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Microwave synthesis process for ZSM-11 molecular sieve

A technology of ZSM-11 and microwave synthesis, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., to achieve the effect of high crystallinity, pure crystal phase and controllable particle size

Inactive Publication Date: 2009-09-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, various pentasil series molecular sieves and molecular sieve membranes such as ZSM-5, TS-1, TS-2, silicalite-1, and silicalite-2 have been successfully obtained through microwave radiation crystallization and microwave-assisted synthesis, and ZSM-11 The direct microwave radiation synthesis has not been reported so far

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  • Microwave synthesis process for ZSM-11 molecular sieve
  • Microwave synthesis process for ZSM-11 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 15g silica sol (SiO 2 25.59 wt%, Na 2 O 0.31wt%, Al 2 o 3 0.10wt%, H 2 (273.99wt%, other 0.01wt%, hereinafter the same), 3.22g tetrabutylammonium bromide (99%), 10.4g deionized water add in the reactor and mix homogeneously, the mol ratio that obtains reaction mixture is: 12 Na 2 O: Al 2 o 3 : 80 SiO 2 : 15 TBABr: 3600 H 2 O (no seed crystals, the same below), under continuous stirring, add a uniform solution prepared by 0.43g aluminum sulfate, 0.74g sodium hydroxide and 20g deionized water, and then add 0.20g ZSM-11 seed crystals (accounting for raw silicon 5% of the total mass of aluminum oxide) was added into 10 g of deionized water for ultrasonic dispersion, and then the above-mentioned raw material mixture was added, and the stirring was continued until the mixture was uniform. Seal the reaction kettle, place it in a hydrothermal synthesis oven, and dynamically synthesize it by rotating the kettle body (100 rpm). After aging for 48 hours at room temperatu...

Embodiment 2

[0022] In Example 1, the amount of seed crystals added was changed to 0.04 g (accounting for 1% of the total mass of the raw material silicon-aluminum oxide), and the composition of other raw materials remained unchanged. The raw materials were mixed evenly, without aging, directly placed into a microwave synthesis reactor, and crystallized at 170°C for 6 hours. The product was ZSM-11 molecular sieve with a crystallinity of 79.2% and a particle size of 2.11 μm.

Embodiment 3

[0024] In Example 1, the raw materials and composition were unchanged. After the raw material mixture is evenly mixed, the kettle body is rotated (100rpm) at room temperature for aging for 9 days, transferred to a microwave synthesis reactor, and crystallized at 170°C for 2h. The product is ZSM-11 molecular sieve with a crystallinity of 99.7% and a particle size of 0.82μm .

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Abstract

The invention relates to a microwave synthesis process for a ZSM-11 molecular sieve. The process uses aluminum source, alkali source, silicon source, tetrabutylammonium bromide and de-ionized water as the raw materials and adopts the heating mode of microwave radiation. The reaction mixture is crystallized for 1 to 8 hours under microwave radiation and self-generated pressure at 130 to 180 DEG C, solid is separated from the mother liquid, and then the product is washed by the de-ionized water until the pH value is 8 to 9, thus obtaining the raw powder of the ZSM-11 molecular sieve. The microwave synthesis process for the ZSM-11 molecular sieve has the advantages of replacing traditional water heating by microwave radiation heating and obtaining the ZSM-11 molecular sieve with the advantages of high crystallinity, pure crystal phase and controllable and wide range of grain size, and the process accelerates the nucleation rate and crystal growth speed obviously and shortens the crystallization time greatly by pre-placing crystal seeds.

Description

technical field [0001] The invention relates to a new microwave synthesis route of ZSM-11 molecular sieve, in particular, it provides a microwave synthesis process of ZSM-11 molecular sieve. Background technique [0002] The silicon-oxygen tetrahedron in the Pentasil molecular sieve framework is connected into a special structural unit, which is composed of 8 five-membered rings. This structure is connected into a chain through a shared edge, and then connected into a sheet. The sheet structure adopts different connection methods (symmetry center correlation and mirror correlation), and two structural configurations of MFI and MEL can be obtained respectively. Pentasil molecular sieves have different names according to their elemental composition. Among them, silicon aluminum is called ZSM-5 (MFI) and ZSM-11 (MEL), and all silicon is called silicalite-1 (MFI) and silicalite-2 (MEL). ), commonly known as TS-1 (MFI) and TS-2 (MEL) of titanium silicon. [0003] ZSM-11 molecul...

Claims

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Application Information

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IPC IPC(8): C01B39/36
Inventor 徐龙伢张玲刘会娟谢素娟刘盛林
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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