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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.

Inactive Publication Date: 2010-08-04
HUAIHAI INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this technology significantly improves the thermal stability of hexabromocyclododecane, the encapsulation process of microcapsules is complicated, the amount of process wastewater is large, and the content of harmful substances in the wastewater is high, which is not friendly to the environment
In addition, the amount of microcapsules used is large, which has a significant impact on the flame retardancy of hexabromocyclododecane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention provides a new washing process for increasing the heat stability of hexabromocyclododecane, is to combine a washing debromination process in a produce process of hexabromocyclododecane, and makes bromization fatty acid barium salt, magnesium salt or calcium salt with a thermal stabilizer action and a fire retardant function be infiltrated into inner of hexabromocyclododecane granuleor uniformly be deposited on the surface of hexabromocyclododecane granule, to realize mixture between bromization fatty acid barium salt, magnesium salt or calcium salt with double functions and hexabromocyclododecane uniformization uniformizing and coating and have a high efficient thermal stability. And at the same time, the invention simplifies the produce of hexabromocyclododecane and a thermal stability treating process, reduces producing and processing cost of hexabromocyclododecane, and decreases the discharge of the three wastes in a producing process of hexabromocyclododecane.

Description

technical field [0001] The invention provides a new washing process for hexabromocyclododecane, in particular to a new washing process for improving the thermal stability of hexabromocyclododecane. It belongs to the field of fine chemical production technology. technical background [0002] Hexabromocyclododecane (HBCD) is an additive aliphatic brominated flame retardant, which can be used for molded or foamed XPS or EPS plastics, and can also be used for textiles in aqueous suspension or latex. Flame retardant treatment. At present, in the industry, cyclododecatriene is mixed in chloroform / isobutanol and other organic solvents, and undergoes bromine addition reaction process, sodium carbonate aqueous solution washing process to remove bromine, water washing process to remove salt, drying and crushing process, etc. The production process produces hexabromocyclododecane products. There are mainly three isomers of α, β and γ in industrial hexabromocyclododecane products, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C23/02C07C17/38
Inventor 张田林李新华姜培琴
Owner HUAIHAI INST OF TECH
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