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Hierarchical porous titanium-silicon molecular sieve catalyst with oxidative desulfurization function and preparation method and application thereof

A titanium-silicon molecular sieve, oxidative desulfurization technology, applied in molecular sieve catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as low sulfur efficiency, and achieve good effects, cheap and easy-to-obtain raw materials, and simple preparation methods. Effect

Active Publication Date: 2019-03-19
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the shortcomings and shortcomings of the low efficiency of oxidation removal of sulfur in dibenzothiophene in the prior art, the primary purpose of the present invention is to provide a highly efficient polysulfide with oxidative desulfurization from the perspective of thermodynamics and kinetics. A method for preparing a mesoporous titanium-silicon molecular sieve catalyst; the method is to prepare a mesoporous molecular sieve by adding aspartic acid in a sodium hydroxide solution as a protective agent and desiliconizing the prepared molecules

Method used

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  • Hierarchical porous titanium-silicon molecular sieve catalyst with oxidative desulfurization function and preparation method and application thereof
  • Hierarchical porous titanium-silicon molecular sieve catalyst with oxidative desulfurization function and preparation method and application thereof
  • Hierarchical porous titanium-silicon molecular sieve catalyst with oxidative desulfurization function and preparation method and application thereof

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Embodiment 1

[0024] A method for preparing a porous titanium-silicon molecular sieve catalyst with oxidative desulfurization, characterized in that it comprises the following steps:

[0025] (1) Mix tetrapropylammonium hydroxide and deionized water evenly, then add ethyl silicate and butyl titanate dropwise together, and stir for 10 hours so that ethyl silicate and butyl titanate are completely decomposed; then The mixture was transferred to a 100 ml polytetrafluoroethylene-lined stainless steel autoclave, and dried in a dry box at 180 °C under static conditions for 2 days; the synthesized solid product was centrifuged at 500 rpm, and the volume Wash fully with a mixture of deionized water and ethanol at a ratio of 1:1, and then dry overnight in an oven at 80°C to obtain molecular sieve TS-1; the ethyl silicate, butyl titanate, tetrapropylammonium hydroxide and deionized The dosage of ionized water is 8.32 grams, 0.680696 grams, 8.785152 grams and 84.2751 grams respectively;

[0026] (2) ...

Embodiment 2

[0031] Embodiment 2: Carry out performance test to the TS-1 hierarchical porous molecular sieve obtained in embodiment 1

[0032] 1. Dissolve 0.2mmol (0.036852g) of dibenzothiophene in 15.0ml of acetonitrile solution, add 0.125ml (0.107g) of 1,3-diisopropylbenzene and 0.025g (25 mg) of the implementation Example 1 gained TS-1 hierarchical porous molecular sieve (mass ratio is dibenzothiophene / molecular sieve catalyst=15), then adding 2.0mmol (198.16mg) mass fraction is 35% H 2 o 2 Aqueous solution, the molar ratio is dibenzothiophene / H 2 o 2 =1 requires 30% hydrogen peroxide (226.67 mg) with a mass fraction equivalent to 204 microliters.

[0033] 2. Then start the reaction (the reaction should be at a higher dilution to prevent the crystallization of dibenzothiophene and the product, while cooling with condensed water) and heat to reflux at 60°C for 4h.

[0034] 3. Finally, take samples every half an hour and analyze them in gas chromatography (designed to take samples at ...

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Abstract

The invention belongs to the technical field of molecular sieves and preparation thereof and discloses a hierarchical porous titanium-silicon molecular sieve catalyst with an oxidative desulfurizationfunction and a preparation method and application thereof. The preparation method includes the steps of mixing tetrapropylammonium hydroxide and deionized water, dropwise adding ethyl silicate and butyl titanate, and stirring; transferring the mixture to a stainless steel high-pressure kettle, and drying in a drying box at 180 DEG C in static state; separating by centrifuging, washing, and dryingovernight in an oven at 80 DEG C to obtain a molecular sieve; mixing the molecular sieve, sodium hydroxide, water and aspartic acid, stirring at room temperature, filtering by centrifuging, drying the filter residue in the oven at 80 DEG C for 10 hours, taking out, and calcining in a muffle furnace for 6 hours at a temperature rate of 2 DEG C / min from room temperature to 550 DEG C to obtain the catalyst herein. The molecular sieve catalyst of Si / Ti=20 is up to 43% in conversion rate 4 hours after sulfide removal; dynamics simulation of the catalyst shows that the reaction is first-order dynamics reaction.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves and their preparation, and in particular relates to a multi-level porous titanium-silicon molecular sieve catalyst with oxidative desulfurization and its preparation method and application. Background technique [0002] Since the 1970s and 1980s, some people have studied titanium-silicon molecular sieves, which have been widely used in catalytic degradation, adsorption separation and degradation of organic sulfides. Titanium-silicon molecular sieves were developed by scientific research enthusiasts in the 1980s. Due to their specific MFI topology, unique pore structure, good hydrothermal stability, good shape selectivity, and application range in the petrochemical field Wide, has a good catalytic effect, and is widely used in the field of catalysis. Some of these molecular sieves have reached the requirements of industrialization. Traditional synthesis methods mainly include hydrotherma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J35/10B01J37/00C07D333/76
CPCC07D333/76B01J29/89B01J37/0018B01J35/647
Inventor 穆巧文刘宝玉谭伟方岩雄
Owner GUANGDONG UNIV OF TECH
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