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ChemicalBook CAS DataBase List Tris(2-ethylhexyl) phosphate
78-42-2

Tris(2-ethylhexyl) phosphate synthesis

4synthesis methods
-

Yield:78-42-2 97.8%

Reaction Conditions:

with magnesium chloride;trichlorophosphate at 20 - 63; under 0 - 16 Torr; for 4.25 h;Sonication;Inert atmosphere;Pressure;Temperature;

Steps:

1; 2; 3; 4 Example 1

Equipped with mechanical stirrer,Constant pressure funnel,Thermometer, condenser,And a vacuum joint with a control valve250mL four-necked round flask was set in an ultrasonic instrument.Nitrogen purge,Isooctanol (148.2 g, 1.14 mol) was placed in a flask,Stirring, magnesium chloride (0.25 g, 0.005 g / g phosphorus oxychloride)And then put phosphorus oxychloride (50g, 0.3257mol) to the constant pressure funnel,Pull vacuum, open the ultrasound system,Cooled to 20 ° C,Start slowly dropped phosphorus oxychloride,Exothermic system significantly.Drops complete, insulation 1h, slowly warmed to 40 ,Incubated 1h, and finally warmed to 60 ,Insulation to the end of the reaction.Gas chromatography analysis,Chloro isooctane content of 0.3483%.Reaction control in Table 1-1,The results of the crude gas chromatographic analysis are shown in Table 1-2. Table 1-1 Reaction parameter table of Example 1
Table 1-2 Results of crude gas chromatographic analysis
Note: In Table 2, the retention time unit is min, the peak height unit is V,Peak area in units of mv * min,The peak with a retention time of 4.232 min was isooctanol,16.4min peak for the product triisooctyl phosphate, the same below;From Table 1-2, it can be concluded that the crude product obtained after the completion of the reaction contains an excess of isooctanol,By vacuum distillation can be recycled,The crude product which was reduced to isooctyl alcohol was washed with a 5% sodium hydroxide solution,Washed, the last vacuum distillation off the water,To obtain the product of triisooctyl phosphate,The yield was about 97.8%, the GC content was 99.6%

References:

CN106380481,2017,A Location in patent:Paragraph 0012; 0016; 0017; 0018; 0019; 0020; 0021-0061

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