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Preparation of Hierarchical Zeolite Aggregates Supported by Highly Dispersed Transition Metal Nanoparticles

A technology of transition metals and nanoparticles, applied in the direction of nanotechnology, nanotechnology, non-metallic elements, etc., can solve the problems of affecting the activity of transition metal-supported catalysts, cumbersome preparation process, unevenness, etc., and achieves significant prospects for industrialization and application. The preparation steps are simple and the effect of not being easy to reunite

Active Publication Date: 2020-10-16
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent (CN104858413 B) discloses a preparation method of silica-loaded noble metal nanoparticles, which adopts the inverse microemulsion method to mix 1-20 nm metal nanoparticles Cu, Au, Ni, Pt, Pd, Rh, Ir, Ru Silica particles loaded at 20-200 nm, the preparation requires the use of expensive reagents such as surfactants and long-chain fatty alcohols, and the preparation process is cumbersome
From the technical content disclosed in the above patent documents, it is not difficult to find that the preparation steps are very cumbersome, and the distribution of nanoparticles of the obtained materials does not clearly indicate the size of the particles.
[0005] To sum up, the transition metal nanoparticle catalysts supported by different molecular sieves prepared in the prior art generally need to synthesize zeolite molecular sieves first, and then carry out loading. The preparation steps are cumbersome, and agglomeration is easy to occur, resulting in larger particle sizes And uneven, greatly affecting the activity of transition metal supported catalysts

Method used

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  • Preparation of Hierarchical Zeolite Aggregates Supported by Highly Dispersed Transition Metal Nanoparticles
  • Preparation of Hierarchical Zeolite Aggregates Supported by Highly Dispersed Transition Metal Nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 0.6 g NiSO 4 And 2.2 g Al 2 (SO 4 ) 3 ·18H 2 Dissolve O in 25 ml pure water, stir to clarify and add dropwise to 28g Na 2 SiO 3 ·9H 2 Add 2 ml of NH to 20 ml of O in water 3 ·H 2 O (concentration of 1 M) adjust the alkalinity, stir for 23 minutes to obtain a nickel-silicate-aluminum sol-gel solution, and then add 0.7 g (13wt%) of the silicate-1 seed solution dropwise to the nickel-silicate-aluminum prepared above Stir in the sol-gel solution for 30 minutes to obtain a precursor solution. The precursor solution is hydrothermally crystallized at 150°C for 20 hours. After the reaction is completed, it is washed and dried to obtain a highly dispersed Ni-ZSM-5 nanometer product. Zeolite aggregate catalyst material.

[0014] See attached figure 1 The XRD spectrum of the Ni-ZSM-5 sample obtained is consistent with the characteristic peaks of the standard MFI molecular sieve, indicating that the transition metal nickel has not entered the framework of the zeolite molecular sieve. T...

Embodiment 2

[0017] Add 0.4 g CuCl 2 ·6H 2 O and 1.1 g Al 2 (SO 4 ) 3 ·18H 2 Dissolve O in 25 ml pure water, stir to clarify and add dropwise to 28 g Na 2 SiO 3 ·9H 2 To 25ml aqueous solution of O, add 2.2 ml NH 3 ·H 2 Adjust the alkalinity with O (concentration of 1 M), stir for 25 minutes to obtain a copper-silica-aluminum sol-gel solution, and then add 0.5 g (13wt%) of ß-zeolite zeolite seed solution dropwise to the nickel-silica-aluminum prepared above Stir in the sol-gel solution for 25 minutes to obtain the precursor solution. The precursor solution is hydrothermally crystallized at 170 ℃ for 26 hours. After the reaction is completed, the product is washed and dried to obtain a highly dispersed Cu-ß-zeolite nano Zeolite aggregate catalyst material.

Embodiment 3

[0019] Add 0.5 g CoCl 2 · 6H 2 O and 0.67 g Al2(SO 4 ) 3 ·18H 2 Dissolve O in 25 ml of pure water, stir to clarify and add dropwise to 27 g of Na 2 SiO 3 ·9H 2 Add 2.1 ml NH to the 23ml aqueous solution of O 3 ·H 2 O (concentration of 1 M) adjust the alkalinity, stir for 20 minutes to obtain the cobalt-silica-aluminum sol-gel solution, and then add 0.4 g (13wt%) silicate-2 zeolite seed solution dropwise to the cobalt-silica-aluminum prepared above Stir in the sol-gel solution for 30 minutes to obtain the precursor solution. The precursor solution is hydrothermally crystallized at 150 ℃ for 20 hours. After the reaction, the product is washed and dried to obtain a highly dispersed Co-ZSM-11 nanometer. Zeolite aggregate catalyst material.

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Abstract

The invention discloses a preparation method of a high-dispersed transition metal nanoparticle-supported hierarchical pore zeolite aggregate. The preparation method comprises adding mixed liquid dropsof an inorganic aluminum source and a transition metal salt into an inorganic silicon source solution drop by drop, adjusting alkalinity through KOH or NaOH, carrying out stirring to obtain a transition metal-silica-alumina sol-gel solution, adding crystal gel with different crystal structures into the mixed solution, and carrying out crystallization at 80-200 DEG C for 10-48h to obtain the high-dispersed transition metal nanoparticle-supported hierarchical pore zeolite aggregate catalytic material with particle sizes of 1.5 to 2 nm. Compared with the prior art, the preparation method furthercontrols the synthesis of the hierarchical pore zeolite molecular sieve material, effectively adjusts and controls the opening degree of channels of hierarchical pore zeolite, and successfully modifies the surface of the hierarchical pore zeolite aggregate material with transition metal nanoparticles to produce the zeolite aggregate catalytic material with multiple active sites and agglomerationdifficulty. The preparation method has simple processes, is easy to operate and separate and has a certain industrial promotion use prospect and a remarkable economic value.

Description

Technical field [0001] The invention relates to the technical field of zeolite molecular sieve synthesis, in particular to the preparation of a high-dispersion transition metal nanoparticle-loaded multi-porous zeolite aggregate. Background technique [0002] Nano-transition metal catalysts have received extensive attention and research due to their excellent catalytic performance. They have become one of the leading catalysts in modern industry and occupy a very key position in the field of catalysts. Metal nanoparticles have high surface energy and are easy to agglomerate. The activity is reduced. In order to solve this problem, the highly active nanoparticles can be immobilized on the carrier, and the aggregation and deactivation of the nanoparticles can be inhibited through the interaction with the carrier. [0003] Nanoparticle loading is mainly synthesized by impregnation method. One is to synthesize the carrier first, then load the metal salt on the carrier by the impregnatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/46B01J29/76C01B39/38C01B39/46C01B39/36B82Y30/00
CPCB01J29/46B01J29/7615B01J2229/186B82Y30/00C01B39/365C01B39/38C01B39/46C01P2002/72C01P2004/04C01P2004/80
Inventor 陈丽
Owner EAST CHINA NORMAL UNIV
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