Method for preparing high-transition metal content molecular sieves

A transition metal and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of uneven distribution of metal ions, uneven surface of molecular sieve, etc., and achieve strong application value , good dispersibility, enhanced selectivity and activity

Inactive Publication Date: 2010-06-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In terms of the synthesis of heteroatom molecular sieves, the domestic patent CN 96117259 adopts the Zr metal element molecular sieve prepared by the ion exchange method, the Na type molecular sieve is ion exchanged into the H type molecular sieve, and then impregnated with a soluble salt solution containing Zr, and the metal Zr is loaded on the On the molecular sieve, the molecular sieve obtained by this method has defects such as uneven surface
CN 98 123933.1, CN 101121526A and US 6773694BI also introduced the heteroatom molecular sieve Fe-ZSM-5 obtained by the direct synthesis method, CN 101073778A in situ synthesis of Ag / Al-ZSM-5, CN 101066532A introduced a skeleton containing Sn ZSM-5 molecular sieve, but the metal content of the molecular sieve prepared by the direct method is generally below 5%, and the distribution of metal ions is uneven

Method used

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  • Method for preparing high-transition metal content molecular sieves
  • Method for preparing high-transition metal content molecular sieves
  • Method for preparing high-transition metal content molecular sieves

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0028] 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 weigh 3.22g of tetrabutylammonium bromide, and associate the metal complex with water-soluble cationic surfactant tetrabutylammonium bromide, and the resulting template association is used as the template for the experiment.

[0029]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- ], then continue to stir for 1.5 hours, add sodium hydroxide to adjust the pH to 9, finally, add water to make the total amount of water be 67ml, the above synthesis process is carried out at room temperature, and after continuous stirring for 3 hours, the obtained gel is transferred into a polymer Static crystallization ...

Embodiment 2

[0031] Weigh 2.96g of cobalt nitrate and dissolve it in 10g of deionized water to complex with sodium edetate solution to generate metal complex Co(EDTA) 2- . Then 12.09g of tetrabutylammonium bromide was weighed, and the metal complex was associated 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 40g of deionized water, stir to dissolve, dissolve the weighed 3g of silicon dioxide in the solution of sodium hydroxide, stir for 1 hour, add template agent [TBA] + 2 [Co(EDTA) 2- ], then continue to stir for 2 hours, add sodium hydroxide to adjust the pH to 9.5, and finally, add water to make the total amount of water be 122ml. The above synthesis process was carried out at room temperature. After continuous stirring for 3 hours, the obtained gel was transferred into a polytetrafluoroethylene-lined reaction tank and sta...

Embodiment 3

[0034] Weigh 2.28g of copper nitrate and dissolve it in 10g of deionized water to complex with sodium edetate solution to generate metal complex Cu(EDTA) 2- . Then 12.09g of tetrabutylammonium bromide was weighed, and the metal complex was associated with water-soluble cationic surfactant tetrabutylammonium bromide, and the resulting template association was used as the template for the experiment.

[0035] Weigh 0.5g of sodium hydroxide and dissolve it in 40g of deionized water, stir to dissolve, dissolve the weighed 3g of silicon dioxide in the solution of sodium hydroxide, stir for 1 hour, add template agent [TBA] + 2 [Cu(EDTA) 2- ], then continue to stir for 2 hours, add sodium hydroxide to adjust the pH to 9.5, finally, add water so that the total amount of water is 122ml, the above synthesis process is carried out at room temperature, and the gel obtained after continuous stirring for 3 hours is transferred into a polymer Static crystallization was carried out at 160°...

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Abstract

The invention relates to a method for preparing high-transition metal content molecular sieves. In the invention, Ni-ZSM-5, Co-ZSM-5 and Cu-ZSM-5 molecular sieves the transition metal contents of which respectively reach up to 15% are successfully designed and synthetized by taking ion association formed by the interaction of the traditional template agent and the metal complex as a template agent for synthetizing the molecular sieves and directly introducing metal ions to the skeletons of the molecular sieves by the template agent. The high-transition metal content heteroatom molecular sieve material has regular crystal structure, uniform bore diameter, bigger specific surface area and pore volume as well as good thermostability and hydrothermal stability.

Description

1. Technical field [0001] The invention relates to a preparation method of molecular sieves with high transition metal content, in particular to a preparation method of Ni-ZSM-5, Co-ZSM-5 and Cu-ZSM-5 molecular sieves with high transition metal content. 2. Background technology [0002] Molecular sieve, also known as zeolite, is abundant in nature and can also be synthesized artificially. Since 1960, molecular sieves, as catalysts and catalyst supports, have been widely valued and developed greatly in all countries in the world. In particular, great achievements have been made in catalytic cracking, catalytic hydrocracking, hydroisomerization and alkylation, and gradually become the core technology of oil refining and petroleum industry. [0003] ZSM-5 molecular sieve is a new type of high-silica zeolite molecular sieve developed by Mobil Corporation of the United States in 1972. The patent U.S. Patent 3702866 first introduced the preparation method of ZSM-5 zeolite molecul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 李保山李潇
Owner BEIJING UNIV OF CHEM TECH
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