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Prepn process of hexabromo-cyclododecane

A technology of hexabromocyclododecane and cyclododeca, which is applied in the field of chemical synthesis of halogenated cycloalkanes, can solve the problems of low melting point, poor thermal stability, and failure to achieve the best effect, and achieve high melting point and high product quality. yield effect

Inactive Publication Date: 2003-07-30
邵林高
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The melting point of the product is low, indicating that the product contains a certain amount of impurities with a low melting point, which makes the thermal stability of the product poor. When it is used as a flame retardant for some plastics (such as high-impact polystyrene), it cannot reach the optimum level. good effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In 1000L reactor, add 400kg mixed solvent, 30% of weight in mixed solvent is carbon tetrachloride, 3% is water, surplus is ethanol, starts agitator and circulating cooling system, and the control mixed solvent temperature is 20 ℃, by Two feeders add 100kg of 1,5,9-cyclodododecatriene and 320kg of liquid bromine to the reactor at a uniform speed at the same time respectively within 6 hours. Because this reaction is an exothermic reaction, the materials in the reactor must be fully stirred and Take effective cooling measures. During the feeding, the material temperature in the reactor was controlled at 20°C. After adding 1,5,9-cyclodododecatriene and liquid bromine, the temperature of the material in the reactor was raised to 30°C, and the reaction was stirred at this temperature for 3 h, and then the material was cooled to 15°C. Stop stirring, filter the material, and remove the solvent to obtain the crude product of hexabromocyclododecane. The crude product is first w...

Embodiment 2

[0020] Different from Example 1: 40% of the weight in the mixed solvent is chloroform, 1% is water, and the balance is n-propanol; liquid bromine and 1,5,9-cyclododetriene are respectively simultaneously Adding; during the feeding, the temperature of the material was controlled at 30°C; after the addition, the material was stirred and reacted at 40°C for 2 hours, and the material was cooled to 25°C. The crude product was first washed with hot water at 70°C, and then washed with hot water at 100°C; the wet hexabromocyclododecane was dried at 70°C and 0.07MPa vacuum for 15 hours to obtain the hexabromocyclododecane product. The yield is 95%, and the melting point is 188--195°C.

Embodiment 3

[0022] Different from Example 1: 1,5,9-cyclodododecatriene 100kg and 310kg of liquid bromine; 35% of weight in the mixed solvent is chloroform, and the balance is n-butanol; liquid bromine and 1,5,9 -Cyclododecatriene was added simultaneously at a constant rate within 9 hours; after the reaction, the material was cooled to 20°C; the crude product was washed with hot water at 65°C first, and then with hot water at 92°C; wet hexabromocyclododecane Dry at 60° C. and 0.08 MPa vacuum for 15 hours to obtain the hexabromocyclododecane product with a yield of 92%. The melting point is 180--187°C.

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Abstract

The present invention belongs to the field of chemical synthesis of cyclo alkane halide. The preparation of hexabromo-cyclododecane includes the following steps: reaction of 1,5,9-cyclododecatriene and liquid bromine in mixed solvent; separation of the reacted mixture to obtain coarse hexabromo-cyclododecane product; washing with hot water; and vacuum drying to obtain hexabromo-cyclododecane product. The present invention has the features of use of mixed solvent containing C2-C4 saturated alcohol, use of no catalyst, no neutralizing step of coarse product, vacuum drying, high product yield and high product smelting point.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of halogenated cycloalkane, in particular to a preparation method of hexabromocyclododecane. Background technique [0002] Hexabromocyclododecane (HBCD) is a widely used high-efficiency flame retardant, which can be used for molded or foamed polyolefin and polystyrene plastics, and can also be used for water suspension or latex flame retardant textiles . The method disclosed in U.S. Patent 4783563 is: in C 4 -C 8 In saturated alcohol, boron trifluoride complex is used as catalyst, and 1,5,9-cyclodododecatriene (CDT) is brominated with liquid bromine, and the reactant is neutralized with non-aqueous alkali to recover crystalline six Bromocyclododecane. The best example disclosed by this patent is: add 420g isobutanol in the reaction flask, which contains 4.2g boron trifluoride etherate complex as catalyst, then 495g (3.09mol) liquid bromine and 162g (1mol) 1, 5,9-Cyclododecatriene w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/02C07C23/02
Inventor 邵林高
Owner 邵林高
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