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Method for catalyzing fuel oil desulfurization by coupling of sulfonic heteropolyacid salt with eutectic solvent

A technology of deep eutectic solvent and heteropolyacid salt, which is applied in the field of desulfurization to achieve the effects of mild reaction conditions, simple operation and simple synthesis

Inactive Publication Date: 2018-06-19
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] At present, the desulfurization methods of fuel oil mainly include hydrodesulfurization and non-hydrodesulfurization. Among them, hydrodesulfurization (HDS), which is widely used in industry, can effectively remove some sulfides in fuel oil, but for dibenzothiophene (DBT) and their derivatives, it is difficult for HDS to remove them

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  • Method for catalyzing fuel oil desulfurization by coupling of sulfonic heteropolyacid salt with eutectic solvent
  • Method for catalyzing fuel oil desulfurization by coupling of sulfonic heteropolyacid salt with eutectic solvent
  • Method for catalyzing fuel oil desulfurization by coupling of sulfonic heteropolyacid salt with eutectic solvent

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preparation example Construction

[0037] Preparation of sulfonic acid heteropoly salt catalyst: Add 0.1mol 1,3-propane sultone into a beaker of 50mL dichloromethane, stir for 10min under an oil bath atmosphere; then add 0.1mol triethylamine dropwise Add it to the above mixture and react at 40°C for 24h. After the reaction, filter, wash with ethyl acetate and ether, and dry in an oven at 100°C to obtain the product PSTEtA. The product PSTEtA was added to the phosphotungstic acid solution, wherein the molar ratio was n:1, stirred for 24 hours, and the final product was placed in an oven for 8 hours. [TBAC] 3 PW 12 o 40 Using the above synthesis [PSTEtA] n h 3-n PW 12 o 40 Prepared by the method, wherein TBAC and H 3 PW 12 o 40 The molar ratio is 3:1. For the synthesis of the remaining catalysts, refer to the above synthesis methods.

[0038] Preparation of choline-based deep eutectic solvent: Mix the quaternary ammonium salt and the hydrogen bond donor together to obtain a uniformly mixed liquid, and ...

Embodiment 1

[0044] Add 5mL DBT model oil (the sulfur content of oil product is 500ppm) in the 50mL round bottom flask, then add the catalyst [PSTEtA]H of 0.01g above-mentioned preparation 2 PW 12 o 40 , 1 mL deep eutectic solvent ChCl / 2Ac, 0.156 mmol H 2 o 2 , the mass fraction is 30%. At this time, the oil phase was in the upper layer, stirred and reacted at 1000rpm at 50°C for 2.5h, the model oil was separated, and the content of DBT in the oil was detected by GC-FID (internal standard method), and the removal rate of sulfur was calculated to be 96.0%.

Embodiment 2

[0046] Add 5mL DBT model oil (the sulfur content of oil product is 500ppm) in 50mL round bottom flask, then add 0.01g above-mentioned prepared catalyst [PSTEtA] 3 PW 12 o 40 , 1 mL deep eutectic solvent ChCl / 3Ac, 0.234 mmol H 2 o 2 , the mass fraction is 30%. At this time, the oil phase was in the upper layer, stirred and reacted at 800rpm at 60°C for 2h, the model oil was separated, and the content of DBT in the oil was detected by GC-FID (internal standard method), and the removal rate of sulfur was calculated to be 99.3%.

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Abstract

The invention belongs to the technical field of desulfurization, and relates to fuel oil desulfurization, in particular to a method for catalyzing fuel oil desulfurization by coupling of a sulfonic heteropolyacid salt with a eutectic solvent. According to the method, a sulfonic heteropolyacid salt catalyst and a choline eutectic solvent are added to fuel oil and uniformly stirred, then an oxidantaqueous hydrogen peroxide solution is added, and continuous stirring and sufficient reaction are performed, wherein the sulfonic heteropolyacid salt is prepared from 1,3-propanesultone and triethylamine by mixing, and the eutectic solvent is prepared from a quaternary ammonium salt and a hydrogen bond donor by mixing. The method adopts mild reaction conditions, can be exerted at room temperature under normal pressure and is simple to operate. After the reaction, the eutectic solvent and an oil product form two phases, the oil product can be separated by simple pouring, and the method is harmless to human and environment. The prepared catalyst and eutectic solvent can be recycled directly and also be used after regeneration. The highest oil product recovery rate can reach 100%, and the method is green.

Description

technical field [0001] The invention belongs to the technical field of desulfurization, relates to fuel oil desulfurization, in particular to a method for catalyzing fuel oil desulfurization with a sulfonic acid heteropoly salt coupled with a deep eutectic solvent. Background technique [0002] Since the 20th century, industries around the world have developed rapidly. A series of global problems have been caused because people have insufficient awareness of the negative impacts of industrial development and have not taken effective preventive measures. In recent years, ecological destruction and environmental pollution have received widespread attention as two major crises, among which the polluting gas NO X , SO X A large amount of emissions is an important reason leading to the above problems. In addition, when the SOx content is too high, it will be highly irritating to the human respiratory tract, leading to a series of respiratory diseases such as bronchitis and pne...

Claims

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Application Information

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IPC IPC(8): C10G27/12
CPCC10G27/12C10G2300/202C10G2300/70C10G2400/02
Inventor 蒋伟贾浩董蕾郭涛朱文帅李华明
Owner JIANGSU UNIV
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