Method for preparing high-content double-transition metal composite molecular sieve

A composite molecular sieve and transition metal technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of poor thermal stability and hydrothermal stability, etc., to increase the content, improve thermal stability and Hydrothermal stability, effect of increasing wall thickness

Inactive Publication Date: 2011-09-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] 1. Purpose of the invention: the present invention provides a high-content double-transition metal composite molecular sieve M 1 -MFI / M 2 -MCM-41(M 1 , M 2 =Ni, Co, Cu, Fe, Zn, Cr etc. one or both) synthetic method, its purpose is to overcome the defect that microporous molecular sieve is limited by pore size and poor thermal stability and hydrothermal stability of mesoporous molecular sieve, simultaneously Incorporation of a large number of metal atoms into the framework of molecular sieves

Method used

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  • Method for preparing high-content double-transition metal composite molecular sieve
  • Method for preparing high-content double-transition metal composite molecular sieve
  • Method for preparing high-content double-transition metal composite molecular sieve

Examples

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Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 2.97g of nickel nitrate and dissolve it in 10g of deionized water to react with sodium ethylenediaminetetraacetate solution to generate the metal complex Ni(EDTA) 2- . Then 12.089g of tetrabutylammonium bromide was weighed, the metal complex was mixed with water-soluble cationic surfactant tetrabutylammonium bromide, and the resulting template association was used as the template for the experiment.

[0032] Weigh 0.5g of sodium hydroxide and dissolve it in 20g of deionized water and stir. After dissolving, dissolve 3g of silicon dioxide weighed in the solution of sodium hydroxide. After stirring for 1 hour, add template agent [TBA] + 2 [Ni(EDTA) 2- ], and then continued to stir for 1.5 hours, using sodium hydroxide solution to adjust the pH to 9. Finally, the total amount of water was adjusted to 121ml, and the above synthesis process was carried out at room temperature. After 3 hours of continuous stirring, the obtained gel was transferred into a polytetrafl...

Embodiment 2

[0035] Dissolve 2.97g of nickel nitrate in 10ml of disodium ethylenediaminetetraacetic acid aqueous solution to generate metal complex Ni(EDTA) 2- . Then 12.089g of tetrabutylammonium bromide was weighed, the metal complex was mixed with water-soluble cationic surfactant tetrabutylammonium bromide, and the resulting product was used as a template for the experiment.

[0036] Weigh 0.5g of sodium hydroxide and dissolve it in 20g of deionized water and stir. After dissolving, dissolve 3g of silicon dioxide weighed in the solution of sodium hydroxide. After stirring for 1 hour, add template agent [TBA] + 2 [Ni(EDTA) 2- ], and then continued to stir for 1.5 hours, using sodium hydroxide solution to adjust the pH to 9. Finally, adjust the total amount of water to 121ml. The above synthesis process was carried out at room temperature, and after continuous stirring for 3 hours, the obtained gel was transferred into a polytetrafluoroethylene-lined reaction tank, statically crystal...

Embodiment 3

[0039] Weigh 2.99g of cobalt nitrate and dissolve it in 10g of deionized water to react with sodium edetate solution to generate the metal complex Ni(EDTA) 2- . Then 12.089g of tetrabutylammonium bromide was weighed, the metal complex was mixed with water-soluble cationic surfactant tetrabutylammonium bromide, and the resulting template association was used as the template for the experiment.

[0040] Weigh 0.5g of sodium hydroxide and dissolve it in 20g of deionized water and stir. After dissolving, dissolve 3g of silicon dioxide weighed in the solution of sodium hydroxide. After stirring for 1 hour, add template agent [TBA] + 2 [Co(EDTA) 2-], and then continued to stir for 1.5 hours, using sodium hydroxide solution to adjust the pH to 9. Finally, the total amount of water was adjusted to 121ml, and the above synthesis process was carried out at room temperature. After 3 hours of continuous stirring, the obtained gel was transferred into a polytetrafluoroethylene-lined re...

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Abstract

The invention relates to a method for preparing a high-content double-transition metal heteroatom composite molecular sieve. By using a stepwise synthesis method, a a MFI primary structure is firstly synthesized; then a M1-MFI molecular sieve is taken as part of silicon sources wherein M1 is one or two selected from the group consisting of Ni, Co, Cu, Fe, Zn, Cr and the like; M1-MFI is introduced into the hole wall of a mesoporous M2-MCM-41 molecular sieve wherein M2 is one or two selected from the group consisting of Ni, Co, Cu, Fe, Zn, Cr and the like; amorphous substances are guided to arrange in order to change defects of amorphous hole wall of the mesoporous molecular sieve, increase the wall thickness and raise heat stability and hydro-thermal stability of the mesoporous M2-MCM-41 molecular sieve. In the mean time, ion association complex formed by the interaction between a traditional template and a metal coordination compound is taken as a template of the synthesis molecular sieve, and metal ion is directly introduced into the molecular sieve skeleton through the template, successfully designing and synthesizing the double-transition metal heteroatom composite molecular sieve. The above composite molecular sieve material has well-regulated crystal structure, high metal content, two uniform mesoporous apertures, large specific surface area and pore volume, and good heat stability and hydro-thermal stability.

Description

1. Technical field [0001] The invention relates to a preparation method of a high-content double-transition metal composite molecular sieve, in particular to a high-content double-transition metal composite molecular sieve M 1 -MFI / M 2 -MCM-41(M 1 , M 2 = one or two of Ni, Co, Cu, Fe, Zn, Cr, etc.) Ni-MFI / Ni-MCM-41, Ni-MFI / Co-MCM-41, Co-MFI / Ni-MCM-41, Co-MFI / Co-MCM-41, Ni-MFI / Fe-MCM-41, Cu-MFI / Fe-MCM-41, Zn-MFI / Cr-MCM-41, Fe-MFI / Cr-MCM-41, etc. Preparation method of composite molecular sieve. 2. Background technology [0002] As we all know, ZSM-5 is an important microporous zeolite molecular sieve shape-selective catalyst in the modern petroleum industry. However, due to the limitation of its pore size, the product molecules are not easy to diffuse out in some reactions, which often leads to the occurrence of side reactions. With the heavy oil, solving the catalytic cracking of heavy oil and residual oil has become the controlling factor of the petroleum catalytic cra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/80
Inventor 李保山李潇
Owner BEIJING UNIV OF CHEM TECH
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