Synthetic method of water soluble ultraviolet light absorber BP-9

[0026] ① Methylation reaction: Put 123kg of 2,2',4,4'-tetrahydroxybenzophenone, 2.95kg of zinc chloride and a mixture of 295L dichloroethane + 295L absolute ethanol into the reaction kettle Solvent 590L, heat and stir to dissolve, heat up to 45~50°C, add 148kg of dimethyl sulfate dropwise, 2h is completed, keep warm for 6h; cool to room temperature, add 148L of water, stir to dissolve, then stand to separate layers, and separate the organic phase , the water phase was extracted twice with dichloroethane, each time 50L, the organic phase was combined, the solvent was recovered by distillation, and cooled to crystallize to obtain 2,2'-dihydroxy-4,4'dimethoxybenzophenone About 130kg, molar yield 95% (based on 2,2',4,4'-tetrahydroxybenzophenone);

[0027] ②Sulfonation reaction: Put 130kg of the methylated product 2,2'-dihydroxy-4,4'dimethoxybenzophenone and 610 L of dichloroethane into the reactor, heat and stir to dissolve , heated up to 60~65°C, put 112kg of sulfamic acid in 3 ...

[0031] ① Methylation reaction: Put 123kg of 2,2',4,4'-tetrahydroxybenzophenone, 2.46kg of copper chloride and a mixture of 276L dichloroethane + 276L absolute ethanol into the reaction kettle Solvent 552L, heat and stir to dissolve, heat up to 45~50°C, add 148kg of dimethyl sulfate dropwise, after 2h dropwise addition, keep warm for 6h reaction; cool to room temperature, add 148L of water, stir to dissolve, then stand for stratification, and separate the organic phase , the aqueous phase was extracted twice with dichloroethane, 50 L each time, the organic phases extracted twice were combined, the solvent was recovered by distillation, and crystallized by cooling to obtain 2,2'-dihydroxy-4,4'dimethoxydi Benzophenone 124kg;

[0032] ②Sulfonation reaction: Put 124kg of the methylated product 2,2'-dihydroxy-4,4'dimethoxybenzophenone and 596L of chloroform into the reactor, heat and stir to dissolve, and heat up To 60~65°C, add 99kg of sulfamic acid in 3 times, keep it warm for 5...

[0035] ①Methylation reaction: Put 123kg of 2,2',4,4'-tetrahydroxybenzophenone, 3.1kg of nickel chloride and a mixture of 307L dichloroethane + 307L absolute ethanol into the reaction kettle Solvent 614L, heat and stir to dissolve, heat up to 45~50°C, add 184.5kg of dimethyl sulfate dropwise, dropwise add 2h, keep warm for 6h; cool to room temperature, add 185L of water and stir to dissolve, then stand for stratification, separate organic phase, the aqueous phase was extracted twice with dichloroethane, 55 L each time, the organic phases were combined twice, the solvent was recovered by distillation, and crystallized by cooling to obtain 2,2'-dihydroxy-4,4'dimethoxydi Benzophenone 127kg;

[0036] ②Sulfonation reaction: Put 127kg of the methylated product 2,2'-dihydroxy-4,4'dimethoxybenzophenone and 610 L of dichloroethylene into the reactor, heat and stir to dissolve, Raise the temperature to 60~65°C, add 112 kg of sulfamic acid in 3 times, keep the temperature for 5 hours, co...