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【资料】硝酸胍的合成

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转自MIT的争议化学实验室。翻译者刘企。


1楼2013-01-15 21:22回复
    硝酸胍 Guanidine nitrate
    CH6N4O3
    melting point :215-216 °C
    explodes at 230 °C
    molecular mass:122.08 g/mol
    density:0.75 g/mL
    sensitivity:low

    Guanidine nitrate is both an explosive compound and a precursor to other explosives similar to this one. The one difficulty in making this compound is obtaining the main ingredient, dicyanodiamide. The preparation of dicyanodiamide is a long and involved process using cyanamide, which is made from potassium cyanide reacted with chlorine then the product is reacted with ammonia, the cyanamide thus produced is reacted with sulfuric acid or ammonium sulfide. I'm not exactly sure about the specifics as of yet. This process was developed at around 1920 or 1921. I do not have many specifics relating to explosive or chemical properties of this compound. Some legitimate uses of this compound include the manufacturing of trimethoprim, folic acid, sulpha guanidine, organic synthetics, photographic chemicals, and disinfectants. Other names for this explosive are guanidine mononitrate, and guanidinium nitrate.
    Place a mixture of 210 g of dicyanodiamide and 440 g of ammonium nitrate in a 1-L Florence flask, the flask is immersed in an oil bath for heating which has athermometer in the oil. The oil bath should be preheated to 110-120 °C before placing the flask in, then it is warmed to 160 °C over 30 minutes, and held at this temp for 2 hours. At the end of that time the flask is removed and allowed to cool, and the contents are extracted on a steam bath by warming with successive portions of water. About 2 L of water will be needed, the hard cake of crystals will dissolve slowly, so sufficient time must be given for each portion of water to become saturated before it is decanted. The combined solution is filtered while hot for the removal of white insoluble material (that being ammeline and ammelide), concentrated to a volume of about 1 liter, and allowed to crystallize. There may be some crystals of guanidine nitrate mixed with the ammeline and ammelide, these can be re-dissolved in hot water and cooled to precipitate the ammeline and ammelide again, the guanidine nitrate will remain in solution. The mother liquors are concentrated to a volume of about 250 mL for a second crop, after the removal of which the residual liquors are discarded. The crude guanidine nitrate may be recrystallized by dissolving it in the least possible amount of boiling water and allowed to cool, or it may be dried thoroughly and used directly for the preparation of nitroguanidine.


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