Fluorine-containing liquid crystal elastomer and preparation method and application thereof
A liquid crystal elastomer, liquid technology, applied in applications, liquid crystal materials, other household appliances, etc., can solve the problem that the working durability of the main chain cross-linked liquid crystal elastomer needs to be improved, so as to improve mechanical properties, improve solubility, and prolong work. effect of time
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Embodiment 1
[0054] Embodiment 1: the synthesis of NIR823
[0055]
[0056] Preparation of compound 3: Add 3.60 g of acrylic acid, 7.80 g of 9-decen-1-ol, 0.61 g of 4-dimethylaminopyridine, 9.60 g of 1-ethyl-(3-di Methylaminopropyl) carbonyl diimide hydrochloride, 13.90 ml triethylamine and 150 ml dichloromethane. Under the protection of nitrogen, the reaction was stirred at room temperature for 12 hours. After the reaction, the solvent was removed by a rotary evaporator. The crude product was then purified by column chromatography (petroleum ether:ethyl acetate=4:1) to obtain compound 3.
[0057] Preparation of compound 5: 3.15 g of compound 3, 545 mg of 3-aminophenol and 150 ml of acetic acid were successively added to a 100 mL round bottom flask. The reaction mixture was stirred at 80° C. for 5 hours. The crude product was then purified by column chromatography (petroleum ether:ethyl acetate=4:1) to obtain compound 5.
[0058] Preparation of NIR823: 0.74 g of compound 5, 100 mg o...
Embodiment 2
[0061] Embodiment 2: Preparation of fluorine-containing liquid crystal polymer
[0062]
[0063] Preparation of compound 9: Add 9.74 grams of hydroquinone (formula 7), 10 grams of p-hydroxybenzoic acid (formula 8), 0.35 grams of boric acid, 0.5 milliliters of sulfuric acid, 10 milliliters of xylene and 40 milliliters of toluene. The mixture was refluxed at 137°C for 5 hours. After the reaction, the solvent was removed by suction filtration, and the solid product was washed with water until it was colorless. The product can be directly used in the next reaction.
[0064] Preparation of compound 11: 4.60 g of compound 9, 13.8 g of potassium carbonate, 6.52 g of 6-bromo-1-hexene and 100 ml of acetonitrile were successively added into a 250 ml three-necked flask. The reaction was refluxed at 90°C for 5 hours. After the reaction, potassium carbonate was removed by suction filtration. The crude product was separated by column chromatography (petroleum ether: ethyl acetate = 4:...
Embodiment 3
[0067] Example 3: Preparation of Fluorinated Liquid Crystal Elastomer
[0068] Dissolve 30 mg of NIR823, 300 mg of CFCI666, and 6 mg of Grubbs second-generation catalyst in 2 mL of toluene and sonicate for 2 min, and pour it into a custom-made polytetrafluoroethylene mold ( Figure 4 a), heated to 60°C under nitrogen protection atmosphere, after two hours of reaction, cooled the mold to room temperature and carefully removed the polymer film ( Figure 4 b-c) to complete the first preliminary cross-linking to obtain a preliminary cross-linked product. Stretch the film to 1.5-1.8 times the original length along the long axis under a certain external force and fix the film ( Figure 4 d), put it into a 120°C vacuum oven for 48 hours to complete the second cross-linking ( Figure 4 e), after the reaction, the film is cooled to room temperature to obtain the corresponding fluorine-containing liquid crystal elastomer film ( Figure 4 f). The flow chart of the above preparation p...
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