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Method for preparing Fe-MFI microporous molecular sieve

A technology of microporous molecular sieve and deionized water, which is applied in the direction of iron silicate and crystalline aluminosilicate zeolite, etc., can solve the problems of application limitation, poor hydrothermal stability, lack of acidity, etc., and achieve good selectivity and cost The effect of low cost and simple preparation method

Inactive Publication Date: 2018-03-30
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limitation of pore size, microporous materials are greatly restricted in the research fields of macromolecular catalytic reactions, especially in fine chemical industry. How to solve this defect has become the research direction of many people.
Later, people prepared zeolite molecular sieves with mesoporous structure, because pure silicon mesoporous materials have many defects, that is, lack of acidity, and the amorphous pore wall structure also leads to poor hydrothermal stability, which makes it widely used in petrochemical industry. App is restricted

Method used

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  • Method for preparing Fe-MFI microporous molecular sieve
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  • Method for preparing Fe-MFI microporous molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Take 2.91g Fe(NO 3 ) 3 ﹒ 9H 2 O and 1.072g TEA are placed in a 50ml beaker, add a small amount of deionized water, and dissolve on a constant temperature magnetic stirrer.

[0031] After the dissolution is complete, put the solution into an ice-water bath, drop 61.54g of tetrapropylammonium hydroxide TPAOH solution (40wt%) in about 30min, add 17.20g of TEOS dropwise after the addition is completed and stir for 1h, at room temperature Under stirring for 10h.

[0032] Place the beaker containing the solution in a magnetic heating stirrer at 80°C to evaporate the ethanol. After the ethanol is evaporated, transfer the solution in the beaker to a polytetrafluoroethylene-lined reaction kettle, add a small amount of deionized water, and place at 80 The reaction was carried out at ℃ for 24 hours, and it was taken out and stored in a refrigerator at low temperature.

[0033] Weigh the above seed crystals, transfer them to a plastic beaker, add A380 white carbon black silica...

Embodiment 2

[0038] Note: Steps 1) to 4) are the same as those in Example 1 and will not be repeated here.

[0039] 5) Transfer the column into a high-pressure reaction kettle for crystallization for 4 hours, take out the sample and cool it, dry it in an oven at 80°C for 24 hours, and roast it at 550°C for 6 hours to obtain the sample and label it as Fe-0.2625-0.025-4h ;(0.2625TPAOH:1SiO 2 :0.025Fe(NO 3 ) 3 ﹒ 9H 2 O: 0.025TEA).

[0040] The prepared Fe-0.2625-0.025-4h sample, because the crystallization time is too short, the crystallinity is not very good. The Fe-0.2625-0.025-4h sample was used to catalyze the reaction of oxidizing toluene to prepare benzaldehyde, the conversion rate of Fe-Si molecular sieve was 0.54%, and the selectivity was 3.68%.

Embodiment 3

[0042] Note: Steps 1) to 4) are the same as those in Example 1 and will not be repeated here.

[0043] 5) Transfer the columnar material into a high-pressure reaction kettle for crystallization for 24 hours, take out the sample and cool it, dry it in an oven at 80°C for 24 hours, and roast it at 550°C for 6 hours to obtain the sample and label it as Fe-0.2625-0.025-24h, (0.2625TPAOH:1SiO 2 :0.025Fe(NO 3 ) 3 ﹒ 9H 2 O: 0.025TEA).

[0044]The prepared Fe-0.2625-0.025-24h sample has achieved a good crystallization effect after 24h of crystallization. Fe-0.2625-0.025-24h is used to catalyze the reaction of oxidizing toluene to prepare benzaldehyde, the conversion rate of iron-silicon molecular sieve is 4.82%, and the selectivity is 52.47%.

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Abstract

The invention discloses a method for preparing a Fe-MFI microporous molecular sieve. The method, with tetraethylorthosilicate (TEOS) as a silicon source, iron nitrate as a heteroatom metal source, triethanolamine (TEA) as a complexing agent and tetrapropylammonium hydroxide (TPAOH) as a structure-directing agent, successfully prepares the iron-containing MFI microporous molecular sieve by extrusion molding by a dry gel method. According to the method for synthesizing the molecular sieve by the dry gel method, a smaller amount of the structure-directing agent TPAOH and a small amount of water are used for molding and synthesis of the iron-containing molded heteroatom molecular sieve in one step. The method can effectively avoid the filtration and washing process in the traditional process,reduce the production cost of the catalyst, minimize the generation of waste water, and belongs to the green environmental protection process.

Description

technical field [0001] The invention belongs to the field of preparation of zeolite molecular sieve microporous materials. Specifically, it relates to a preparation method of Fe-MFI microporous molecular sieve. Background technique [0002] According to the definition, zeolite molecular sieves can be divided into three parts according to the pore size, namely microporous molecular sieves (<2nm), mesoporous molecular sieves (2-50nm) and macroporous molecular sieves (>50nm). [0003] In the 1850s, people discovered natural microporous materials, namely natural zeolite. Later, people concluded in long-term practical activities that this material has ion exchange properties and the function of adsorbing gas and moisture. In recent years, the preparation of high-efficiency, "environmentally friendly" new catalytic materials has become one of the hotspots in the field of catalyst research. Zeolite porous materials have broad development space in this field. However, due ...

Claims

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Application Information

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IPC IPC(8): C01B39/08
CPCC01B39/087C01P2002/72C01P2002/82
Inventor 卢德力林静静颜松刘平张小杰刘玥冉常伟姚璐连俊韩生蔺华林
Owner SHANGHAI INST OF TECH
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