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Synthesis method of supported MoS2 catalyst

A synthesis method and catalyst technology, which is applied in the field of MoS2 catalyst synthesis, can solve the problems of imperfect preparation methods of multi-stage molecular sieves, and achieve the effects of low synthesis cost, strong process economy, and safe and convenient operation

Inactive Publication Date: 2016-07-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, so far, the preparation method of hierarchical porous molecular sieves is not perfect, and there is no report on the ionothermal synthesis of hierarchical porous AFI molecular sieves, and there is no report on the use of hierarchical porous AFI molecular sieves as MoS 2 carrier report

Method used

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  • Synthesis method of supported MoS2 catalyst
  • Synthesis method of supported MoS2 catalyst

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Effect test

Embodiment 1

[0024] At 80°C, 1.5 g of phosphoric acid, 0.88 g of aluminum isopropoxide, 0.4 g of ethanolamine and 0.05 g of hydrofluoric acid with a mass concentration of 40% were added to 33 g of 1-butyl-3-methylimidazolium bromide ionic liquid and mixed , and stir until a homogeneous precursor mixture is obtained. The above mixture was transferred to a stainless steel reaction kettle with a polytetrafluoroethylene lining, and then placed in an oven at 150°C for crystallization. After crystallization for 6 hours, it was taken out, the reaction kettle was cooled, and then 200ml of deionized water was added to the reaction mixture. After ultrasonic washing, the reactant was filtered to obtain a white solid, which was repeatedly washed three times with deionized water and washed with 50 ml of ethanol. The final white solid was dried in an oven at 110°C to finally obtain a white powdery solid, which was determined by XRD, as figure 1 As shown, characteristic diffraction peaks with 2θ angles...

Embodiment 2

[0026] At 80°C, 1.8 g of phosphoric acid, 1.0 g of aluminum isopropoxide, 0.5 g of ethanolamine and 0.05 g of hydrofluoric acid with a mass concentration of 40% were added to 20 g of 1-butyl-3-methyl imidazolium bromide ionic liquid and mixed , and stir until a homogeneous precursor mixture is obtained. The above mixture was transferred to a stainless steel reactor with a polytetrafluoroethylene lining, and then placed in an oven at 160°C for crystallization. After crystallization for 4 hours, it was taken out, the reactor was cooled, and then 300ml of deionized water was added to the reaction mixture. After ultrasonic washing, the reactant was filtered to obtain a white solid, which was repeatedly washed three times with deionized water and washed with 50 ml of ethanol. The final white solid was dried in an oven at 110°C, and finally a white powdery solid was obtained, which was determined by XRD test, as figure 2 As shown, the characteristic diffraction peaks with 2θ angle...

Embodiment 3

[0028] 0.5 ml of ammonium tetrathiomolybdate solution with a concentration of 0.01 g / ml was impregnated on 0.4 g of the hierarchical porous AFI molecular sieve carrier synthesized in Example 2. The impregnated catalyst was air-dried at room temperature, and then transferred to a vacuum oven at 70°C for 4 hours. The dried catalyst was placed in a tube furnace under N 2 Under the condition of purging, the temperature was raised to 450°C and kept for 8 hours to prepare MoS supported by multi-level porous AFI molecular sieves. 2 catalyst.

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Abstract

The invention relates to a synthesis method of a supported MoS2 catalyst. The method comprises the following steps: preparing a macropore-mesopore-micropore composite hierarchical pore aluminum phosphate AFI molecular sieve carrier at normal pressure or a low authigenic pressure through adopting an ionothermal synthesis technology; and dipping the prepared hierarchical pore aluminum phosphate AFI molecular sieve carrier in a sulfur-containing mother liquor, drying the immersed carrier, and carrying out high temperature roasting to prepare the hierarchical pore molecular sieve supported MoS2 catalyst. The ionothermal synthesis technology has the advantages of recovery and repeated use of an ionic liquid, low synthesis cost, no discharge of acids, alkalis or waste liquids in the synthesis process, and environmental protection. The hierarchical pore molecular sieve supported MoS2 catalyst prepared in the invention has the advantages of large specific surface area, large pore volume, and potential application values in hydrodesulfurization, hydrocracking and other catalytic reactions.

Description

technical field [0001] The invention relates to a loaded MoS 2 The synthesis method of catalyst, specifically relates to a kind of MoS supported by hierarchical porous aluminum phosphate AFI molecular sieve 2 Catalyst synthesis method. Background technique [0002] With the rapid growth of China's economy, the demand for middle distillates continues to increase. At present, oil resources are in short supply, crude oil is increasingly heavy and inferior, and environmental protection requirements are increasing. Therefore, it is particularly important to develop efficient heavy oil conversion technology to produce clean fuels. For heavy oil conversion technology, active components such as Co, Mo or Ni are usually loaded on the carrier. Commonly used supports are usually alumina, silica, microporous molecular sieves and amorphous silica-alumina. The invention relates to a MoS supported by a molecular sieve with a hierarchical porous AFI structure 2 In the preparation of th...

Claims

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Application Information

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IPC IPC(8): C01G39/06
Inventor 徐仁顺田志坚马怀军王炳春曲炜李鹏王从新潘振栋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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