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Synthetic method of iron silicon molecular sieve with MFI structure

The technology of an iron-silicon molecular sieve and a synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite and the like, can solve the problems of easy loss, complicated operation and high cost, and achieve the effects of short production cycle, simple operation and high utilization rate.

Inactive Publication Date: 2012-02-15
SHENZHEN UNIV
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Problems solved by technology

The first two methods have been studied more, but the obtained materials are generally considered to be located in the pores and cages of molecular sieves, rather than on the skeleton, and are more likely to be lost.
Isomorphic substitution is to modify the composition of the molecular sieve framework. It can adopt gas-solid displacement reaction and liquid-solid displacement reaction. It belongs to the secondary synthesis, the operation is cumbersome, and the cost is high. It is generally used for heteroatom molecular sieves that cannot be directly hydrothermally synthesized.

Method used

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  • Synthetic method of iron silicon molecular sieve with MFI structure
  • Synthetic method of iron silicon molecular sieve with MFI structure
  • Synthetic method of iron silicon molecular sieve with MFI structure

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preparation example Construction

[0014] A method for synthesizing iron-silicon molecular sieve with MFI structure, characterized in that: the synthesis method includes the following steps:

[0015] Step 1: Weigh the silicon source, iron source, sodium hydroxide and organic template according to the stoichiometric ratio;

[0016] Step 2: Under stirring at room temperature, the substances in Step 1 are added to deionized water in sequence and mixed uniformly to form a mixture;

[0017] Step 3: Transfer the mixture in Step 2 to a closed hydrothermal reactor, and crystallize for 3 to 7 days under the conditions of a temperature range of 140°C to 190°C to obtain crude iron silicate crystals;

[0018] Step 4: Take the crude iron-silicon molecular sieve crystal product, and obtain the iron-silicon molecular sieve product through separation, washing, drying and roasting procedures.

[0019] The molar ratio of silicon source, iron source, sodium hydroxide, organic template agent and deionized water is 1.00:0.05~0.25:3.60:0.07~0...

Embodiment 1

[0021] A method for synthesizing Fe-Si molecular sieve with MFI structure. The steps are as follows: Under stirring at room temperature, according to the molar ratio of raw materials n(SiO 2 ): n(Fe 2 O 3 ): n(Na 2 O): n(HAD): n(H 2 O) = 1.00: 0.05: 3.60: 0.225: 30 The silicon source (fumed silica or silica sol), iron source (Fe(NO 3 ) 3 ·9H 2 O or FeSO 4 .7H 2 O), sodium hydroxide, organic template (1,6-hexamethylene diamine) and deionized water are mixed and stirred vigorously for 1 to 4 hours; after the mixture is uniform, the mixture is transferred to a closed hydrothermal reactor; After crystallization at 140°C for 7 days, the crude iron-silicon molecular sieve crystals are obtained; then, the crude iron-silicon molecular sieve crystals are taken as the crystalline product, and the finished product of the iron-silicon molecular sieve is finally obtained through separation, washing, drying, and roasting.

Embodiment 2

[0023] A method for synthesizing Fe-Si molecular sieve with MFI structure. The steps are as follows: Under stirring at room temperature, according to the molar ratio of raw materials n(SiO 2 ): n(Fe 2 O 3 ): n(Na 2 O): n(HAD): n(H 2 O) = 1.00: 0.25: 3.60: 0.30: 60 The silicon source (fumed silica or silica sol), iron source (Fe(NO 3 ) 3 ·9H 2 O or FeSO 4 .7H 2 O), sodium hydroxide, organic template (1,6-hexamethylenediamine) and deionized water are mixed and stirred vigorously for 1 to 4 hours; after the mixing is uniform, the mixture is transferred to a closed hydrothermal reactor; Under the condition of 190℃, crystallize for 3 days to obtain crude iron-silicon molecular sieve crystals. Then, the crude product of the crystalline product of the iron-silicon molecular sieve crystal is taken, and the finished product of the iron-silicon molecular sieve is finally obtained through the processes of separation, washing, drying and roasting.

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Abstract

The invention relates to a synthetic method of an iron silicon molecular sieve with an MFI structure. The method comprises the following steps of: step1. weighing silicon source, iron source, sodium hydroxide and organic template according to a stoichiometric ratio; step 2. stirring at a room temperature, and adding the substances of step 1 into deionized water successively, and mixing well to form a mixture; step 3. transferring the mixture from step 2 into an enclosed hydro-thermal reaction kettle, crystallizing for 3-7 days at a temperature scope of 140-190 DEG C to obtain a iron silicon molecular sieve crystal crude product. The invention employs a one-step hydro-thermal synthesis method, which can settle a matter at one go and has characteristics of low costs, high utilization rate and short production period, etc.

Description

Technical field [0001] The invention relates to the technical field of inorganic synthesis, in particular to a method for synthesizing iron-silicon molecular sieve, which can be used to prepare microporous materials. Background technique [0002] The introduction of heteroatoms into the framework is an important method of molecular sieve modification. It can not only adjust the acidity and pore structure of the molecular sieve, and improve the activity and selectivity of the molecular sieve. At the same time, the introduced heteroatoms can act as active centers and play a dual catalytic role. [0003] In the 1980s, Enichem first introduced transition metal titanium into the molecular sieve framework, synthesized the titanium silicate molecular sieve TS-1 with MFI structure, and successfully used it in the selective oxidation of hydrocarbons with hydrogen peroxide. This makes molecular sieve expand from the field of acid-base catalysis to the field of redox catalysis, becoming a mil...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 魏波徐宏刘振
Owner SHENZHEN UNIV
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