Preparation method of multi-stage pore channel beta molecular screen

A technology of molecular sieves and channels, which is applied in the field of preparation of multi-stage channel molecular sieves, can solve the problems of discontinuous intercrystalline pores and the decrease of micropore volume of Beta molecular sieves, and achieve the goal of avoiding the loss of molecular sieve quality, reducing synthesis costs, and simplifying synthesis steps Effect

Active Publication Date: 2012-12-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

This treatment method is simple, but after the treatment, the pore volume of the Beta molecular sieve micropores decreases, and the formed intercrystalline pores may be discontinuous

Method used

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  • Preparation method of multi-stage pore channel beta molecular screen
  • Preparation method of multi-stage pore channel beta molecular screen
  • Preparation method of multi-stage pore channel beta molecular screen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] First mix 4g of fumed silica, 1.48g of aluminum sulfate and 11.21g of an aqueous solution with a mass fraction of 35% tetraethylammonium hydroxide, and then add 0.132g of sodium hydroxide to obtain the original solution of aluminosilicate. than SiO 2 :Al 2 o 3 :TEA + :OH - =1:0.033:0.4:0.45, stirred at room temperature for 1 hour, then evaporated to dryness at 70°C to obtain "pseudo-solid phase" aluminosilicate, and measured the water content H 2 O and SiO 2 The molar ratio was 2.1. Take 5g of the obtained "pseudo-solid phase" aluminosilicate, and transfer it to a closed static reaction kettle, and crystallize at a crystallization temperature of 140°C for 60h. After the crystallization is completed, the synthesized sample is The rate of 2°C / min was raised from room temperature to 550°C for 4 h at constant temperature to obtain the final sample with a yield of 98%.

[0031] X-ray diffraction showed that the sample was Beta molecular sieve (attached figure 1 ), an...

Embodiment 2

[0033]First mix 4g of fumed silica, 0.74g of aluminum sulfate and 11.21g of an aqueous solution with a mass fraction of 35% tetraethylammonium hydroxide, and then add 0.132g of sodium hydroxide to obtain the original solution of aluminosilicate. than SiO 2 :Al 2 o 3 :TEA + :OH - =1:0.0167:0.4:0.45, stirred at room temperature for 6 hours, and then evaporated to dryness at 70°C to obtain a "pseudo-solid phase" aluminosilicate, and the water content H 2 O and SiO 2 The molar ratio is 2.1. Take 5g of the obtained "pseudo-solid phase" aluminosilicate, and transfer it to a closed static reaction kettle, and crystallize at a crystallization temperature of 140°C for 60h. After the crystallization is completed, the synthesized sample is The rate of 2°C / min was raised from room temperature to 550°C for 4 h at constant temperature to obtain the final sample with a yield of 98%.

[0034] X-ray diffraction shows that the obtained sample is a Beta molecular sieve, and the specific s...

Embodiment 3

[0036] First mix 33.33g of 30% silicon dioxide, 3.70g of aluminum sulfate and 28.02g of 35% tetraethylammonium hydroxide in water, mix well and then add 0.33g of sodium hydroxide to obtain the original aluminosilicate solution, the molar ratio of raw materials is SiO 2 :Al 2 o 3 :TEA + :OH - =1:0.033:0.4:0.45, stirred at room temperature for 1 hour, then evaporated to dryness at 70°C to obtain "pseudo-solid phase" aluminosilicate, and measured the water content H 2 O and SiO 2 The molar ratio was 3.0. Take 5g of the obtained "pseudo-solid phase" aluminosilicate, and transfer it to a closed static reaction kettle, and crystallize at a crystallization temperature of 140°C for 60h. After the crystallization is completed, the synthesized sample is placed in a muffle furnace Calcined at a constant temperature from room temperature to 550 °C for 4 h at a rate of 2 °C / min, the yield was 99%.

[0037] X-ray diffraction shows that the obtained sample is a Beta molecular sieve, a...

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Abstract

A preparation method of a multi-stage pore channel beta molecular screen belongs to the technical field of preparation of a multi-stage pore channel molecular screen. The preparation method is as follows: synthesizing the multi-stage pore channel beta molecular screen in one step by pseudo solid phase aluminosilicate; the molecular screen comprises a honeycomb-shaped structure or a plurality of particles in the size of 5micron to 60micron, the honeycomb-shaped structure or particles are polymerized by small crystal particles of a nano-level molecular screen, and the size of the small crystal particles of the nano-level molecular screen is 10nm to 100nm; and the aperture of one of meso pores formed by the polymerization of the small crystal particles of the nano-level molecular screen is 3nm to 45nm, and the aperture of a micro-pore is 0.6nm to 0.8nm. A second template agent is not in need during the synthesis process, so that the synthesis cost is reduced and the synthesis step is simplified; and in addition, the filtering is not in need after the crystallization is finished, therefore, the yield of the molecular screen is greatly enhanced.

Description

technical field [0001] The invention belongs to the technical field of preparation of multi-stage pore molecular sieves. In particular, it relates to a method for one-step synthesis of a multi-level channel Beta molecular sieve in a "pseudo-solid phase" without a second template agent. Background technique [0002] Traditional microporous molecular sieves are widely used as catalysts in fine chemical and petrochemical fields. But when the molecule of the reactant is close to or larger than the aperture of the microporous molecular sieve (generally less than 1.5nm), the reaction rate largely depends on the diffusion degree of the reactant molecule in the microporous molecular sieve, and the reactant in the micropore Diffusion limitation in molecular sieves can easily cause "carbon deposition" and deactivate molecular sieve catalysts, greatly reducing the service life of molecular sieve catalysts. Therefore, it is necessary to improve the diffusion of reactant molecules in mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B82Y30/00
Inventor 李英霞王煊王艺诺陈标华
Owner BEIJING UNIV OF CHEM TECH
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