Process for preparing methyl ethylphosphinate and methyl ethylphosphinate aluminum salt
A technology of ethyl methyl ethyl phosphinate and methyl ethyl phosphinic acid, which is applied in the field of dialkyl phosphinate flame retardant materials, can solve the problems of slow reaction rate, undisclosed reaction time, There are no problems such as the possibility of industrialized production, and the effects of high phosphorus content, reduced procedures, and reduced costs are achieved.
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[0049]
[0050]Add 100g of methyl diethylphosphinate (MDEP, purity 92.1%) and 2g of sodium iodide into a 250mL four-neck flask, protect it with nitrogen, and heat up to 140°C. After 6h, use GC to detect the reaction, and the conversion rate is 99.8%. Distill product, reclaim catalyst, the product methyl ethyl hypophosphite ethyl ester (MEEP) (product GC content 91.9%) that distills out is directly used in next step;
[0051]
[0052] Put 35.95g of anhydrous aluminum trichloride and 400g of trimethylbenzene in a 1L four-necked flask, and add 100g of MEEP dropwise. During the reaction, ethyl chloride gas is generated, which is absorbed by an exhaust device. After the drop is completed, the temperature is raised to 100°C. After reacting for 5 hours, raise the temperature to recover 300 g of trimethylbenzene by distillation; lower the temperature to 70°C, add 600 g of ethanol, react for 1 hour, filter, precipitate and dry to obtain the product with a yield of 96%, and recover...
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