A method for alkyl derivatization and separation of sulfur-containing compounds in petroleum components
A compound and derivatization technology, applied in material separation, petroleum industry, analytical materials, etc., can solve the problems of reaction time affecting application, achieve short reaction time, solve the analysis of trace sulfide-containing molecular composition, and have strong stability
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Embodiment 1
[0033] This embodiment provides a method for methyl derivatization and molecular composition analysis of sulfur-containing compounds in refined diesel oil. The specific steps are as follows:
[0034] First, add 0.1 g of national VI diesel oil with a total sulfur content of 10 ppm and 1 ml of dichloromethane into a 2 ml vial, then add 0.1 g of silver hexafluoroantimonate, add 0.2 ml of methyl iodide with a syringe, and put the lid on The stoppered vial was stirred and reacted for 2 hours in the dark.
[0035] Take 20 μL of the supernatant and dissolve it in a mixed solvent of toluene and methanol (volume ratio is 1:3) for positive ion electrospray ionization source combined with Fourier transform ion cyclotron resonance mass spectrometry. The operating conditions of this analysis are routinely used in the art. The molecular composition of the sulfide in the national VI diesel oil obtained through statistics and calculation is as follows: figure 1 shown. DBE is the number of e...
Embodiment 2
[0037] This embodiment provides an example of analyzing the composition of sulfur-containing compounds in Kuwait crude oil based on the methyl derivatization method of the present invention, and its specific steps are as follows:
[0038] First, add 10 mg of Kuwait crude oil with a total sulfur content of 3.5 wt % and 1 ml of dichloromethane into a 2 ml vial, then add 50 mg of silver hexafluoroantimonate, add 0.1 ml of methyl iodide with a syringe, and put the cap on The stoppered vial was stirred and reacted for 20 minutes in the dark.
[0039] Take 20 μL of the supernatant and dissolve it in a mixed solvent of toluene and methanol (volume ratio is 1:3) for positive ion electrospray ionization source combined with Fourier transform ion cyclotron resonance mass spectrometry. The operating conditions of this analysis are routinely used in the art. The molecular composition of sulfides in Kuwait crude oil obtained through statistics and calculation is as follows: figure 2 show...
Embodiment 3
[0041] This embodiment provides an example of analyzing sulfide and thiophene sulfur-containing compounds in Kuwait VGO based on the methyl derivatization method of the present invention. The specific steps are as follows:
[0042] First, add 200 mg of Kuwait VGO and 20 ml of dichloromethane into a 40 ml vial, then add 0.3 g of silver hexafluoroantimonate, add 0.5 ml of methyl iodide with a syringe, and place the vial with the stopper under dark conditions The reaction was stirred for 0.5 hours.
[0043]After the reaction was finished, the silver iodide precipitate in the reaction solution was removed by filtration, and the dichloromethane in the filtrate was removed by a rotary distillation apparatus. Add 10 mL of n-hexane to the remaining oil, shake vigorously and cool to 0°C. Sulfonium salts will precipitate out under these conditions and accumulate at the bottom of the bottle under centrifugation. Polar sulfonium salts can be isolated by pouring the unreacted oily phase ...
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