Mordenite and preparation method thereof

A technology of mordenite and zeolite, which is applied in the direction of mordenite crystalline aluminosilicate zeolite, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problem of little research on mordenite grain morphology, harsh synthesis conditions, and unfavorable environment Protection and other issues, to achieve the effect of eliminating dislocations and lattice defects, high selectivity of isomerization activity, and improving catalytic performance

Inactive Publication Date: 2011-05-18
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Abstract
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  • Claims
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Problems solved by technology

[0009] Chinese patent 200510023802.5 (publication number CN 1673081A) discloses a synthesis method of high-silicon mordenite, which provides a method for preparing high-silicon mordenite in an all-inorganic system by vapor phase spin crystallization (vapor phase transport method, namely VPT) , the method does not use organic templates and fluorides, and the silicon-aluminum ratio of the synthesized mordenite is SiO 2 /Al 2 o 3 =20-40, but the synthesis conditions of this method are harsh and difficult for industrialization
[0016] Throughout various public documents, it can be found that the research on molecular sieve materials including mordenite has attracted great attention in this field. In order to improve the catalytic performance of these molecular sieves, especially mordenite,

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  • Mordenite and preparation method thereof

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Embodiment 1

[0050] First, 0.5g of sodium hydroxide (96%) was added to a certain amount of deionized water and mixed uniformly to obtain a sodium hydroxide solution, to which 5g of silica-alumina microspheres (commercially purchased) were added, stirred for 2 hours and mixed uniformly to obtain an initial gel Glue mixture, which is placed in a closed reaction kettle to prepare for crystallization, the molar composition of the crystallization reaction system is:

[0051] Na 2 O: SiO 2 : Al 2 o 3 :H 2 O=1.3:10:1:67

[0052] The crystallization reaction material is self-pressurized and crystallized in a closed reaction kettle. First, the first-stage crystallization reaction is carried out at a controlled temperature of 80°C. Crystallization takes 8 hours to form zeolite microcrystals, and then the temperature is raised to 180°C to continue crystallization for 24 hours. After the reaction, the product was filtered, washed, dried, and calcined at 550° C. for 5 hours in an air atmosphere to...

Embodiment 2

[0060] At first the sodium hydroxide (96%) of 0.65g is joined into a certain amount of deionized water and mixed uniformly to form a sodium hydroxide solution, add 5g of silica-alumina microspheres, stir for 2 hours, then add 1.5g of white carbon black, Continue to stir evenly to form an initial gel mixture, and place it in a closed reaction kettle for crystallization: carry out the first stage of crystallization at 90°C, crystallize for 6 hours to form zeolite microcrystals, and then heat up to 170°C for crystallization for 48 hours . The molar composition of this crystallization reaction system is:

[0061] Na 2 O: SiO 2 :Al 2 o 3 :H 2 O=0.85:20:1:67

[0062] After the reaction, the product was filtered, washed, dried, and calcined to obtain a mordenite molecular sieve sample 2 with a special structure and morphology of high silicon. The morphology of the sample was similar to Example 1.

[0063] Catalytic reaction results: ethylbenzene conversion rate 20%, p-xylene ...

Embodiment 3

[0065] First, 0.6g of sodium hydroxide (96%) is added to a certain amount of deionized water and mixed uniformly to form a sodium hydroxide solution, and 5g of silicon-aluminum microspheres are added, stirred evenly and then placed in a closed reaction kettle for crystallization. The molar composition of this crystallization reaction system is:

[0066] Na 2 O: SiO 2 : Al 2 o 3 :H 2 O=1.6:10:1:65

[0067] After crystallization at 60° C. for 10 hours, after cooling, 2.10 g of tetrapropylammonium bromide (TPABr) was added and stirred evenly, and then the temperature was raised to 200° C. for crystallization for 24 hours. After the reaction, the product was filtered, washed, and dried to obtain a mordenite molecular sieve sample 3 with a special structure and morphology with a grain size of about 5-7 μm. See details image 3 . Such as image 3 The SEM photo shows that this sample 3 is a uniform ellipsoid grain (a), in which each small grain is formed by many strip crysta...

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Abstract

The invention provides mordenite and a preparation method thereof. The mordenite has an ellipsoidal structural topography formed by stacking a plurality of strip zeolite crystals in the one-dimensional direction in order; and the method for preparing the mordenite with the special structural topography comprises that: a solid silicon-aluminum source raw material is subjected to two-stage crystallization reaction in an extremely thick system, the molar ratio of water to silicon dioxide in the crystallization system is 1-7, the structural topography of the obtained mordenite is obviously difference from that of the conventional product by optimizing and controlling synthesis process and condition parameters, and mesopores and macropores are introduced into the mordenite structure to contribute to solving the problems of dislocation and surface defects of the mordenite structure and better contribute to improving the catalytic performance in xylene isomerization reaction. The invention also provides application of the mordenite with the special structural topography to catalysis in the xylene isomerization reaction.

Description

technical field [0001] The invention relates to the technical field of preparation of zeolite molecular sieves, and in particular provides a mordenite with special structure and morphology and a preparation method thereof. Background technique [0002] About 80% of modern petrochemical processes are related to catalytic processes. The fundamental core technology is the selection and use of catalysts, and the characteristics of catalytic materials themselves are the key to determining their catalytic performance. At present, a consensus has been reached in the field of petroleum processing and catalyst technology that as crude oil becomes increasingly heavy, the conversion of heavy oil macromolecules requires catalysts to provide abundant macropores or even ultra-macropore systems to adapt to the catalytic cracking of larger molecules At the same time, further shape-selective catalysis of catalytic cracking molecules is required, which requires the catalyst to provide a pore ...

Claims

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Application Information

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IPC IPC(8): C01B39/26B01J29/18B01J32/00C07C5/27C07C15/08
CPCY02P20/52
Inventor 巩雁军窦涛刘素燕
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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