Preparation method of pentabromobenzyl acrylate
A technology of pentabromobenzyl acrylate and pentabromotoluene, which is applied in the field of compound synthesis, can solve problems such as high cost, complicated separation process, and impact on yield, and achieve the effects of difficult polymerization, high purity, and easy product separation
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Embodiment 1
[0022] Add 170ml of chlorobenzene, 100g of pentabromotoluene, 14ml of bromine, 40ml of water, 2g of azobisisobutyronitrile (AIBN) into a 250ml four-necked flask equipped with a condenser, mechanical stirring and a thermometer, and stir for 20min at room temperature. Then, the reaction system was heated to 80°C and stirred for 3 hours. When the reaction system was cooled to room temperature, a certain amount of sodium bisulfite aqueous solution was added to wash until the lotion was colorless and transparent, and the upper aqueous solution was separated. Under the protection of nitrogen, 70ml of 30wt% sodium acrylate aqueous solution and 1.4g of cetyltrimethylammonium bromide (CTAB) were added to the system, heated to 80°C, kept stirring for 4h, and the reaction was completed. When the system was cooled to 5°C, it was filtered to obtain a solid product. The solid product was repeatedly washed with distilled water until the washing solution was colorless and transparent, and the...
Embodiment 2
[0024] Add 170ml of dichloromethane, 100g of pentabromotoluene, 14ml of bromine, 40ml of water, 2g of azobisisobutyronitrile (AIBN) into a 250ml four-neck flask equipped with a condenser, mechanical stirring and a thermometer, and stir for 20min at room temperature , and then the reaction system was heated to 100 ° C and stirred for 2 h. When the reaction system was cooled to room temperature, a certain amount of sodium hydroxide aqueous solution was added to wash until the lotion was colorless and transparent, and the upper aqueous solution was separated. Add 70ml of 30% sodium acrylate aqueous solution and 1.4g of cetyltrimethylammonium chloride (CTAC) to the system under nitrogen protection, heat to 100°C, keep stirring for 3h, and the reaction is completed. When the system was cooled to 0°C, it was filtered to obtain a solid product. The solid product was repeatedly washed with distilled water until the washing solution was colorless and transparent, and the product obtain...
Embodiment 3
[0026] That is, in the 250ml four-necked bottle equipped with condenser tube, mechanical stirring and thermometer, add 170ml dibromoethane, 120g pentabromotoluene, 17.71ml bromine, 48ml water, 1.63g benzoyl peroxide (BPO), Stir at room temperature for 20 minutes. Then the reaction system was heated to 60°C, stirred for 3 hours, and when the reaction system was cooled to room temperature, a certain amount of sodium carbonate aqueous solution was added, washed until the lotion was colorless and transparent, and the upper aqueous solution was separated. Add 110ml of 30% sodium acrylate aqueous solution and 2.68g of methyltrioctylammonium chloride to the system under the protection of nitrogen, heat to 90°C, keep stirring for 4h, and the reaction is completed. When the system was cooled to 5°C, it was filtered to obtain a solid product. The solid product was repeatedly washed with distilled water until the washing solution was colorless and transparent, and the product obtained w...
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