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Aerosol-assisted synthesis method of Beta molecular sieve

An aerosol and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., to achieve the effect of high utilization rate, simple synthesis process and reduced sewage discharge

Inactive Publication Date: 2015-04-29
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current aerosol method is mainly used to mix raw materials and templates to form an aerosol to synthesize mesoporous and macroporous molecular sieves, and it has not been reported that this method is directly used in the synthesis process of Beta molecular sieves.

Method used

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  • Aerosol-assisted synthesis method of Beta molecular sieve
  • Aerosol-assisted synthesis method of Beta molecular sieve
  • Aerosol-assisted synthesis method of Beta molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Mix 0.83g sodium metaaluminate, 20g silica sol, and 68.67g water and stir for 1 hour to form a mixed solution, in which SiO 2 : Al 2 o 3 : H 2 The O molar ratio is 1:0.033:38.15. Then an aerosol is formed by an aerosol generator, and silicon-aluminum oxide is obtained by drying. 0.8g of silicon-aluminum oxide is put into a 1.35ml stainless steel synthesis kettle with a polytetrafluoroethylene liner, and then 1.11g of a mass fraction of 25% is added. Aqueous solution of tetraethylammonium hydroxide, silicon aluminum oxide in SiO 2 The mol ratio with tetraethylammonium hydroxide is 1: 0.15, sealed at 145 DEG C and carry out crystallization reaction 72h, the gained solid product is washed with deionized water and then dried at 100 DEG C for more than 12 hours to obtain the final product Beta (Si / Al=30) Molecular sieve 0.72g, equivalent to 1L crystallization kettle can produce about 530g Beta molecular sieve. figure 1 For the XRD spectrum of this product, it can be se...

Embodiment 2

[0028] Mix 0.5g sodium metaaluminate, 20g silica sol, and 37.68g water and stir for 1 hour to form a mixed solution, in which SiO 2 : Al 2 o 3 : H 2 The O molar ratio is 1:0.02:28.7. Then an aerosol is formed by an aerosol generator, and silicon-aluminum oxide is obtained by drying. 0.8g of silicon-aluminum oxide is put into a stainless steel synthesis kettle with a polytetrafluoroethylene lining, and then 1.13g of 25% tetraethylene oxide is added. Aqueous ammonium hydroxide solution, SiO in silicon aluminum oxide 2 The mol ratio with tetraethylammonium hydroxide is 1: 0.15, sealed at 145 DEG C and carry out crystallization reaction 72h, the gained solid product is washed with deionized water and then dried at 100 DEG C for more than 12 hours to obtain the final product Beta (Si / Al=50) molecular sieve. figure 2 For the XRD spectrum of this product, it can be seen that there are 6 diffraction peaks at 2theta of 7.8°, 12.0°, 13.6°, 21.0°, 22.4°, and 29.4° on the XRD spect...

Embodiment 3

[0030] Mix 0.313g of sodium metaaluminate, 20g of silica sol, and 17g of water and stir for 1 hour to form a mixed solution, in which SiO 2 : Al 2 o 3 : H 2 The O molar ratio is 1:0.0125:9.4. Then an aerosol is formed by an aerosol generator, and silicon-aluminum oxide is obtained by drying. 0.8g of silicon-aluminum oxide is put into a stainless steel synthesis kettle with a polytetrafluoroethylene lining, and then 1.15g of 25% tetraethylene oxide is added. Aqueous ammonium hydroxide solution, SiO in silicon aluminum oxide 2 The mol ratio with tetraethylammonium hydroxide is 1: 0.15, sealed at 145 DEG C and carry out crystallization reaction 72h, the gained solid product is washed with deionized water and then dried at 100 DEG C for more than 12 hours to obtain the final product Beta (Si / Al=80) molecular sieve. Figure 4For the XRD spectrum of this product, it can be seen that there are 6 diffraction peaks at 2theta of 7.8°, 12.0°, 13.6°, 21.0°, 22.4°, and 29.4° on the X...

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Abstract

The invention provides an aerosol-assisted synthesis method of a Beta molecular sieve. The current industrial Beta molecular sieve is mainly synthesized by adopting a hydrothermal method, but the hydrothermal method has the problems of long hydrolysis time, large template used amount, low reactor utilization rate, high production cost, complex operation and serious waste water pollution. Aiming to solve the technical problems, the invention provides the aerosol-assisted synthesis method of the Beta molecular sieve. According to the synthesis method, a molecular sieve precursor is prepared by using aerosol, and the molecular sieve precursor is crystallized by using a template which is tetraethylammonium hydroxide to synthesize the Beta molecular sieve. The synthesis method provided by invention can be used for preparing the Beta molecular sieve with high crystallinity and controllable ratio of silicate to aluminium. The synthesis method has the advantages of simplicity in operation, small template used amount, little pollution, high yield of Beta molecular sieve, high single-reactor utilization rate and low production cost and has a good industrial application prospect.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for aerosol-assisted synthesis of Beta molecular sieves. Background technique [0002] Beta molecular sieve, as the only high-silicon molecular sieve with macroporous three-dimensional structure discovered so far, has a unique topological structure, both acid catalytic properties and structural selectivity, and has a wide range of applications. Beta molecular sieve has moderate acidity, good thermal, acid and hydrothermal stability and hydrophobicity, and can show excellent catalytic properties such as not easy to coke and long service life in catalytic reactions. At present, Beta molecular sieves are widely used in many aspects such as alkylation, transalkylation reaction, hydrocarbon cracking, esterification, etherification, disproportionation isomerization, etc. A class of molecular sieves. [0003] Beta molecular sieves currently used in industry are mainl...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 熊光赵瑞雪郭振东
Owner DALIAN UNIV OF TECH
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