Method for preparing hexabromocyclododecane
A technology for hexabromocyclododecane and cyclododecatriene, which is applied in the field of preparing hexabromocyclododecane, can solve the problems of high boiling point, high viscosity of polyalcohol, difficult solvent handling, etc., and achieves simple operation and low cost. Low and easy industrial application effect
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Embodiment 1
[0020] In a four-neck flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, add 95g of 2-ethoxyethanol and 30g of hydrobromic acid, start the stirring device, and simultaneously add 71.2g of bromine dropwise at 1 to 50°C Prime (Br 2 ) and 23g cyclododecatriene, control the rate of addition, so that the two are dropped simultaneously within 1 to 5 hours, heat up to 50 to 70°C after the heat preservation reaction for about 1 to 4 hours, keep warm for 4 to 8 hours, and then heat up Heat at 70-90°C and keep warm for 2-6 hours until the material turns light yellow. A colorless or light yellow solid was obtained by suction filtration, and the filtrate was used for other purposes. The solid is washed with 10-20g of mixed solvent (i.e. 95g of 2-ethoxyethanol and 30g of hydrobromic acid), 5-20g of aqueous ammonia with a concentration of 40% (m / m), 80-150g of water, and 80 Dry at ~90°C with a yield of 87% to obtain hexabromocyclododecane with a melting ...
Embodiment 2
[0022] In the four-neck flask equipped with agitator, thermometer and constant pressure dropping funnel, apply the solvent in Example 1 (i.e. the suction filtrate in Example 1), add 10~30g of 2-ethoxyethanol, 2~10g of hydrobromic acid, start the stirring device, drop 70g of bromine and 23g of cyclododecatriene at the same time under the condition of 1~50℃, control the dropping speed, so that the two are dropped simultaneously within 1~5 hours , keep warm for about 1-4 hours, then heat up to 50-70°C, keep warm for 4-8 hours, then heat up to 70-90°C, keep warm for 2-6 hours, until the material is light yellow. Suction filtration to obtain a colorless or light yellow solid, the solid is washed with 10-20g protic solvent (2-ethoxyethanol), 10-25g ammonia water with a concentration of 40% (m / m), 80-150g water, and 80-20g Dry at 90°C with a yield of 92% to obtain hexabromocyclododecane with a melting point of 190-195°C.
Embodiment 3
[0023] Example 3. In a four-neck flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, add 100 g of 2-methoxyethanol and 30 g of hydrobromic acid, start the stirring device, and drop simultaneously at 1 to 50 ° C. Add 71.2g of bromine and 23g of cyclododecatriene, and control the rate of addition so that the two are dropped simultaneously within 1 to 4 hours. After the heat preservation reaction is about 2 to 4 hours, the temperature is raised to 50 to 70°C, and the temperature is kept for 4 to 8 hours. hour, then heat up to 70-90°C, and keep warm for 2-6 hours until the material turns light yellow. Suction filtration obtains colorless or light yellow solid, and solid is 40% (m / m) with 10~20g mixed solvent (being the mixed solvent that 100g 2-methoxyethanol and 30g hydrobromic acid form), 15~20g concentration Ammonia, washed with 80-150g of water, dried at 80-90°C, the yield is 85%, and hexabromocyclododecane is obtained, with a melting point of...
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