3032-55-1Relevant articles and documents
Preparation method of trimethylol ethane trinitrate
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Paragraph 0014; 0015; 0016; 0023-0040, (2018/09/21)
The invention discloses a preparation method of trimethylol ethane trinitrate (TMETN). The preparation method takes trimethylol ethane as a raw material and comprises the following steps: firstly dissolving trimethylol ethane into water, so that trimethylol ethane aqueous solution with the mass fraction of 20-40% is obtained, then adding concentrated sulfuric acid into a reaction bottle, sequentially adding concentrated nitric acid and the trimethylol ethane aqueous solution, carrying out nitration reaction, after the reaction is completed, extracting with dichloromethane, washing with water for three times, and carrying out reduced pressure dichloromethane removal, so that the TMETN is obtained, wherein the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid to the trimethylol ethane aqueous solution to the dichloromethane is (1.1-2.2):(1.3-2.6):1:(1.6-3.2), reaction temperature is 10-15 DEG C, and reaction time is 10 minutes. The invention aims at solving theproblems that reaction conditions of a preparation process of the TMETN are harsh, solvent dosage is high and cost is high, and the preparation method disclosed by the invention is mainly used for preparation of the TMETN.
Sila-Substitution of Alkyl Nitrates: Synthesis, Structural Characterization, and Sensitivity Studies of Highly Explosive (Nitratomethyl)-, Bis(nitratomethyl)-, and Tris(nitratomethyl)silanes and Their Corresponding Carbon Analogues
Evangelisti, Camilla,Klapoetke, Thomas M.,Krumm, Burkhard,Nieder, Anian,Berger, Raphael J.F.,Hayes, Stuart A.,Mitzel, Norbert W.,Troegel, Dennis,Tacke, Reinhold
experimental part, p. 4865 - 4880 (2010/08/06)
A series of analogous nitratomethyl compounds of carbon and silicon of the formula types Me3ElCH2ONO2 (1a/1b), Me 2El(CH2ONO2)2 (2a/2b), MeEl(CH 2ONO2)3 (3a/3b), (CH2) 4El(CH2ONO2)2 (4a/4b), and (CH 2)5El(CH2ONO2)2 (5a/5b) were synthesized [El = C (a), Si (b); (CH2)4El = (sila)cyclopentane-1,1-diyl; (CH2)5El = (sila)cyclohexane-1,1-diyl]. All compounds were characterized by using NMR, IR, and Raman spectroscopy and mass spectrometry. In addition, the crystal structures of Me2C(CH2ONO2)2 (2a), (CH2)4C(CH2ONO2)2 (4a), Me2Si(CH2ONO2)2 (2b), and (CH 2)5Si(CH2ONO2)2 (5b) were determined by single-crystal X-ray diffraction. The gas-phase structures of the C/Si analogues 1a and 1b were determined by electron diffraction and compared with the results of quantum chemical calculations at different levels of theory. The thermal stabilities of the C/Si pairs 1a/1b-5a/5b were investigated by using DSC. In addition, their friction and impact sensitivities were measured with standard BAM methods. The extreme sensitivities of the silicon compounds 1b-5b compared to those of the corresponding carbon analogues 1a-5a were discussed in terms of the structures of the C/Si analogues and possible geminal Si???O interactions.
