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Novel method for synthesizing bromo-triazine

A technology of bromotriazine and synthesis method, which is applied in the field of synthesis of triazine compounds, can solve problems such as pollution and difficulty in recycling, and achieve the effects of stable process, easy operation and high efficiency

Inactive Publication Date: 2012-12-26
孔庆池
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, a large amount of DMF enters the water phase, and it is difficult to recover due to the good compatibility between DMF and water, causing greater pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] Add 200ml of benzene into a 500ml four-necked flask equipped with a condenser, thermometer and stirring rod, then add 107.6g of tribromophenol, cool down to 15°C, slowly add 20g of cyanuric chloride, after the addition, raise the temperature to 60°C , add 33g of triethylamine dropwise, after the dropwise addition, keep the temperature for 3 hours, add ice water to cool to 20°C, filter, remove the generated triethylamine hydrochloride by filtration, and wash the solid triethylamine hydrochloride once with benzene , combined the organic phase, washed the organic phase with water twice, then added 200ml of water, heated and distilled, benzene was evaporated, bromotriazine was crystallized, filtered, and dried. The melting point of the product is 229-230°C, and the yield is 97%.

example 2

[0036] Add 180ml of dichloromethane to a 500ml four-necked flask equipped with a condenser, thermometer and stirring rod, then add 109g of tribromophenol, cool down to 5°C, slowly add 20g of cyanuric chloride, after the addition, heat up to reflux , add 33g of triethylamine dropwise, after the dropwise addition is completed, keep warm for 3h, add 200ml of water, then add sodium hydroxide to the solution pH = 10, distill, distill methylene chloride and triethylamine, and bromotriazine crystallizes Precipitated, filtered, and the product was washed once with water and dried. The melting point of the product is 229-231°C, and the yield is 99%.

example 3

[0038]Add 100ml of chloroform in a 500ml four-neck flask equipped with a condenser, a thermometer and a stirring rod, then add 108g of tribromophenol, heat up to reflux temperature, dissolve 20g of cyanuric chloride in 120ml of chloroform, and Slowly add it dropwise to the chloroform solution of tribromophenol in the state, after the addition is completed, add 33g of triethylamine dropwise, after the dropwise addition is completed, keep the temperature for 3h, add 200ml of water, and then add sodium hydroxide until the solution pH= 9. Distill, distill off chloroform and triethylamine, bromotriazine crystallizes out, filter, wash the product with water once more, and dry. The melting point of the product is 228-231°C, and the yield is 99%.

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Abstract

The invention discloses a novel method for synthesizing bromo-triazine, which belongs to the field of flame retardant synthesis; the novel method for synthesizing the bromo-triazine is characterized by comprising the following steps of: adding tribromophenol and cyanuric chloride to an organic solvent containing no water in sequence; dripping an organic base into the organic solvent; after finishing the dripping, heating the organic solvent to 40 DEG C to backflow temperature; taking reaction for 1-3 hour by heat preservation; separating out organic base hydrochloride or adding sodium hydroxide aqueous solution to a reaction product, so that the pH value of the solution is 7-10; by using distilling or other separating methods, separating the organic solvent and the organic base from the water; and then centrifuging, washing and drying an obtained product so as to obtain a bromo-triazine finished product, wherein the quantity ratio of substances of the cyanuric chloride and the tribromophenol is 1:3-3.3, the quantity ratio of substances of the cyanuric chloride and the organic base is 1:2-3.3, the selected organic solvent obtains good dissolubility for the tribromophenol, the cyanuric chloride and the bromo-triazine; and the tribromophenol, the cyanuric chloride and the bromo-triazine can be completely dissolved by the selected organic solvent. As no water is available in the whole reaction system, the hydrolysis possibility of the cyanuric chloride is prevented.

Description

technical field [0001] The invention relates to a method for synthesizing triazine compounds, in particular to a method for synthesizing a flame retardant bromotriazine. Background technique [0002] The chemical name of bromotriazine is tris(tribromophenoxy)-cyanurate, which is an excellent flame retardant with excellent flame retardant properties. A lot of research has been done on its synthesis methods at home and abroad . [0003] The synthesis methods reported at present all use cyanuric chloride and tribromophenol as raw materials. Generally, tribromophenol is reacted with sodium hydroxide to generate sodium salt, and then reacted with cyanuric chloride to generate bromotriazine. [0004] In the disclosed technology of U.S. Yabao Company in US5965731, acetone is used as solvent, first tribromophenol is added in anhydrous acetone, and then sodium hydroxide aqueous solution is added to make tribromophenol sodium acetone solution, and tribromophenol sodium acetone is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/30
Inventor 孔庆池杨森李汝奕
Owner 孔庆池
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