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    PETN Synthesis of

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    Patrik
    The document describes the synthesis of pentaerythritol tetranitrate (PETN), a primary high explosive. PETN was synthesized through the nitration of pentaerythritol with 90% nitric acid and 96% sulfuric acid at 0°C over 2 hours. This produced PETN in near quantitative yield (99%) as white needles with a melting point of 140°C, matching the literature value. The synthesis allows for facile scale up to produce 50-100g of PETN.

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    PETN Synthesis of

    Uploaded by

    Patrik
    47 views2 pages
    The document describes the synthesis of pentaerythritol tetranitrate (PETN), a primary high explosive. PETN was synthesized through the nitration of pentaerythritol with 90% nitric acid and 96% sulfuric acid at 0°C over 2 hours. This produced PETN in near quantitative yield (99%) as white needles with a melting point of 140°C, matching the literature value. The synthesis allows for facile scale up to produce 50-100g of PETN.

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    The document describes the synthesis of pentaerythritol tetranitrate (PETN), a primary high explosive. PETN was synthesized through the nitration of pentaerythritol with 90% nitric acid and 96% sulfuric acid at 0°C over 2 hours. This produced PETN in near quantitative yield (99%) as white needles with a melting point of 140°C, matching the literature value. The synthesis allows for facile scale up to produce 50-100g of PETN.

    Copyright:

    © All Rights Reserved
    Download as RTF, PDF, TXT or read online from Scribd
    Download as rtf, pdf, or txt
    47 views2 pages

    PETN Synthesis of

    Uploaded by

    Patrik
    The document describes the synthesis of pentaerythritol tetranitrate (PETN), a primary high explosive. PETN was synthesized through the nitration of pentaerythritol with 90% nitric acid and 96% sulfuric acid at 0°C over 2 hours. This produced PETN in near quantitative yield (99%) as white needles with a melting point of 140°C, matching the literature value. The synthesis allows for facile scale up to produce 50-100g of PETN.

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    © All Rights Reserved
    Download as RTF, PDF, TXT or read online from Scribd
    Download as rtf, pdf, or txt
    of 2

    Synthesis and Characterization of Blowing Agents and Hypergolics

    http://ir.canterbury.ac.nz/bitstream/10092/581/1/12605854_307.doc

    The following preparation is transcribed from the reference above

    Synthesis of PETN , Pentaerythritol tetranitrate,

    o
    Pentaerythritol (4.80 g, 0.015 moles) and urea (0.03 g) were added at 0 C

    to 19.80 g of 90% concentrated nitric acid. Stirring was continued for 15 min.,

    then 96% concentrated sulfuric acid (19.80 g) was added, and the reaction

    mixture was left to stir at 0 oC for 2h. The whole was poured onto ice, filtered

    and washed with water (400 mL). The precipitate was dissolved in 250 mL of

    acetone containing 0.75 g of ammonium carbonate by heating in a water bath

    at 50 oC. Ethanol (72 mL) and water (108 mL) were then added.

    Pentaerythritol tetranitrate (7) crystallized out over 2h. Filtration and washing

    the precipitate with ethanol afforded a near quantitative yield (99%) of

    pentaerythritol tetranitrate (7) as white needles, mp 140 oC, (Lit.29 mp 141 oC).

    1
    H NMR (Acetone-d6 / DMSO-d6,) δ ppm: 4.77 (s, 8H);
    13
    C NMR (Acetone-d6 / DMSO-d6,) δ ppm: 68.6 (4C), 41.0.

    Elemental analysis: Theory: % C, 19.00; % H, 2.55; % N, 17.72.

    Found: % C, 19.29; % H, 2.44; % N, 17.35.

    Synthesis of PETN (7) was accomplished in near quantitative yield (99%) using

    excess fuming nitric (90%) and concentrated sulfuric acid (96%) in a 1 to 1 (w/w)

    ratio (Scheme 1). A note of caution is that the reaction is pH sensitive, if 86%

    H2SO4 is used instead of 96%, a mixture of the trinitrate and tetranitrate will be
    obtained. Scale up of the procedure to provide 50−100 g is facile; Camp et al.29

    have previously described kilogram scale synthesis.

    OH ONO2

    HNO3 90% O2NO ONO2


    HO OH
    H2SO4 96%
    OH ONO2

    19 7

    References

    1. Plastics and Rubber Processing and Applications, Kok, C. M., Tok, I. F., and Toh,
    H. K. 1985. 5: 281-284.
    Chem. Abstr., 1986, 104: 20537.

    13. Katritzky, A. R., Cundy, D. J., Chen. J. 1993. J. Energetic Materials, 11: 345-
    352.

    29. Camp, A.T., Marans, N. S., Elrick, D. E., and Preckel, R. F. 1955. J. Am. Chem.
    Soc., 77: 751-752.

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