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Transition-metal-doped chiral germanium silicate molecular sieve and synthesis method thereof

A germanosilicate and transition metal technology, applied in the field of molecular sieve and its synthesis, can solve the problems of expensive raw materials, long synthesis time, difficult synthesis of ionic liquids, etc., and achieve the effect of simple experimental process

Inactive Publication Date: 2014-11-26
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the synthesis of germanosilicate molecular sieve SU-32, the obtained STW structure is unstable, and the skeleton structure is easy to collapse, and another phase of Beta molecular sieve SU-15 is also generated during the synthesis. The two structures compete with each other, and it is impossible to obtain pure STW. Mutually
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 difficult to synthesize. longer time

Method used

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  • Transition-metal-doped chiral germanium silicate molecular sieve and synthesis method thereof
  • Transition-metal-doped chiral germanium silicate molecular sieve and synthesis method thereof
  • Transition-metal-doped chiral germanium silicate molecular sieve and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Synthesis of transition metal doped chiral germanosilicate molecular sieve Co-STW:

[0020] (1) Add 1.65g OSDA (organic structure directing agent) N,N diethylethylenediamine and 0.1g water into a 50ml beaker, add 0.1g germanium dioxide (GeO 2 ) mixed well for 2h, then added 0.08gCuCl 2 ·5H 2 O or 0.057gCoCl 2 2H 2 O stirred for 1h, then added 0.186g tetraethyl orthosilicate Si (OC 2 h 5 ) 4 , stirred for 15 minutes, and finally added 0.17g HF and stirred for 20 minutes to obtain a precursor mixture of molecular sieves

[0021] (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;

[0022] (3) The product is washed and dried to obtain light blue (Cu-STW) or light pink (Co-STW) powder, that is, pure phase of Cu-STW or Co-STW type germanosilicate molecular sieve.

Embodiment 2

[0024] Synthesis of transition metal doped chiral germanosilicate molecular sieve Cu-STW:

[0025] (1) Add 3.3g OSDA (organic structure directing agent) N,N diethylethylenediamine and 0.4g water into a 50ml beaker, add 0.2g germanium dioxide (GeO 2 ) mixed well for 2h, then added 0.16gCuCl 2 ·5H 2 O or 0.114gCoCl 2 2H 2 O stirred for 1h, then added 0.372g tetraethyl orthosilicate Si(OC 2 h 5 ) 4 , stirred for 20 minutes, and finally added 0.34g HF and stirred for 30 minutes to obtain a precursor mixture of molecular sieves;

[0026] (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;

[0027] (3) The product is washed and dried to obtain light blue (Cu-STW) or light pink (Co-STW) powder, that is, pure phase of Cu-STW or Co-STW type germanosilicate molecular sieve.

Embodiment 3

[0029] Synthesis of transition metal doped chiral germanosilicate molecular sieve Cu-STW:

[0030] (1) Add 1.65g OSDA (organic structure directing agent) N,N diethylethylenediamine and 0.2g water into a 50ml beaker, add 0.1g germanium dioxide (GeO 2 ) mixed well for 2h, then added 0.08gCuCl 2 ·5H 2 O or 0.057gCoCl 2 2H 2 O stirred for 1h, then added 0.186g tetraethyl orthosilicate Si (OC 2 h 5 ) 4 , stirred for 15 minutes, and finally added 0.17g HF and stirred for 20 minutes to obtain a precursor mixture of molecular sieves

[0031] (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;

[0032] (3) The product is washed and dried to obtain light blue (Cu-STW) or light pink (Co-STW) powder, that is, pure phase of Cu-STW or Co-STW type germanosilicate molecular sieve.

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Abstract

The invention relates to a transition-metal-doped chiral germanium silicate molecular sieve and a synthesis method thereof. The synthesis method comprises the following steps: uniformly mixing N,N-diethylethylenediamine, water and GeO2, adding tetraethyl orthosilicate, stirring, adding doping metal salt CuCl2.5H2O and / or CoCl2.2H2O, sufficiently stirring, adding HF and stirring to obtain a molecular sieve precursor mixture; and adding the molecular sieve precursor mixture into a high-pressure stainless steel reaction kettle, crystallizing at 150-200 DEG C for 7-9 days, taking out of the reaction kettle, cooling to room temperature, washing the product, and drying to obtain the Co / Cu-STW germanium silicate molecular sieve pure phase. The transition metal ions copper and cobalt are successfully doped into the STW germanium silicate molecular sieve to obtain the pure phase; and meanwhile, the cost is lowered.

Description

technical field [0001] The invention relates to a molecular sieve and a synthesis method thereof, belonging to the technical field of catalyst synthesis. Background technique [0002] Molecular sieve materials belong to the microporous material part of porous materials, and their pore size is about 0.3-2.0 nanometers. Molecular sieve materials have a rich pore structure, regular pore distribution, and high stability, so they have unique application properties in various fields (adsorption, separation, catalysis, photoelectric materials, functional materials, host-guest materials, etc.), and contribute to social development. Created immeasurable value. Catalysis is the core of the chemical industry, and the soul of catalytic reactions is the catalyst. As one of the most important catalysts, the importance of molecular sieve materials can be imagined. [0003] Molecular sieves doped with transition metals are often used as selective catalysts in industrial catalysis and envi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/08
Inventor 石磊张娜
Owner QILU UNIV OF TECH