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Method for preparing hierarchical porous SAPO-11 molecular sieve through ultrasonic assistance

A SAPO-11, ultrasonic-assisted technology, applied in the field of ultrasonic-assisted preparation of multi-stage SAPO-11 molecular sieves, can solve the problem of low mesopore increase, achieve high crystallinity, reduce waste water production, and increase single-pot yield Effect

Active Publication Date: 2018-06-08
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for ultrasonically assisted preparation of hierarchically porous SAPO-11 molecular sieves, which solves the technical problem that the degree of mesopore increase is not high in the preparation method of SAPO-11 molecular sieves in the prior art

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  • Method for preparing hierarchical porous SAPO-11 molecular sieve through ultrasonic assistance
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  • Method for preparing hierarchical porous SAPO-11 molecular sieve through ultrasonic assistance

Examples

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Embodiment 1

[0030] This example provides a method for preparing SAPO-11 hierarchically porous molecular sieves by an ultrasonic-assisted method, which specifically includes: first mixing 4.085g of aluminum isopropoxide and 3.16g of deionized water, and then adding 1.7mL of phosphoric acid and 3.16g of deionized water 0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g hexadecyltrimethylammonium bromide were added successively, and then the mixed liquid was ultrasonicated at room temperature for 1h (ultrasonic power was 53KHz , 350W). Continue to stir, dry at 80°C, hydrothermally crystallize at 200°C for 24 hours, and calcine at high temperature (600°C) to remove the template agent.

[0031] The specific surface area of ​​the hierarchical porous SAPO-11 molecular sieve obtained in this embodiment is 296.4m 2 / g, the external specific surface area is 80.6m 2 / g, the total pore volume is 0.225cm 3 / g, the mesopore volume is 0.139cm 3 / g.

Embodiment 2

[0033] This example provides a method for preparing SAPO-11 hierarchically porous molecular sieves by an ultrasonic-assisted method, which specifically includes: first mixing 4.085g of aluminum isopropoxide and 3.16g of deionized water, and then adding 1.7mL of phosphoric acid and 3.16g of deionized water 0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g hexadecyltrimethylammonium bromide were added successively, and then the mixed liquid was ultrasonicated at room temperature for 2h (ultrasonic power is 53KHz, 350W). Continue to stir, dry at 80°C, hydrothermally crystallize at 200°C for 24 hours, and calcine at high temperature (600°C) to remove the template agent.

[0034] figure 1 Shown is the XRD characterization result of the hierarchically porous SAPO-11 molecular sieve synthesized in this example. It can be seen that the product has a typical AEL structure and has good crystallinity. figure 2 The scanning electron micrograph of the hierarchically por...

Embodiment 3

[0037] This example provides a method for preparing SAPO-11 hierarchically porous molecular sieves by an ultrasonic-assisted method, which specifically includes: first mixing 4.085g of aluminum isopropoxide and 3.16g of deionized water, and then adding 1.7mL of phosphoric acid and 3.16g of deionized water A mixed solution composed of ionic water; 0.45mL tetraethyl orthosilicate, 1.6mL di-n-propylamine and 0.018g cetyltrimethylammonium bromide were successively added, and then the mixed liquid was ultrasonicated at room temperature for 3h (ultrasonic power was 53KHz, 350W). Continue to stir, dry at 80°C, hydrothermally crystallize at 200°C for 24 hours, and calcine at high temperature (600°C) to remove the template agent.

[0038] The specific surface area of ​​the hierarchical porous SAPO-11 molecular sieve obtained in this embodiment is 286.4m 2 / g, the external specific surface area is 64.8m 2 / g, the total pore volume is 0.231cm 3 / g, the mesopore volume is 0.143cm 3 / g...

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Abstract

The invention discloses a method for preparing a hierarchical porous SAPO-11 molecular sieve through ultrasonic assistance. The method comprises the following steps of: mixing an aluminum source, a phosphor source, a silicon source, deionized water, a microporous template agent and a mesoporous template agent in proportion, performing ultrasonic treatment, mixing at the room temperature until a mixture is changed into sol, drying, grinding, performing hydrothermal crystallization, and separating, drying and roasting a product to remove the mesoporous template agent, thereby obtaining the hierarchical porous SAPO-11 molecular sieve. Ultrasonic treatment conditions are as follows: ultrasonic power is 200-400 w, ultrasonic frequency is 20-60 kHz, and ultrasonic time is 0.5-4 hours. The hierarchical porous SAPO-11 molecular sieve prepared by the method has a complete AEL structure of the SAPO-11 molecular sieve and relatively high degree of crystallinity, and has a more mesoporous structures; besides, a very little water is used in a molecular sieve synthesis process; and generation of wastewater in a production process is reduced, and the yield and the single-kettle yield are increased greatly.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve porous materials, and in particular relates to an ultrasonic-assisted method for preparing multi-level porous SAPO-11 molecular sieves. Background technique [0002] Since the development of silicoaluminophosphate-based SAPO-11 molecular sieve in the 1980s, it has been widely researched and paid attention to, and is known as the "third-generation new molecular sieve". The framework structure of SAPO-11 molecular sieve is different from that of the traditional silica-alumina zeolite ZSM-5. It is composed of aluminum and phosphorus as the main elements alternately arranged. The introduced silicon atoms break the neutral balance of the phosphorus-aluminum framework, making it exchangeable. The charge that forms the unique molecular sieve's acidic and catalytic applications. SAPO-11 molecular sieve is a non-zeolite medium-pore molecular sieve with AEL structure, which belongs to the orthorhom...

Claims

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Application Information

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IPC IPC(8): C01B39/54
CPCC01B39/54C01P2002/72C01P2004/03C01P2006/12C01P2006/14
Inventor 杜燕燕李久盛
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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