Preparation method and application of 4-methyl-5-vinyl thiazolyl polymerization ionic liquid
An ionic liquid and thiazolyl-based technology is applied in the preparation of ionic liquid and its catalytic application field, and achieves the effects of low catalyst dosage, good catalytic activity and high catalytic activity
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[0039] The preparation method of 4-methyl-5-vinylthiazolyl polymerized spherical ionic liquid catalyst comprises the steps:
[0040] (1) Synthesis of ylide: use 1,3-propane sultone, ethyl acetate and 4-methyl-5-vinylthiazole as raw materials to prepare ylide;
[0041] (2) Synthesis of ionic liquid monomer: react the ylide obtained in step (1) with Brønsted acid to obtain ionic liquid monomer;
[0042] (3) Synthesis of polymerized spherical ionic liquid: Fe modified by the ionic liquid monomer prepared in step (2), divinylbenzene and 3-(methylpropyloxy)propyltrimethoxysilane 3 o 4 The polymerized spherical ionic liquid is obtained by ultrasonically dispersing in a solvent, adding an initiator, and heating and polymerizing.
[0043] More specifically, the preparation method of 4-methyl-5-vinylthiazolyl polymerized spherical ionic liquid catalyst comprises the following steps:
[0044] (1) Synthesis of ylide: Dissolve 0.05~0.1 mol of 1,3-propane sultone in 50~300mL of ethyl ac...
Embodiment 1
[0057] 4-Methyl-5-vinylthiazolyl polymerized spherical ionic liquid catalyst, its structural formula is as follows:
[0058] ;
[0059] Where R- represents trifluoromethanesulfonate.
[0060] The preparation method of 4-methyl-5-vinylthiazolyl polymerized spherical ionic liquid catalyst comprises the steps:
[0061] (1) Synthesis of ylide: Dissolve 0.1 mol of 1,3-propane sultone in 250 mL of ethyl acetate in an ice-water bath, and add 0.1 mol of 4-methyl-5 -Vinylthiazole, at 60°C, stir the reaction for 48 h, after the reaction stops, filter, wash the solid product with ethyl acetate three times, and dry it in vacuum for 12 h to obtain the ylide;
[0062] (2) Synthesis of ionic liquid monomer: Dissolve the ylide obtained in step (1) in 350 mL of deionized water under ice-water bath conditions, and add equimolar trifluoromethane dropwise under full stirring Sulfonic acid was reacted at 70°C for 24 hours under the protection of nitrogen. After the reaction stopped, the disti...
Embodiment 2
[0070] 4-Methyl-5-vinylthiazolyl polymerized spherical ionic liquid catalyst, its structural formula is as follows:
[0071]
[0072] Where R- represents hydrogen sulfate.
[0073] The preparation method of 4-methyl-5-vinylthiazolyl polymerized spherical ionic liquid catalyst comprises the steps:
[0074] (1) Synthesis of ylide: Dissolve 0.08 mol of 1,3-propane sultone in 100 mL of ethyl acetate in an ice-water bath, and add 0.08 mol of 4-methyl-5 -Vinylthiazole, at 80°C, stir the reaction for 24 h, after the reaction stops, filter, wash the solid product with ethyl acetate three times, and dry it in vacuum for 8 h to obtain the ylide;
[0075] (2) Synthesis of ionic liquid monomer: Dissolve the ylide obtained in step (1) in 200 mL of deionized water under the condition of ice-water bath, and add equimolar concentrated sulfuric acid drop by drop under full stirring. React at 90 °C for 12 h under the protection of nitrogen. After the reaction is stopped, distilled water is...
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