Polyphenol ether oligomer and products comprising same
An oligomer, polyphenol ether technology, applied in the direction of polyether coatings, polyether adhesives, adhesive types, etc., can solve problems such as poor compatibility, and achieve the effect of improving poor solubility
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Embodiment 1
[0054] [Example 1] Synthesis of polyphenol ether oligomer 1
[0055] Take monovalent copper bromide (3.42 grams, 24mmol) and put it into a 1000ml double-necked flask, add diethylamine (70.7g, 0.96mol), 1,3,5 trihydroxybenzene (6 grams, 47.5mmol) and toluene (500mL) as a solvent, heated to 50°C under an oxygen system, and then added monomer 2,6-dimethylphenol (58.1 grams, 470mmol), 2-allyl-6-methylphenol (22 grams, 96mmol) and a little hydrochloric acid, precipitated in a large amount of methanol.
[0056] The obtained precipitated product was collected by gravity filtration, dried and stored at 50°C to obtain polyphenol ether oligomer 1 with a yield of 52%; please refer to Table 1 for relevant synthesis experiments and electrical property data, dielectric constant (Dk )=3.05; dielectric loss factor (Df)=0.004; glass transition temperature (Tg)=196°C. The above reaction can be expressed as follows:
[0057]
[0058]
[0059] (Wherein, Y can be the same or different gro...
Embodiment 2
[0064] [Example 2] Synthesis of polyphenol ether oligomer 2
[0065] Get monovalent copper bromide (3.42 grams, 24mmol) and put it into a 1000ml double-necked flask, add diethylamine (70.7g, 0.96mol), 1,3,5 trihydroxybenzene (6 grams, 47.5mmol) and toluene ( 500mL) as a solvent, heated to 50°C under an oxygen system, then added monomer 2,6-dimethylphenol (58.1 grams, 470mmol), 2-allyl-6-methylphenol (22 grams, 96mmol ) and a little hydrochloric acid, precipitated in a large amount of methanol. The resulting precipitated product was collected by gravity filtration, dried and sealed at 50°C.
[0066] Epichlorohydrin (10 g, 100 mmol) was put into a 100 ml two-necked bottle, and the above product (1 g, 0.154 mmol) was added for terminal group modification. The above mixture was heated and reacted to 60° C. under a nitrogen system. Next, epichlorohydrin (2-(chloromethyl)oxirane, 1 g, 13 mmol) was added, and then the solvent was removed by vacuum distillation, then dissolved in t...
Embodiment 3
[0076] [Example 3] Synthesis of polyphenol ether oligomer 3
[0077] Get monovalent copper bromide (3.42 grams, 24mmol) and put it into a 1000ml double-necked flask, add diethylamine (70.7g, 0.96mol), 1,3,5 trihydroxybenzene (6 grams, 47.5mmol) and toluene ( 500mL) as a solvent, heated to 50°C under an oxygen system, then added monomer 2,6-dimethylphenol (58.1 grams, 470mmol), 2-allyl-6-methylphenol (22 grams, 96mmol ) and a little hydrochloric acid, precipitated in a large amount of methanol. The resulting precipitated product was collected by gravity filtration, dried and sealed at 50°C.
[0078] Take the above product (1 g, 0.154 mmol) into a 100 ml double-neck flask, add 10 mL of tetrahydrofuran (THF) solvent, and heat to 60° C. under a nitrogen system. Next, 0.2 g of a 50% aqueous sodium hydroxide solution was added, followed by the slow addition of p-chloromethylstyrene (0.8 mL, 1.1 mmol). After the reaction, the solution was washed with deionized water to remove impu...
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