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Method for one-step synthesis of ZSM-5 molecular sieve in solid phase system

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high energy consumption, complicated operation steps, large pollution, etc., and achieve product crystallization The effect of high efficiency, elimination of high-voltage safety hazards, and improvement of utilization rate and product yield

Inactive Publication Date: 2021-03-09
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main purpose of the present invention is to provide a method for synthesizing ZSM-5 molecular sieve in one step in a solid phase system, so as to solve the problems of complex operation steps, high energy consumption and large pollution of ZSM-5 molecular sieve synthesized by hydrothermal method

Method used

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  • Method for one-step synthesis of ZSM-5 molecular sieve in solid phase system
  • Method for one-step synthesis of ZSM-5 molecular sieve in solid phase system
  • Method for one-step synthesis of ZSM-5 molecular sieve in solid phase system

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 0.2g tetrapropylammonium bromide (TPABr), 0.336g ammonium bifluoride (NH 4 HF 2 ), 1g sodium metasilicate nonahydrate (Na 2 SiO 3 9H 2 O), 0.0744g aluminum isopropoxide, poured in the mortar, after grinding and mixing for 15 minutes, the pasty or pasty mixture after mixing was moved in the steel reaction kettle of polytetrafluoroethylene lining, at 160 ℃ After crystallization for 24 hours, the reaction product was washed with ethanol and deionized water, and the filter cake was transferred to a blast drying oven at a drying temperature of 60°C for 12 hours or more to obtain the final product. In this system, the molar ratio of raw materials is: n(TPABr):n(NH 4+ ): n(SiO 2 ): n (water of crystallization) = 0.20: 1.60: 1.0: 8.60; Si / Al = 10.

[0026] attached figure 1 It is the XRD characterization result of Example 1. From the characteristic diffraction peaks, it can be known that the product is a pure phase of MFI and has a high degree of crystallinity.

Embodiment 2

[0028] Weigh 0.2g tetrapropylammonium bromide (TPABr), 0.336g ammonium bifluoride (NH 4 HF 2 ), 1g sodium metasilicate nonahydrate (Na 2 SiO 3 9H 2 O), 0.0744g aluminum isopropoxide, 0.226g fumed silica, pour into a mortar, grind and mix for 15 minutes, transfer the mixed paste or paste mixture to a Teflon-lined steel In a reaction kettle, crystallize at 160°C for 24 hours, wash the reaction product with ethanol and deionized water, and transfer the filter cake to a blast drying oven at a drying temperature of 60°C for 12 hours or more to obtain the final product. In this system, the molar ratio of raw materials is: n(TPABr):n(NH 4+ ): n(SiO 2 ): n (water of crystallization) = 0.10: 0.80: 1.0: 4.30; Si / Al = 20.

[0029] attached figure 2 It is the XRD characterization result of Example 2. From the characteristic diffraction peaks, it can be known that the product is MFI pure phase, and the crystallinity is relatively high. attached image 3 It is a scanning electron ...

Embodiment 3

[0031] Weigh 0.2g tetrapropylammonium bromide (TPABr), 0.336g ammonium bifluoride (NH 4 HF 2 ), 1g sodium metasilicate nonahydrate (Na 2 SiO 3 9H 2 (2), 0.037g aluminum isopropoxide, 0.226g silicon micropowder, pour in the mortar, after grinding and mixing for 15 minutes, move the mixed paste or pasty mixture to the steel reactor of polytetrafluoroethylene lining crystallization at 160°C for 24 hours, the reaction product was washed with ethanol and deionized water, and the filter cake was transferred to a blast drying oven at a drying temperature of 60°C for 12 hours or more to obtain the final product. In this system, the molar ratio of raw materials is: n(TPABr):n(NH 4+ ): n(SiO 2 ): n (water of crystallization) = 0.10: 0.80: 1.0: 4.30; Si / Al = 40.

[0032] attached Figure 4 It is the XRD characterization result of Example 3. From the characteristic diffraction peaks, it can be seen that the product is MFI pure phase, and the crystallinity is relatively high. attac...

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Abstract

The invention provides a method for one-step synthesis of a ZSM-5 molecular sieve in a solid phase system, which is characterized by comprising the following steps: uniformly mixing a silicon source,an aluminum source, a mineralizing agent, an alkali source and a template agent, crystallizing the mixture at the crystallization temperature of 100 DEG C and 180 DEG C for 6-48h, and washing and drying the obtained product to obtain the ZSM-5 molecular sieve. The preparation process only relates to grinding and mixing of the raw materials, the steps of stirring, aging and the like required in thehydrothermal synthesis process are not needed, no solvent is added, a sample can be obtained by directly grinding and mixing at a certain temperature for a certain period of time, the utilization rate of the raw materials and the product yield are greatly improved, seed crystals do not need to be added to induce crystallization in the crystal forming process, the product crystallization rate is high, and the crystal form is good.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation, in particular to a method for synthesizing ZSM-5 molecular sieve in one step in a solid phase system. Background technique [0002] Molecular sieve is a very important inorganic material, which is widely used in the field of petroleum refining and chemical catalysis. ZSM-5 molecular sieve, because of its uniform pore structure, good hydrophobicity, and large specific surface area, makes it suitable for many important industrial fields, such as the adsorption and separation of organic substances, methane aromatization and other catalytic reactions. The modified ZSM-5 molecular sieve also has good shape selectivity and catalytic performance for specific reactions. As an adsorption material, it can be used for the separation of pollutants in industry and the environment, the purification of gas or sewage, and the drying of humid environments; As a catalytic material, it is gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03
Inventor 方奕文李伟可丁客鑫罗昀皓谢桐汤晓雯宋一兵
Owner SHANTOU UNIV
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