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Preparation method of hierarchical pore ZSM-5/ZSM-11 eutectic zeolite molecular sieve

A technology of ZSM-11 and eutectic zeolite is applied in the directions of molecular sieve catalyst, crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., to achieve the effects of simple process, low cost, and easy operation and realization.

Active Publication Date: 2018-01-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method requires the addition of a structure directing agent and two firings

Method used

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  • Preparation method of hierarchical pore ZSM-5/ZSM-11 eutectic zeolite molecular sieve
  • Preparation method of hierarchical pore ZSM-5/ZSM-11 eutectic zeolite molecular sieve

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Embodiment 1

[0025] Silica sol (SiO 2 weight percentage content 40%) as silicon source, aluminum source then selects sodium metaaluminate, template agent adopts tetrabutyl ammonium hydroxide, according to 150SiO 2 :1Al 2 o 3 :6 template agent: 12M 2 O (M=K or Na, K / Na=0.5): 2300 molar ratio of deionized water was weighed. After mixing well, crystallize at 160°C for 48 hours, wash and dry, treat with 0.2mol / L NaOH solution at 65°C for 30min, filter, wash and dry, continue to use 1mol / L NH 3 NO 3 The solution was treated at 65° C. for 6 hours, and finally put into a muffle furnace and calcined at 500° C. for 5 hours to obtain a hierarchically porous ZSM-5 / ZSM-11 eutectic zeolite molecular sieve. Obtained XRD pattern, N 2 The adsorption isotherm diagram is shown in figure 1 , figure 2 . It can be seen from the XRD pattern that there are strong diffraction peaks at 2θ=7.90°, 8.82°, 23.04°, 23.88°, and 45.82° respectively, which are the characteristic diffractions of multi-level hole ...

Embodiment 2

[0027] Tetraethyl orthosilicate is selected as the silicon source, aluminum chloride is selected as the aluminum source, and tetrabutylammonium bromide is used as the template agent, according to 120SiO 2 :1Al 2 o 3 :7 template agent: 16M 2 O (M=K or Na, K / Na=0.7): 2700 Deionized water molar ratio weighing. After mixing well, crystallize at 180°C for 24 hours, wash and dry, treat with 0.25mol / l NaOH solution at 70°C for 45min, filter, wash and dry, continue to use 1mol / l NH 3 NO 3 The solution was treated at 65° C. for 6 hours, and finally put into a muffle furnace and calcined at 550° C. for 5 hours to obtain a hierarchically porous ZSM-5 / ZSM-11 eutectic zeolite molecular sieve. Its XRD pattern, N 2 The adsorption isotherm is similar to figure 1 , figure 2 .

Embodiment 3

[0029] Silica sol (SiO 2 weight percentage content 40%) as silicon source, aluminum source then selects aluminum sulfate, template agent adopts tetrapropyl ammonium hydroxide, according to 180SiO 2 :1Al 2 o 3 :8 template agent: 18M 2 O (M=K or Na, K / Na=1.2): 3000 deionized water molar ratio weighing. After mixing well, crystallize at 160°C for 96 hours, wash and dry, treat with 0.3mol / l NaOH solution at 75°C for 45min, filter, wash and dry, continue to use 1mol / l NH 3 NO 3 The solution was treated at 65° C. for 6 hours, and finally put into a muffle furnace and calcined at 580° C. for 4 hours to obtain a hierarchically porous ZSM-5 / ZSM-11 eutectic zeolite molecular sieve. Its XRD pattern, N 2 The adsorption isotherm is similar to figure 1 , figure 2 .

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Abstract

The invention relates to a preparation method of a hierarchical pore ZSM-5 / ZSM-11 eutectic zeolite molecular sieve, mainly solves the problems that in the mode of preparing the hierarchical pore ZSM-5 / ZSM-11 eutectic zeolite molecular sieve by using double template agents or adding seed crystal, steps are tedious, and the price is high, and belongs to the technical field of preparation of inorganic materials. The preparation method comprises the following steps: preparing an aluminum source, a silicon source, an organic template, sodium hydroxide and potassium hydroxide into a raw material mixture; fully stirring the raw material mixture into gel and then transferring the gel into a high-temperature kettle for hydrothermal crystallization; and after washing and filtering, carrying out acid-alkali treatment modification so as to obtain the hierarchical pore ZSM-5 / ZSM-11 eutectic zeolite molecular sieve finally. The preparation method is simple and convenient in process, easy to operateand implement and low in cost, and is environmentally friendly.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a preparation method of a multi-stage porous ZSM-5 / ZSM-11 eutectic zeolite molecular sieve. Background technique [0002] ZSM-5 molecular sieve is widely used in oil refining industry, environmental protection and fine chemical industry because of its wide range of silicon-aluminum ratio, high hydrothermal stability, high specific surface area and high catalytic performance. ZSM-5 molecular sieve belongs to the orthorhombic crystal system, and there are two kinds of pore systems in its skeleton, which are the ten-membered ring straight cylindrical channel with an elliptical cross-section parallel to the y-axis (the channel size is 0.54nm×0.56nm) and the channel parallel to the y-axis. The cross-section of the x-axis is approximately a circular Z-shaped channel (the size of the channel is 0.52nm×0.58nm), and the two kinds of channels cross each other, and the size o...

Claims

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Application Information

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IPC IPC(8): C01B39/40C01B39/36B01J29/40
Inventor 李婷婷殷玉圣孙中华
Owner CHINA PETROLEUM & CHEM CORP
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