Preparation method of catalyst with Fe nanoparticles inlaid into hierarchical pore molecular sieve crystal particles

A nanoparticle and molecular sieve technology, which is applied in the direction of molecular sieve catalysts, molecular sieve compounds, molecular sieves and base exchange compounds, etc., can solve the problems of easy aggregation and deactivation of loaded metal oxides, blockage of molecular sieve channels, etc., and achieve high selectivity, high pore volume, high The effect of specific surface area

Inactive Publication Date: 2017-09-19
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the problems in the prior art that loaded metal oxides are easy to agglomerate, deactivate and block the pores of molecula

Method used

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  • Preparation method of catalyst with Fe nanoparticles inlaid into hierarchical pore molecular sieve crystal particles
  • Preparation method of catalyst with Fe nanoparticles inlaid into hierarchical pore molecular sieve crystal particles
  • Preparation method of catalyst with Fe nanoparticles inlaid into hierarchical pore molecular sieve crystal particles

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Experimental program
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Effect test

Embodiment 1

[0027] Mix the complexing agent with the iron source solution and stir for 0.5h; add the template solution and stir for 2h; add the silicon source and stir for 12h; add the alkali source and continue stirring for 2h, the final molar ratio of the reactants is SiO 2 : 0.01 Fe: 0.02EDTA: 0.30TBAB: 111 H 2 O: 0.5NaOH The mixed gel was put into a synthesis kettle, and crystallized at 180° C. for 2 days under autogenous pressure; after the crystallization was completed, the solid product was separated by washing, and the product was washed with 95% ethanol solution, Then transfer the product to a quartz glass tube and reduce it with hydrogen gas at 400°C. The reduction time is 4 hours. Add the obtained product to the alkali solution; add the mixed solution to the template solution and stir for 3 hours; add silicon source, Stir for 3h; add alkali source, stir for 1h; the final molar ratio of reactants is SiO 2 : 0.30 CTAB : 111 H 2 O: 0.2NaOH Put the mixed gel into a synthesis kett...

Embodiment 2

[0029] Mix the complexing agent with the iron source solution and stir for 0.5h; add the template solution and stir for 2h; add the silicon source and stir for 12h; add the alkali source and continue stirring for 2h, the final molar ratio of the reactants is SiO 2 : 0.02 Fe: 0.04EDTA: 0.30 TBAB: 111 H 2 O: 0.5 NaOH Put the mixed gel into a synthesis kettle, and crystallize at 160°C for 24 hours under autogenous pressure; after the crystallization is completed, wash and separate the solid product, wash the product with 100% ethanol, and then Transfer the product to a quartz glass tube and reduce it with hydrogen at 400°C. The reduction time is 4 hours. Add the obtained product to the alkali solution; add the mixed solution to the template solution and stir for 3 hours; add silicon source and stir 3h; add alkali source and stir for 1h; the final molar ratio of reactants is SiO 2 : 0.30 CTAB : 111 H 2O: 0.2 NaOH Put the mixed gel into a synthesis kettle, crystallize at 180° C. ...

Embodiment 3

[0031] Mix the complexing agent with the iron source solution and stir for 0.5h; add the template solution and stir for 2h; add the silicon source and stir for 12h; add the alkali source and continue stirring for 2h, the final molar ratio of the reactants is SiO 2 : 0.01 Fe: 0.02EDTA: 0.30TMAOH: 111 H 2 O: 0.5 NaOH Put the mixed gel into a synthesis kettle, and crystallize at 200°C for 36 hours under autogenous pressure; after the crystallization is completed, wash and separate the solid product, and wash the product with 98% ethanol solution, Then transfer the product to a quartz glass tube and reduce it with hydrogen gas at 400°C. The reduction time is 4 hours. Add the obtained product to the alkali solution; add the mixed solution to the template solution and stir for 3 hours; add silicon source, Stir for 3h; add alkali source, stir for 1h; the final molar ratio of reactants is SiO 2 : 0.30 CTAB : 111 H 2 O: 0.2 NaOH Put the mixed gel into a synthesis kettle, crystallize ...

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Abstract

The invention provides a preparation method of a catalyst with Fe nanoparticles inlaid into hierarchical pore molecular sieve crystal particles. The preparation method mainly comprises four steps: firstly, a micropore part unit is prepared with tetrabutylammonium bromide as a template agent; secondarily, a complex formed by a complexing agent and Fe ions is inlaid into the template agent in a molecule sieve, and then, Fe atoms are reduced into a molecular sieve crystal lattice under the hydrogen introduction condition; finally, a mesopore part unit is prepared with hexadecyl trimethyl ammonium bromide as the template agent, and Fe particles and a microporous unit are inlaid into a mesoporous framework. The preparation method has the benefits as follows: the catalyst has two kinds of pores, namely, mesopores and micropores, and has higher specific surface area and pore volume, and the Fe nanoparticles among the molecular sieve particles have higher catalytic activity and are applicable to the hydrogenation catalysis and cracking reaction process of residual oil. The granulated and formed catalyst can be used for a hydrogenation catalysis and cracking reaction of the residual oil and has high activity and high selectivity for gasoline and diesel.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of a multi-stage molecular sieve grain-embedded Fe nanoparticle catalyst. Background technique [0002] In my country's resource structure, petroleum resources account for a large proportion, and the current situation of my country's petroleum resources is that more than 60% of crude oil in petroleum resources has a large proportion, and the content of light oil products is low, which prompts my country's The smelting process of the petroleum smelting enterprises is further developed to the deep processing of petroleum. The advancement of science and technology has further improved the catalytic fission technology in petroleum smelting technology. However, it can be clearly seen that in today's world where the market economy dominates, my country's oil consumption has increased tremendously, and the use of light crude oil is even more pr...

Claims

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Application Information

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IPC IPC(8): C01B37/00C01B39/00B01J29/80
CPCC01B37/005B01J29/044B01J29/46B01J29/80C01B39/00C01P2002/54C01P2002/72C01P2004/04
Inventor 王静徐俊青吴宁王志鹏李熠杰
Owner TIANJIN POLYTECHNIC UNIV
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