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Catalytic oxidation desulfurization catalyst and preparation method thereof

A technology for catalytic oxidative desulfurization and catalyst, applied in the field of emulsion catalytic system and its preparation, can solve the problems of hindering oxidation of oxidant, reducing catalytic ability of catalyst, adverse catalytic activity of catalyst, etc., and achieves the effect of improving catalytic activity and good cycle stability

Inactive Publication Date: 2014-08-27
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the catalyst structure synthesized by this type of surfactant, the density of the alkyl chain at the catalytic active center is either too low or too high to simultaneously take into account the formation of the active peroxygen center and the contacting catalytic center of the low-polarity sulfide
According to previous literature and patent reports, when the density of alkyl chain-wrapped polyacids is low, although it is beneficial for hydrogen peroxide to contact polyacids to form active catalytic centers, it is not conducive to the contact between low-polarity sulfur-containing organics and catalysts, reducing the The catalytic ability of the catalyst; when the density of the alkyl chain wrapped polyacid is high, it will seriously hinder the oxidant from oxidizing the heteropolyacid to peroxypolyacid, and it is also not conducive to improving the catalytic activity of the catalyst

Method used

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  • Catalytic oxidation desulfurization catalyst and preparation method thereof
  • Catalytic oxidation desulfurization catalyst and preparation method thereof
  • Catalytic oxidation desulfurization catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Catalyst (C 18 -C 2 -C 18 ) 2 ·Br·(AsMo 12 o 40 ) preparation:

[0049] As an illustrative example, the catalyst (C 18 -C 2 -C 18 ) 2 ·Br·(AsMo 12 o 40 ) can be prepared as follows: Dissolve 5.5mmol of 1-bromooctadecane in 50mL of ethanol solution, then slowly add 5mmol of N,N,N,N-tetramethylethylenediamine dropwise, and then at 80°C Stir and heat in an oil bath for 48 h, and finally evaporate to dryness with a rotary evaporator, and crystallize in a chloroform / ethyl acetate system to obtain C 18 -C 2 -C 18 ; 0.096mmol of C to be obtained 18 -C 2 -C 18 Dissolve in 5 mL of ethanol solution, then slowly add 0.048 mmol of H 3 AsMo 12 o 40 , a bright yellow precipitate was obtained (C 18 -C 2 -C 18 ) 2 ·Br·(AsMo 12 o 40) (referred to as AsMo 12 C 18 C 2 ), then reacted for 12h, and finally obtained AsMo by suction filtration, washing and drying 12 C 18 C 2 , and the yield is about 62%. C during the reaction 18 -C 2 -C 18 with H 3 AsMo 12...

Embodiment 2

[0051] As an illustrative example, the catalyst (C 18 -C 4 -C 18 ) 2 ·Br·(AsMo 12 o 40 ) preparation:

[0052] With embodiment 1, with N, N-dimethyl octadecylamine acetate, 1,4-dibromoalkane, H 3 AsMo 12 o 40 Synthesis (C 18 -C 4 -C 18 ) 2 ·Br·(AsMo 12 o 40 ).

[0053] Dissolve 5.5mmol of 1,4-dibromoalkane in 50mL of ethanol solution, then slowly add 5mmol of N,N,N,N-tetramethylethylenediamine dropwise, then stir and heat in an oil bath at 80°C 48h, finally evaporated to dryness with a rotary evaporator, and crystallized in a chloroform / ethyl acetate system to obtain C 18 -C 4 -C 18 ; 0.096mmol of C to be obtained 18 -C 4 -C 18 Dissolve in 5 mL of ethanol solution, then slowly add 0.048 mmol of H 3 AsMo 12 o 40 , to obtain a bright yellow precipitate, then reacted for 12h, and finally obtained by suction filtration, washing and drying (C 18 -C 4 -C 18 ) 2 ·Br·(AsMo 12 o 40 ).

Embodiment 3

[0055] As an illustrative example, the catalyst (C 18 -C 6 -C 18 ) 2 ·Br·(AsMo 12 o 40 ) preparation:

[0056] With embodiment 1, with N, N-dimethyl octadecylamine acetate, 1,4-dibromohexane, H 3 AsMo 12 o 40 Synthesis (C 18 -C 6 -C 18 ) 2 ·Br·(AsMo 12 o 40 ).

[0057] Dissolve 5.5mmol of 1,4-dibromohexane in 50mL of ethanol solution, then slowly add 5mmol of N,N,N,N-tetramethylethylenediamine dropwise, then stir and heat in an oil bath at 80°C 48h, finally evaporated to dryness with a rotary evaporator, and crystallized in a chloroform / ethyl acetate system to obtain C 18 -C 6 -C 18 ; 0.096mmol of C to be obtained 18 -C 6 -C 18 Dissolve in 5 mL of ethanol solution, then slowly add 0.048 mmol of H 3 AsMo 12 o 40 , to obtain a bright yellow precipitate, then reacted for 12h, and finally obtained by suction filtration, washing and drying (C 18 -C 6 -C 18 ) 2 ·Br·(AsMo 12 o 40 ).

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Abstract

The invention discloses a catalytic oxidation desulfurization catalyst and a preparation method thereof. The chemical formula of the catalytic oxidation desulfurization catalyst is (Cn-Cs-Cn)2 Y XM12O40), wherein Cn-Cs-Cn is a gemini surfactant, the spacer s is equal to 2 or 4 or 6, the alkyl chain n is equal to 14 o 16 or 18, the counter anion atom Y is a halogen atom, the heteroatom X is phosphorus or silicon or boron or iron or cobalt or arsenic or germanium, and the donor atom M is molybdenum or tungsten. The catalytic oxidation desulfurization catalyst not only is suitable for oxidation desulfurization of sulfur-containing organic matter, but also extends emulsion to the other organic synthesis fields, such as reactions of alkene epoxidation, alcohol oxidation, acid catalysis and isomerization. As long as the system is conducted in the oil-water two-phase, and the suitable heteropolyacid and the gemini surfactant with the suitable alkyl chain length and the suitable spacer length are adopted, the catalyst high in catalytic efficiency can be formed; after the reaction, the catalyst can be separated out through static demulsification; after the catalyst is recycled ten times, the catalytic efficiency can still be kept to be 95.7% of original catalytic efficiency.

Description

technical field [0001] The invention relates to a recyclable emulsion catalytic system for the oxidation of organic sulfides and a preparation method thereof, in particular to a recyclable and reusable catalytic system prepared from gemini surfactants and polyacid compounds as raw materials Catalytic oxidation desulfurization catalyst and its preparation method. Background technique [0002] Ultra-deep desulfurization of gasoline and diesel has become one of the urgent research topics in the world. The sulfur compounds in fuel oil are inevitably released into the air in the form of gas during the combustion process. These oxidizing gases react with moisture in the air to form sulfate, which in turn forms acid rain, damages buildings, acidifies soil, causes forest degradation, and destroys ecosystems. Therefore, it is of great significance to develop ultra-deep desulfurization of diesel oil. Ultra-deep desulfurization of gasoline and diesel is not only for the production o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18C10G27/12
Inventor 胡平安邱云峰李晓光马卓
Owner HARBIN INST OF TECH
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