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A kind of hierarchical porous zsm-5 nano-aggregate microsphere and its preparation method

A ZSM-5 and aggregate technology, applied in the field of preparation of ZSM-5 microspheres, can solve the problems of complex molecular sieve production process, large molecular diffusion resistance, difficult separation, etc., and achieve easy separation of products, improved diffusion capacity, and cheap raw materials. Effect

Active Publication Date: 2021-02-02
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems of complex production process of molecular sieves, high cost, difficult separation and high molecular diffusion resistance, the present invention discloses a preparation method of ZSM-5-based nano-aggregated microspheres, which effectively solves the above problems

Method used

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  • A kind of hierarchical porous zsm-5 nano-aggregate microsphere and its preparation method
  • A kind of hierarchical porous zsm-5 nano-aggregate microsphere and its preparation method
  • A kind of hierarchical porous zsm-5 nano-aggregate microsphere and its preparation method

Examples

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Effect test

Embodiment 1

[0030]Alkali source: silicon source: aluminum source: template: bioalcohol: deionized water = 10:100:3:10:20:2000 in molar ratio, dissolve 0.89g sodium metaaluminate in 10.35g TPAOH solution, add 2.33mL A 10mol / L NaOH solution has been prepared, then 2.00mL of water is added, and stirred for half an hour to form a uniform, clear and transparent solution. Finally, 24g of silica sol is slowly added dropwise to the above solution. After rapid stirring for 3h, 1.7mL of bioglycerin is added. Continue to stir for 1 hour, then transfer to a hydrothermal synthesis kettle with PTFE lining, and place it in a 170°C oven for crystallization for 1 day. After the crystallization is completed, the upper alkaline clear liquid is poured out, and the lower solid product is washed with water to neutrality, dried, and calcined to finally obtain multi-porous ZSM-5 nano aggregate microspheres. The final product yield reached 91.2%, the size of the microspheres was about 2um, and the size of the nanocryst...

Embodiment 2

[0032]The steps for preparing the multi-stage porous ZSM-5 nano-aggregate in this example are basically the same as those in Example 1, with the only difference being the ratio of silicon to aluminum. Alkali source: silicon source: aluminum source: templating agent: bioalcohol: deionized water = 10:100:1:10:20:2000 in molar ratio, 0.27g sodium metaaluminate dissolved in 10.35g TPAOH solution, add 2.33mL A 10mol / L NaOH solution has been prepared, then 2.00mL of water is added, and stirred for half an hour to form a uniform, clear and transparent solution. Finally, 24g of silica sol is slowly added dropwise to the above solution. After rapid stirring for 3h, 1.7mL of bioglycerin is added. Continue to stir for 1 hour, then transfer to a hydrothermal synthesis kettle with PTFE lining, and place it in a 170°C oven for crystallization for 1 day. After the crystallization is completed, the upper alkaline clear liquid is poured out, and the lower solid product is washed with water to neutra...

Embodiment 3

[0034]In this example, the steps for preparing the multi-stage porous ZSM-5 nano-aggregate are basically the same as those in Example 1, except that the amount of glycerin added is different. Alkali source: silicon source: aluminum source: templating agent: bioalcohol: deionized water = 10:100:3:10:40:2000 in molar ratio, dissolve 0.89g sodium metaaluminate in 10.35g TPAOH solution, add 2.33mL A solution with a concentration of 10mol / L NaOH has been prepared, and then 2.00mL of water is added, and stirred for half an hour to form a uniform, clear and transparent solution. Finally, 24g of silica sol is slowly added dropwise to the above solution, after rapid stirring for 3h, 3.4mL of bioglycerin is added, and continue After stirring for 1 hour, it was transferred to a hydrothermal synthesis kettle with polytetrafluoroethylene lining, sealed and placed in a 170°C oven for crystallization for 1 day. After the crystallization is completed, the upper alkaline clear liquid is poured out, ...

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Abstract

The invention provides a multi-level porous ZSM‑5 nano-aggregate microsphere and a preparation method. Specifically, the silicon source, aluminum source, alkali source, and template are mixed uniformly to form a gel, and a small amount of bioalcohol is added, and nano-aggregate microspheres with a multi-level structure are synthesized in one simple step through precise regulation of the synthetic liquid precursor. The hierarchically porous ZSM-5 nano-aggregate microspheres prepared by the method are self-assembled nano-aggregate microspheres composed of nanocrystals with a size of 20-100nm and a shape of a cube or a sphere, and the microspheres have good uniform dispersion , and there are a large number of gaps between the nanocrystals to form abundant mesopores, and the addition of bioalcohol can adjust the size of the microspheres arbitrarily. The method for preparing the hierarchically porous ZSM-5 is simple in operation and low in cost, and the yield of the prepared nano-aggregate microspheres is as high as 90%, and the silicon-aluminum ratio can be adjusted in a wide range, which has good application and development value.

Description

Technical field[0001]The invention belongs to the technical field of inorganic porous materials, and specifically relates to a method for preparing ZSM-5 microspheres with special morphologies formed by the aggregation of nanoparticles.Background technique[0002]ZSM-5 molecular sieve has excellent shape selectivity and good hydrothermal stability due to its specific ten-membered ring pore structure, and plays a huge role in the fields of adsorption and separation, shape-selective catalysis, ion exchange and fine chemicals. However, for the conventional micron-sized ZSM-5, due to the small pore size of the molecular sieve, the transmission of macromolecular reactants and products in the pores is restricted, and the diffusion resistance is increased, and it is easy to generate carbon deposits to cover the catalytic active sites of the ZSM-5 molecular sieve. The catalyst is deactivated.[0003]Reducing the particle size of the molecular sieve to prepare nano-scale ZSM-5 can shorten the di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40B82Y40/00
CPCB82Y40/00C01B39/40C01P2004/32C01P2004/45C01P2004/61C01P2004/62C01P2004/64
Inventor 张雄福王金山刘海鸥
Owner DALIAN UNIV OF TECH
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