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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

Inactive Publication Date: 2008-09-24
ZHENJIANG SANWA FLAME RETARDANT ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent after recycling is difficult to handle. The polyalcohol in the selected solvent has a relatively high viscosity and a high boiling point. After the solvent with a low boiling point is evaporated, the polyalcohol is not easy to recycle, which increases the production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The present invention discloses a preparation method of hexabromocyclododecane. In the method, bromine and cyclododecatriene are simultaneously dropped in the mixed solvent of substances, which are used for providing halogen ions, and protic solvent; the molar ratio of the bromine and the cyclododecatriene is equal to 3 to from 3.5 to 1; thus the hexabromocyclododecane can be prepared through the reaction. Compared with the hexabromocyclododecane prepared in the prior art, the hexabromocyclododecane prepared in the method has an increased melting point, which reaches above 186 DEG C. The preparation method has the advantages of low cost, simple operation, safety, environmental protection, and suitability for the industrial application.

Description

technical field [0001] The invention belongs to the field of flame retardants and relates to a method for preparing hexabromocyclododecane. Background technique [0002] Hexabromocyclododecane is an additive flame retardant with high thermal decomposition temperature and good flame retardant effect. It can be used for flame retardancy of polystyrene, polypropylene fiber foam, etc. Commercially available hexabromocyclododecane usually has a melting point of ≥175°C and cannot withstand higher processing temperatures. [0003] Hexabromocyclododecane is composed of three stereoisomers of α, β and γ, and the γ isomer is the main one, usually containing 10-18% by mass of the α isomer and 6-14% of the β isomer , 71-78% of the gamma isomer. The alpha isomer has a melting point of 171-173°C, the beta isomer has a melting point of 169-171°C, and the gamma isomer has a melting point of 208-210°C. Generally, the greater the content of γ isomer, the higher the melting point of the so...

Claims

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Application Information

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IPC IPC(8): C07C23/02C07C17/02
Inventor 杨锦飞章庚柱杨建伟程学波于春红黄东平
Owner ZHENJIANG SANWA FLAME RETARDANT ENG TECH CO LTD
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