Tetraethyl-p-cyclobenzene Molecular Grade Conformal Coating Material and Its Application
A coating material and cyclobenzene technology, applied in the field of tetraethyl-p-cyclobenzene molecular-level conformal coating materials, can solve the problem of reducing the mechanical properties, electrical insulation properties and protective properties, light reflectivity, The problem of strong refraction and high optical birefringence can achieve the effect of flexible and easy film-forming protection, good physical and mechanical properties, and good solubility
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Embodiment 1
[0038] Embodiment 1: Synthesis of tetraethyl-p-cyclobenzene compounds by catalytic hydrogenation method
[0039]
[0040] 1. Carry out bromination reaction of cyclobenzene to obtain 12,15,42,45-tetrabromo-p-cyclobenzene: Install a conduit connected to the hydrogen bromide gas absorption device on a 250mL three-neck round bottom flask, and then add 30mL (589mmol, 94.2g) of bromine and 150mg (0.6mmol) of iodine, sealed and magnetically stirred under ice water cooling, and the reaction was placed in a dark place as much as possible. When the temperature was below 10°C, 10.0 g (48 mmol) p-cyclobenzene was added in 10 times within 12 hours. Note the rapid evolution of hydrogen bromide gas at this point. After the addition of p-cyclobenzene was completed, return to room temperature and continue stirring for 3 days, and track the reaction by TLC until completion. After completion of the reaction, decompose the reaction with 300 mL of 20% aqueous sodium hydroxide solution, collec...
Embodiment 2
[0051] Embodiment 2: Synthesis of tetraethyl-p-cyclobenzene compound by coupling method
[0052]
[0053] Add 50mmol (1.20g) of magnesium strips and 50mL of anhydrous ether into a 150mL round-bottomed flask, and drop 20 drops of a mixture consisting of 10mL of anhydrous ether and 50mmol (7.80g) of ethyl iodide into the round-bottomed flask. After the reaction is started, the ethyl iodide solution is added dropwise to the reaction bottle in batches to react with the magnesium bars. After the dropwise addition, continue to react for a certain period of time to obtain the Grignard reagent of ethyl iodide.
[0054] 10 mmol (5.24 g) of tetrabromo-p-cyclobenzene and 5% mmol of [1,3-bis(diphenylphosphine) propane]-nickel(II) chloride (Ni(dppp)Cl 2 ) was added to a 250mL round bottom flask, and 50mL of anhydrous ether was added to dissolve it. Under cooling in an ice bath, the Grignard reagent prepared above was added dropwise to the reaction mixture with stirring. Return to roo...
Embodiment 3
[0056] Using a vacuum vapor deposition process, the tetraethyl-p-cyclobenzene-based molecular-level conformal coating material obtained in the above-mentioned embodiment 1-2 is placed in the sublimation chamber of the coating equipment, and the vacuum base pressure is lower than 10 -6 Under the state of Torr degree, first vacuum gasification at 110-120°C, then crack at 640-650°C when passing through the cracking chamber, and then polymerize into high-molecular polymers in the deposition chamber at 3mTorr deposition pressure and normal temperature, and grow On the sample to be protected, a protective film is formed, with uniform thickness, dense and pinhole-free, transparent and stress-free, excellent electrical insulation and protection, good physical and mechanical properties, low friction coefficient, solvent resistance and acid and alkali resistance Excellent properties.
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