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Method for synthesizing mesoporous material with MCM-22 zeolite structured forerunner

A technology of MCM-22 and mesoporous materials, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of preparing mesoporous materials from precursors, and achieve the effect of good application prospects.

Inactive Publication Date: 2011-05-18
JIANGSU POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no mesoporous material prepared from its precursor in the prior art

Method used

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  • Method for synthesizing mesoporous material with MCM-22 zeolite structured forerunner

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Effect test

example 1

[0008] The synthesis of example 1 MM (25)

[0009] The first step of crystallization: 4.00mL hexamethyleneimine (HMI), 0.4574g NaAlO 2 Mix with 14.4mL water, slowly drop 24g (25wt%) silica sol into the mixed solution under strong stirring, the molar ratio of its material is SiO 2 : 0.02Al 2 o 3 :0.35HMI:18H 2 O. Stir continuously for another 1-2 hours, put it into a stainless steel reaction kettle with polytetrafluoroethylene lining, and crystallize at 150°C under rotation (120 revolutions / min) for 22-24 hours. After cooling to room temperature, the product was taken out to obtain the precursor of MCM-22 zeolite structure.

[0010] The second step of crystallization: take out the product MCM-22 zeolite structural unit of the first step after cooling, about 6 grams, and stir for 30 minutes. Under the condition of 50~60℃, dissolve 5.1024g CTAB in 21.46mL distilled water and add 4.988mL 4.01mol.L -1 NaOH solution. Add it dropwise to the MCM-22 zeolite structure precursor ...

example 2

[0011] The synthesis of example 2 MM (15)

[0012] The first step of crystallization: 3.50mL hexamethyleneimine (HMI), 0.762g NaAlO 2 Mix with 16mL of water, slowly drop 24g (25wt%) silica sol into the mixture under strong stirring, the molar ratio of the material is SiO 2 : 0.033Al 2 o 3 :0.30HMI:20H 2 O. Stir continuously for another 1-2 hours, put it into a stainless steel reaction kettle with polytetrafluoroethylene lining, and crystallize at 150°C under rotation (120 revolutions / min) for 22-24 hours. After cooling to room temperature, the product was taken out to obtain the precursor of MCM-22 zeolite structure.

[0013] The second step of crystallization: take out the product MCM-22 zeolite structural unit of the first step after cooling, about 6 grams, and stir for 30 minutes. Under the condition of 50~60℃, dissolve 5.1024g CTAB in 24mL distilled water and add 4.988mL 4.01mol.L -1 NaOH solution. Add it dropwise to the MCM-22 zeolite structure precursor under sti...

example 3

[0019] The synthesis of example 3 MM (50)

[0020] The first step of crystallization: 5.60mL hexamethyleneimine (HMI), 0.2287g NaAlO 2Mix with 15mL of water, slowly add 24g (25wt%) silica sol dropwise into the mixture under strong stirring, the molar ratio of the material is SiO 2 : 0.01Al 2 o 3 :0.40HMI:19H 2 O. Stir continuously for another 1-2 hours, put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallize at 140°C for 24 hours while rotating (120 revolutions / min). After cooling to room temperature, the product was taken out to obtain the precursor of MCM-22 zeolite structure.

[0021] The second step of crystallization: take out about 6 grams of the product of the first step after cooling, and stir for 30 minutes. Dissolve 6.37g of CTAB in 30.5mL of distilled water at 50-60°C. Add it dropwise to the MCM-22 zeolite structure precursor under stirring, and then continue to stir for 1 to 2 hours and then put it into the reactor. ...

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Abstract

The invention relates to a synthetic method adopting an MCM-22 zeolite structure precursor to compound a mesopore material MM(x). The synthetic method of the invention is a two-step crystallized synthetic method. On the basis of synthetizing an MCM-22 zeolite structure unit body, a cetyltrimethylammonium bromide (CTAB) solution with a certain concentration is utilized to transform the MCM-22 zeolite structure unit body to a mesopore material, and the structure is similar to an MCM-41 mesopore molecular sieve. After exchange processing into a hydrogen form, the MCM-22 zeolite structure unit body becomes the mesopore material with stronger acid site. In alkylation of cumene cracking, 2,4 di-tert-butylphenol and tertiary butyl alcohol, the catalytic activity of samples prepared is higher than that of the MCM-41 which is synthetized by a conventional method, thereby indicating that the mesopore material synthetized by the MCM-22 zeolite structure unit body has better application prospect for giant molecule acid catalytic reactions.

Description

technical field [0001] The invention relates to a preparation method of a mesoporous material, in particular to a method for synthesizing a mesoporous material with an MCM-22 zeolite structure precursor. Background technique [0002] The synthesis of mesoporous molecular sieves has broadened the pore size range of the original microporous molecular sieves, and has become a new milestone in the field of porous materials research. Mesoporous molecular sieves have a large specific surface, adjustable pore size and good thermal stability, which lays the foundation for their application in the field of materials and catalysis. Similar to microporous zeolite molecular sieves, conventional silica-alumina mesoporous molecular sieves also have certain acidity, but because the molecular sieve framework is in an amorphous state, its acid strength is much lower than that of microporous zeolite molecular sieves with a crystal framework structure, which is equivalent to amorphous The aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 李工佟惠娟
Owner JIANGSU POLYTECHNIC UNIVERSITY