反应 #425228

反应方程式

diethylphosphinic acid aluminum(III) salt

aluminum

ammonium peroxodisulfate

ethylene

ethylene

ethylene

ammonium peroxodisulfate

sodium hypophosphite monohydrate

→

ethylphosphonous acid aluminum(III) salt

收率 96.3%

溶剂

water

water

反应条件

后处理

1. 1
   其他a reducing valve set to 20 bar
2. 2
   其他a temperature of 100-110° C.
3. 3
   温度After cooling to about 90° C.
4. 4
   过滤Subsequently, the resulting solid is filtered off
5. 5
   洗涤washed with 2 l of hot water
6. 6
   其他dried at 130° C. under reduced pressure

实验过程

1500 g (14 mol) of sodium hypophosphite monohydrate are dissolved in 7.5 kg of water and initially charged in a 16 l steel-enamel jacketed pressure reactor. After heating the reaction mixture to 100° C., a reducing valve set to 20 bar is used to introduce ethylene into the reactor up to saturation. While stirring constantly at an ethylene pressure of 20 bar and a temperature of 100-110° C., a solution of 32 g (1 mol %) of ammonium peroxodisulfate in 300 g of water is metered in homogeneously. At a conversion of ethylene of 90%, the metered addition of ammonium peroxodisulfate is stopped and the reactor is decompressed. After cooling to about 90° C., 3000 g (4.67 mol of aluminum) of a 46% aqueous solution of Al2(SO4)3.14H2O is added within 60 minutes. Subsequently, the resulting solid is filtered off, washed with 2 l of hot water and dried at 130° C. under reduced pressure. The resulting mixture comprises diethylphosphinic acid aluminum(III) salt and ethylphosphonous acid aluminum(III) salt in a ratio of 87.3% by weight of diethylphosphinic acid aluminum(III) salt and 12.7% by weight of ethylphosphonous acid aluminum(III) salt (96.3% yield).

来源