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Preparation method of ZSM-5 molecular sieve

A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of low solid phase content of hydrothermal slurry, poor product quality and high product yield. Low-level problems, to achieve the effect of shortening the crystallization reaction time, high single-pot yield, and a wide range of sources

Active Publication Date: 2015-08-19
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] It is generally believed in the prior art that the continuous medium is an essential conduction medium for the transfer of matter and energy. Therefore, most of the crystallization processes of existing ZSM-5 molecular sieves are hydrothermal crystallization, but the preparation period of hydrothermal crystallization is relatively long. , the solid phase content in the hydrothermal slurry is low, the product yield is low, and a large amount of waste liquid containing organic templates will be generated.
[0013] In the prior art, when synthetic raw materials are used to prepare high-crystallinity ZSM-5 molecular sieves, the process is relatively complicated, the yield is low, and the amount of waste liquid is huge; and when natural aluminosilicates are used as the composite silicon-aluminum source, the quality of the obtained products is poor , the cycle is longer

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Examples

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Embodiment 1

[0064] A kind of preparation method of ZSM-5 molecular sieve, described method is silicon-aluminum source with amorphous silicon dioxide and boehmite, specifically comprises the following steps:

[0065] (1) Homogenization of ingredients: Mix amorphous silica, boehmite, NaOH, tetrabutylammonium hydroxide (TBAOH) and H 2 O mixed and homogenized to obtain the ZSM-5 molecular sieve precursor, SiO in the precursor 2 、Al 2 o 3 , NaOH, TBAOH, H 2 The ratio of the amount of substance of O is 100:25:19:1.6:300;

[0066] (2) Solid-phase thermal crystallization: the ZSM-5 molecular sieve precursor obtained in step (1) was placed in a closed reaction kettle, and the temperature was raised to 130°C for solid-phase thermal crystallization for 0.5h to obtain a crystallized product;

[0067] (3) Washing and drying the crystallized product obtained in step (2) twice with water to obtain nano ZSM-5 molecular sieves. The particle size of ZSM-5 obtained in this example is about 10-30 nm, an...

Embodiment 2

[0069] A kind of preparation method of ZSM-5 molecular sieve, described method is silicon-aluminum source with fumed silica and aluminum sulfate, specifically comprises the following steps:

[0070] (1) Homogenization of ingredients: Mix fumed silica, aluminum sulfate, sodium hydroxide, triethylamine (TEN) and water, grind and homogenize with a mortar to obtain a ZSM-5 molecular sieve precursor, the precursor Medium SiO 2 、Al 2 o 3 , NaOH, TEN, H 2 The ratio of the amount of substance of O is 100:1:15:18:300;

[0071] (2) Solid-phase thermal crystallization: the ZSM-5 molecular sieve precursor obtained in step (1) was placed in a closed reaction kettle, and the temperature was raised to 210°C for solid-phase thermal crystallization for 3 hours to obtain a crystallized product;

[0072] (3) Washing the crystallized product obtained in step (2) three times with water, and drying to obtain nano ZSM-5 molecular sieve.

[0073] The particle size of ZSM-5 obtained in this examp...

Embodiment 3

[0077] A kind of preparation method of nano ZSM-5 molecular sieve, described method is silicon-aluminum source with white carbon black and aluminum hydroxide, specifically comprises the following steps:

[0078](1) Homogenization of ingredients: Mix white carbon black, aluminum hydroxide, sodium hydroxide, TBAOH and water, and use a mixer to homogenize to obtain a ZSM-5 molecular sieve precursor. The SiO in the precursor 2 、Al 2 o 3 , NaOH, TBAOH and H 2 The ratio of the amount of substance of O is 100:3.6:14:1.9:80;

[0079] (2) Solid-state thermal crystallization: The ZSM-5 molecular sieve precursor obtained in step (1) was placed in a closed reaction kettle, and the temperature was raised to 160°C for solid-state thermal crystallization for 10 hours to obtain a crystallized product.

[0080] (3) Washing the crystallized product obtained in step (2) with water four times, and drying to obtain nano ZSM-5 molecular sieve.

[0081] The particle size of ZSM-5 obtained in thi...

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Abstract

The invention relates to a preparation method of a ZSM-5 molecular sieve. The method comprises performing solid-phase thermal crystallization of a ZSM-5 molecular sieve precursor to obtain a sodium-type ZSM-5 molecular sieve. The preparation method of the ZSM-5 molecular sieve is high in reaction speed and short in crystallization time, is high in single-reactor yield and production efficiency, and is not limited by silicon-aluminum sources. According to the invention, the prepared ZSM-5 molecular sieve has advantages of nanoscale, high crystallization degree, and excellent physical and chemical performance.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 molecular sieve, and further relates to a preparation method of nanometer or submicron ZSM-5 molecular sieve. Background technique [0002] ZSM-5 molecular sieve was first reported by Mobil in 1972. It is a five-membered ring zeolite. Its basic structural unit is composed of 8 five-membered rings. This basic structural unit is connected into a chain structure through oxygen bridges, and then Surrounded by a zeolite framework, it has a two-dimensional 10×10 ring channel structure (0.56nm×0.53nm and 0.55nm×0.51nm). ZSM-5 zeolite has become an important catalytic material due to its unique pore structure and acidity, and has been widely used in organic catalytic reactions. ZSM-5 zeolite with small grain size shows good catalytic performance in catalytic reaction, therefore, it is necessary to develop small grain size ZSM-5 zeolite especially with nanometer size. [0003] At present, the preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
Inventor 卢旭晨潘锋王体壮
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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