steel reaction kettle. After 2 days of crystallization, the resulting solid product was washed with distilled water until neutral, filtered, dried, and then calcined in a muffle furnace at 550°C for 5 hours with air to obtain hollow ZSM-5 zeolite microspheres.

[0028] The XRD diffraction pattern shows that the obtained sample is ZSM-5 zeolite crystal phase, and no other miscellaneous crystals are formed; the scanning electron microscope characterization shows that the obtained ZSM-5 zeolite is spherical, and the sphere is formed by the interlaced growth of about 200nm×100nm crystals. After the sample was extruded with a pressure of 20 MPa, it was observed that the inside of the sample presented a hollow structure. Figure 4 The TE...

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Abstract

The invention provides a preparation method for hollow ZSM-5 zeolite microspheres. Hollow zeolite microspheres are obtained by mixing water, a silicon source, an aluminium source, sodium hydroxide and ethylenediamine in the mass ratio of 86:(10-25):(0.13-1.65):(0.3-1.2):(2-6), performing hydrothermal crystallization to obtain a solid product, and roasting the obtained solid product. According to the preparation method, the silicon and aluminium sources and a template are synthesized by utilizing traditional micro-porous zeolite; crystal nucleation and growth orientation are adjusted by precisely controlling the composition of a gel; a polycrystal ZSM-5 zeolite shell layer which is formed by staggered growth of strip-shaped ZSM-5 zeolite crystals and hollow ZSM-5 zeolite microspheres with internal hollow structures which are formed by coating of the polycrystal ZSM-5 zeolite shell layer are synthesized through a one-step hydrothermal method; moreover, the internal hollow structures can be communicated with the external through zeolite micro pore channels.

Description

technical field [0001] The invention relates to the preparation of ZSM-5 zeolite, in particular to a method for one-step hydrothermal synthesis of ZSM-5 zeolite microspheres with an inner hollow structure by utilizing a silicon-aluminum source synthesized by a traditional microporous zeolite and a template. Background technique [0002] The hollow microsphere material has a hollow core that can store species and a shell that can selectively control species transfer, and has great application value in drug embedding and sustained release, protection of bioactive reagents and special catalyst assembly design, so attracted the interest of many researchers. Hollow zeolite microspheres are an important part of hollow microsphere materials. Its uniform micropores, good molecular sieving performance, high thermal stability and mechanical strength make it suitable for use in catalysis, controlled release, bioreactors, etc. Fields can play an irreplaceable role. Therefore, the prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/04C01P2004/34
Inventor 李瑞丰潘梦郑家军白亚东刘芝平王广帅
Owner TAIYUAN UNIV OF TECH