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Hydrogen type germanium-silicon molecular sieve with ZSM-5 structure and preparation method thereof

A ZSM-5, molecular sieve technology, applied in the field of hydrogen-type germanium-silicon molecular sieve and its preparation, can solve the problems of few instances, etc., and achieve the effects of high crystallinity, controllable grain size and high purity

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the synthesized molecular sieves mainly focus on the molecular sieve types with Si-O and Al-O as the framework elements, but there are relatively few examples of synthesizing molecular sieves with Ge-O as the framework elements.

Method used

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  • Hydrogen type germanium-silicon molecular sieve with ZSM-5 structure and preparation method thereof
  • Hydrogen type germanium-silicon molecular sieve with ZSM-5 structure and preparation method thereof
  • Hydrogen type germanium-silicon molecular sieve with ZSM-5 structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0027] Mix 7g of germanium dioxide, 48.9g of tetrapropylammonium bromide (TPABr), 12.2g of n-butylamine and 360ml of deionized water evenly, add 20g of solid silica gel under stirring, stir vigorously, age at 25°C for 2h, and then transfer to the reaction Kettle, hydrothermal crystallization at 160°C for 4 hours, cooling to 100°C for hydrothermal crystallization for 8 hours, then heating up to 180°C for 12 hours.

[0028] After hydrothermal crystallization, quickly cool to 30°C, the reaction product is centrifuged, the obtained solid is washed with water until the pH of the washing solution is 8-9, and dried at 100°C for 12 hours to obtain hydrogen with a crystal phase of ZSM-5 structure Type germanium silicon molecular sieve GZ-1, its X-ray powder diffraction pattern is shown in figure 1 , the anhydrous chemical composition (in oxide molar ratio) is: GeO 2 15.6SiO2 2 , the relative crystallinity is 92%, and the grain size is 3.5μm.

example 2

[0030] Mix 1.4g of germanium dioxide, 48.9g of tetrapropylammonium bromide, 12.2g of n-butylamine and 360ml of deionized water evenly, add 20g of solid silica gel under stirring, stir vigorously, age at 25°C for 2h, and then move it into the reaction kettle. It was hydrothermally crystallized at 150°C for 6 hours, cooled to 120°C for 6 hours, and then heated to 180°C for 12 hours.

[0031] After hydrothermal crystallization, quickly cool to 30°C, the reaction product is centrifuged, the obtained solid is washed with water until the pH of the washing solution is 8-9, and dried at 100°C for 12 hours to obtain hydrogen with a crystal phase of ZSM-5 structure Type germanium silicon molecular sieve GZ-2, its anhydrous chemical composition (calculated by oxide molar ratio) is: GeO 2 40.3SiO2 2 , the relative crystallinity is 93%, and the grain size is 2.3μm.

example 3

[0033] Mix 0.7g of germanium dioxide, 48.9g of tetrapropylammonium bromide, 12.2g of n-butylamine and 360ml of deionized water evenly, add 20g of solid silica gel under stirring, stir vigorously, age at 25°C for 2h, and then transfer to the reaction kettle. It was hydrothermally crystallized at 140°C for 8 hours, cooled to 120°C for 6 hours, and then heated to 180°C for 10 hours.

[0034] After hydrothermal crystallization, quickly cool to 30°C, the reaction product is centrifuged, the obtained solid is washed with water until the pH of the washing solution is 8-9, and dried at 100°C for 12 hours to obtain hydrogen with a crystal phase of ZSM-5 structure Type germanium silicon molecular sieve GZ-3, its anhydrous chemical composition (calculated by oxide molar ratio) is: GeO 2 72.6SiO2 2 , the relative crystallinity is 93%, and the grain size is 1.8μm.

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Abstract

The invention provides a hydrogen type germanium-silicon molecular sieve with a ZSM-5 structure. The non-aqueous chemical structural expression is GeO2.xSiO2, wherein x ranges from 10 to 400, and the grain size of the germanium-silicon molecular sieve is 1 to 4 microns. The molecular sieve is relatively large in grain size; a catalyst prepared after loading platinum is applied to catalytic reforming of naphtha, and the paraxylene selectivity is good.

Description

technical field [0001] The invention relates to a heteroatom molecular sieve and a preparation method thereof, in particular to a hydrogen-type germanium silicon molecular sieve with a ZSM-5 structure and a preparation method thereof. Background technique [0002] At present, the synthesized molecular sieves mainly focus on the molecular sieve types with Si-O and Al-O as the framework elements, but there are relatively few examples of synthesizing molecular sieves with Ge-O as the framework elements. Germanium is in the same main group of silicon, with adjacent periods, has similar chemical properties, but is more metallic than silicon, which is conducive to the formation of some unique structures of germanate molecular sieves. As a new class of molecular sieves, germanate molecular sieves are quite different from aluminosilicate molecular sieves in structure and properties. [0003] ZSM-5 is a molecular sieve developed by Mobil in 1972 that contains two intersecting ten-me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
Inventor 王嘉欣张大庆臧高山张玉红王涛
Owner CHINA PETROLEUM & CHEM CORP
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