Production of polycyclic aromatic acetyl compounds
A vinyl compound and polycyclic aromatic technology, applied in the field of polycyclic aromatic vinyl compounds, can solve difficult problems such as polycyclic aromatic compounds, and achieve low dielectric loss, low dielectric constant, and high refractive index Effect
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Embodiment 1
[0030]Table 1 shows the composition of crude divinylbiphenyl as a raw material. 625 g of crude divinylbiphenyl was dissolved in 625 g of toluene, and cooled to 5° C. while stirring. After cooling, 500 g of bromine was slowly added dropwise while maintaining the reaction temperature at 5 to 20°C. When about half of the bromine has just been dripped, crystallization begins. After bromine was added dropwise, white crystals were recovered by filtration. Further, recrystallization was performed twice using toluene as a solvent to obtain 114.5 g of 3,3'-bis(1,2-dibromoethyl)biphenyl.
[0031] Add 114.5 g of recrystallized and refined 3,3'-bis(1,2-dibromoethyl)biphenyl and 0.3 g of tert-butylcatechol to a mixed solvent of 458 g of toluene and 19.8 g of pure water, and stir Heat to 80°C. While keeping the reaction temperature at 80-90°C, add zinc powder little by little until it no longer dissolves. After the addition of zinc was completed, the mixture was washed three times with...
Embodiment 2
[0035] 625 g of the same crude divinylbiphenyl as in Example 1 was dissolved in 156 g of toluene and 156 g of n-heptane, and cooled to 5° C. while stirring. After cooling, 500 g of bromine was slowly added dropwise while keeping the reaction temperature at 5-20°C. When about half of the bromine has just been dripped, crystallization begins. After bromine was added dropwise, white crystals were recovered by filtration. Further, recrystallization was performed twice using toluene as a solvent to obtain 126.0 g of 3,3'-bis(1,2-dibromoethyl)biphenyl.
[0036] Add 126.0 g of refined 3,3'-bis(1,2-dibromoethyl)biphenyl and 0.3 g of tert-butylcatechol to a mixed solvent of 458 g of dioxane and 45.8 g of pure water, and stir Heat to 80°C. While maintaining the reaction temperature at 80-90°C, add zinc powder little by little until it does not dissolve. After the addition of zinc, wash with 1000ml of water for 3 times, use a rotary evaporator to distill off dioxane to obtain purity ...
Embodiment 3
[0044] Table 3 shows the composition of crude acenaphthylene as a raw material. 500 g of crude acenaphthylene was dissolved in 500 g of toluene, and cooled to 5° C. while stirring. After cooling, slowly add 474 g of bromine dropwise while keeping the reaction temperature at 5-10°C. When about half of the bromine has just been dropped, crystallization begins. After adding bromine dropwise, filter and recover the crystals. Further, recrystallization was performed twice using toluene as a solvent to obtain 321 g of 1,2-dibromoacenaphthylenene.
[0045] 321 g of purified 1,2-dibromoacenaphthylene and 0.2 g of tert-butylcatechol were added to a mixed solvent of 321 g of tetrahydrofuran and 15.8 g of pure water, and heated to 80°C while stirring. While keeping the reaction temperature at 80-90°C, add zinc powder little by little until it does not dissolve. After the addition of zinc was completed, the mixture was washed three times with 1000 ml of water, and tetrahydrofuran was d...
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