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Oxidation desulfurization method based on Lewis acid ion liquid

An acidic ionic liquid and oxidative desulfurization technology, which is applied in the fields of refining oxygenated compounds, petroleum industry, refining hydrocarbon oil, etc., can solve the problems of difficult recovery of acid catalysts, fuel oil pollution, catalyst loss, etc., and achieve broad practical industrial application prospects , Overcome the effect of recycling difficulties

Active Publication Date: 2014-01-15
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has some disadvantages. For example, the commonly used acid catalyst is difficult to recover and has a certain solubility in oil, which will not only cause the loss of the catalyst, but also pollute the fuel oil.

Method used

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  • Oxidation desulfurization method based on Lewis acid ion liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 6g [Bmim]Cl / FeCl 3 , 1-Butyl-3-methylimidazolium chloride / FeCl 3 , added to 12g simulated diesel oil (the sulfur compound is dibenzothiophene, the sulfur content is 505ppm), and then added 0.17gH 2 o 2 The aqueous solution (30%) was magnetically stirred at 318K and normal pressure for 10 minutes, then stood still, separated, and detected by high performance liquid chromatography. The results showed that the sulfur content in the fuel oil was reduced to 12ppm, and the desulfurization rate was 97.7%. After the desulfurization is completed, the ionic liquid phase is separated, and the ionic liquid is back-extracted with carbon tetrachloride, poured and separated, and the ionic liquid is vacuum-dried at 80° C. to obtain a regenerated ionic liquid for the next recycling; Carbon chloride gives the product sulfone.

Embodiment 2

[0014] 6g [Bmim]Cl / 2ZnCl 2 , 1-Butyl-3-methylimidazolium chloride / 2ZnCl 2 , added to 12g simulated diesel oil (the sulfide is dibenzothiophene, the sulfur content is 505ppm), and then 0.17g H 2 o 2 The aqueous solution (30%) was magnetically stirred at 318K and normal pressure for 3 hours, then stood still, separated, and detected by high performance liquid chromatography. The results showed that the sulfur content in the fuel oil was reduced to 15ppm, and the desulfurization rate was 96.9%. After the desulfurization is completed, the ionic liquid phase is separated, and the ionic liquid is back-extracted with carbon tetrachloride, poured and separated, and the ionic liquid is vacuum-dried at 80° C. to obtain a regenerated ionic liquid for the next recycling; Carbon chloride gives the product sulfone.

Embodiment 3

[0016] 6g [Bmim]Cl / 3ZnCl 2 , 1-Butyl-3-methylimidazolium chloride / 3ZnCl 2 , added to 12g simulated diesel oil (the sulfide is dibenzothiophene, the sulfur content is 521ppm), and then 0.17g H 2 o 2 The aqueous solution (30%) was magnetically stirred at 363K and normal pressure for 3 hours, then stood still, separated, and detected by high performance liquid chromatography. The results showed that the sulfur content in the fuel oil was reduced to 4ppm, and the desulfurization rate was 99.2%. After the desulfurization is completed, the ionic liquid phase is separated, and the ionic liquid is back-extracted with carbon tetrachloride, poured and separated, and the ionic liquid is vacuum-dried at 80° C. to obtain a regenerated ionic liquid for the next recycling; Carbon chloride gives the product sulfone.

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PUM

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Abstract

The present invention relates to an oxidation desulfurization method based on a Lewis acid ion liquid. The oxidation desulfurization method comprises: adopting a Lewis acid ion liquid as an extraction agent and a catalyst, and adopting a H2O2 aqueous solution as an oxidant to carry out oxidation removing on thiophene sulfides in fuel oil, wherein the Lewis acid ion liquid adopts butyl imidazole as cations and adopts Lewis acidic MxCly<-> as anions, a molar ratio of the H2O2 to the initial S in the fuel oil is 0.1-100, a mass ratio of the Lewis acid ion liquid to the fuel oil is 1:20-10:1, the oxidation desulfurization temperature is 273-373 K, the pressure is 0.1-50 atm, and the time is 5 min-24 h. According to the method, the thiophene sulfide removal rate is up to 90%, and the sulfur content is reduced to less than 10 ppm.

Description

technical field [0001] The present invention relates to a kind of with Lewis acidic ionic liquid as extraction agent and catalyst, H 2 o 2 Aqueous solution is used as an oxidizing agent to oxidize and remove sulfur compounds in fuel oil. Background technique [0002] Fuel oil usually contains a certain amount of sulfide, which will be converted into an important air pollutant - SO during the combustion process. X , and the acid rain formed by it will cause serious damage to the ecological environment. In addition, sulfur oxides can also corrode and damage engine components, poison the locomotive exhaust gas treatment catalyst, reduce its catalytic activity, increase the emission of particle pollution, and aggravate the pollution of the urban environment. To this end, countries are formulating increasingly stringent fuel oil standards to reduce the sulfur content in fuel oil. For example, most European and American countries currently require the sulfur content in fuel oi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G27/12C10G21/20
Inventor 陈晓春宋丹丹于光认
Owner PETROCHINA CO LTD
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