Phase transfer catalyst for oxidative desulfurization of activated carbon supported heteropolyacid quaternary ammonium salt diesel and preparation method of phase transfer catalyst

A technology of phase transfer catalyst and heteropolyacid quaternary ammonium salt, which is applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, chemical instrument and method, etc. Load activated carbon and other issues to achieve the effects of easy separation and recovery, improved diesel yield and desulfurization rate, and high dispersion

Inactive Publication Date: 2014-03-05
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The heteropoly acid quaternary ammonium salt phase transfer catalyst is solid and cannot be directly loaded on the activated carbon, so the heteropoly acid is loaded on the activated carbon first, and then reacted with the quaternary ammonium salt to prepare the supported heteropoly acid quaternary ammonium salt phase transfer catalyst At present, there is no report on the related research on the preparation of activated carbon-supported heteropolyacid quaternary ammonium salt phase transfer catalyst by two-step method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] ① Weigh the activated carbon, impregnate the activated carbon with 10% by weight nitric acid solution in an equal volume ratio for 24 hours, heat in a water bath for 2-3 hours, filter with suction, wash with water until neutral, put it in an oven, and dry it at 120 °C;

[0021] ②Weigh 0.3g of phosphomolybdic acid and fully dissolve in 40ml of 30% ethanol solution, add 1g of pretreated activated carbon to the above solution, first stir at 60°C for 2 hours, then raise the temperature to 85°C to evaporate the solution Dry, dry at 110°C for 24 hours to obtain activated carbon-supported phosphomolybdic acid catalyst;

[0022] ③ Weigh 0.08g of cetyltrimethylammonium bromide and fully dissolve it in 30% ethanol solution of 40ml, add the prepared activated carbon-loaded phosphomolybdic acid catalyst into the above solution, stir at 70°C for 2 hours, Then, it was suction-filtered, washed with water until neutral, and dried at a constant temperature of 100°C for 24 hours to obtai...

Embodiment 2

[0024] ① Weigh the activated carbon, impregnate the activated carbon with 10% by weight nitric acid solution in an equal volume ratio for 24 hours, heat in a water bath for 2-3 hours, filter with suction, wash with water until neutral, put it in an oven, and dry it at 120 °C;

[0025] ②Weigh 0.3g of phosphotungstic acid and fully dissolve in 40ml of 30% ethanol solution, add 1g of pretreated activated carbon to the above solution, stir at 70°C for 2 hours, then raise the temperature to 85°C to evaporate the solution Dry, dry at 110°C for 24 hours to obtain activated carbon-supported phosphotungstic acid catalyst;

[0026] ③ Weigh 0.004g of tetrabutylammonium bromide and fully dissolve it in 30% ethanol solution of 40ml, add the prepared activated carbon-supported phosphotungstic acid catalyst into the above solution, stir at 75°C for 2 hours, and then filter with suction. Wash with water until neutral, and dry at a constant temperature of 100°C for 24 hours to obtain an activa...

Embodiment 3

[0028] ① Weigh the activated carbon, impregnate the activated carbon with 10% by weight nitric acid solution in an equal volume ratio for 24 hours, heat in a water bath for 2-3 hours, filter with suction, wash with water until neutral, put it in an oven, and dry it at 120 °C;

[0029] ② Weigh 0.2g of phosphomolybdic acid and fully dissolve in 40ml of 30% ethanol solution, add 1g of pretreated activated carbon to the above solution, stir at 65°C for 2 hours, then raise the temperature to 80°C to evaporate the solution Dry, dry at 110°C for 24 hours to obtain activated carbon-supported phosphomolybdic acid catalyst;

[0030] ③ Weigh 0.04g of tetrabutylammonium bromide and fully dissolve it in 30% 40ml ethanol solution, add the prepared activated carbon-supported phosphomolybdic acid catalyst into the above solution, stir at 70°C for 2 hours, and then filter with suction. Wash with water until neutral, and dry at a constant temperature of 100 °C for 24 hours to obtain an activate...

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Abstract

The invention discloses a phase transfer catalyst for oxidative desulfurization of activated carbon supported heteropolyacid quaternary ammonium salt diesel and a preparation method of the phase transfer catalyst. The catalyst is prepared from an activated carbon carrier and a heteropolyacid quaternary ammonium salt active component, wherein the content of the heteropolyacid quaternary ammonium salt is 20-40% of the content of the activated carbon; the aperture of the catalyst is 1-2nm; the specific surface area of the catalyst is 500-700 m<2>/g. According to the invention, the activated carbon is taken as a support, and the heteropolyacid quaternary ammonium salt is taken as an active component, so as to prepare the phase transfer catalyst for oxidative desulfurization for the diesel, so that the defects that a non-supported phase transfer catalyst is fine in particles, low in specific surface area, and not easy to recycle are overcome. The heteropolyacid quaternary ammonium salt is supported on the activated carbon by adopting a two-step impregnation method. Firstly, heteropolyacid is supported to the activated carbon, and then reacts with the quaternary ammonium salt, so as to prepare the supported heteropolyacid quaternary ammonium salt phase transfer catalyst. The obtained catalyst is high in specific surface area; the active components are high in dispersity on the support, easy to separate and recycle, and less in oil loss. Thus, the diesel efficiency and the desulphurization rate are improved.

Description

1. Technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to an active carbon-loaded heteropolyacid quaternary ammonium salt diesel oil oxidation desulfurization phase transfer catalyst and a preparation method thereof. 2. Background technology [0002] Although catalytic oxidation desulfurization is a typical non-hydrogenation desulfurization method, due to the immiscibility of the oxidant system and the oil system, the effective mixing degree of the oxidant in the water phase and the sulfur-containing compound is poor, and the oxidation reaction only occurs in the water phase-organic phase. At the interface, it not only affects the desulfurization rate but also affects the yield of diesel oil. [0003] Heteropolyacid quaternary ammonium salts are hydrophilic and lipophilic, and also have strong acidity and strong oxidizing properties, which can effectively solve the above problems. However, the heteropolyacid quaternary...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/34C10G27/12
Inventor 李剑杨丽娜
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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