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Step type pore ZSM-5 zeolite and preparation method thereof

A technology of ZSM-5 and cascaded pores, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of stability improvement and achieve strong acid strength and multi-acid active sites Effect

Active Publication Date: 2017-03-29
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Their research results show that the nano-HZSM-5 catalyst modified by the combination of hydrothermal treatment and metal oxide has good desulfurization performance, but its stability still needs to be improved

Method used

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  • Step type pore ZSM-5 zeolite and preparation method thereof
  • Step type pore ZSM-5 zeolite and preparation method thereof
  • Step type pore ZSM-5 zeolite and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] This embodiment provides a kind of stepped pore ZSM-5 zeolite, which is prepared through the following steps:

[0044] Mix 50g deionized water, 1.45g three polyquaternium C 16 C 6 C 6 C 16 Br 3 With 0.38g double-ended polyquaternium C 16 C 6 C 16 Br 2 Mix well to obtain a solution;

[0045] Add 0.7g of sodium hydroxide to the solution, stir evenly, add 0.6g of aluminum sulfate octadecahydrate, then add a mixture of 12.4g of ethanol and 8.2g of ethyl orthosilicate, stir at 40-60°C for 4-6h to obtain a condensate glue mixture;

[0046] The gel mixture was transferred to a polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally crystallized at 150°C for 4 days;

[0047] The product obtained by hydrothermal crystallization was suction-filtered, washed with deionized water until pH<9, then dried at 120°C for 12h, and the dried sample was put into a muffle furnace for calcination at 550°C for 4h to obtain Na-type ZSM- 5 zeolites;

[0048] The Na-...

Embodiment 2

[0051] This embodiment provides a kind of stepped pore ZSM-5 zeolite, which is prepared through the following steps:

[0052] The preparation method is generally the same as in Example 1, the difference is that the template agent is replaced by 1.77g four-head cationic polyquaternary ammonium surfactant and 0.38g double-head cationic surfactant, and other conditions remain unchanged, and the prepared H-type The stepped pore ZSM-5 zeolite is denoted as Z-2.

[0053] The powder XRD test result of the step hole ZSM-5 zeolite Z-2 that the present embodiment obtains is as follows figure 1 with figure 2 Shown, N 2 Adsorption-desorption isotherms such as image 3 As shown, the ammonia temperature-programmed desorption curve is as follows Figure 4 shown.

Embodiment 3

[0055] This embodiment provides a kind of stepped pore ZSM-5 zeolite, which is prepared through the following steps:

[0056] The preparation method is generally the same as that in Example 1, except that the template agent is replaced with 1.94 g of three-head cationic polyquaternium salt, and other conditions remain unchanged, and the prepared H-type stepped pore ZSM-5 zeolite is recorded as Z-3.

[0057] The powder XRD test result of the step hole ZSM-5 zeolite Z-3 that the present embodiment obtains is as follows figure 1 with figure 2 Shown, N 2 Adsorption-desorption isotherms such as image 3 As shown, the ammonia temperature-programmed desorption curve is as follows Figure 4 shown.

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Abstract

The present invention provides a step type pore ZSM-5 zeolite and a preparation method thereof. The preparation method comprises: mixing a templating agent and water to obtain a solution; adding sodium hydroxide, an aluminum source, a short chain alcohol and a silicon source to the solution, and mixing to form a gel mixture, wherein a molar ratio of the sodium hydroxide to the aluminum source (calculated as Al2O3) to the silicon source (calculated as SiO2) to the templating agent to the short chain alcohol to the water is (5-15):1:(30-100):(0.5-3):(70-500):(1000-8000); crystallizing the gel mixture, separating the solid product, washing, and drying to obtain ZSM-5 zeolite raw powder; and calcining the ZSM-5 zeolite raw powder to obtain the step type pore ZSM-5 zeolite. The invention further provides the step type pore ZSM-5 zeolite prepared through the preparation method. According to the present invention, the step type pore ZSM-5 zeolite has the ordered large mesopores so as to easily achieve the effective diffusion and the reaction of the macromolecular compound.

Description

technical field [0001] The invention relates to a zeolite and a preparation method thereof, in particular to an ordered mesoporous-micropore step-pore ZSM-5 zeolite and a preparation method thereof, belonging to the technical field of zeolite preparation. Background technique [0002] Microporous zeolites are widely used in petroleum refining and petrochemical fields due to their regularly arranged micropore channels, highly crystalline pore walls and a large number of evenly distributed active sites. In the 1970s, Mobil first developed ZSM zeolite by using organic additives to synthesize gels. HZSM-5 zeolite has an acid center and has hydrogenation performance after loading active metals, so it is widely used in petrochemical fields such as catalytic cracking and catalytic hydrogenation. However, conventional ZSM zeolites generally have small pore sizes, which prevent the mass transfer of molecules with large kinetic diameters, and cannot exhibit good catalytic performance...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 范煜姚丽群李建华曾佑富吴耀光马婷牛文忠朱凌辉张琴托罗别克郭宝华杨欢
Owner PETROCHINA CO LTD
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