C14H4Br8 and synthesizing process

A technology of octabromodiphenylethane and diphenylethane, which is applied in the field of engineering plastics, can solve the problems of high melting point, uneven dispersion, and reduced plastic strength, and achieves the effects of simple operation method, good dispersion effect and reduced loss.

Active Publication Date: 2009-10-14
山东兄弟科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to solve the disadvantages of high bromine content flame retardants in the prior art, which have a high melting point and exist in solid form during use and processing, and tend to be unevenly dispersed during use and easily cause a decrease in plastic strength. In the method, a solvent with higher solubility is used, thus making the process simpler, and avoiding the use of a large amount of solvents, saving costs

Method used

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  • C14H4Br8 and synthesizing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) In a 1000mL four-necked bottle, put 72.8g of diphenylethane into 400mL of dibromomethane and dissolve it in 400mL of dibromomethane, then add 7.28g of iron powder, cool down with ice water, slowly add 175mL of bromine dropwise, keep the temperature below 20°C during the dropwise addition, add After keeping warm for 2 hours, add 50mL of 15% sodium sulfite to neutralize until the system is white or colorless, then separate into layers at rest, discard the water layer, and separate the materials;

[0040] (2) Add 100mL of 15% hydrochloric acid and 50mL of water respectively, raise the temperature and reflux for 30min, let the layers stand still, discard the water layer, and separate the materials;

[0041] (3) Add 300mL of water and 10mL of OS (MS-1) surfactant respectively, heat up and distill, raise to 85°C, the material precipitates, filter with suction, and dry in an oven at 100°C to obtain a white powder of octabromodiphenylethane 320g, yield 93.46%.

[0042] ana...

Embodiment 2

[0051] Others are the same as in Example 1, and the organic solvent is changed to 600ml of dichloromethane to obtain 322g of octabromodiphenylethane as a white powder, with a yield of 96.40%.

[0052] Analysis test: bromine content 80.06%, melting point 165-175 ℃, volatile matter 0.15%, whiteness 90.4.

Embodiment 3

[0054] Others are the same as in Example 1, the catalyst is replaced by 20 g of iron tribromide to obtain 320 g of white powder octabromodiphenylethane, the yield is 93.46%, the bromine content is 80.10%, the melting point is 165-175°C, the volatile matter is 0.15%, and the whiteness 90.4.

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Abstract

The invention relates to an additive flame retardant, in particular to octabromodiphenylethane and a synthesis method thereof, which are used in the field of engineering plastics. The invention dissolves raw materials and products with organic solvent, adopts iron powder and iron tribromide as catalyst, has short reaction time and good reaction effect; during crystallization, the solvent is recovered by concentrated distillation, which greatly reduces the loss of organic solvent. The raw material cost is low, the operation method is simple, the prepared product octabromodiphenylethane is off-white, the bromine content is 78-80%, the melting point is between 150-180 ° C, exists in a solid form, and is easy to store and transport. It is also relatively low, exists in molten form during use and processing, has good compatibility with plastics, has good dispersion effect, and will not change the strength of the added plastics.

Description

technical field [0001] The invention relates to an additive flame retardant, specifically octabromodiphenylethane and its synthesis method, which are used in the field of engineering plastics. Background technique [0002] Brominated flame retardants are the most important and effective ones among halogen-containing flame retardants. They have high flame retardancy, low addition amount, and little influence on product processing and use characteristics. [0003] Many studies have shown that the refractory effect of halogenated organic compounds decreases in the order of iodine, bromine, chlorine, and fluorine. But in fact, iodide is unstable and in short supply, so it has not been used in practice. Chlorine and fluorine compounds are not as flame retardant as bromine. The flame retardant effect of bromine is generally 2.5-4 times higher than that of chlorine. This is because in structure, the binding strength of H-Br is greater than that of H-Cl, so the flame retardant eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C25/18C07C17/12C08K5/02
Inventor 郭秀安杨喜生柴家启
Owner 山东兄弟科技股份有限公司
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