1,2,5,6,9,10-Hexabromocyclododecane synthesis

Yield:3194-55-6 96%

Reaction Conditions:

with bromine in dichloromethane;2-methyl-propan-1-ol;chloroform; pH=7 at 14 - 15;Large scale;

Steps:

3 Example 3
The isobutanol and chloroform mixed solvent was added to the reactor, the mixed solvent pH = 7, the total amount of mixed solvent was 1419.50kg,Isobutanol and dichloroethane mass ratio of 1.0: 1, turn on the frozen salt water pump to cool to 6-8 ,The reactor speed was adjusted to 65 r / min, bromine 835kg and cyclododecatriene 266kg (bromine and cyclododecatriene molar ratio of 3.19: 1) into the metering tank, close the feed valve and vacuum Valve, open the vent valve.When feeding to the reactor, first slowly added to participate in the reaction of bromine 6% -9% of the total mass of bromine, this embodiment is first added 50kg bromine,Then cyclododecatriene and the remaining bromine were added at the same time, keeping the bromine and cyclododecatriene drop mass ratio of 3: 1, 120kg per hour of bromine, cyclododecatriene per Hour 40kg, dropping in 6.5-7 hours is completed.During the reaction, the temperature was controlled at 14 ° C. After the reaction was completed, the freezer was turned off and the reaction temperature was raised to 15 ° C for 1.5 to 2 hours.Bromination reaction after the separation, the reaction of the material was suction filtered, the filtered material was poured into the centrifuge, the material after centrifugation followed by caustic washing, washing.After the separation of materials through suction filtration drying, sieve powder,The product HBCD was 1000kg, the yield was 95.0% and the melting point was 193 .The difference between Example 1 and Example 1 is that the ratio of raw materials is changed by taking 825.53 kg of bromine and 266 kg of cyclododecatriene (the molar ratio of bromine and cyclododecatriene is 3.15: 1), the corresponding mixed solvent The total amount of 1403.40kg, other process conditions the same. The product, hexabromocyclododecane, was obtained in an amount of 1010.76 kg, a yield of 96% and a melting point of 195 ° C.

References:

Shandong Dongxin Chemical Co., Ltd.;Guo Shaojun;Li Xiaoying;Zhang Wenshui;Wang Chuantao;Zhong Kunpeng CN105949031, 2016, A Location in patent:Paragraph 0015; 0016; 0023; 0024

FullText