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Preparation method of hierarchical pore heteroatom aluminum phosphate molecular sieve for oxidative desulfurization

A technology of aluminum phosphate molecular sieve and heteroatom, which is applied in the direction of molecular sieve-specific aluminum phosphate, refining with halogen compounds, molecular sieve and alkali exchange phosphate, etc., which can solve the waste of internal active sites, deactivation of catalyst carbon deposition, and limit reactants and products Molecular diffusion and other problems to achieve the effect of easy recovery, high selectivity, and shortened crystallization time

Active Publication Date: 2018-03-09
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the small pore size of traditional zeolite molecular sieves, macromolecules can only be catalyzed on the outer surface or pores, resulting in a waste of a large number of internal active sites.
In addition, the crystal size of traditional zeolite molecular sieves is on the micron scale, and its relatively long and narrow micropore channels limit the diffusion of reactant and product molecules.
Therefore, while improving the shape selectivity of the zeolite molecular sieve, it also causes serious problems such as the "secondary reaction" of the product in the outward diffusion process and the carbon deposition and deactivation of the catalyst.

Method used

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  • Preparation method of hierarchical pore heteroatom aluminum phosphate molecular sieve for oxidative desulfurization
  • Preparation method of hierarchical pore heteroatom aluminum phosphate molecular sieve for oxidative desulfurization
  • Preparation method of hierarchical pore heteroatom aluminum phosphate molecular sieve for oxidative desulfurization

Examples

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Effect test

Embodiment 1

[0026] This example uses dynamic hydrothermal synthesis of microporous AlPO 4 -5 molecular sieves were used as crystal seeds, and hierarchically porous CoAPO-5 molecular sieves were synthesized statically and hydrothermally.

[0027] The first step, dynamic hydrothermal synthesis of AlPO 4 -5 seeds:

[0028] Hydrate 2.96g of pseudo-boehmite with 36mL of distilled water, stir magnetically at 25°C for 12h, add 4.62g of phosphoric acid solution, continue stirring for 2h, add 2.02g of microporous template agent triethylamine, and prepare molecular sieve synthetic solution, continue After stirring for 3 hours, the reactant was transferred to a dynamic hydrothermal reaction kettle, crystallized at 180°C and 500r / min for 3h, filtered with suction, washed with deionized water until neutral, dried at 110°C, and calcined at 550°C 5h, the microporous AlPO prepared by dynamic method was obtained 4 -5 molecular sieve with a particle size of 2*5μm.

[0029] figure 2 Microporous AlPO s...

Embodiment 2

[0036] The first step, dynamic hydrothermal synthesis of AlPO 4 -5 seeds:

[0037] Hydrate 2.96g of pseudo-boehmite with 36mL of distilled water, stir magnetically at 25°C for 12h, add 4.62g of phosphoric acid solution, continue stirring for 2h, add 2.02g of triethylamine as a microporous template agent, and prepare a molecular sieve synthetic solution. After continuing to stir for 3 hours, transfer the reactant to a dynamic hydrothermal reactor, crystallize at 185°C and 400r / min for 4h, filter with suction, wash with deionized water until neutral, dry at 110°C, and dry at 550°C Calcined for 5h to obtain microporous AlPO prepared by dynamic method 4 -5 molecular sieves.

[0038] In the second step, the method of statically synthesizing the hierarchically porous CoAPO-5 molecular sieve is the same as in Example 1.

[0039] Catalytic oxidation removal of sulfide in simulated oil is the same as in Example 1, and the removal rates of thiophene, benzothiophene and dibenzothiophe...

Embodiment 3

[0041] The first step, dynamic hydrothermal synthesis of AlPO 4 -5 seeds:

[0042] Hydrate 2.96g of pseudo-boehmite with 36mL of distilled water, stir magnetically at 25°C for 12h, add 4.62g of phosphoric acid solution, continue stirring for 2h, add 2.02g of triethylamine as a microporous template agent, and prepare a molecular sieve synthetic solution. After continuing to stir for 3 hours, transfer the reactant to a dynamic hydrothermal reaction kettle, crystallize at 160°C and 500r / min for 3h, filter with suction, wash with deionized water until neutral, dry at 110°C, and dry at 550°C Calcined for 5h to obtain microporous AlPO prepared by dynamic method 4 -5 molecular sieves.

[0043] The second step of static synthesis of hierarchically porous CoAPO-5 molecular sieves is the same as in Example 1.

[0044] Catalytic oxidation removal of sulfide in simulated oil is the same as in Example 1, and the removal rates of thiophene, benzothiophene, and dibenzothiophene are 69.25%...

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Abstract

The invention belongs to the technical field of chemical catalysts, and specifically relates to a preparation method of a hierarchical pore heteroatom aluminum phosphate molecular sieve for oxidativedesulfurization. The method comprises the following steps: synthesizing a microporous aluminum phosphate molecular sieve through a dynamic hydrothermal crystallization manner; and preparing the hierarchical pore heteroatom aluminum phosphate molecular sieve in a mesoporous template agent and metal source synthesizing system by taking the prepared microporous aluminum phosphate molecular sieve as aseed crystal. According to the method, the synthesizing time is reduced; the prepared molecular sieve is controllable and uniform in crystal particles; and the desulfurization effect is high in catalytic oxidative desulfurization reaction.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a preparation method and related applications of a multi-level porous heteroatom aluminum phosphate molecular sieve. Background technique [0002] The sulfides in fuel oil will cause water pollution, acid rain, smog and other environmental pollution, and due to the strong corrosiveness of sulfides, the life of industrial machines will be shortened. With the increase of human demand for fuel oil, it is of great significance to remove sulfur compounds in fuel oil. There are many methods for fuel oil desulfurization, such as traditional hydrodesulfurization, extraction desulfurization, adsorption desulfurization, membrane separation desulfurization, biological desulfurization and oxidative desulfurization. Among them, oxidative desulfurization has the characteristics of mild conditions, simple operation, non-hydrogenation, etc., and has attracted widespread a...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/04C10G27/02
CPCC01B37/04C01B39/54C01P2002/54C01P2002/72C01P2004/03C01P2004/61C10G27/02C10G2300/202C10G2300/70
Inventor 韶晖郑静静陆杨王俊孙雪妮黄春香
Owner CHANGZHOU UNIV
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