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Preparation method of high-thermal-stability STW type germanosilicate molecular sieve

A high thermal stability, germanosilicate technology, applied in crystalline aluminosilicate zeolite and other directions, can solve the problems of expensive raw materials, easy collapse of skeleton structure, difficult synthesis of ionic liquids, etc., and achieves improved thermal stability and simple synthesis method. Effect

Inactive Publication Date: 2014-12-17
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the synthesis of silicon germanate molecular sieve SU-32, the obtained STW structure is unstable, and the skeleton structure is easy to collapse. In addition, another phase of Beta molecular sieve (β molecular sieve) SU-15 is formed during the synthesis. The two structures compete with each other. Unable to get STW pure phase
In the synthesis of HPM-1, although the STW structure of pure silicon has been obtained and has high thermal stability, the ionic liquid used in the structure synthesis is not easy to synthesize, and the synthetic structure directing agent is not only expensive in raw materials, but also long synthesis time

Method used

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  • Preparation method of high-thermal-stability STW type germanosilicate molecular sieve
  • Preparation method of high-thermal-stability STW type germanosilicate molecular sieve
  • Preparation method of high-thermal-stability STW type germanosilicate molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of high thermal stability STW type germanosilicate molecular sieve, take N,N-diethylethylenediamine as template agent and solvent, F - As a mineralizer, the STW topology molecular sieve is synthesized under hydrothermal conditions, and the steps are as follows:

[0026] (1) Add 2.46g OSDA (organic structure directing agent) N,N diethylethylenediamine and 0.12g water into a 50ml beaker, add 0.1g germanium dioxide (GeO 2 ) After mixing well for 2h, add 0.149g tetraethyl orthosilicate Si(OC 2 h 5 ) 4 , stirred for 15 minutes, added 0.17g HF and stirred for 20 minutes to obtain a precursor mixture of molecular sieves;

[0027] (2) Transfer the precursor mixture into a 25ml high-pressure stainless steel reactor, crystallize at 170°C for 7 days, and cool to room temperature;

[0028] (3) washing and drying the product to obtain STW type germanosilicate molecular sieve with high thermal stability.

[0029] Such as figure 1 , figure 2 As sho...

Embodiment 2

[0031] A kind of preparation method of high thermal stability STW type germanosilicate molecular sieve, take N,N-diethylethylenediamine as template agent and solvent, F - As a mineralizer, the STW topology molecular sieve is synthesized under hydrothermal conditions, and the steps are as follows:

[0032] (1) Add 7.38g OSDA (organic structure directing agent) N,N diethylethylenediamine and 0.18g water in a 50ml beaker, add 0.15g germanium dioxide (GeO 2 ) After mixing well for 2h, add 0.223g tetraethyl orthosilicate Si(OC 2 h 5 ) 4 , stirred for 20 minutes, added 0.246g HF and stirred for 20 minutes to obtain a precursor mixture of molecular sieves;

[0033] (2) Transfer the precursor mixture into a 25ml high-pressure stainless steel reactor, crystallize at 150°C for 9 days, and cool to room temperature;

[0034] (3) washing and drying the product to obtain STW type germanosilicate molecular sieve with high thermal stability.

Embodiment 3

[0036] A kind of preparation method of high thermal stability STW type germanosilicate molecular sieve, take N,N-diethylethylenediamine as template agent and solvent, F - As a mineralizer, the STW topology molecular sieve is synthesized under hydrothermal conditions, and the steps are as follows:

[0037] (1) Add 2.46g OSDA (organic structure directing agent) N,N diethylethylenediamine and 0.4g water into a 50ml beaker, add 0.1g germanium dioxide (GeO 2 ) After mixing well for 2h, add 0.149g tetraethyl orthosilicate Si(OC 2 h 5 ) 4 , stirred for 15 minutes, added 0.17g HF and stirred for 20 minutes to obtain a precursor mixture of molecular sieves;

[0038] (2) Transfer the precursor mixture into a 25ml high-pressure stainless steel reactor, crystallize at 200°C for 7 days, and cool to room temperature;

[0039] (3) The product is washed and dried to obtain a STW type germanosilicate molecular sieve with high thermal stability.

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Abstract

The invention discloses a preparation method of a high-thermal-stability STW type germanosilicate molecular sieve. The preparation method comprises the following steps: (1), uniformly mixing OSDA: N, N-diethyl ethylenediamine, water and GeO2, and then adding Si(OC2H5)4, stirring the mixture for 15-25 minutes, and adding HF into the mixture to prepare a precursor mixture of the molecular sieve, wherein the molar ratio of the raw materials of GeO2 to Si(OC2H5)4 to OSDA to H2O to HF is equal to 1 to 0.8 to 43.4 to (6-24) to 3; (2), filling the precursor mixture prepared in the step (1) into a high-pressure reaction kettle, crystallizing for 7-9 days at 150-200 DEG C, and cooling to the room temperature; and (3), washing and drying the cooled products to obtain the high-thermal-stability STW type germanosilicate molecular sieve. The preparation method can be used for obtaining a pure phase of the STW type germanosilicate molecular sieve, increasing a silicon-germanium (Si / Ge) ratio (molar ratio) of the STW type germanosilicate molecular sieve to 1.25 and improving the thermal stability to 800 DEG C; and moreover, the preparation method is simple.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve inorganic materials, and in particular relates to a preparation method of STW type germanosilicate molecular sieve with high thermal stability. Background technique [0002] Zeolite molecular sieve is a kind of porous material, which generally has unique properties such as high specific surface area, high porosity and open structure, and can be widely used in various fields, such as industrial catalysis, adsorbent, environmental treatment, Various carriers and ion exchangers, etc. [0003] Silicate has excellent thermal stability, germanate structure is not stable, but germanate has a special germanium cluster structure, easy to form Ge 5 Cluster, Ge 7 Cluster, Ge 8 Cluster, Ge 9 Cluster and Ge 10 Clusters, etc., can synthesize germanate open framework compounds with novel topological structures. Since germanium and silicon have many different properties, compared with the four-coord...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 石磊张娜
Owner QILU UNIV OF TECH