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Preparation method of MCM-22 (Multiple Chip Module 22)/silicon-oxide compound

A technology of MCM-22 and silicon oxide, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc., can solve the problems of low mechanical strength, low production efficiency, and difficult interconnection, etc., and achieve low price, The effect of simple reaction conditions and mature technology

Active Publication Date: 2012-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, a common key disadvantage of this type of 3DOM materials is that their mechanical strength is very low and the preparation efficiency is very low.
However, in this patent, carbon particles are physically dispersed in the microporous molecular sieve precursor as a porogen, and the mesopores or macropores of the prepared multi-stage molecular sieve are difficult to communicate with each other.

Method used

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  • Preparation method of MCM-22 (Multiple Chip Module 22)/silicon-oxide compound
  • Preparation method of MCM-22 (Multiple Chip Module 22)/silicon-oxide compound
  • Preparation method of MCM-22 (Multiple Chip Module 22)/silicon-oxide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Synthesis of MCM-22 molecular sieves. Add silica sol, sodium hydroxide, sodium aluminate, and hexamethyleneimine (HMI) into the beaker in a certain proportion and order, and the reaction mixture consists of n(SiO 2 ):n(Al 2 o 3 ):n(HMI):n(NaOH):n(H 2 (0)=1: 0.04: 0.12: 0.35: 20, stir evenly and pack into a 500mL dynamic stainless steel reactor. The stirring speed was 100 rpm, the reaction temperature was 170° C., and the crystallization time was 62 hours. After the reaction, the samples were taken out, washed repeatedly, and filtered with suction until the pH of the washing liquid was close to 7. Put the filtered white paste product in an oven at 100°C and dry it for 24 hours to obtain the MCM-22 precursor. The precursor was then placed in a muffle furnace at a heating rate of 2°C / min, and calcined at 550°C for 6 hours in an air atmosphere to remove the template agent to obtain the MCM-22 molecular sieve.

Embodiment 2-4

[0034] Synthesis of MCM-22 / silica complexes. First, 10 g of the MCM-22 molecular sieve prepared in Example 1 was uniformly dispersed in 100 g of distilled water, then 1 g of phenol was added to the suspension under stirring, and after stirring for 30 minutes, 1.5 g of phenol was added to the mixture Containing 5% sodium hydroxide and 25% tetraethylammonium hydroxide aqueous solution, stir well and then add 10 grams of tetraethyl orthosilicate (TEOS), then add dropwise the equivalent of phenol molar amount in the mixed solution 2 times the formaldehyde. After stirring evenly, the temperature was slowly raised to 75°C under continuous stirring until a thick gel was formed; after the gel was aged at 75°C for 24 hours, it was transferred to an autoclave for hydrothermal treatment at 130°C for 12 hours. After the hydrothermal reaction, the product was separated, dried, and calcined at 500° C. for 10 hours in an air atmosphere to obtain the MCM-22 / silicon oxide composite, which was...

Embodiment 5-7

[0037] Synthesis of MCM-22 / silica complexes. First, 10 g of MCM-22 molecular sieves prepared in Example 1 were evenly dispersed in distilled water, then 1.2 grams of phenol was added to the suspension under stirring, and after stirring for 30 minutes, 1.5 grams of phenol was added to the mixture. Containing 8% sodium carbonate and 25% tetrapropyl ammonium hydroxide aqueous solution, after stirring evenly, add 8 grams of tetramethyl orthosilicate (TMOS), and then add dropwise the equivalent of phenol molar amount in the mixed solution 1.5 times the formaldehyde. After stirring evenly, the temperature was slowly raised to 80° C. under continuous stirring until a thick gel was formed; the gel was aged at 80° C. for 12 hours, and then dried at 120° C. for 10 hours. Afterwards, transfer to an autoclave for hydrothermal treatment at 180° C. for 24 hours. After the hydrothermal reaction, the product was separated, dried, and calcined at 600° C. for 5 hours in an air atmosphere to o...

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Abstract

The invention discloses a preparation method of an MCM-22 (Multiple Chip Module 22) / silicon-oxide compound. The method comprises the following steps of: in the compounding process of MCM-22 zeolite and silicon oxide, introducing phenol and formaldehyde to be used as the precursors of phenolic resin as an organic pore-forming agent; under the action of a catalyst, subjecting the precursors of the phenolic resin to the cross-linked polymerization reaction to generate the phenolic resin in a three-dimensional network structure to be in homogeneous coexistence with silicon-oxide gel; and then removing the phenolic resin through roasting to prepare the MCM-22 / silicon-oxide compound with a mutually-penetrated three-dimensional mesoporous network. Through the compound prepared with the method disclosed by the invention, the mutually-penetrated mesoporous network enables reactants and an active center to have stronger accessibility and is beneficial to the rapid diffusion of the reactants andproducts.

Description

technical field [0001] The invention relates to a method for preparing a zeolite composition, in particular to a method for preparing an MCM-22 / silicon oxide composite, and belongs to the field of inorganic material preparation. Background technique [0002] According to the classification standard of the International Union of Pure and Applied Chemistry, molecular sieve porous materials are divided into three categories according to the pore size: micropores with a pore size <2nm, mesoporous with a pore size between 2-50nm, and macropores with a pore size >50nm. Material. At present, Y, β, ZSM-5, ZSM-35, L zeolite, mordenite, L zeolite, A-type zeolite, MCM-22 zeolite and SPAO series zeolite are all microporous zeolites that are widely used in industry. These crystalline microporous molecular sieves have played an important role in catalysis, adsorption and separation industries. [0003] However, in the field of petrochemical industry, with the increasingly heavy an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70B01J37/00B01J35/10
Inventor 杨卫亚沈智奇凌凤香王丽华王丽君孙万付
Owner CHINA PETROLEUM & CHEM CORP