Tetrabromophthalic anhydride synthesis

Yield:632-79-1 95.1%

Reaction Conditions:

with sulfuric acid;bromine;tin(IV) chloride at 30 - 80; for 13 h;Reagent/catalyst;Temperature;

Steps:

1 Example 1
This example provides a process for producing tetrabromophthalic anhydride.First 50g of fuming sulfuric acid 50g added to the reactor, add 10g of phthalic anhydride to stir all the phthalic anhydride dissolved after the addition of tin tetrachloride catalyst 0.1g, continue to stir to mix evenly, and then three-step temperature and three ways to join the reactants The reaction temperature is 30 , the mass of bromine is 5g, the reaction time is 4 hours; the temperature of the second stage is 60 , the quality of bromine is 5g, the reaction time is 4 hours; The temperature of three-stage heating is 80 , the quality of bromine is 4g of phthalic anhydride, the reaction time is 5 hours, the tetrabromophthalic anhydride seed is added in the third stage, and the mass of tetrabromophthalic anhydride is 0.5g After the reaction, the temperature was lowered to 50 ° C and suction filtration was carried out.The filtering device used in the invention is a quartz material, 25 * 25 filter brick seamless combination, its diameter is equivalent to 120 mesh filter screen, transfer device is through the 2m glass-lined pipe, pipeline with nitrogen inlet, through Nitrogen into the pipeline to prevent the occurrence of clogging phenomenon.The filter cake obtained by filtration was added to 25% sodium hydroxide aqueous solution, adjusted to a temperature of 80C and adjusted to a pH of 8. Then, 0.5 g of activated charcoal was added and stirred until the mixture was homogeneous. After filtration, the filtrate was added to 30% aqueous hydrochloric acid, To 93 ° C and adjust the pH to 0.1 for acidification, cooling to room temperature after adding 50g of ethyl acetate extraction, the four-bromo phthalic acid crude.Ethyl acetate was distilled under vacuum at a temperature of 0.09 MPa and at a temperature of 100 ° C and dehydrated at a high temperature of 150 ° C to obtain a finished product of tetrabromophthalic anhydride.

References:

Shandong Runke Chemical Co., Ltd.;Wu, Duokun;Zhang, Guoqiang;Qin, Shanbao;Yang, Hong;Yang, Lili CN105418565, 2016, A Location in patent:Paragraph 0021; 0026

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