A thermosensitive nanogel based on hydroxyimidazole ionic liquid and its preparation method
A technology of ionic liquid and nanogel, which is applied in the field of new materials, can solve the problems of toxicity of organisms and non-adjustable temperature range, and achieve the effects of adjustable particle size, convenient operation and simple process
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Embodiment 1
[0031] Embodiment 1, based on hydroxyl imidazole ionic liquid nanogel (CLPNx 1 -OH) Preparation
[0032] (1) Preparation of 1-vinyl-3-hydroxyethylimidazole bromide ionic liquid ([VEOIm]Br): 1-vinylimidazole (1.4050g, 14.93mmol) and 2-bromoethanol (2.0077g, 16.06 mmol) were mixed and added to a 50mL round bottom flask, and then 20mL of absolute methanol was added. in N 2 Under protection, the reaction was stirred and refluxed at 65°C for 48h. After the reaction, the mixture was poured into 50 mL of diethyl ether for precipitation, and then the solid was recrystallized from diethyl ether to obtain a white crystal [VEOIm]Br. Yield: 76.4%. The synthetic reaction formula is as follows:
[0033]
[0034] (2) Preparation of 4-vinylbenzyl-triphenylphosphonium chloride ionic liquid ([VBTP]Cl): 4-chloromethylstyrene (1.5276g, 10mmol) and triphenylphosphine (3.1465g , 12mmol) were mixed and added to a 100mL round bottom flask, and then 50mL of acetone was added. in N 2Under pr...
Embodiment 2
[0039] Embodiment 2, based on hydroxyl imidazole ionic liquid nanogel (CLPNy 1 -OH) Preparation
[0040] (1) Preparation of 1-vinyl-3-hydroxyethylimidazolium bromide ionic liquid ([VEOIm]Br): same as Example 1.
[0041] (2) Preparation of 1-vinyl-3-(4-vinylbenzyl)imidazolium chloride ionic liquid ([VVBIm]Cl): 4-chloromethylstyrene (3.0524g, 20mmol) and 1-ethylene Kimidazole (2.2560 g, 24 mmol) was mixed and added to a 100 mL round bottom flask, followed by 50 mL of absolute methanol. in N 2 Under protection, the reaction was stirred and refluxed at 70°C for 48h. After the reaction, the mixture was poured into 150 mL of diethyl ether, the product was washed with diethyl ether, and then placed in a vacuum oven at room temperature to dry overnight to obtain a yellow liquid, which was [VVBIm]Cl. Yield: 88.6%. The synthetic reaction formula is as follows:
[0042]
[0043] (3) The target product——preparation of nanogel based on hydroxyimidazole ionic liquid: [VEOIm]Br (0.1...
Embodiment 3
[0046] Embodiment 3, based on hydroxyl imidazole ionic liquid nanogel (CLPNx 2 -OH) Preparation
[0047] (1), (2) are the same as embodiment 1;
[0048] (3) Preparation of hydroxyimidazole-based ionic liquid nanogel: [VEOIm]Br (0.8771g, 4.00mmol), [VBTP]Cl (0.2071g, 0.50mmol) and cross-linking agent EGDMA (0.2056g, 1.04mmol) Mix and add to a 100mL round bottom flask, add 50mL of absolute methanol and AIBN (0.0090g, 0.055mmol), in N 2 Under protection, the reaction was stirred and refluxed at 70°C for 64h. At the end of the reaction, a light yellow emulsion is obtained, which is the target product CLPNx 2 -OH, yield: 64.56%. Synthetic reaction formula is the same as embodiment 1. In the structural formula, m=19, p=9, q=73. It was determined that the UCST of the nanogel was 0°C.
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