Trisodium Trimetaphosphimate 1-hydrate

Submitted by Morris L. Nielsen and T. J. Morrow Checked by Oscar T. QuiMBYf 

The hydrolysis of trimeric phosphonitrile chloride dissolved in ether and shaken with aqueous sodium acetate solution was described by Stokes.1 It is slow and uncertain, however, and the substitution of dioxane for ether, as practiced by de Fiequelmont in related preparations,2 is preferred. 

The sodium salt is prepared in a manner similar to that for the potassium salt. A solution of 60 g. of trimeric phosphonitrile chloride in 240 ml. of dioxane is stirred with a solution of 300 g. of sodium acetate 3-hydrate in 480 ml. of water at 45 to 55°. After 3 hours, crystals amounting to 47 to 55 g. are recovered, and after an additional 16 hours a second crop can be recovered for a total of 59 g. (91%). The product is found to be free of sodium chloride by x-ray diffraction analysis. Anal. Calcd. for Na3(P02NH)3-H20 N, 11.22 P, 24.77 Na, 18.40. Found N, 11.01 P, 24.99 Na, 18.2. 

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Ps06(NH)3K3 Tripotassium tri-metaphosphimate, 6 97 Pa06(NH)3Na8 Trisodium tri-metaphosphimate, 1-hydrate, 6 99 4-hydrate, 6 105 P,0 (NH)3Na,NaOH-7H20 Trisodium trimetaphosphimate, 6 80... 

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