2,6-dimethyl-4-(tri(3,5-dimethyl-phenyl)methyl)phenol, preparation and end-functional polyarylether
A technology of dimethylphenyl and dimethylbromobenzene, which is applied in the field of terminal-functionalized polyarylethers, can solve the problem of few types of polyarylethers, and achieve excellent heat resistance and good application prospects
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Embodiment 1
[0034] Example 1: Synthesis of 2,6-dimethyl-4-(tri(3,5-dimethylphenyl)methyl)phenol
[0035] The first step reaction: in a strictly anhydrous, oxygen-free and argon protective atmosphere, add 15.40mL 3,5-dimethylbromobenzene and 300mL refined tetrahydrofuran to a 1000mL round bottom flask equipped with magnetic stirring, and use liquid nitrogen- Acetone bath lowered the temperature of the system to -78°C. After the temperature stabilized, slowly add 49.90 mL of n-hexane solution with a concentration of 2.5 mol / L n-butyl lithium dropwise, and stirred for half an hour. During this period, liquid nitrogen was continuously added to keep the temperature stable. Then add 4.36mL of diethyl carbonate, wait for the system to cool down naturally, and continue to stir for 10 hours. After the reaction is complete, pour it into 500mL of ionized water, and extract it with dichloromethane for 3 times. g, that is, tris(3,5-dimethylphenyl)methanol.
[0036] The second step reaction: add 3.45g...
Embodiment 2
[0038] Example 2: Synthesis of end-capped polyethersulfone with tetrakis(3,5-dimethylphenyl)methane structure
[0039] 0.0852 g (0.19 mmol) of 2,6-dimethyl-4-(tris(3,5-dimethylphenyl)methyl)phenol, 4,4'- Dihydroxydiphenylsulfone 2.5027g (10mmol), 4,4'-difluorodiphenylsulfone 2.666g (10.095mmol), potassium carbonate 1.6585g (0.012mol), solvent sulfolane 16.71mL, toluene 10mL as azeotropic dehydrating agent. The reaction was carried out under the protection of argon, and the toluene was distilled off after 4 hours with water at 155°C, and the temperature was raised to 210°C for 8 hours, and the material was discharged in deionized water to obtain a strip-shaped solid, which was washed 5 times with deionized water and ethanol. Vacuum-dried at 80°C to obtain a polyarylether having a tetrakis(3,5-dimethylphenyl)methane structure at the end group as shown in the following structural formula.
[0040]
Embodiment 3
[0041] Example 3: Preparation of polyethersulfone with bromomethylphenyl end groups
[0042] Under the protection of an inert atmosphere, put 1g of end-capped polyethersulfone and 20mL of 1,1,2,2-tetrachloroethane into a 50mL three-necked flask equipped with mechanical stirring, and raise the temperature to 80°C until the solid is completely dissolved , cool down to room temperature, put in 0.2134g N-bromosuccinimide and 0.0508g dibenzoyl peroxide, raise the temperature to 80°C, the reaction time is 8 hours, cool down the reaction vessel to room temperature; pour the solution into 100mL without in water and methanol, filtered, washed 5 times with ethanol, and dried to obtain a polyethersulfone polymer containing bromomethyl phenyl groups with the following structural formula.
[0043]
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