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Preparation method of open macroporous Beta molecular sieve

A molecular sieve, open technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as the preparation method of open large-pore Beta molecular sieves, etc.

Pending Publication Date: 2020-04-17
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many patents for post-processing or special templates to assist in the preparation of hierarchically porous Beta molecular sieves, but there is no preparation method for open macroporous Beta molecular sieves

Method used

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  • Preparation method of open macroporous Beta molecular sieve
  • Preparation method of open macroporous Beta molecular sieve
  • Preparation method of open macroporous Beta molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of open macropore Beta molecular sieve, comprises the following steps:

[0027] Mix deionized water, aluminum oxide, sodium hydroxide, tetraethylammonium hydroxide (R), cetyltrimethylammonium bromide (X), tetraethyl orthosilicate and seed crystals and transfer to crystal Crystallization in the kettle. The molar ratio of each component in the gel is: SiO 2 :Al 2 o 3 :Na 2 O:TEAOH:X:H 2 O=1:0.03:0.3:0.2:0.001:15. The added mass of seed crystal accounts for 8% of the silica mass in the gel. Rapidly raise the temperature to 160°C with a heating rate of 5°C / min, adjust the back pressure valve to a pressure of 0.3MPa, and keep the temperature constant for 24h. After the crystallization is completed, pass low-temperature cooling water into the crystallization solution at a cooling rate of -4°C / min. After cooling down to room temperature, the crystallized product is separated, washed, dried and calcined to obtain Beta molecular sieve, which ...

Embodiment 2

[0029] A kind of preparation method of open macropore Beta molecular sieve, comprises the following steps:

[0030] Mix deionized water, aluminum isopropoxide, sodium hydroxide, tetraethylammonium bromide (R), ammonium bicarbonate (X), water glass and seed crystals evenly, then transfer to a crystallization tank for crystallization. The molar ratio of each component in the gel is: SiO 2 :Al 2 o 3 :Na 2 O:TEAOH:X:H 2 O=1:0.01:0.05:0.1:0.1:1. The added mass of seed crystal accounts for 7% of the silica mass in the gel. Rapidly raise the temperature to 170°C with a heating rate of 6°C / min, adjust the back pressure valve to a pressure of 0.35MPa, and keep the temperature constant for 12h. After the crystallization is completed, pass low-temperature cooling water into the crystallization solution at a cooling rate of -4°C / min. After cooling down to room temperature, the crystallized product is separated, washed, dried, and calcined to obtain a Beta molecular sieve, which is ...

Embodiment 3

[0033] A kind of preparation method of open macropore Beta molecular sieve, comprises the following steps:

[0034] Mix deionized water, aluminum hydroxide, sodium hydroxide, tetraethylammonium hydroxide (R), isopropanol (X), silica gel and seed crystals evenly and transfer them to a crystallization kettle for crystallization. The molar ratio of each component in the gel is: SiO 2 :Al 2 o 3 :Na 2 O:TEAOH:X:H 2 O=1:0.1:0.1:0.3:0.05:30. The added mass of seed crystal accounts for 9% of the silica mass in the gel. Rapidly raise the temperature to 150°C with a heating rate of 4°C / min, adjust the back pressure valve to a pressure of 0.25MPa, and keep the temperature constant for 36h. After the crystallization is completed, pass low-temperature cooling water into the crystallization solution at a cooling rate of -3°C / min. After cooling down to room temperature, the crystallized product is separated, washed, dried, and calcined to obtain a Beta molecular sieve, which is design...

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Abstract

The invention relates to a preparation method of an open macroporous Beta molecular sieve, belonging to the field of molecular sieve catalyst preparation. The preparation method comprises the following steps: a) uniformly mixing deionized water, an aluminum source, an alkali source, a template agent, a filler, a silicon source and a seed crystal, and transferring the obtained mixture into a crystallization kettle for crystallization; b) conducting crystallization for 6-72 hours at 140-180 DEG C, wherein a heating rate is not lower than 2 DEG C / min and not higher than 10 DEG C / min; c) when a pressure in the kettle is increased to 0.2-0.4 MPa, starting to release pressure to recover amine and water vapor, wherein the pressure in the kettle is maintained at 0.2-0.4 MPa in the crystallizationprocess; and d) after the crystallization is finished, rapidly cooling product slurry, and separating, washing, drying and roasting a crystallized product to obtain the open macroporous Beta molecularsieve. The molecular sieve has excellent hydrothermal stability and relatively high crystallinity. Compared with a macroporous or hierarchical-pore Beta molecular sieve prepared by using a post-treatment method, the method has the characteristics of simple process, high raw material utilization rate and high product yield.

Description

technical field [0001] The invention relates to a preparation method of an open macroporous Beta molecular sieve, belonging to the field of preparation of molecular sieve catalysts. Background technique [0002] Beta molecular sieves are molecular sieves with a twelve-membered ring three-dimensional pore structure. Due to its high hydrothermal stability, good shape selectivity and acidity, Beta molecular sieves can be used in hydroisomerization, hydrocracking, cumene from benzene and propylene, alkylation of aromatics, disproportionation of toluene, etc. showed excellent catalytic performance (CN 106430230A). In the catalytic process of molecular sieves, in addition to acidic factors, diffusion limitation is the main reason for the deactivation of molecular sieve catalysts. In order to solve the diffusion problem, researchers try to micronize and nanosize molecular sieves, and reduce the particle size of molecular sieves as much as possible. However, the solid-liquid sepa...

Claims

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Application Information

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IPC IPC(8): C01B39/48
CPCC01B39/48C01P2006/12C01P2006/14C01P2006/16
Inventor 王龙陈文勇苗植平彭立石倩翡周泳冰冯春晓郭淄龙
Owner SHANDONG QILU HUAXIN HIGH TECH
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