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Method for synthesizing 3-tribromophenoxy cyanurate

A technology of tribromophenoxy and cyanurate, which is applied in the direction of organic chemistry, can solve the problems of yellow color, strong pungent odor, and high total product cost, so as to achieve the promotion of flame retardant effect, increase nitrogen content, and reduce cost Effect

Inactive Publication Date: 2006-09-13
南通联华阻燃科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional synthetic method: add cyanuric chloride (C 3 N 3 Cl 3 ), after it dissolves, add excess tribromophenol (C 6 h 5 Br 3 0), warming up to a certain temperature, after several hours, the solid product is separated out, and the solid-liquid separation is carried out with a closed centrifuge, and the solid product is dried, pulverized and packaged; generally speaking, the obtained product has a melting point Generally below 225°C, the yield is generally <88%, and the color is yellower, with a strong pungent smell, and the total cost of the final product is also high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] a) add 250L toluene in 1000L kettle;

[0009] b) Add 397kg (1200mol) of tribromophenol, and stir for 30 minutes to fully dissolve it;

[0010] c) Add 53.18 kg (412mol) of cyanuric acid at 50°C;

[0011] d) adding 0.2 kilograms of aluminum trichloride;

[0012] e) heating up to 90°C and keeping the temperature for 6 hours;

[0013] f) rapidly cool down to normal temperature, and separate the solid with a closed centrifuge;

[0014] g) Rinse twice with 1000 kg of water;

[0015] h) Dried to moisture <0.5%, pulverized to an average particle size of 0.5 microns to obtain 384 kg of tris-tribromophenoxy-cyanurate product with a yield of 90%, a melting point of 227°C and a whiteness of 95 %.

Embodiment 2

[0017] a) add 400L toluene in 1000L kettle;

[0018] b) Add 397kg (1200mol) of tribromophenol, and stir for 30 minutes to fully dissolve it;

[0019] c) Add 53.44 kg (414mol) of cyanuric acid at 60°C;

[0020] d) adding 0.22 kilograms of antimony trioxide;

[0021] e) Heating up to 100°C and keeping warm for 8 hours;

[0022] f) rapidly cool down to normal temperature, and separate the solid with a closed centrifuge;

[0023] g) Rinse twice with 1000 kg of water;

[0024] h) Dried to moisture <0.5%, crushed to an average particle size of 10 microns to obtain 388.4 kg of tris-tribromophenoxy-cyanurate product with a yield of 91%, a melting point of 229° C., and a whiteness of 93 %;

Embodiment 3

[0026] a) add 480L toluene in 1000L kettle;

[0027] b) Add 397kg (1200mol) of tribromophenol, and stir for 30 minutes to fully dissolve it;

[0028] c) Add 53.69 kg (416mol) of cyanuric acid at 70°C;

[0029] d) adding 0.24 kg of ammonium fluozirconate;

[0030] e) be heated up to 110 ℃, keep warm for 10 hours;

[0031] f) rapidly cool down to normal temperature, and separate the solid with a closed centrifuge;

[0032] g) Rinse twice with 1000 kg of water;

[0033] h) Dried to moisture < 0.5%, crushed to an average particle size of 25 microns to obtain 392.7 kg of tris-tribromophenoxy-cyanurate product with a yield of 92%, a melting point of 225°C and a whiteness of 94 %.

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Abstract

A process for preparing high-purity 3-tribromophenoxy-cyanurate with low cost features that the cyanruic acid is used as raw material and toluene is used as solvent.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a synthesis method of tris-tribromophenoxy-cyanurate. Background technique [0002] Tri-tribromophenoxy-cyanurate, the chemical name is 2,4,6-tris(2,4,6-tribromophenoxy)-1,3,5 triazine, the English name is 2, 4,6-tris(2,4,6-tribromophenoxy)-1,3,5triazine, CAS number: 25713-60-4, molecular formula C 21 h 6 Br 9 N 3 o 3 , molecular weight: 1067.2, bromine content > 67%, melting point 225-230 ° C, appearance is white crystalline powder, non-toxic, chemically stable, often used as a high-efficiency flame retardant, suitable for HIPS, ABS, PBT, PS, PET, Flame retardant modification in various fields such as PP, epoxy resin, unsaturated resin and rubber. Traditional synthetic method: add cyanuric chloride (C 3 N 3 Cl 3 ), after it dissolves, add excess tribromophenol (C 6 h 5 Br 3 0), warming up to a certain temperature, after several hours, the solid product is separated out, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/34
Inventor 丁邦瑞
Owner 南通联华阻燃科技有限公司
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