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Method for preparing polybromophenoxy-substituted striazine fire-retardant compound

A technology of polybromophenoxy and bromophenoxy, which is applied in the field of preparation of flame retardant compounds, can solve the problems of unavoidable cyanuric chloride feeding pollution, troublesome separation operation process, insufficient homogeneous method, etc., and achieves a good Market application prospects, avoiding high reaction temperature, and avoiding the effect of high product cost

Active Publication Date: 2007-11-14
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Jiang Hongquan of Qingdao University of Science and Technology and others added cyanuric chloride in batches to a mixed solvent of dichloromethane and toluene, and reacted with 2,4,6-tribromophenol to obtain tribromophenoxy-substituted s-triazine inhibitors. Combustible compounds, the yield reaches 92%, but this method cannot avoid the problem of cyanuric chloride feeding pollution, the separation operation process is troublesome, and the energy consumption is high
[0006] To sum up, domestic and foreign researches are mostly focused on the use of cyanuric chloride and 2,4,6-tribromophenol to synthesize tribromophenoxy-substituted s-triazine flame retardant compounds, and no cyanuric chloride Reports on the preparation of a series of polybrominated phenoxy-substituted s-triazine flame retardant compounds from cyanide and other polybrominated phenols; the preparation methods used are different, but there are certain deficiencies in both the homogeneous method and the phase transfer catalytic method

Method used

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  • Method for preparing polybromophenoxy-substituted striazine fire-retardant compound
  • Method for preparing polybromophenoxy-substituted striazine fire-retardant compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 500mL four-neck flask equipped with a stirrer, thermometer, reflux condenser, and dropping funnel, add 25g (0.136mol) cyanuric chloride, 135g (0.408mol) 2,4,6-tribromophenol, 0.44g (0.00136mol) tetrabutylammonium bromide, 100ml solvent 1, 2-dichloroethane began to stir and cooled, when the temperature was cooled below 10°C, add dropwise from 16.3g (0.408mol) hydroxide in advance through the dropping funnel 5% alkaline aqueous solution prepared with sodium, control the addition rate, keep the system temperature not exceeding 10°C, after about 0.5h after the dropwise addition, raise the temperature to 30°C-60°C and continue the reaction for 2h, then distill and recover the solvent, and then cool down the system to room temperature, filter and add an appropriate amount of water to wash the filter cake until the filtrate becomes clear, collect the filter cake, and dry to obtain 143.3 g of white crystalline powder, with a yield of 98.7%, a melting point of 227°C-229°C, a...

Embodiment 2

[0030] 2,4,6-tribromophenol addition is increased to 140g (0.422mol), and sodium hydroxide is increased to 16.9g (0.422mol), and other is with embodiment 1, slightly, obtains product 142.3g, and yield is 98.5%.

Embodiment 3

[0032] Catalyst tetrabutylammonium bromide is increased to 4.4g (0.0136mol), and other is with embodiment 1, example 2, omission, and product yield reaches 97.8%.

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Abstract

The invention relates to the more monobromo-benzene oxygen radical substitutions even triazine flame retardance compound's preparation method. Its characteristic is: The reactant three will gather the chlorine cyanogens, the multi-bromophenols, shift the catalyst according to 1:2.5-3.1:0.01-0.1 a mole of allocated proportion to take the quantity, with the right amount organic solvent one and joins to a reactor, stir and cool it to 10 degree C below; Take the 5%-30% sodium hydroxide peroxide solution which mole of quantity sodium hydroxide compounds the weight percentage concentration with the multi-bromophenols, add by drops in the reactor stated, and maintain the system temperature not to surpass 10 degree C when adding by drops in the process; After the installment, heat the reaction material to 30-60 degree C ,and respond 1h-5h again; Then distillate to clean the resolve, cool, filtrate, the solid which the filtration obtains after the washing, drying is the system results in the product. This invention uses a method of 'a pot synthesis', the operation is simple, the pollution is reduced, the resolve may recycle repeatedly, the cost is small, and it is suitable for the industrialization production.

Description

technical field [0001] The invention relates to the preparation of a flame retardant compound, in particular to a preparation method of a polybrominated phenoxy substituted s-triazine flame retardant compound. Background technique [0002] Among the many types of flame retardants, brominated flame retardants are famous for their excellent flame retardant performance, wide application range, not too much influence on the physical and mechanical properties and electrical properties of the substrate, and the cost performance is far superior to other flame retardants. It has been widely used and still occupies the main position of flame retardant application in the world. However, the brominated flame retardant will cause the UV stability of the flame retardant base material to decline, and there will be secondary hazards such as smoke and corrosive toxic gases during combustion, which poses a serious threat to the environment and personal safety, especially the use of polybromi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/10C07D251/30
Inventor 黄杰唐安斌马庆柯支肖琼
Owner SICHUAN DONGFANG INSULATING MATERIAL
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