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Preparation method and application of superacid compound ionic liquid

An ionic liquid and composite technology, which is applied in the field of preparation of super acid composite ionic liquid catalytic systems, can solve problems such as being unsuitable for large-scale application, inability to achieve deep desulfurization, and a gap in desulfurization performance, and achieve a simple preparation method and contact Sufficient and mild reaction conditions

Inactive Publication Date: 2015-08-12
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN102993101A adds ferrous chloride tetrahydrate into imidazolium bromide according to the molar ratio of imidazolium bromide and inorganic ferrous chloride tetrahydrate at a molar ratio of 1: (0.5-1.5), to synthesize imidazole-based ferrous chloride-type ionic liquid and It can be used for extractive desulfurization and can be recycled for more than 10 times, but it cannot reach the index of deep desulfurization
CN102690676A uses rhenic acid imidazolium salt ionic liquid as catalyst, hydrogen peroxide as oxidant, controls the reaction temperature at 60-80°C, and stirs for 0.5-2 hours to make the desulfurization rate reach more than 95%. This type of ionic liquid is expensive and not suitable for large-scale scale application
CN101220293A provides an extraction catalytic oxidation desulfurization system composed of tungsten, molybdenum polyoxometalate catalyst and hydrogen peroxide aqueous solution in ionic liquid, and a method for reducing the sulfur content in gasoline through extraction catalytic oxidation. This type of catalyst is used before and after the reaction. It can be dissolved in ionic liquid, but its acidity is low, which has a great influence on the performance of oxidative desulfurization
US7553406, US7001504, US7198712, US7749377, and US7758745 also involve the application of ionic liquids in oxidative desulfurization, but there is still a certain gap in desulfurization performance compared with similar technologies

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  • Preparation method and application of superacid compound ionic liquid
  • Preparation method and application of superacid compound ionic liquid
  • Preparation method and application of superacid compound ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Synthesis of N-methylimidazolium propanesulfonate (PSMIM):

[0048] Synthesis of ionic liquid PSMIM with N-methylimidazole and 1,3-propane sultone: Add equimolar N-methylimidazole and 1,3-propane sultone into a three-necked flask, and then add 40ml of toluene as a solvent , stirred at 50°C for 24 hours under nitrogen protection, filtered to obtain a white solid precipitate, washed with ethyl acetate, 40°C rotary evaporation, and vacuum dried to obtain a white solid PSMIM.

[0049] Synthesis of N-methylimidazolidine sulfonate (BSMIM) The synthesis method is the same as above.

[0050] Put the synthesized ionic liquid and simulated sulfur solution into a test tube at a mass ratio of 1:5, stir with a shear for 10 minutes at 80°C, cool and let stand, separate the two phases, remove the upper oil phase, and measure the sulfur content and calculate the desulfurization rate. The desulfurization rate is shown in Table 1.

Embodiment 2

[0052] Preparation of sulfated sulfonic acid type ionic liquid (PSMIMHSO 4 - ):

[0053] Weigh the sulfonic acid-type ionic liquid of Example 1 and sulfuric acid in equal moles, control the reaction temperature to 90° C., and reflux and stir for 8-12 hours to obtain the sulfated sulfonic acid-type ionic liquid.

[0054] Synthesis of sulfated N-methylimidazolidine sulfonate (BSMIMHSO 4 - ) The synthesis method is the same as above.

[0055] The desulfurization method is as in Example 1. The desulfurization rate is shown in Table 1.

Embodiment 3

[0057] Preparation of Superacid Composite Ionic Liquid

[0058] ZrO 2 、TiO 2 , Fe 2 o 3 or SnO 2 Grind into a fine powder of less than 100 meshes, and add to the PSMIMHSO prepared above in an amount of 1:1 by weight 4 , mixed at 160°C for 1 h to prepare a superacid complex ionic liquid. where ZrO 2 、TiO 2 , Fe 2 o 3 , SnO 2 A solid superacid is formed with sulfuric acid in an ionic liquid.

[0059] The desulfurization method is as in Example 1. The desulfurization rate is shown in Table 2.

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Abstract

The invention discloses a superacid compound ionic liquid, and a preparation method and application thereof. The preparation method comprises a first step of adding metal oxide ZrO2, TiO2, Fe2O3 or SnO2 into a sulfated sulfonic acid ionic liquid and a second step of carrying out mixing. The invention has the following advantages: the preparation method is simple; the superacid compound ionic liquid has a high acid value, fully contacts with reactant and has good desulphurization activity; after completion of desulphurization, the superacid compound ionic liquid is subjected to simple settlement and separation, and after simple filtering and washing, the superacid compound ionic liquid can be repeatedly used; reaction conditions are mild; and the superacid compound ionic liquid has no corrosivity to equipment, is stable in moisture and air and nonvolatile, does not need hydrogen peroxide oxidizing agent, has an acid site and oxidation and extraction centers and can realize greenization in the whole process of desulphurization.

Description

technical field [0001] The invention relates to a new technology for reducing the sulfur content in fuel oil, in particular to a preparation method of a superacid composite ionic liquid catalytic system. Background technique [0002] Reducing the sulfur content of oil Catalytic hydrogenation is currently the main means of desulfurization of fuel oil in industry, but it is difficult to remove benzothiophene, dibenzothiophene and their derivatives. Deep catalytic hydrogenation will also reduce the content of olefins and aromatics, which will cause a sharp drop in the octane number of gasoline and diesel, a large investment in equipment and a sharp increase in operating costs. Therefore, the key to deep desulfurization is to develop new desulfurization technologies, such as adsorption desulfurization, complexation desulfurization, reactive desulfurization (oxidative desulfurization, alkylation reaction desulfurization, etc.), ionic liquid extraction and other non-hydrogenation ...

Claims

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Application Information

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IPC IPC(8): B01J31/38B01J31/28B01J31/26C10G29/28
Inventor 高艺茏唐博合金吴建祥张炜谭月月杨锡铎郑新萌门勇
Owner SHANGHAI UNIV OF ENG SCI