Abstract:
510,854. Glycerine esters. I.G. FARBENINDUSTRIE AKT.-GES. Feb. 7, 1939, No. 3993. Convention date, Feb. 10, 1938. [Class 2 (iii)] Nitric acid esters of mono acyl glycerines are prepared by reacting glycide nitrate with organic acids, e.g., aliphatic and aromatic carboxylic acids such as formic, acetic and substituted and unsubstituted benzoic acids, preferably at elevated temperatures, e.g., 60‹-120‹C. and preferably in the presence of a little metallic chloride, e.g., ferric chloride, with or without the addition of an inert solvent. The mononitric acid esters formed may be converted into the dinitric acid esters by nitrating with concentrated nitric acid, preferably in the presence of concentrated sulphuric acid. The products render glycerine trinitrate and other liquid explosives which tend to solidify at low temperatures more difficult to freeze In examples (i) and (ii) glycerine monoformate mononitrate and glycerine monoacetate mononitrate, the major part of which probably contain the acyl radicle in the alpha-position, are prepared by reacting formic and glacial acetic acid with glycide nitrate in the presence of a little ferric chloride at 95‹-100‹C. for 15 minutes, (iii) glycerine mononitrobenzoate mononitrate, the major part of which probably contains the nitrobenzoic acid radicle in the alpha-position, is prepared by heating glycide nitrate, meta-nitrobenzoic acid and ferric chloride at 100‹-110‹C. for 2 hours, (iv) glycerine monoacetate dinitrate, the major part of which is probably alpha-acetyl compound, is prepared by introducing glycerine monoacetate mononitrate (see example (ii)) into a mixture of nitric acid (S.G. 1.5) and oleum at 25‹C.
Abstract:
284,700. Schmid, A., and Meissner, J., (Assignees of Dynamit-Akt.-Ges. vorm. A. Nobel & Co.). Feb. 5, 1927, [Convention date]. Nitrates of glycerol and similar alcohols.-In nitrating glycerine, glycol and similar alcohols, glycerine, &c. is introduced by a pipe 9 and nitrating acid through openings 7 into a current of reacting mixture circulating between a reaction chamber 4 and a cooling chamber 5 separated by a partittion which may be formed of cooling tubes 3 placed closed together. Excess of the reaction mixture overflows through the outlet 2. The circulation is maintained by a stirrer 6 or by injection of air. The cooling-chamber 5 may be tubes through which cooling medium is circulated or may be arranged so that the reaction mixture passes through tubes surrounded by a cooling medium.