Process for the production of hexanitrostilbene

Details Process for the production of hexanitrostilbene Process for the production of hexanitrostilbene

1979-03-06

1981-03-10

Kyle, Deborah L.

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

Organic compounds

Oxygen containing

149105, 149111, C07C 7602, C07C 7910

Patent

active

042553580

ABSTRACT:
A process for the production of 2, 2', 4, 4', 6, 6'-hexanitrostilbene, which gives a readily isolable product and in which solvent recovery is relatively straightforward, is described.
An alkali or alkaline earth hypochlorite was reacted with 2, 4, 6-trinitrotoluene in an aqueous organic solvent, preferably containing tetrahydrofuran. The reactant mixture was allowed to stand for at least 30 minutes when a solution of a mineral acid, especially sulphuric acid, was added, with stirring, to acidify the mixture to a final pH of less than 5, preferably between 0.5 and 1.0, especially 0.7. This acidification caused agglomeration of the hexanitrostilbene. When complete mixing of the solutions had been obtained, the stirring was stopped and the mixture allowed to settle and separate into two layers. The top layer, which contained little solid product, was run off through a filter and the filtrate was treated separately to recover solvents, especially tetrahydrofuran. The bottom layer, which contained most of the solid product, was then passed through the filter to collect the agglomerated solid.
Washing the product afforded hexanitrostilbene that has a surface area of between 3 and 6 meter.sup.2 gm.sup.-1 when measured by gas adsorption techniques.

REFERENCES:
patent: 3505413 (1970-04-01), Shipp
patent: 3699176 (1972-10-01), Syrop
patent: 4085152 (1978-04-01), Salter

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