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Preparation method of hexabromocyclododecane

A kind of technology of hexabromocyclododecane and cyclododecatriene, applied in the field of organic bromide preparation and synthesis

Active Publication Date: 2015-09-09
TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the problem of low melting point of the existing hexabromocyclododecane products, the present invention provides a method for preparing hexabromocyclododecane with a high melting point, which uses a solvent washing method to entrain the unbrominated bromide that will affect the melting point of the product. Remove impurities, improve product purity, and increase product melting point

Method used

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Embodiment Construction

[0016] The technical solution of the present invention is further illustrated by examples. Example:

[0017] Take by weighing 63.6g ethylene dichloride and 26.6g isobutanol and be mixed with mixed solvent, then add 12.3g bromine in mixed solvent, then use the method of adding 30.5g cyclododecatriene and remaining 79.7g elemental bromine respectively Add cyclododecatriene and bromine dropwise into the mixed solvent through two constant pressure funnels. Raise the temperature to 30°C±2°C, add dropwise for 40 minutes; raise the temperature to 40°C±2°C, add dropwise for 40 minutes; raise the temperature to 50°C±2°C, continue dropwise to the end, the total dropping time is 115 minutes. Keep at 50℃±2℃ for aging for 2h. After the aging is completed, let it stand until the solid phase and the liquid phase are separated, and the liquid phase is thrown out. Add 30g of mixed solvent to the solid phase, stir for 1-2min, let it stand for solid-liquid separation, and then remove the uppe...

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Abstract

The invention discloses a preparation method of hexabromocyclododecane. The preparation method comprises three steps of bromination, washing separation and drying, wherein the bromination step comprises the steps of respectively dropwise adding raw materials including cyclododecatriene and bromine into a mixed solvent of isobutanol and dichloroethane, and heating to 50+ / -2 DEG C in three stages of the dropwise adding process, wherein the molar ratio of bromine to cyclododecatriene is (3.05-3.08) to 1, and the total reaction time is 3-4 hours; the washing separation step comprises the steps of adding a solid phase separated from a finished solution of the bromination reaction into the prepared mixed solvent of dichloroethane and isobutanol, after uniformly stirring and mixing, separating the solid phase out, adding ethanol, and washing twice, so as to obtain the filtered solid phase; the drying step comprises the step of drying the solid phase obtained in the washing separation step at 80+ / -2 DEG C, so as to obtain a white solid powder product. According to the preparation method of hexabromocyclododecane, completely-bromized impurities which are entrained by the product and can influence the melting point are removed by virtue of a solvent washing method, so that the product impurity is improved, and the melting point of products is increased.

Description

technical field [0001] The invention belongs to the preparation and synthesis technology of organic bromides. technical background [0002] Hexabromocyclododecane is a special flame retardant for expanded polystyrene and extruded polystyrene. Commercially available hexabromocyclododecane products have a low melting point, mostly around 150°C, and are easily decomposed during material processing, affecting the appearance and performance of the finished product. Contents of the invention [0003] Aiming at the problem of low melting point of the existing hexabromocyclododecane products, the present invention provides a method for preparing hexabromocyclododecane with a high melting point, which uses a solvent washing method to entrain the unbrominated bromide that will affect the melting point of the product. Impurities are removed, the purity of the product is improved, and the melting point of the product is raised. [0004] The preparation method of hexabromocyclododeca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/02C07C17/38C07C23/02
Inventor 蔡荣华姚颖吴丹路绍琰刘伟黄西平
Owner TIANJIN SEA WATER DESALINATION & COMPLEX UTILIZATION INST STATE OCEANOGRAPHI
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