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Low-cost green method for synthesizing Fe-ZSM-5 molecular sieve

A green synthesis, fe-zsm-5 technology, applied in the direction of gallium aluminosilicate/iron aluminosilicate, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., to achieve energy consumption Reduction, reduction of toxic effects, low cost effect

Inactive Publication Date: 2016-07-06
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, diatomite is used as raw material, tetrapropylammonium bromide is used as a template to obtain Fe-ZSM-5 molecular sieve through hydrothermal crystallization. Use of organic templating agents

Method used

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  • Low-cost green method for synthesizing Fe-ZSM-5 molecular sieve
  • Low-cost green method for synthesizing Fe-ZSM-5 molecular sieve
  • Low-cost green method for synthesizing Fe-ZSM-5 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0036] First, mix the diatomite raw material with a 10% sodium hydroxide solution according to a solid-to-liquid ratio of 1:5 (g / ml), stir evenly, dissolve in alkali at 150°C for 4 hours, and filter with suction to obtain diatomite Alkali-soluble supernatant. Then, add ZSM-5 molecular sieve seed crystals and deionized water to the upper supernatant, and the preparation composition is n(H 2 O) / (SiO 2 )=50, ZSM-5 molecular sieve seed crystal / SiO 2 =6% (mass ratio), the initial gel system with a pH value of 9.5 (adjusted by sulfuric acid), stirred evenly and crystallized at 170° C. for 36 hours. Finally, cool, filter, wash and dry to obtain a crystallized product. According to the XRD analysis, the crystallized product has a typical MFI structure diffraction peak, which proves that the product is a ZSM-5 molecular sieve; it can be seen from the SEM photo that the Fe-ZSM-5 molecular sieve is in the shape of a hexagonal prism; The ZSM-5 molecular sieve framework was formed and ...

Embodiment 2

[0039] Firstly, the diatomite raw material is mixed with a 20% sodium hydroxide solution, stirred uniformly and dissolved in alkali at 100° C. for 6 hours, and suction-filtered to obtain a diatomite alkali-dissolved supernatant. Then, NaY molecular sieve seed crystals and deionized water were added to the upper supernatant to prepare n(H 2 O) / (SiO 2 )=40, NaY molecular sieve seed crystal / SiO 2 =8% (mass ratio), the initial gel system with a pH value of 10.5 (adjusted by sulfuric acid), stirred evenly and crystallized at 170° C. for 96 hours. Finally, cool, filter, wash and dry to obtain a crystallized product. According to the XRD analysis, the crystallized product has a typical MFI structure diffraction peak, which proves that the product is a ZSM-5 molecular sieve; it can be seen from the SEM photo that the Fe-ZSM-5 molecular sieve is in the shape of a hexagonal prism; The ZSM-5 molecular sieve framework was formed and mainly existed in the form of isolated trivalent Fe i...

Embodiment 3

[0043] Firstly, the diatomite raw material is mixed with a 20% sodium hydroxide solution, stirred uniformly and dissolved in alkali at 100° C. for 6 hours, and suction-filtered to obtain a diatomite alkali-dissolved supernatant. Then, add a certain amount of deionized water to the upper supernatant, and prepare the composition as n(H 2 O) / (SiO 2 )=40, ZSM-5 molecular sieve seed crystal / SiO 2 =0% (mass ratio) (note: that is, without adding any seed crystals), the initial gel system with a pH value of 10.5 (adjusted by sulfuric acid), and crystallized at 170° C. for 120 hours after stirring evenly. Finally, cool, filter, wash and dry to obtain a crystallized product. According to the XRD analysis, the crystallized product has a typical MFI structure diffraction peak, which proves that the product is a ZSM-5 molecular sieve; it can be seen from the SEM photo that the Fe-ZSM-5 molecular sieve is in the shape of a hexagonal prism; The ZSM-5 molecular sieve framework was formed a...

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Abstract

The invention belongs to the technical field of molecular sieves and preparation methods thereof, and particularly relates to a technique for preparing an Fe-ZSM-5 molecular sieve. According to the method, natural mineral diatomite is used as the raw material to provide all of the silicon source, aluminum source and iron source required by synthesis of Fe-ZSM-5, and conventional hydrothermal crystallization is carried out under the condition of not adding any organic template. The natural mineral diatomite is used as the raw material to provide all the silicon and aluminum sources required by the synthesis of the molecular sieve, the Fe2O3 impurity contained in the diatomite raw material is fully utilized as the iron source, and a conventional hydrothermal process is carried out under the condition of not adding any organic template, thereby preparing the framework-iron-containing ZSM-5 molecular sieve (Fe-ZSM-5 molecular sieve). The method has obvious advantages in the aspects of widening the molecular sieve synthesis raw material range, enhancing the added value of the natural mineral product, lowering the molecular sieve production cost, reducing the environmental pollution and the like.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves and their preparation methods. It specifically involves using natural mineral diatomite as raw material to provide all the silicon sources, aluminum sources and iron sources required for the synthesis of Fe-ZSM-5, and preparing Fe through conventional hydrothermal crystallization without adding any organic template. - The process of ZSM-5 molecular sieve. Background technique [0002] ZSM-5 zeolite molecular sieve is an inorganic crystalline material developed by Mobil Corporation. It is widely used as an FCC catalyst promoter because of its regular pore structure, strong acidity, good hydrothermal stability and excellent selectivity. , methanol to olefins catalysts and other fields. Modification by introducing Fe into the ZSM-5 molecular sieve framework can effectively adjust its acidic properties and can be used as NH 3 Selective Catalytic Reduction of NO x Catalysts for reaction, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38C01B39/06
CPCC01B39/065C01B39/38C01P2002/84C01P2004/03C01P2002/72C01P2004/40
Inventor 王有和阎子峰历阳白鹏邢伟刘欣梅乔柯
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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