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Amphiphilic cobalt-containing sandwich type heteropolyacid and application thereof

A sandwich type, heteropolyacid technology, applied in the refining of oxygenated compounds, treatment of hydrocarbon oils, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of less research and achieve high desulfurization and desulfurization efficiency reduced effect

Active Publication Date: 2016-08-24
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, sandwich polyacid K 10 co 4 (H 2 O) 2 (PW 9 o 34 ) 2 There are few studies on desulfurization

Method used

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  • Amphiphilic cobalt-containing sandwich type heteropolyacid and application thereof
  • Amphiphilic cobalt-containing sandwich type heteropolyacid and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The concrete synthetic steps of described a kind of amphipathic cobalt-containing sandwich type heteropolyacid are as follows:

[0023] (1) Synthesis of cobalt-containing sandwich heteropolyacids ：

[0024] Dissolve 0.41g of cobalt nitrate in 15ml of ionized water, and add 2.0g of phosphotungstic acid (A-PW 9 ), heating the solution to a homogeneous burgundy color, adding excess potassium chloride (4-6g) to the above solution to generate a blue-purple precipitate, cooling to room temperature and drying by suction, redissolving the solid powder in 5-10ml In hot water, recrystallize at 5°C, and collect blue-purple crystals. Dry in a vacuum oven for 2 hours;

[0025] (2) Synthesis of amphiphilic cobalt-containing sandwich heteropolyacids:

[0026] Concentration is the ethanol solution of surfactant of 1mol / L and slowly adds dropwise in the aqueous solution of cobalt-containing sandwich-type heteropolyacid that is 0.1mol / L with the same volume concentration, wherein the...

Embodiment 2

[0027] Example 2: Extraction and catalytic oxidation desulfurization experiment of simulated oil containing benzothiophene:

[0028] Take 0.73g benzothiophene and 0.5g biphenyl dissolved in n-octane, prepare 500mL simulated oil containing benzothiophene 500ppm, then mix 23mg catalyst prepared above, 21μL hydrogen peroxide, 1mL ionic liquid [Bmim]PF 6 , 5mL simulated oil was added to a 25mL round-bottomed flask in sequence, and the reaction was carried out under magnetic stirring at 60°C for 60 minutes. The supernatant was taken out every 10 minutes, and analyzed by gas chromatography. The experimental results are shown in Table 1. After the reaction is over, use the pouring method to pour out the remaining simulated oil. After washing several times with dichloromethane, the catalyst and the ionic liquid were centrifuged and separated, and placed in a vacuum drying oven for 6 hours, and the catalyst was obtained again for the next round of reaction. The catalytic efficiency di...

Embodiment 3

[0029] Example 3: Extraction and catalytic oxidation desulfurization experiment of simulated oil containing dibenzothiophene:

[0030] Get 1.0g dibenzothiophene and 0.5g biphenyl to be dissolved in n-octane, be mixed with 500mL the simulated oil product that contains dibenzothiophene 500ppm, then 23mg catalyst prepared above, 21μL hydrogen peroxide, 1mL ionic liquid [Bmim ]PF 6 , 5mL simulated oil was added to a 25mL round bottom flask in turn, and the reaction was performed under magnetic stirring at 60°C for 80 minutes. The supernatant was taken out every 10 minutes, and analyzed by gas chromatography. The experimental results are shown in Table 1. After the reaction is over, use the pouring method to pour out the remaining simulated oil. After washing with dichloromethane for several times, the catalyst and the ionic liquid were centrifuged and separated, and placed in a vacuum drying oven for 8 hours, and the catalyst was obtained again for the next round of reaction. Th...

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Abstract

The invention belongs to the fields of preparation of functional catalytic materials and fuel purification and relates to amphiphilic cobalt-containing sandwich type heteropolyacid and an application of heteropolyacid in catalytic desulfurization. The molecular formula of the catalyst is [C18H37N(CH3)3]10[Co4(H2O)2(PW9O34)2], and amphiphilic cobalt-containing sandwich type heteropolyacid is obtained through self-assembly of cobalt-containing sandwich type heteropolyacid K10[Co4(H2O)2(PW9O34)2] and a cationic surfactant, namely, octadecyl trimethyl ammonium chloride through ion exchange under electrostatic force. The catalyst is mixed with hydrogen peroxide and an ionic liquid [Bmim]PF6 to form an extraction, catalytic oxidation and desulfurizing system, and the purpose of super-deep desulfurization can be achieved at normal temperature. The preparation method of the catalyst is simple, the desulfurization reaction condition is mild, the catalytic system can be at least used 6 times without remarkable reduction of catalytic efficiency, and the preparation method is an efficient, economical and environment-friendly production process.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional catalytic materials and catalytic desulfurization, and in particular relates to an amphiphilic cobalt-containing sandwich type heteropolyacid and its application in catalytic desulfurization. Background technique [0002] Fuel oil mainly includes gasoline, diesel oil, etc. Sulfur is one of the main impurity elements commonly found in fuel oil. Sulfur compounds in fuel burn to form sulfur oxides (SO x ), not only will cause the formation of acid rain, but also will reduce the effect of automobile exhaust catalysts on nitrogen oxides NO x , incomplete combustion of hydrocarbons and particulate matter, etc., which will aggravate environmental pollution. The world has established increasingly stringent environmental protection regulations, limiting the sulfur content of vehicle fuels, and the production of low-sulfur "green fuels" has become an inevitable trend. [0003] At presen...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J27/188C07C211/63C07C209/00C10G21/06C10G27/12
CPCB01J27/188B01J31/0239C07C209/00C07C211/63C10G21/06C10G27/12C10G2300/202C10G2300/70
Inventor 张宏徐琰马雯雯
Owner NORTHEAST NORMAL UNIVERSITY
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