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Core-shell structured nano monocrystal ZSM-5@Silicalite-1 molecular sieve and preparation method thereof

A nano-single-crystal, core-shell structure technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, refined hydrocarbon oil, etc., can solve the problems of loss, molecular sieve activity and adverse effects on stability, etc., and achieve small diffusion resistance and excellent catalytic performance , highly selective effect

Inactive Publication Date: 2018-02-09
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this type of method will inevitably cause the loss of acid sites in the channels, and will have an adverse effect on the activity and stability of molecular sieves.

Method used

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  • Core-shell structured nano monocrystal ZSM-5@Silicalite-1 molecular sieve and preparation method thereof
  • Core-shell structured nano monocrystal ZSM-5@Silicalite-1 molecular sieve and preparation method thereof
  • Core-shell structured nano monocrystal ZSM-5@Silicalite-1 molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The invention provides a method for preparing a nano single crystal ZSM-5@Silicalite-1 molecular sieve with a core-shell structure, comprising the following steps:

[0043] S101: Weigh 50 g of nano ZSM-5 molecular sieves with a silicon-aluminum ratio of 35 and a grain size of 150 nm as an uncalcined template, add 500 ml of hydrochloric acid solution with a concentration of 5 mol / L, and stir for 5 hours at a temperature of 50°C.

[0044] S102: filter and wash the molecular sieve obtained in S101 until the pH value is 7, and dry at 80° C. for 12 hours to obtain ZSM-5 molecular sieve Z-1 with pretreated outer surface.

[0045] S103: Weigh 2.33g of tetrapropylammonium hydroxide (25wt%), 35.23g of ethanol and 205g of water, after mixing and dissolving, slowly add 2.88g of fumed silica under stirring condition, and obtain the shell Silicalite- 1 molecular sieve of Growth Solution A.

[0046] S104: Add the pretreated nuclear phase Z-1 to the growth solution A, wherein the mas...

Embodiment 2

[0050] The invention provides a method for preparing a nano single crystal ZSM-5@Silicalite-1 molecular sieve with a core-shell structure, comprising the following steps:

[0051] S101: Weigh 50 g of nano ZSM-5 molecular sieves with a silicon-aluminum ratio of 35 and a grain size of 150 nm as an uncalcined template, add 500 ml of hydrochloric acid solution with a concentration of 5 mol / L, and stir for 5 hours at a temperature of 50°C.

[0052] S102: filter and wash the molecular sieve obtained in S101 until the pH value is 7, and dry at 80° C. for 12 hours to obtain ZSM-5 molecular sieve Z-1 with pretreated outer surface.

[0053] S103: Weigh 2.33g of tetrapropylammonium hydroxide (25wt%), 35.23g of ethanol and 205g of water, after mixing and dissolving, slowly add 2.88g of fumed silica under stirring condition, and obtain the shell Silicalite- 1 molecular sieve of Growth Solution A.

[0054] S104: Add the pretreated nuclear phase Z-1 into the growth solution A, wherein the m...

Embodiment 3

[0057] The invention provides a method for preparing a nano single crystal ZSM-5@Silicalite-1 molecular sieve with a core-shell structure, comprising the following steps:

[0058] S101: Weigh 50 g of nano-ZSM-5 molecular sieves with a silicon-aluminum ratio of 70 and a grain size of 150 nm as an uncalcined template, add 500 ml of hydrochloric acid solution with a concentration of 0.5 mol / L, and stir for 5 hours at a temperature of 50°C.

[0059] S102: filter and wash the molecular sieve obtained in S101 until the pH value is 7, and dry at 80° C. for 12 hours to obtain ZSM-5 molecular sieve Z-2 with pretreated outer surface.

[0060] S103: Weigh 2.33g of tetrapropylammonium hydroxide (25wt%), 35.23g of ethanol and 205g of water, after mixing and dissolving, slowly add 2.88g of fumed silica under stirring condition, and obtain the shell Silicalite- 1 molecular sieve of Growth Solution A.

[0061] S104: Add the pretreated nuclear phase Z-2 into the growth solution A, wherein the...

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Abstract

The invention relates to a core-shell structured nano monocrystal ZSM-5@Silicalite-1 molecular sieve and a preparation method thereof. According to the preparation method, a nano ZSM-5 molecular sieveis used as a core phase, and the grain size is 50 to 800 nm; a nano Silicalite-1 molecular sieve is used as a shell phase, and a shell layer is 5 to 100 nm in thickness; after the outer surface of the core-phase ZSM-5 molecular sieve is pretreated with a weakly acidic solution, the core-phase ZSM-5 molecular sieve is subjected to hydrothermal crystallization in a shell-layer molecular sieve growth solution system, so that the nano monocrystal ZSM-5@Silicalite-1 molecular sieve containing a compact shell layer is prepared. The molecular sieve provided by the invention has the characteristics of a continuous porous channel, low diffusion resistance, high integration mechanical intensity and high selectivity; furthermore, the molecular sieve can be effectively applied to a catalytic crackinggasoline hydrogenation modification process, and has excellent catalysis performance on aspects of aromatics shape-selective disproportionation, shape-selective alkylation, shape-selective isomerization, catalytic cracking gasoline hydrogenation modification and the like.

Description

technical field [0001] The invention relates to the technical field of composite catalytic materials, in particular to a nano single crystal ZSM-5@Silicalite-1 molecular sieve with a core-shell structure and a preparation method thereof. Background technique [0002] As a typical high-silicon molecular sieve developed by Mobil Corporation of the United States, ZSM-5 molecular sieve has three-dimensional intersecting channels. The diameter of the channel intersection is 0.9nm. With the help of special pore structure and acidity, ZSM-5 molecular sieves are used as catalysts and shape-selective catalysts for acid-catalyzed reactions, and are widely used in petrochemical, fine chemical and environmental protection. [0003] As we all know, the size of nanoparticles is generally less than a few hundred nanometers, and the size is between atomic clusters and macroscopic objects. Compared with conventional particles, the physical and chemical properties of nanoparticles are obviou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/80C10G45/12
CPCC10G45/12B01J29/005B01J29/40B01J29/0308C10G2300/1037B01J35/396
Inventor 刘宾谢清清柴永明刘晨光李奕川柳云骐殷长龙董斌
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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