Novel washing technique for improving thermal stability of hexabromocyclododecane
A technology of hexabromocyclododecane and thermal stability, which is applied in the disproportionation separation/purification of halogenated hydrocarbons, organic chemistry, etc. It can reduce the production and processing costs, improve the thermal stability effect, and meet the requirements of multi-purpose.
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Embodiment 1
[0013] first washing process
[0014] In the washing kettle, inject 800 kilograms of calcium chloride aqueous solution with a mass percentage concentration of 0.8%, start stirring, and send 550 kilograms of hexabromocyclododecane crude product that is centrifuged out of the bromination reaction mother liquor into the washing kettle, and stir for 1 After one hour, open the ammonia cylinder valve and feed ammonia to the material in the scrubber, and the flow rate of ammonia is controlled at 2.5 liters / minute. At the same time, when the pH value of the material in the washing kettle is checked to be 9.0, the valve of the ammonia cylinder is closed. Turn on the steam heating system of the washing kettle. After the temperature of the material in the washing kettle rises to 90-95°C, keep it warm for 2 hours. After the distillation and recovery of the organic solvent entrained by the crude hexabromocyclododecane is completed, turn off the steam heating system of the washing kettle. ...
Embodiment 2
[0019] According to the operating procedures and steps of the first washing process and the second washing process in Example 1, the calcium chloride aqueous solution mass percentage concentration is increased to 1.5%, and 2,3-dibromo-1,4-butanedi The mass percentage concentration of the acid ethanol solution is increased to 6%, and the analysis result of the hexabromocyclododecane product with high thermal stability is finally produced: the appearance is a white powder, the melting point is 182°C, the thermal decomposition temperature is 209°C, and the bromine content 72.47%.
Embodiment 3
[0021] According to the operating procedures and steps of the first washing process and the second washing process in Example 1, the calcium chloride aqueous solution with a mass percentage concentration of 0.8% is changed to a barium chloride aqueous solution with a mass percentage concentration of 0.8% , the mass percent concentration of 2,3-dibromo-1,4-butanedioic acid ethanol solution is adjusted to 1.7% by 3.3%, finally produces the high hexabromocyclododecane product analysis result of thermal stability: The appearance is white powder, the melting point is 181°C, the thermal decomposition temperature is 202°C, and the bromine content is 73.32%.
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