External surface modification method of microporous molecular sieve

A technology of microporous molecular sieve and molecular sieve, which is applied in the field of surface modification of microporous molecular sieve, can solve the problem of high cost, achieve the effects of controlling acidity, increasing the ratio of silicon to aluminum, and simple operation

Active Publication Date: 2012-11-28
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses organosilicon compounds dissolved in organic solvents, and the cost is relatively high
In addition, the flammability of organic solvents and potential safety hazards are also an aspect worth improving

Method used

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  • External surface modification method of microporous molecular sieve
  • External surface modification method of microporous molecular sieve
  • External surface modification method of microporous molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] At 30°C, 30g of commercially available alkaline silica sol (Beijing Xingdaxin Special Materials Co., Ltd., SiO 2 The content is 30wt%) and 90g deionized water in the beaker and mix uniformly, then add the ZSM-5 molecular sieve of 15g Na type under stirring (surface silicon aluminum ratio is 18, purchased from Beijing Bowen Kefeng Technology Development Co., Ltd. ), continue to stir for 4h, stop stirring, stand still at room temperature for 24h, filter, dry at 120°C for 12h, and roast at 540°C for 4h to obtain ZSM-5 molecular sieve with external surface modification, marked as SLD-1. X-ray diffraction (XRD, see figure 1 ) Determination, its phase belongs to ZSM-5 molecular sieve.

Embodiment 2

[0035] At 20°C, 20g of commercially available alkaline silica sol (Beijing Xingdaxin Special Materials Co., Ltd., SiO 2 The content is 30wt%) and 106g deionized water in a beaker and mix evenly, then add the ZSM-5 molecular sieve of 20g Na type under stirring (surface silicon aluminum ratio is 113, purchased from Beijing Bowen Kefeng Technology Development Co., Ltd. ), continue to stir for 4h, stop stirring, stand still at 20°C for 24h, filter, dry at 120°C for 12h, and roast at 540°C for 2h to obtain ZSM-5 molecular sieve with external surface modification, marked as SLD-2. As determined by X-ray diffraction (XRD), its phase belongs to ZSM-5 molecular sieve.

Embodiment 3

[0037] At 35°C, 7.5g of commercially available alkaline silica sol (Beijing Xingdaxin Special Materials Co., Ltd., SiO 2 content is 30wt%) and 84.75g deionized water are mixed evenly, then add the ZSM-5 molecular sieve of 15g Na type (surface silicon aluminum ratio is 88, purchased from Beijing Bowen Kefeng Technology Development Co., Ltd.), stir 4h, stop Stir, stand still at 35°C for 24h, filter, dry at 120°C for 12h, and calcinate at 500°C for 4h to obtain ZSM-5 molecular sieve with modified outer surface, marked as SLD-3. As determined by X-ray diffraction (XRD), its phase belongs to ZSM-5 molecular sieve.

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Abstract

The invention provides an external surface modification method of a microporous molecular sieve, which comprises the following steps: mixing silicasol and a microporous molecular sieve, carrying out liquid deposition to initiate physical adsorption between the molecular sieve and the silicasol, filtering, drying and roasting to prepare the external-surface-modified microporous molecular sieve. In the invention, colloidal particles of the silicasol are larger than pores of the selected molecular sieve, thereby preventing the colloidal particles from entering the inside of the pores; and when the silicasol particles are adsorbed onto the external surface of the molecular sieve, drying and roasting are utilized to remove water in the colloidal particles, so that the colloidal particles are firmly attached onto the external surface of the molecular sieve. The XPS (X-ray photoelectron spectroscopy) measurement indicates that the modified molecular sieve has obviously higher surface phase silica-alumina ratio than the un-modified molecular sieve. The improved Hammett tracer method measurement on the acid quantity of the external surface of the molecular sieve before and after modification proves that the modified molecular sieve has lower acid quantity on the external surface.

Description

technical field [0001] The invention relates to a method for modifying the outer surface of a microporous molecular sieve, in particular to a method for preparing a microporous molecular sieve whose outer surface has been modified by using silica sol as a raw material, through liquid phase deposition, and taking physical adsorption as the main process. It also relates to the microporous molecular sieve with modified outer surface prepared according to the method and its application as an active component of catalytic cracking catalyst. Background technique [0002] At present, most of the microporous silica-alumina molecular sieves (zeolites) prepared including ZSM-5 molecular sieves have the characteristics of rich aluminum on the surface, that is, the distribution of silica-alumina in the molecular sieve crystal grains is uneven, and the surface-phase silica-alumina ratio (referred to in the present invention) The silicon-aluminum ratio refers to SiO 2 / Al 2 o 3 oxide m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J29/85C10G11/05
Inventor 申宝剑李德富高雄厚王宝杰王双刘宏海赵红娟申波俊
Owner BC P INC CHINA NAT PETROLEUM CORP
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