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Method for preparing nano Fe-ZSM-5 zeolite molecular sieve

A zeolite molecular sieve and nanotechnology, applied in the direction of molecular sieve catalysts, nanostructure manufacturing, nanotechnology, etc., can solve the problem of long time-consuming crystallization of small-grained molecular sieves, to overcome the long time of low-temperature crystallization, reduce production difficulty, and simplify operations conditional effect

Inactive Publication Date: 2008-02-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] Aiming at the deficiencies in the prior art, the purpose of the present invention is to provide a preparation method of nano-Fe-ZSM-5 zeolite molecular sieve, which makes the operation method safe and simple, and overcomes the shortcoming of long time-consuming crystallization at low temperature for the preparation of small-grain molecular sieves. Capable of preparing small-grained molecular sieves with grains smaller than 100nm

Method used

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  • Method for preparing nano Fe-ZSM-5 zeolite molecular sieve
  • Method for preparing nano Fe-ZSM-5 zeolite molecular sieve

Examples

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Embodiment 1

[0051] Mix 4.4g of sulfuric acid, 20g of deionized water, and 1.1g of ferric sulfate at room temperature, stir until the ferric sulfate is completely dissolved, and the solution becomes clear; then dissolve 17.1g of sodium silicate in 32g of deionized water, and the silicon-containing aqueous solution Add dropwise into the above-mentioned iron-containing solution, stir the two to mix evenly, then add 3 g of tetrapropylammonium hydroxide solution with a concentration of 30%, and continue stirring to obtain a uniform gel mixture. The molar composition of each component in the raw material is:

[0052] Fe2O3:SiO2:Na2O:(TPA)OH:H2O=1:25:30:4:1600

[0053] The resulting gel mixture was transferred into a stainless steel autogenous pressure crystallizer, kept at 100°C for 30 hours, and then heated to 180°C for 25 hours to complete the crystallization process. Cool the crystallizer with cold water, filter and wash the obtained product until the pH value reaches 7-8; put the solid pro...

Embodiment 2

[0055] Mix 4.4g of sulfuric acid, 25g of deionized water, and 1.1g of ferric sulfate at room temperature, stir until the ferric sulfate is completely dissolved, and the solution becomes clear; then dissolve 20.5g of sodium silicate in 46.2g of deionized water, and the Add the aqueous solution dropwise to the above iron-containing solution, stir the two to mix evenly, add 1.2g tetrapropylammonium bromide, and continue stirring to obtain a uniform gel mixture. The molar composition of each component in the raw material is:

[0056] Fe2O3:SiO2:Na2O:(TPA)Br:H2O=1:30:35:5:2200

[0057] The resulting gel mixture was transferred into a stainless steel autogenous pressure crystallizer, kept at a constant temperature of 90°C for 40 hours, and then heated to 180°C for 30 hours to complete the crystallization process. Cool the crystallizer with cold water, filter and wash the obtained product to a pH value of 7-8, put it in an oven at 110°C for 10 hours to dry the product, and bake it in...

Embodiment 3

[0059] 4.2g of sulfuric acid, 20g of deionized water, and 1.1g of ferric sulfate were mixed at room temperature, stirred until ferric sulfate was completely dissolved, and the solution became clear; then 12.3g of water glass with a modulus of 3.2 was dissolved in deionized water, and Add the silicon-containing aqueous solution dropwise to the above-mentioned iron-containing solution, stir the two to mix evenly, and then add 6 g of tetrapropylammonium hydroxide solution with a concentration of 30%, and continue to stir to obtain a uniform gel mixture. The molar composition of the fraction is:

[0060] Fe2O3:SiO2:Na2O:(TPA)OH:H2O=1:30:20:8:1800

[0061] The resulting gel mixture was transferred into a stainless steel autogenous pressure crystallizer, kept at a constant temperature of 120°C for 20 hours, and then heated to 180°C for 30 hours to complete the crystallization process. Cool the crystallizer with cold water, filter and wash the obtained product to a pH value of 7-8, ...

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Abstract

The present invention relates to the technical field of a zeolite molecular sieve synthesis, concretely speaking, relating to a preparation method of a zeolite molecular sieve of a nano heteroatom. A sodium silicate or a soluble glass, an inorganic acid, an inorganic ferric salt, an organic amine and deionized water serve as the material. After the steps of liquor preparation, two variable temperature crystallizations, washing-up centrifugalization, drying and roasting, the zeolite molecular sieve of nano Fe-ZSM-5 is produced with a grain size less than 100nm. The present invention can be used in the petrochemical industry, fine chemical industry and the environmental protection field.

Description

technical field [0001] The invention relates to the technical field of synthesis of zeolite molecular sieves, in particular to a preparation method of nanometer heteroatom zeolite molecular sieves. Background technique [0002] Zeolite molecular sieve catalysts have unique molecular shape-selective properties, high catalytic activity and hydrothermal stability, and occupy a major position in industrial catalysis. ZSM-5 zeolite molecular sieve is a kind of medium-pore zeolite molecular sieve with high silicon-aluminum ratio developed by Mobil Petroleum Company of the United States. It has unique structure and physical and chemical properties, and is widely used in petrochemical, fine chemical and environmental protection. [0003] In recent years, with the in-depth research on zeolite molecular sieves, molecular sieves with small grains have received more attention. Compared with large-grain molecular sieves, small-grain molecular sieves have a large specific surface area, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/42B82B3/00
Inventor 张飞姜健准黄文氢张敬梅张明森
Owner CHINA PETROLEUM & CHEM CORP
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