A kind of synthetic method of bisphenols
A synthesis method and phenol technology, applied in the field of organic synthesis, can solve the problems of reduced service life, complex process and high cost of heat transfer oil, and achieve the effects of improving purity and yield, simplifying operation process and reducing reaction cost
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Embodiment 1
[0024] While stirring, 284g (3.0mol) of phenol and 0.5g of benzenesulfonic acid were heated to 130°C under nitrogen protection, and 100g (1.0mol) of 98% sulfuric acid was added dropwise therein, and the dropwise reaction time was 3h . The sulfonated reaction solution is kept warm in an oil bath and dehydrated with a slight negative pressure of -0.005MPa. After dripping the sulfuric acid, keep it warm for 2.5 hours, then raise the temperature to 175°C, and keep it warm for 5.5 hours until the system becomes molten. Samples are taken and analyzed by HPLC. The results showed that the composition (weight ratio) of 4,4'-dihydroxydiphenylsulfone / 2,4'-dihydroxydiphenylsulfone / trihydroxytriphenyldisulfone=92.5 / 7.0 / 0.5. All the excess phenol has been distilled off, and there is no residue in the system, and the crude product of 4,4'-dihydroxydiphenyl sulfone is obtained. The steamed phenol is used for the next application.
[0025] Dissolve the crude product in dilute lye, adjust th...
Embodiment 2
[0027] While stirring, 284g (3.0mol) of phenol and 0.45g of benzenesulfonic acid were heated up to 135°C under nitrogen protection, and 100g (1.0mol) of 98% sulfuric acid was added dropwise thereto, and the dropwise reaction time was 2.8 h. The sulfonated reaction solution is kept warm in an oil bath and dehydrated with a slight negative pressure of -0.006MPa. After dripping the sulfuric acid, keep it warm for 3 hours, then raise the temperature to 180°C, and keep it warm for 5 hours until the system becomes molten. Samples are taken and analyzed by HPLC. The results showed that the composition (weight ratio) of 4,4'-dihydroxydiphenylsulfone / 2,4'-dihydroxydiphenylsulfone / trihydroxytriphenyldisulfone=92.4 / 7.0 / 0.6. All the excess phenol has been distilled off, and there is no residue in the system, and the crude product of 4,4'-dihydroxydiphenyl sulfone is obtained. The steamed phenol is used for the next application.
[0028] Dissolve the crude product in dilute lye, adjust ...
Embodiment 3
[0030] While stirring, 237g of phenol and 0.4g of benzenesulfonic acid were heated up to 122°C under nitrogen protection, and 100g of 98% sulfuric acid was added dropwise thereto, and the dropwise reaction time was 3.5h. The sulfonated reaction solution is kept warm in an oil bath and dehydrated with a slight negative pressure of -0.005MPa. After dripping the sulfuric acid, keep it warm for 2.5 hours, then raise the temperature to 170°C, and keep it warm for 5.8 hours until the system becomes molten. Samples are taken and analyzed by HPLC. The results showed that the composition (weight ratio) of 4,4'-dihydroxydiphenylsulfone / 2,4'-dihydroxydiphenylsulfone / trihydroxytriphenyldisulfone=92.3 / 7.1 / 0.6. All the excess phenol has been distilled off, and there is no residue in the system, and the crude product of 4,4'-dihydroxydiphenyl sulfone is obtained. The steamed phenol is used for the next application.
[0031] Dissolve the crude product in dilute lye, adjust the pH to 9.0, ob...
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