4,4'-Sulphonylbis(2,6-dibromophenol) synthesis

Yield: 99.5%

Reaction Conditions:

with dihydrogen peroxide;bromine in dichloromethane;2-methyl-propan-1-ol;water at 25 - 37; for 7.58333 h;Temperature;

Steps:

1.1; 1.2; 2.1; 2.2; 3.1; 3.2; 1.1; 1.2; 2.1; 2.2; 3.1; 3.2 A synthesis method of tetrabromobisphenol S includes the following steps:
(1) Add 50g of bisphenol S, 300g of the recovered mother liquor of Example 1 and 100g of water to a four-necked flask, mix well, and warm to 25 ° C; slowly add 56g of hydrogen peroxide and 68g of bromine in double drops.The dropping temperature was controlled at 25 ° C, and the dropping time was 95 min. After the dropping, the temperature was continued to 37 ° C, and the reaction was stirred for 6 hours.(2) After the reaction is completed, the reaction system is brought to room temperature, a mass fraction of 9% sodium sulfite solution is added to neutralize the excess bromine, and the pH of the system is adjusted to 6-7 with 9% mass fraction sodium carbonate solution. The solid was washed twice with water, and then dried at 75 ° C for 8 hours to obtain tetrabromobisphenol S, and the recovered mother liquor was directly recycled and applied.The purity of tetrabromobisphenol S prepared in this example was 98.6%, and the yield was 99.5%.

References:

Shandong Xurui Xincai Co., Ltd.;Yang Qingbo;Yang Kai;Li Hongrui;Zhang Ronghua;Yang Zhenzhen;Li Jinzhong;Wang Qiang CN111072529, 2020, A Location in patent:Paragraph 0031-0059