Preparation method and application of high-strength anti-icing organogel
An organogel, anti-icing technology, applied in the field of functional polymer materials, can solve the problems of complex preparation process, poor mechanical properties, limited application, etc., and achieves controllable molecular weight, mild and controllable reaction conditions, and gelation time. short effect
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Embodiment 1
[0045] Preparation of fluorine-containing organogels
[0046] Preparation of norbornenyl trifluoroethyl ester:
[0047] Take 5-norbornene-2-carboxylic acid (4.49g), trifluoroethanol (1.65g) and trimethylacetic anhydride (TA) (3.35g) in a 25ml flask, add 10ml of tetrahydrofuran (THF) to dissolve , keep stirring at room temperature and introduce nitrogen gas, then dissolve 4-dimethylaminopyridine (DMAP) (19.54mg) in 2ml THF, add it to the flask, gradually heat up to 60 ℃ and react for 24h, then cool to room temperature to remove the solvent, An appropriate amount of dichloromethane was added, washed three times with saturated NaHCO3 solution, saturated NaCl solution and deionized water respectively, dried and filtered to remove the solvent, and dried at 40°C to obtain a white viscous liquid, namely norbornenyl trifluoroethyl ester, Figure 4 It can be seen that the synthesis was successful.
[0048] Synthesis of Dinorbornenyl Glycol Esters:
[0049]Take 5-norbornene-2-carboxy...
Embodiment 2
[0054] Preparation of fluorine-containing organogels
[0055] Preparation of norbornenyl octafluoropentyl ester:
[0056] Take 5-norbornene-2-carboxylic acid (6.91g), octafluoropentanol (11.37g) and trimethylacetic anhydride (TA) (9.31g) in a 25ml flask, add 10ml of tetrahydrofuran (THF) to make it Dissolve, keep stirring at room temperature and pass nitrogen gas, then dissolve 4-dimethylaminopyridine (DMAP) (59.86mg) in 2ml THF, add it to the flask with a syringe, keep stirring and pass nitrogen gas for 30min, remove nitrogen gas, and gradually heat up to After 60 °C to stabilize the reaction for 24 h, the instrument was removed and cooled to room temperature for rotary evaporation, an appropriate amount of dichloromethane was added, washed three times with saturated NaHCO3 solution, saturated NaCl solution and deionized water respectively, dried and filtered to remove the solvent, and dried at 50 °C. After drying, a white viscous liquid is obtained, namely norbornenyl octaf...
Embodiment 3
[0063] Preparation of fluorine-containing organogels
[0064] Preparation of norbornenyl dodecafluoroheptyl ester:
[0065] Take 5-norbornene-2-carboxylic acid (6.91g), dodecafluoroheptanol (16.27g) and trimethylacetic anhydride (TA) (9.31g) in a 25ml flask, add 10ml of tetrahydrofuran (THF) It was dissolved, kept stirring at room temperature and passed nitrogen, and then 4-dimethylaminopyridine (DMAP) (59.86 mg) was dissolved in 2 ml of THF, added to the flask with a syringe, kept stirring for 30 min, and then the nitrogen was removed, and the temperature was gradually increased. After the reaction was stabilized at 60 °C for 24 h, the instrument was removed and cooled to room temperature for rotary evaporation, an appropriate amount of dichloromethane was added, washed three times with saturated NaHCO3 solution, saturated NaCl solution and deionized water, respectively, dried and filtered to remove the solvent, at 60 °C After drying, a white viscous liquid is obtained, name...
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