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Preparation method of nano-rod-shaped ZSM-48 molecular sieve

A nano-rod-shaped, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, can solve problems such as increasing cost and polluting the environment, and achieve the effect of high crystallinity and short diffusion path

Inactive Publication Date: 2014-08-27
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Usually, in order to prepare ZSM-48 with nanorod-shaped small grains, more additives need to be introduced, such as alkylating agents, polymers and inorganic additives. The above-mentioned methods not only increase the cost but also pollute the environment.

Method used

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  • Preparation method of nano-rod-shaped ZSM-48 molecular sieve
  • Preparation method of nano-rod-shaped ZSM-48 molecular sieve
  • Preparation method of nano-rod-shaped ZSM-48 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0030] Prepare the initial gel in the following molar ratios: SiO 2 / Al 2 o 3 =100,OH - / SiO 2 =0.3, R / SiO 2 =0.2, H 2 O / SiO 2 Sodium aluminate, sodium hydroxide, and 1,4-(N-methylpiperidinyl)butane bromide were dissolved in deionized water at a ratio of =30, and then white carbon black was added under constant stirring. Afterwards, the above mixture was charged into a 100 ml crystallization kettle and reacted at 160° C. for 168 hours.

[0031] Put the cooled reaction solution in a water bath for 5 hours, after obvious layering, the yellow solid in the lower layer is ZSM-48 molecular sieve, which is separated, washed, dried, and calcined. After XRD analysis, it is confirmed to be nanorods Stacked ZSM-48 molecular sieve particles with a silicon-aluminum molar ratio of 29; characterized by SEM, the particle length is 1.5 μm, and the nanorod size is 30 nm. The yield of -48-1 was 90%.

Embodiment 2

[0033] Prepare the initial gel in the following molar ratios: SiO 2 / Al 2 o 3 =60,OH - / SiO 2 =0.3, R / SiO 2 =0.25, H 2 O / SiO 2 Sodium aluminate, sodium hydroxide, and 1,10-(N-methylpiperidinyl)decane bromide were dissolved in deionized water at a ratio of 40, and then white carbon black was added under constant stirring. Afterwards, the above mixture was charged into a 100 ml crystallization kettle and reacted at 175° C. for 192 hours.

[0034] Put the cooled reaction solution in a water bath for 10 hours, after obvious stratification, the off-white solid in the lower layer is ZSM-48 molecular sieve, which is separated, washed, dried, and calcined. After XRD analysis, it is confirmed to be nano Rod-shaped ZSM-48 molecular sieve with a molar ratio of silicon to aluminum of 23; characterized by SEM, the particle size is 700 nm, and the nanorod length is 50 nm. Numbering is ZSM-48-2, and the productive rate of ZSM-48-2 is 82% in terms of the silica weight of feeding.

Embodiment 3

[0036] Prepare the initial gel in the following molar ratios: SiO 2 / Al 2 o 3 =200,OH - / SiO 2 =0.5, R / SiO 2 =0.16, H 2 O / SiO 2 Dissolve sodium aluminate, sodium hydroxide, and the above organic templates in deionized water at a ratio of =15, add silicic acid without stirring, and then put the above mixture into a 100 ml crystallization kettle at 160°C Reaction for 120 hours.

[0037] Put the cooled reaction solution in a water bath for 10 hours, and after obvious stratification, the white solid in the lower layer is ZSM-48 molecular sieve, which is separated, washed, dried, and roasted and then analyzed by XRD to confirm that it is a nanorod The rice grain-shaped ZSM-48 molecular sieve formed by stacking has a silicon-aluminum molar ratio of 80; after SEM characterization, the particle size is 600 nm, and the length of the nano-sized grains is 50 nm. Numbering is ZSM-48-3, and the productive rate of ZSM-48-3 is 94% in terms of the silica weight of feeding.

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Abstract

The invention belongs to the technical field of inorganic materials, and in particular relates to a preparation method of a nano-rod-shaped ZSM-48 molecular sieve. The method comprises the following steps: mixing a silicon source, an aluminum source, an alkali source, an organic template and a water phase by virtue of adopting a hydro-thermal synthesis method, and stirring into a gel-like mixture used as a raw material for synthesizing the ZSM-48 molecular sieve. The chemical composition of the nano ZSM-48 molecular sieve with high degree of crystallinity is TO2:aY2O3:bM2 / nO, wherein T represents at least one quadrivalent element, Y represents at least one trivalent element, M represents at least one alkaline metal (or) alkaline-earth metal element of which the valence state is n. Prepared ZSM-48 disclosed by the invention not only has neat appearance, relatively short diffusion process, ultra-high degree of crystallinity and relatively rich specific surface area, but also can be used for improving the whole catalytic utilization efficiency of the molecular sieves.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and in particular relates to a preparation method of nanorod ZSM-48 molecular sieves. Background technique [0002] ZSM-48 molecular sieve is a microporous crystalline molecular sieve with a one-dimensional ten-membered ring channel structure. At the same time, ZSM-48 molecular sieve also has high thermal stability, hydrothermal stability and adjustable acidity. Therefore, ZSM-48 molecular sieve shows high practical value in the fields of small molecule shape-selective catalysis, aromatic hydrocarbon alkylation, toluene disproportionation and fine chemical processing. [0003] At present, most of the ZSM-48 molecular sieves used in industry are bulky particles. The large grains lead to low catalytic utilization of one-dimensional molecular sieves and easy to cause carbon deposition. When used in catalytic reactions, reactants or products The diffusion resistance of molecules on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 唐颐王磊王培丞田海雯张宏斌吕新春
Owner FUDAN UNIV
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