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A kind of microporous-mesoporous layered zeolite material and its preparation method and application

A zeolite material and a mesoporous technology, which are applied in the field of micropore-mesoporous level zeolite materials and their preparation, can solve the problems of difficulty in enlarging the synthesis process and high synthesis cost, and achieve the effect of saving costs.

Active Publication Date: 2022-03-18
PEKING UNIV SHENZHEN GRADUATE SCHOOL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both surfactants and polymers are mesoscopic templates, which are encapsulated in mesoporous channels through physical steric hindrance. Due to the special template structure, the synthesis cost is relatively high, and the synthesis process is difficult to scale up.
Therefore, the current synthetic methods all have certain limitations

Method used

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  • A kind of microporous-mesoporous layered zeolite material and its preparation method and application
  • A kind of microporous-mesoporous layered zeolite material and its preparation method and application
  • A kind of microporous-mesoporous layered zeolite material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 3

[0048] Example 1 Synthesis of microporous-mesoporous LTA zeolite using trifluoroacetic acid as a mesoporous agent

[0049] Dissolve 12.54ml of silica sol (25%) in 10ml of deionized water, stir mechanically for more than 15 minutes to disperse evenly, and mark it as silicon source; dissolve 2.0g of sodium hydroxide and 4.1g of sodium metaaluminate in 35ml of deionized water , stirred for 10 minutes until clear, then 2.85 g of trifluoroacetic acid was added. Finally, the above solution was added to the silicon source, kept stirring, aged at room temperature for 3 hours, then started heating, and reacted at 100° C. for 18 hours. After the reaction, the reaction liquid was collected and centrifuged, washed with water to collect the white solid, and dried at 60° C. to obtain the hierarchically porous LTA zeolite.

[0050] The D / Max-2200 PC X-ray diffractometer of Rigaku Company was used to carry out XRD measurement on the above-mentioned microporous-mesoporous layered zeolite mate...

Embodiment 2

[0053] Example 2 Synthesis of microporous-mesoporous LTA zeolite using p-toluenesulfonic acid as a mesoporous agent

[0054] Dissolve 12.54ml of silica sol (25%) in 10ml of deionized water, stir mechanically for more than 15 minutes to disperse evenly, and mark it as silicon source; dissolve 2.0g of sodium hydroxide and 4.1g of sodium metaaluminate in 35ml of deionized water , stirred for 10 minutes until clear, then 2.353 g p-toluenesulfonic acid was added. Finally, the above solution was added to the silicon source, kept stirring, aged at room temperature for 3 hours, then started heating, and reacted at 100° C. for 18 hours. After the reaction, the reaction liquid was collected and centrifuged, washed with water to collect the white solid, and dried at 60° C. to obtain the hierarchically porous LTA zeolite.

[0055] The D / Max-2200 PC X-ray diffractometer of Rigaku Company was used to carry out XRD measurement on the above-mentioned microporous-mesoporous layered zeolite ma...

Embodiment 3 6

[0058] Example 3 Synthesis of microporous-mesoporous LTA zeolite using hexafluoroisopropanol as mesoporous agent

[0059]Dissolve 12.54ml of silica sol (25%) in 10ml of deionized water, stir mechanically for more than 15 minutes to disperse evenly, and mark it as silicon source; dissolve 2.0g of sodium hydroxide and 4.1g of sodium metaaluminate in 35ml of deionized water , stirred for 10 minutes until clear, then 4.2 g of hexafluoroisopropanol was added. Finally, the above solution was added to the silicon source, kept stirring, aged at room temperature for 3 hours, then started heating, and reacted at 100° C. for 18 hours. After the reaction, the reaction liquid was collected and centrifuged, washed with water to collect the white solid, and dried at 60° C. to obtain the hierarchically porous LTA zeolite.

[0060] The D / Max-2200 PC X-ray diffractometer of Rigaku Company was used to carry out XRD measurement on the above-mentioned microporous-mesoporous layered zeolite materi...

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Abstract

A microporous-mesoporous layered zeolite material and its preparation method and application, the preparation method comprising: introducing an anion precursor into a zeolite synthesis liquid including a silicon source and an aluminum source as an organic mesoporous agent, the anion precursor can be used in the Stable organic negative ions are formed in the zeolite synthesis liquid, and the organic negative ions are used as nucleophiles to attack the Si-O / Al-O sites in the zeolite framework, so that the framework is partially dissolved to form intracrystalline mesopores, and a microporous-mesoporous hierarchical zeolite material is obtained , which includes a zeolite structure and optionally dispersed anion precursors living in pores of the zeolite structure, the zeolite structure includes a microporous structure and a mesoporous structure, and at least part of the mesoporous structure is located inside the crystal. A new mechanism is proposed, which avoids the problems of phase separation, complex synthesis steps and high cost, and the post-treatment does not need to remove the template by calcination, and the hierarchical porous zeolite can be obtained only by washing with deionized water.

Description

technical field [0001] The invention relates to the technical field of zeolite materials, in particular to a microporous-mesoporous hierarchical zeolite material and its preparation method and application. Background technique [0002] Zeolite (Zeolite) is made from [TO 4 ]([SiO 4 ], [AlO 4 ] or [PO 4 ], etc.) tetrahedrons share vertices to form a three-dimensional four-linked framework with periodic channels of aluminosilicate crystals. Because of its uniform pore structure, internal adjustable acid sites, excellent shape selectivity, high specific surface area, thermal stability, chemical stability and mechanical stability, zeolites are widely used in catalysis, adsorption and ion exchange. field has a wide range of applications. Most zeolites need to be synthesized with organic amines or quaternary ammoniums as structure-directing agents, but traditional microporous zeolites have small pore sizes, usually less than 1nm, which will seriously hinder the diffusion of ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02B01J29/06B01J20/18B01J39/14
CPCB01J39/14B01J20/18B01J29/06C01B39/02
Inventor 洪梅陈超董磊王彦顶张健陈柱文钱微
Owner PEKING UNIV SHENZHEN GRADUATE SCHOOL
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