Preparation method of high-dispersed transition metal nanoparticle-supported hierarchical pore zeolite aggregate

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 effect of simple preparation steps and easy materials

Active Publication Date: 2018-06-15
EAST CHINA NORMAL UNIV
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  • 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 cu

Method used

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  • Preparation method of high-dispersed transition metal nanoparticle-supported hierarchical pore zeolite aggregate
  • Preparation method of high-dispersed transition metal nanoparticle-supported hierarchical pore zeolite aggregate

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Embodiment 1

[0013] 0.6 g NiSO 4 and 2.2 g Al 2 (SO 4 ) 3 18H 2 O was dissolved in 25 ml of pure water, stirred and clarified, and added dropwise to 28 gNa 2 SiO 3 9H 2 In 20 ml aqueous solution of O, add 2 ml NH 3 ·H 2 O (concentration of 1 M) was used to adjust the alkalinity, and stirred for 23 minutes to obtain a nickel-silicon-alumina sol-gel solution, and then 0.7 g (13wt%) of silicate-1 seed solution was added dropwise to the above-prepared nickel-silicon-alumina Stir in the sol-gel solution for 30 minutes to obtain the precursor solution. The precursor solution is subjected to hydrothermal crystallization reaction at 150°C for 20 hours. After the reaction is completed, it is washed and dried, and the obtained product is highly dispersed Ni-ZSM-5 nanometer Zeolite aggregate catalyst material.

[0014] See attached figure 1 , the XRD spectrum of the obtained product Ni-ZSM-5 sample is consistent with the characteristic peaks of the standard MFI molecular sieve, indicating t...

Embodiment 2

[0017]0.4 g CuCl 2 ·6H 2 O and 1.1 g Al 2 (SO 4 ) 3 18H 2 O was dissolved in 25 ml pure water, stirred and clarified, then added dropwise to 28 g Na 2 SiO 3 9H 2 In 25ml aqueous solution of O, add 2.2ml NH 3 ·H 2 O (concentration of 1 M) was used to adjust the alkalinity, and stirred for 25 minutes to obtain a copper-silicon-alumina sol-gel solution, and then 0.5 g (13wt%) ß-zeolite zeolite seed solution was added dropwise to the above-prepared nickel-silicon-alumina The precursor solution was obtained by stirring in the sol-gel solution for 25 minutes, and the precursor solution was subjected to hydrothermal crystallization reaction at 170 °C for 26 hours. After the reaction was completed, it was washed and dried, and the obtained product was highly dispersed Cu-ß-zeolite nanometer Zeolite aggregate catalyst material.

Embodiment 3

[0019] 0.5 g CoCl 2 · 6H 2 O and 0.67 g Al2(SO 4 ) 3 18H 2 O was dissolved in 25 ml of pure water, stirred and clarified and added dropwise to 27 g of Na 2 SiO 3 9H 2 In 23ml aqueous solution of O, add 2.1ml NH 3 ·H 2 O (concentration of 1 M) was used to adjust the alkalinity, and stirred for 20 minutes to obtain a cobalt-silicon-alumina sol-gel solution, and then 0.4 g (13wt%) silicate-2 zeolite seed solution was added dropwise to the cobalt-silicon-alumina sol-gel solution prepared above The precursor solution was obtained by stirring in the sol-gel solution for 30 minutes, and the precursor solution was hydrothermally crystallized at 150°C for 20 hours. After the reaction was completed, it was washed and dried, and the obtained product was 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 synthesis of zeolite molecular sieves, in particular to the preparation of highly dispersed transition metal nanoparticle-loaded multi-stage zeolite aggregates. Background technique [0002] Nano-transition metal catalysts have received extensive attention and research because of their excellent catalytic performance, and have become one of the leading catalysts in modern chemical industry, and occupy a very key position in the field of catalysts. Because metal nanoparticles have high surface energy and are easy to agglomerate, making The activity is reduced. In order to solve this problem, highly active nanoparticles can be immobilized on the carrier, and the aggregation and inactivation of the nanoparticles can be inhibited by interacting with the carrier. [0003] Nanoparticle loading is mainly synthesized by impregnation. One is to synthesize the carrier first, then load the metal salt on the carrier ...

Claims

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Application Information

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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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