Isocyanates from oxalyl chloride and amines

Details Isocyanates from oxalyl chloride and amines Isocyanates from oxalyl chloride and amines

1986-08-25

1987-05-05

Siegel, Alan

Organic compounds -- part of the class 532-570 series

Organic compounds

Isocyanate esters

C07C 7100

Patent

active

046634738

ABSTRACT:
An isocyanate compound of the general formula R(NCO).sub.n, wherein R is her an aliphatic or an aromatic radical or a combination of both, and n is 1 or a larger integer is prepared by the process comprising dissolving in a high temperature boiling point solvent contained in an agitated, jacketed reactor vessel, an amine of the formula R(NH.sub.2).sub.n, completing a hydrochlorination and precipitation step to form a colloidal suspension of microcrystalline salt particles of amine hydrochloride salt R(NH.sub.2).sub.n.nHCl, introducing oxalyl chloride with agitation and by subsurface injection into the amine hydrochloride salt solution to form an intermediate of amine oxamyl chloride in situ which is thermally decomposed to yield an isocyanate of the general formula R(NCO).sub.n, and separating and purifying the isocyanate by distillation. The unreacted oxalyl chloride and high temperature reaction solvent are recovered by distillation and by absorption from the HCl by-product and are recycled. The by-product HCl is also partially recycled and used for hydrochlorination.

REFERENCES:
patent: 4322365 (1982-03-01), Franzmerger et al.
A. J. Speziale and L. R. Smith, J. Org. Chem., 28, 1805 (1963).
J. Goerdeler and H. Schenk, Angew. Chem., 75, 675 (1963).
Ulrich von Gizycki, Angew. Chem. Int. Ed. Engl., 10, 403 (1971).

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