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Method for preparing ZSM-5 zeolite molecular sieve, product and purpose thereof

A technology of ZSM-5 and zeolite molecular sieve, which is applied in the field of molecular sieve to achieve the effect of high catalytic activity

Active Publication Date: 2015-02-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, there have been no reports on the use of symmetrical twin surfactants as mesoporous directing agents (ie, gemini-type cation mesoporous directing agents).

Method used

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  • Method for preparing ZSM-5 zeolite molecular sieve, product and purpose thereof
  • Method for preparing ZSM-5 zeolite molecular sieve, product and purpose thereof
  • Method for preparing ZSM-5 zeolite molecular sieve, product and purpose thereof

Examples

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preparation example Construction

[0025] The invention provides a method for synthesizing a ZSM-5 zeolite molecular sieve with a hierarchical pore structure, the hierarchical pore structure includes micropores and mesopores, and may also contain macropores; wherein the diameter of the micropores is 0.51-0.58nm , the mesopore diameter is 2~50nm, and the macropore diameter is 50~200nm; The method comprises the following steps:

[0026] (1) Preparation of initial gel: Add silicon source and aluminum source to a certain amount of water according to a certain ratio, after stirring evenly, add alkali to adjust the pH value of the system to alkaline (preferably range 8 to 13), then add ZSM-5 zeolite molecular sieve template and gemini-type cationic mesoporous directing agent, and continue stirring for 1 to 8 hours to obtain an initial gel;

[0027] (2) Hydrothermal crystallization: transfer the initial gel prepared in step (1) to a high-pressure synthesis kettle, and conduct hydrothermal crystallization under autogen...

Embodiment 1

[0046] Example 1: Preparation of ZSM-5 zeolite molecular sieve samples 1-12

[0047] Add silicon source and aluminum source to a certain amount of water according to a certain ratio, and after stirring evenly, add alkali under continuous stirring at 30°C to adjust the pH value of the reaction system to pH=8-13 (the specific values ​​are listed in Table 1 middle), then add ZSM-5 zeolite molecular sieve template agent and gemini-type cation mesoporous directing agent, and continue to stir for 5 hours to obtain the initial gel; move the prepared reaction sol into a stainless steel high-pressure synthesis kettle and seal it in 100~180℃, hydrothermal crystallization under autogenous pressure for 1~5 days. The hydrothermal crystallized solid product was centrifuged, washed with deionized water until neutral, dried in air at 110°C for 36h, and finally calcined in a muffle furnace at 550°C for 8h to remove ZSM-5 zeolite A molecular sieve template and a gemini-type cation mesoporous d...

Embodiment 2

[0050] Example 2: Chemical composition of samples 1-12 prepared in Example 1

[0051] Samples 1-12 prepared in Example 1 are carried out chemical composition measurement by an elemental analyzer, and the adopted instrument is a Magix (PHILIPS) type X-ray fluorescence analyzer. + The standard-free quantitative analysis program corresponds the fluorescence intensity of the standard sample to its standard composition, and deducts the influence of interference spectral lines.

[0052] The result measured by the elemental analyzer is the percentage content of oxides of each element. The chemical composition of the sample can be obtained by inverting the percentage content of the oxide of the element. The chemical composition conforms to the general formula Na X Si Y Al Z o T or K X Si Y Al Z o T , wherein, Y≥10; T=1 / 2·X+2Y+3 / 2·Z.

[0053] Take samples 9 and 12 as examples. In sample 9, the weight percentage of each element is Na 2 O%=0.12%, SiO 2 %=98.16%, Al 2 o 3 %...

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Abstract

The invention relates to a method for preparing ZSM-5 zeolite molecular sieve with a multistage pore structure, its product and a purpose thereof, more specifically, the ZSM-5 zeolite molecular sieve with the multistage pore structure employs a gemini cationic surfactant as a meso-structure guiding agent, and is obtained through a hydro-thermal synthesis method under alkaline condition. According to the invention, the total specific surface area of the ZSM-5 zeolite molecular sieve is 240-1000m<2>.g<-1>, the total pore volume is 0.30-1.40cm<3>.g<-1>, the service life of the ZSM-5 zeolite molecular sieve used as a catalyst in a methanol-to-olefins (MTO) can be greatly prolonged, and can be used in other fields such as coal chemical, petroleum chemical catalysis, natural gas conversion, adsorption and separation.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to a method for preparing ZSM-5 zeolite molecular sieves with a hierarchical pore structure, molecular sieve products and catalysts obtained by the method, and applications of these catalysts. Background technique [0002] Zeolite molecular sieves are widely used in petrochemical-related catalysis, natural gas conversion, adsorption and separation, and ion exchange due to their regular micropore structure, large specific surface area, high hydrothermal stability, and adjustable acidity. Waiting for the process. However, with the gradual increase of the proportion of heavy oil components in the raw materials of petroleum and petrochemical industries, higher requirements are put forward for the catalyst's catalytic conversion activity of macromolecules. The limited pore diameter of traditional microporous molecular sieves restricts the entry of larger molecules into the pores, which i...

Claims

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Application Information

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IPC IPC(8): C01B39/38B01J29/40
Inventor 王全义魏迎旭刘中民李金哲徐舒涛陈景润张莹周游王金棒张默之
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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