Method for preparing grain size-controllable solid phase synthetic molecular sieve

A technology of solid-phase synthesis and grain size, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of adverse effects of molecular sieves in practical application and difficult control of grain size, etc. Achieve good economic and social benefits, reduce waste water discharge, and reduce production costs

Active Publication Date: 2017-08-04
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the solid-phase synthesis of ZSM-5 molecular sieves, the grain size is difficul

Method used

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  • Method for preparing grain size-controllable solid phase synthetic molecular sieve
  • Method for preparing grain size-controllable solid phase synthetic molecular sieve
  • Method for preparing grain size-controllable solid phase synthetic molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Take by weighing 13.15g sodium silicate nonahydrate, 3.47g fumed silica gel, 0.25g sodium metaaluminate, 2.40g tetrapropylammonium bromide (TPABr), 4.2g ammonium chloride (SiO 2 :Al 2 o 3 : organic templating agent: NH 4 + The added molar ratio is 1:0.015:0.09:0.79) mixed as reaction raw materials, added to a mechanical pulverizer for pulverization, so that the solid reactants are uniformly mixed. Then the raw material was transferred to a 100ml polytetrafluoroethylene-lined stainless steel autoclave, and placed in an oven for crystallization at 180°C for 48h. The obtained product was calcined at 550° C. for 6 h to obtain the final product.

[0046] attached figure 1 According to the XRD characterization results of the above product, it can be seen that the product has a typical MFI structure and has a good crystallinity.

[0047] attached figure 2 It is the SEM scanning electron microscope photo of the above product, it can be seen that the particle of the prod...

Embodiment 2

[0050] Weigh 13.15g sodium silicate nonahydrate, 3.47g fumed silica gel, 0.25g sodium metaaluminate, 2.40g tetrapropylammonium bromide (TPABr), 4.2g ammonium chloride, 0.25gZSM-5 molecular sieve seed crystal mix as reaction Raw materials are added to a mechanical pulverizer for pulverization, so that the solid reactants are evenly mixed. Among them, SiO 2 :Al 2 o 3 : organic templating agent: NH 4 + The added molar ratio is 1:0.015:0.09:0.79; the mass percentage of ZSM-5 molecular sieve seed crystals in the reaction raw materials is 1%. Then the raw material was transferred to a 100ml polytetrafluoroethylene-lined stainless steel autoclave, and placed in an oven for crystallization at 180°C for 48h. The obtained product was calcined at 550° C. for 6 h to obtain the final product.

[0051] attached Figure 5 According to the XRD characterization results of the above product, it can be seen that the product has a typical MFI structure and has a good crystallinity.

[005...

Embodiment 3

[0056] Weigh 13.15g sodium silicate nonahydrate, 3.47g fumed silica gel, 0.25g sodium metaaluminate, 2.40g tetrapropylammonium bromide (TPABr), 4.2g ammonium chloride, 0.50g ZSM-5 molecular sieve seed crystals and mix as reaction Raw materials are added to a mechanical pulverizer for pulverization, so that the solid reactants are evenly mixed. Among them, SiO 2 :Al 2 o 3 : organic templating agent: NH 4 + The added molar ratio is 1:0.015:0.09:0.79; the mass percentage of ZSM-5 molecular sieve seed crystals in the reaction raw materials is 2%. Then the raw material was transferred to a 100ml polytetrafluoroethylene-lined stainless steel autoclave, and placed in an oven for crystallization at 180°C for 48h. The obtained product was calcined at 550° C. for 6 h to obtain the final product.

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Abstract

The invention belongs to the field of material chemistry, and relates to a method for preparing a grain size-controllable solid phase synthetic molecular sieve. The invention provides the grain size-controllable solid phase synthetic molecular sieve; the preparation method of the molecular sieve concretely comprises the following steps: adding a solid silicon source, an aluminum source, a template agent and an alkali source, crushing the added materials together with a seed crystal, mixing and taking the obtained mixture as a reaction raw material; carrying out a crystallization reaction, roasting the product of the crystallization reaction and removing the template agent so as to obtain the grain size-controllable solid phase synthetic molecular sieve. The method for preparing the grain size-controllable solid phase synthetic molecular sieve can be used for obtaining the ZSM-5 molecular sieve, which is high in relative crystallinity and has a grain size controllable within a certain range, by controlling the adding amount of the ZSM-5 seed crystal, thus improving the catalytic selectivity of the ZSM-5 molecular sieve; furthermore, by adopting solid-phase synthesis, the method can reduce the discharge of waste water, thus realizing a green molecular sieve synthesis route.

Description

technical field [0001] The invention belongs to the field of material chemistry and relates to a method for solid-phase synthesis of molecular sieves with controllable grain size, in particular to a method for solid-phase synthesis of ZSM-5 molecular sieves with controllable grain size. Background technique [0002] Zeolite molecular sieves are widely used in the fields of ion exchange and catalytic chemistry due to their regular micropore structure and huge specific surface area, especially in petroleum refining and petrochemical fields. Among them, the pore size of ZSM-5 molecular sieve is about 0.55nm, which matches the molecular size of most reactions. Its surface acidity and unique pore structure make it have excellent catalytic performance, and it is widely used as a catalyst for various chemical reactions, such as cracking , Dewaxing, MTG / A, MTO catalytic reaction, etc. [0003] At present, the synthesis methods of conventional ZSM-5 molecular sieves mainly include h...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/38C01P2004/61C01P2006/12C01P2006/17
Inventor 任淑陈新庆刘子玉吴丹丘明煌金秋魏伟孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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