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

Abstract

The invention relates to an iron-based metal-organic framework immobilized ionic liquid, which comprises: an iron-based metal-organic framework and an ionic liquid fixed on the iron-based metal-organic framework, and the iron-based metal-organic framework is NH 2 ‑MIL‑88B(Fe), the ionic liquid is [Ps‑Bz(Me) 2 ] TSA. Its preparation method comprises dissolving 1,3-propane sultone in ethyl acetate, adding dimethylbenzylamine to react, then adding p-toluenesulfonic acid solution to react to generate ionic liquid [Ps-Bz(Me) 2 ] TSA, dissolving ionic liquid, ferric chloride, 2-aminoterephthalic acid and acetic acid in N,N-dimethylformamide and then crystallizing to obtain the iron-based metal-organic framework immobilized ionic liquid. Applied in the deep desulfurization of gasoline, the required reaction conditions are mild, the effect of deep desulfurization is good, easy to recycle, and the activity does not decrease significantly after being recycled for 8 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...

Examples

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...

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...

Examples

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...