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Preparation method of iron-based metal organic framework immobilization ionic liquid and application thereof

An ionic liquid, organic framework technology, applied in refining to remove heteroatoms, petroleum industry, treatment of hydrocarbon oil, etc., can solve problems such as endangering public health, rising gasoline costs, frequent haze weather, etc., and achieve good application prospects, Good effect and low equipment investment

Active Publication Date: 2019-10-15
FUQING BRANCH OF FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Since the 21st century, automobiles have brought great convenience to human beings, but the burning of sulfur-containing gasoline has caused frequent smog and haze, seriously endangering public health
To achieve deep desulfurization, it needs to be carried out under harsh conditions, such as high temperature and high pressure, high hydrogen consumption, expensive precious metal catalysts, etc., which will lead to an increase in gasoline costs

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0032] A method for preparing an iron-based metal-organic framework immobilized ionic liquid, comprising the following steps:

[0033] S1, ionic liquid [Ps-N-Bz(Me) 2 ] Generation of TSA: Dissolve 0.1 molar parts of 1,3-propane sultone in 100 volume parts of ethyl acetate, slowly add 0.1 molar parts of N, N-dimethylbenzylamine under ice bath, in React at 50-70°C for 8-12 hours, centrifuge, wash, and vacuum-dry to obtain a white precursor salt solid; add 20-30 parts by volume of distilled water to the white precursor salt solid, and slowly add it dropwise with the white precursor salt Solid equimolar p-toluenesulfonic acid solution, react at 75-95°C for 10-16 hours, remove water by rotary evaporation, wash 3 times with 2-3 times ethyl acetate, remove ethyl acetate by rotary evaporation and vacuum Dry to obtain ionic liquid [Ps-N-Bz(Me) 2 ]TSA;

[0034] S2, the generation of iron-based metal-organic framework immobilized ionic liquid: the liquid obtained in step S1 [Ps-Bz(Me)...

Embodiment 1

[0037] A method for preparing an iron-based metal-organic framework immobilized ionic liquid, comprising the following steps:

[0038] S1, ionic liquid [Ps-N-Bz(Me) 2 ] Formation of TSA: Dissolve 0.1 mol of 1,3-propane sultone in 100 ml of ethyl acetate, slowly add 0.1 mol of N,N-dimethylbenzylamine under ice-cooling, at 50°C React for 8 hours, centrifuge, wash, and vacuum-dry to obtain a white precursor salt solid; add 20ml of distilled water to the white precursor salt solid, and slowly add p-toluenesulfonic acid solution that is equimolar to the white precursor salt solid, React at 75°C for 10 hours, remove water by rotary evaporation, wash 3 times with 2 times ethyl acetate, remove ethyl acetate by rotary evaporation and vacuum dry to obtain ionic liquid [Ps-N-Bz(Me) 2 ]TSA;

[0039] S2, generation of iron-based metal-organic framework-immobilized ionic liquid: 0.08mol of the liquid obtained in step S1 [Ps-Bz(Me) 2]TSA, 0.08mol ferric chloride, 0.1mol 2-aminoterephthali...

Embodiment 2

[0042] A method for preparing an iron-based metal-organic framework immobilized ionic liquid, comprising the following steps:

[0043] S1, ionic liquid [Ps-N-Bz(Me) 2 ] Formation of TSA: Dissolve 0.1 mol of 1,3-propane sultone in 100 ml of ethyl acetate, slowly add 0.1 mol of N,N-dimethylbenzylamine under ice bath, at 60°C React for 10 hours, centrifuge, wash, and vacuum-dry to obtain a white precursor salt solid; add 30ml of distilled water to the white precursor salt solid, and slowly add p-toluenesulfonic acid solution that is equimolar to the white precursor salt solid, React at 85°C for 12 hours, remove water by rotary evaporation, wash 3 times with 3 times ethyl acetate, remove ethyl acetate by rotary evaporation and vacuum dry to obtain ionic liquid [Ps-N-Bz(Me)2]TSA;

[0044] S2, iron-based metal-organic framework immobilized ionic liquid: 0.12mol of the liquid [Ps-Bz(Me)2]TSA obtained in step S1 and 0.12mol of ferric chloride, 0.1mol of 2-aminoterephthalic acid and 0...

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Abstract

The invention relates to iron-based metal organic framework immobilization ionic liquid. The iron-based metal organic framework immobilization ionic liquid comprises an iron-based metal organic framework, and ionic liquid fixed to the iron-based metal organic framework, wherein the iron-based metal organic framework is NH2-MIL-88B(Fe); the ionic liquid is [Ps-Bz(Me)2]TSA. The preparation method comprises the following steps: dissolving 1,3-propane sultone to ethyl acetate; adding dimethyl benzylamine to react; then adding p-methylbenzene sulfonic acid solution; carrying out a reaction to generate the ionic liquid [Ps-Bz(Me)2]TSA; dissolving the ionic liquid, ferric chloride, 2-aminoterephthalic acid and acetic acid in N,N-dimethyl formamide; crystallizing to obtain the iron-based metal organic framework immobilization ionic liquid. The iron-based metal organic framework immobilization ionic liquid is applicable to deep desulfuration of gasoline; the reaction conditions are mild; the deep desulfuration effect is good; the recovery is easily carried out; the activity is not obviously reduced after cyclically using in eight times.

Description

technical field [0001] The invention relates to an immobilized ionic liquid, in particular to a preparation method and application of an immobilized ionic liquid. Background technique [0002] NH 2 -MIL-88B(Fe): It is a kind of MOFs (metal organic framework compound) material. [0003] Ionic liquids refer to salts that are liquid at or near room temperature and are composed entirely of anions and cations, also known as low-temperature molten salts. As an ionic compound, the main reason for the low melting point of ionic liquid is that the asymmetry of some substituents in its structure prevents the ions from stacking regularly into crystals. [0004] Immobilized ionic liquid: the immobilized ionic liquid is immobilized on some kind of solid carrier, so as to obtain the further use of the immobilized ionic liquid. Immobilized ionic liquid is a liquid film formed by filling ionic liquid into the gap of porous organic or inorganic carrier. Immobilized ionic liquid can increa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10G45/04C08G83/00
CPCC08G83/008C10G45/04C10G2300/202
Inventor 杨金杯俞舒月陈文韬王昌伟余美琼陈玉成
Owner FUQING BRANCH OF FUJIAN NORMAL UNIV
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