Preparation method of high-purity 4, 4 '-biphenol
A biphenol-based biphenol-based technology, applied in the field of high-purity 4, can solve the problems of complex and uncontrollable production operations, large production energy consumption, increased production costs, etc., and achieve low equipment requirements and meet large batches Manufacturing needs, easy-to-achieve effects
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[0034] The preparation method of the high-purity 4,4'-diphenol provided by the application comprises the following steps:
[0035] S1: Preparation of 2,6-di-tert-butylphenol
[0036] Add phenol and aluminum materials into the reaction vessel, raise the temperature to 140-160°C, stir for 1-2 hours, lower the reaction temperature in the reaction vessel to 110-120°C, feed isobutylene into the reaction vessel, and control the temperature in the reaction vessel. The pressure is 0.4-0.6Mpa. After reacting for 4-6 hours, continue to reduce the reaction temperature in the reaction vessel to 50-60°C and react for 1-2 hours to obtain the crude product of 2,6-di-tert-butylphenol. Add sodium hydroxide to the crude product of tert-butylphenol, react at 180-220°C for 1-2 hours, filter the reaction product and distill under reduced pressure to obtain purified 2,6-di-tert-butylphenol;
[0037] S2: Preparation of 3,3',5,5'-tetra-tert-butylbiphenol by oxidative coupling reaction
[0038] Take...
Embodiment 1
[0054] S1: Preparation of 2,6-di-tert-butylphenol
[0055] Add 0.3mol of phenol and 0.006mol of aluminum powder into the reaction vessel, raise the temperature to 150°C, stir the reaction at a low speed of 200rpm / min for 1h, then reduce the reaction temperature in the reaction vessel to 120°C, and pass into the reaction vessel 0.6mol isobutene, control the pressure in the reaction vessel to 0.6Mpa, after 4 hours of reaction, continue to reduce the reaction temperature in the reaction vessel to 60°C, and react for 1 hour to obtain the crude product of 2,6-di-tert-butylphenol, which is Add 0.02mol sodium hydroxide to the crude product of tert-butylphenol, configure it as a 20% sodium hydroxide solution by mass fraction, react at 200°C for 1 hour, and filter and distill the reaction product under reduced pressure to obtain 2,6-di-tert-butylphenol Purified butylphenol;
[0056] S2: Preparation of 3,3',5,5'-tetra-tert-butylbiphenol by oxidative coupling reaction
[0057] Get 0.2m...
Embodiment 2
[0061] S1: Preparation of 2,6-di-tert-butylphenol
[0062] Add 0.3mol of phenol and 0.007mol of aluminum chloride into the reaction vessel, raise the temperature to 150°C, stir the reaction at a low speed of 250rpm / min for 1.5h, then reduce the reaction temperature in the reaction vessel to 110°C, and pour Feed 0.65mol of isobutene, control the pressure in the reaction vessel to be 0.5Mpa, after reacting for 4 hours, continue to reduce the reaction temperature in the reaction vessel to 60°C, react for 1 hour, and obtain the crude product of 2,6-di-tert-butylphenol, which can be obtained at 2,6 - Add 0.03 mol of sodium hydroxide to the crude product of di-tert-butylphenol to form a 20% by mass sodium hydroxide solution and react at 200°C for 1 hour. The reaction product is filtered and distilled under reduced pressure to obtain 2,6- Purified di-tert-butylphenol;
[0063] S2: Preparation of 3,3',5,5'-tetra-tert-butylbiphenol by oxidative coupling reaction
[0064] Get 0.2mol o...
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