Optimized production method of Tri (tribromophenyl) cyanurate

Abstract

The invention relates to an optimized production method of Tri (tribromophenyl) cyanurate. Chlorobenzene is added into a reactor, phenol is added, hydrogen peroxide and bromine are dropwise added into the reactor in a staggering manner, extraction is performed by the aid of the chlorobenzene, a tribromophenol and chlorobenzene mixed liquid is obtained, cyanuric chloride is added into the mixed liquid, an initiating agent CTAB (cetyl trimethyl ammonium bromide), anhydrous sodium carbonate and methylbenzene are added for reaction, and a crude product is transferred to a heating kettle, the product is subjected to pressure reduction and suction filtration in a heating and dissolving state and is finally transferred to a distillation kettle and stirred and crystallized, edulcoration is realized before unit cell arrangement, and the product is obtained. According to the optimized production method of Tri (tribromophenyl) cyanurate, the produced by-products are reduced, the yield is improved, and the product quality is higher.

Description

technical field [0001] The invention relates to the technical field of flame retardant production, in particular to an optimized bromotriazine production method. Background technique [0002] At present, with the enhancement of fire prevention awareness, safety and fire prevention in various industries are placed in the first place. The consumption structure of flame retardants in various regions of the world is different. The largest consumption in Europe is inorganic flame retardants, while the largest consumption in the United States, Japan, and Asia (excluding Japan) is brominated flame retardants. The United States and Japan account for 35% and 40% of the total consumption, but as high as 60% in Asia. [0003] The main trend in the development of flame retardants in the next 10 years is: halogenated flame retardants (including halogen-containing phosphates) will continue to be used, and many brominated flame retardant manufacturers have embarked on internationalization...

AI Technical Summary

Problems solved by technology

In the production, bromine chloride must first be synthesized, and secondly, a large amount of hydrogen chloride will be produced during the reaction of bromine chloride and phenol solution, which is easy to cause accumulation in the reaction system, thus affecting the reaction speed and product quality

Although this method improves the utilization rate of bromine, the process operation of synthesizing bromine chloride is complicated, the consumption of raw materials is large, and the obtained tribromophenol contains a small amount of chlorinated substances, and the product quality is poor

[0012] 3. There are many reports in the literature about the synthesis of 2,4,6-tribromophenol from salicylic acid, but there is no real industrial application, because the salicylic acid bromination method is more complicated and costly than phenol bromination, but some enterprises use it The waste water from the production of salicylic acid is concentrated and then brominated, because the waste water from the production of salicylic acid contains both raw material phenol and a certain amount of salicylic acid

[0028] 1. Phenol bromination is carried out by phenoxy anions. Although its concentration is very low, its reactivity is high, and the bromination speed is faster than that of phenol. After bromine atoms are introduced into the benzene ring, the balance of the corresponding aryloxy anions As the concentration increases, the rate of bromination continues to be faster than that of unsubstituted phenoxy anions, and it is easy to further brominate until the final generation of cyclohexadienone derivatives, which also leads to the etherification of tribromophenol in the extracted aqueous phase. There are many side reactions in continuous production, resulting in unstable quality after reuse, and the melting point of the final product is low and fluctuates greatly;

[0029] 2. Those skilled in the art know that tribromophenol is almost insoluble in water, so most tribromophenols are obtained by filtration, and then the next step of reaction is carried out; The solubility is up to 14g / 100g, and the tribromophenol dissolved in water is extremely difficult to remove, and the COD of the water phase has reached 3600 by the sewage treatment station, which is very polluting to the environment;

[0030] 3. In the traditional process, the small incremental feeding of the original proportion will cause the melting point of the finished product to fluctuate greatly, and the process parameters are not easy to control;

[0031] 4. Due to the long overall process, the probability of introducing impurities is high, resulting in very high impurity content in the final product, poor color quality, and greatly affected performance

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