- Preparation method of trimethylol ethane trinitrate
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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.
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Paragraph 0014; 0015; 0016; 0023-0040
(2018/09/21)
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- METHODS OF PRODUCING NITRATE ESTERS
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Methods of forming a nitrate ester include combining at least one nitrate salt and sulfuric acid to form a nitrating solution and adding an aliphatic polyol to the nitrating solution. Nitrate esters formed by this method may be, for example, triethylene glycol dinitrate (TEGDN), pentaerythritol tetranitrate (PETN), diglycerol tetranitrate (DGTN), 1,1,1-tris(methylol)ethane trinitrate (TMETN), 1,2,4-butanetriol trinitrate (BTTN), nitroglycerin (NG), diethylene glycol dinitrate (DEGDN), ethylene glycol dinitrate (EGDN), metriol trinitrate (MTN), nitrocellulose (NC), or 1,2-propanediol dinitrate (PDDN).
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Page/Page column 5
(2012/06/01)
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- 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
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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.
- Evangelisti, Camilla,Klapoetke, Thomas M.,Krumm, Burkhard,Nieder, Anian,Berger, Raphael J.F.,Hayes, Stuart A.,Mitzel, Norbert W.,Troegel, Dennis,Tacke, Reinhold
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experimental part
p. 4865 - 4880
(2010/08/06)
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- Preparation of di- and polynitrates by ring-opening nitration of oxetanes by dinitrogen pentoxide (N2O5)
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Ten oxetanes bearing various substituents were reacted with N2O5 in chlorinated hydrocarbon solvents to yield 1,3-dinitrate esters (I) by ring-opening nitration. The yields ranged from 73 to 88% for di-/trinitrates derived from oxetanes unsubstituted in the 2-position, to only 15 to 21% for oxetanes bearing such substituents. Although selective ring cleavage of oxetanes bearing non-hydroxylic substituents (epoxy (oxiranyl), spiro-oxetane and alkene) was not, in general, possible, selective nitration of hydroxyalkyloxetanes was achievable under the conditions employed to yield nitrato-methyloxetanes useful as precursors for energetic polyethers. A semi-quantitative reactivity comparison with representative epoxides indicated that the reactivity of oxetanes towards N2O5 was lower, as expected on account of their lower ring strain.
- Golding,Millar,Paul,Richards
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p. 7051 - 7062
(2007/10/02)
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