Polyoxometalate-based loading-type catalyst for oil product desulfurization and preparing method thereof

A supported catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as easy decomposition, easy loss of acid, loss of catalytic activity, etc., and achieve high catalytic efficiency , good mechanical strength

Inactive Publication Date: 2016-11-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, when synthesized by impregnation method, the binding force between polyacid and carrier alumina is weak and it is easy to be dissolved in polar solvents, so it cannot be reused; while polyacid is loaded in alumina carrier by sol-gel method, polyacid will It decomposes due to the strong alkalinity on the surface of the alumina carrier and loses its catalytic activity
[0005] For addressing POMs@Al 2 o 3 In the process of use, it is easy to lose and polyacid is easy to decompose and it is difficult to be used in industrial production. We first bond the 3-aminopropyl functional group on the alumina carrier to make the alumina functionalized. On this basis, through impregnation Method load POMs, got POMs-NH 2 -Al 2 o 3 catalyst

Method used

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  • Polyoxometalate-based loading-type catalyst for oil product desulfurization and preparing method thereof
  • Polyoxometalate-based loading-type catalyst for oil product desulfurization and preparing method thereof
  • Polyoxometalate-based loading-type catalyst for oil product desulfurization and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Put about 0.8g of pretreated γ-Al in a 50mL three-neck round bottom flask 2 o 3 and 25mL dry toluene, add 0.75mL 3-aminopropyltriethoxysilane under nitrogen atmosphere, heat and stir to reflux for 24h;

[0016] (2) Take out the treated γ-Al in step (1) 2 o 3 Pellet, in N 2 Wash with freshly prepared absolute ethanol for 10 h under atmosphere to remove γ-Al 2 o 3 Dry the pellets in a constant temperature drying oven at 80°C for 12 hours to obtain amino-modified γ-Al 2 o 3 , denoted as NH 2 -Al 2 o 3 ;

[0017] (3) NH prepared in step (2) 2 -Al 2 o 3 Add it into the dilute hydrochloric acid solution with pH=4.0, soak for 4 hours, take out the pellet and dry it under vacuum at room temperature.

[0018] (4) Weigh 0.2g of phosphotungstic acid to prepare an aqueous solution of phosphotungstic acid, and add the NH 2 -Al 2 o 3 After soaking the pellets for 4 hours, take them out and wash them three times with deionized water, 10 mL each time, and dry them ...

Embodiment 2

[0020] (1) Put about 0.8g of pretreated γ-Al in a 50mL three-neck round bottom flask 2 o 3 and 25mL dry toluene, add 0.75mL 3-aminopropyltrimethoxysilane under nitrogen atmosphere, heat and stir to reflux for 24h;

[0021] (2) Take out the treated γ-Al in step (1) 2 o 3 Pellet, in N 2 Wash with freshly prepared absolute ethanol for 10 h under atmosphere to remove γ-Al 2 o 3 Dry the pellets in a constant temperature drying oven at 80°C for 12 hours to obtain amino-modified γ-Al 2 o 3 , namely NH 2 -Al 2 o 3 ;

[0022] (3) NH prepared in step (2) 2 -Al 2 o 3 Add it into the dilute hydrochloric acid solution with pH=4.0, soak for 4 hours, take out the pellet and dry it under vacuum at room temperature.

[0023] (4) Weigh 0.2g of silicotungstic acid to prepare an aqueous solution of silicotungstic acid, and add the NH 2 -Al2 o 3 After soaking for 4 hours, the pellets were taken out and washed three times with deionized water, 10 mL each time, and vacuum-dried at ro...

Embodiment 3

[0025] (1) Put about 0.8g silicon-containing Al into a 50mL three-neck round bottom flask 2 o 3 (denoted as SiO 2 @Al 2 o 3 ) and 25mL dry toluene, add 0.75mL 3-aminopropyltriethoxysilane under nitrogen atmosphere, heat and stir to reflux for 24h;

[0026] (2) Take out the SiO treated in step (1) 2 @Al 2 o 3 , at N 2 Wash with freshly prepared absolute ethanol for 10 h under atmosphere to remove SiO 2 @Al 2 o 3 Dry in a constant temperature drying oven at 80°C for 12 hours to obtain amino-modified γ-Al 2 o 3 , namely NH 2 -SiO 2 @Al 2 o 3 ;

[0027] (3) NH prepared in step (2) 2 -SiO 2 @Al 2 o 3 Add it into the dilute hydrochloric acid solution with pH=4.0, soak for 4 hours, take out the pellet and dry it under vacuum at room temperature.

[0028] (4) Weigh 0.2g of phosphotungstic acid to prepare an aqueous solution of phosphotungstic acid, and add the NH 2 -SiO 2 @Al 2 o 3 After soaking the pellets for 4 hours, take out the pellets and wash them three...

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Abstract

The invention discloses a polyoxometalate loading-type catalyst having the good removing effect on a sulfur-containing compound in an oil product and a preparing method thereof, and belongs to the technical field of functional materials. According to the material, amino-modified gamma-Al2O3, pseudo boehmite and SiO2-doped-type gamma-Al2O3 or one of amino-modified gamma-Al2O3, pseudo boehmite and SiO2-doped-type gamma-Al2O3 serves as a carrier, and the catalyst is prepared in the mode that polyoxometalate is loaded with the soaking method; the preparing method includes the steps that under the inert atmosphere, the carrier and an active chemical reagent containing a 3-aminopropyl group are reacted, and an amino group is bonded on the surface of the carrier in a covalent mode; the product is washed, dried and soaked in a dilute acid solution, and positive charge is loaded on the surface of the carrier accordingly; then the carrier is soaked in a polyoxometalate water solution, washed and dried, and the catalyst POMs-NH2-Al2O3 is obtained. If the catalyst is used for an oxidation sweetening reaction, the catalyst is high in catalytic oxidation efficiency, capable of being recycled and low in cost, and as the catalyst has the good mechanical performance, separating, recovering and reusing are quite convenient.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a multi-acid-based supported catalyst with good removal effect on sulfur-containing compounds in oil products and a preparation method thereof. Background technique [0002] Fuel desulfurization technology, as the main means to reduce the content of sulfur oxides in automobile exhaust, has become a current research hotspot. with H 2 o 2 Extraction as an oxidant combined with catalytic oxidation desulfurization Oxidative desulfurization technology Compared with the traditional hydrodesulfurization method, it has mild reaction conditions, high desulfurization rate, low corrosion, simple process, easy operation, low equipment investment, low operating cost, low carbon, energy saving and environmental protection And many other advantages, it has become the main means of deep desulfurization technology development, and the catalyst in the catalytic oxidation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24
Inventor 周云山郑扬张立娟秦立波李殿卿
Owner BEIJING UNIV OF CHEM TECH
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