Monodisperse mesoporous silica composite zeolite core-shell material and preparation method thereof

A mesoporous silica and composite zeolite technology, applied in chemical instruments and methods, molecular sieve catalysts, fatty acid esterification, etc., can solve problems such as deactivation and small surface pores

Pending Publication Date: 2021-09-14
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to propose a monodisperse mesoporous silica composite zeolite core-shell material and its preparation method, to solve the problems of relatively small surface pores and zeolite dealumination, desiliconization, crystallization and deactivation of prior art materials, Realizing the Free Regulation of the Pore Size of Mesoporous Silica Composite Zeolite Material

Method used

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  • Monodisperse mesoporous silica composite zeolite core-shell material and preparation method thereof
  • Monodisperse mesoporous silica composite zeolite core-shell material and preparation method thereof
  • Monodisperse mesoporous silica composite zeolite core-shell material and preparation method thereof

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Effect test

Embodiment 1

[0035] A monodisperse mesoporous silica composite zeolite core-shell nanosphere material, the core is nano-scale zeolite crystal grains, and the shell is radial-shaped mesoporous channel silica. Prepared by the following method:

[0036] Dissolve 5 g of tetramethylammonium hydroxide and 0.75 g of aluminum isopropoxide in 7 g of water, and then add a pre-prepared aqueous solution of ethyl orthosilicate (2.25 g of ethyl orthosilicate mixed with 2 g of water ), after stirring at room temperature for 5 minutes, add 0.6 g of 1M aqueous sodium hydroxide solution, continue stirring at room temperature for 5 hours, and move to a hydrothermal kettle. Place in an oven at 80°C for 72 hours. After the reaction is finished, it is naturally cooled to room temperature, and washed three times with ethanol and water to obtain LTA-type zeolite grains, which are then dried for use.

[0037] 10 g of cetyltrimethylammonium bromide, 100 mg of LTA zeolite grains and 0.8 mL of triethanolamine were ...

Embodiment 2

[0039] A preparation method of a monodisperse mesoporous silica composite zeolite core-shell nanosphere material, comprising:

[0040] Dissolve 0.63 g of tetrapropylammonium hydroxide and 1.6 g of ethanol completely in 4.2 g of water, then add 1.8 g of tetraethyl orthosilicate to it, stir at room temperature for 24 hours, and move to a hydrothermal kettle. Place in a 90°C oven and heat for 48 hours. After the reaction was completed, it was naturally cooled to room temperature, and washed three times with ethanol and water to obtain MFI zeolite grains with a size of 40 nm, which were redispersed in water for later use.

[0041] Dissolve 8 g of cetyltrimethylammonium chloride, 120 mg of MFI zeolite grains and 0.75 mL of triethanolamine into 150 mL of deionized water successively, and ultrasonically stir evenly to form a pale white homogeneous and transparent aqueous phase solution; Put the solution into the reactor, stir at 80°C for 0.5 hours; take another 1 ml of fumed silica ...

Embodiment 3

[0043] A method for preparing a monodisperse mesoporous silica composite zeolite core-shell nanosphere material, comprising:

[0044] Completely dissolve 8.1 g of tetrapropylammonium hydroxide in 40 g of water, then add 23 g of ethyl orthosilicate therein, stir at room temperature for 3 hours, and move to a hydrothermal kettle. Put it in an oven at 120°C and heat it for 2 hours, then raise the temperature to 170°C and heat it for 24 hours. After the reaction was completed, it was naturally cooled to room temperature, and washed three times with ethanol and water to obtain MFI type zeolite crystal grains with a size of 100 nm, which were dried for later use.

[0045] 2 g of octadecyltrimethylammonium chloride, 20 mg of MFI zeolite grains and 0.5 mL of triethanolamine were successively dissolved in 36 mL of deionized water, and ultrasonically stirred evenly to form a pale white homogeneous and transparent aqueous phase solution; Put the solution into the reactor, and stir at 70...

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Abstract

The invention belongs to the technical field of zeolite molecular sieve catalysts, and particularly relates to a monodisperse mesoporous silica composite zeolite core-shell material and a preparation method thereof. The composite material is characterized in that zeolite crystal grains serving as a core and a silicon dioxide layer constructed on the outer surfaces of the zeolite crystal grains by utilizing an oil-water two-phase layered interface assembly method and has divergent mesoporous channels form a multi-stage grading hole zeolite material with a core-shell structure, the multi-stage grading hole zeolite material comprises inner core zeolite micropores, shell layer mesopores and bulk gap accumulation holes, four quantity levels are reached, the shell layer pore channels are a radially developed gradient mesoporous pore channels, and the material still ensures the high crystal phase and strong acidity of the original zeolite crystal grains. According to the invention, a brand-new synthesis strategy, namely an oil-water two-phase interface assembly method, is adopted, organic amine is adopted for catalytic synthesis, stone grains are prevented from being etched and decomposed in the coating process, the high crystalline phase and strong acidity of original zeolite grains are reserved, and the composite material has quite high applicability when being used as a catalyst for macromolecular catalysis or multi-stage series catalytic reaction.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve catalysts, and in particular relates to a monodisperse mesoporous silica composite zeolite core-shell material and a preparation method thereof. Background technique [0002] Zeolite is an important micro-mesoporous material with the characteristics of high porosity, large specific surface area, stable chemical properties and high acidity. It has an irreplaceable position in chemical catalysis, especially in petroleum refining and petrochemical product synthesis. From the structural point of view, the zeolite structure is mostly based on aluminosilicate, characterized by silicon oxide (SiO 4 ) tetrahedron and alumina (AlO 4 ) Tetrahedral two units to form a network structure, and some zeolites are composed of aluminophosphate; the structure is open, there are many holes and channels connecting the holes in the crystal structure, benefiting from the special hole The porous structu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70B01J29/035B01J35/08B01J35/10B01J35/02C11C3/00
CPCB01J29/70B01J29/035C11C3/003B01J35/1023B01J35/1047B01J35/1061B01J35/023B01J35/0073B01J35/08
Inventor 赵东元洪锦德
Owner FUDAN UNIV
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