Invetigation Of New Synthesis Technics On Geminal-Dintro Compound

Geminal-dinitro compound is an excellent energy-containing material with middle energy, stable features and have been widely used in a wide variety of applications. As one of the most important energy-containing material, 2,2-dinitropropanol is the important intermediate product of geminal -dinitro energetic compound. Therefore it has great value to reducing the cost of producing energetic materials, which that researches a kind of simple, feasible, cost-effective synthesis method. By far, the synthesis of 2,2-dinitropropanol adopt oxidative nitration reaction using silver nitrate and potassium ferricyanide as oxidants according to existing literature. In this thesis, we proposed a new procedure to synthesize 2,2-dinitropropanol by using ion-exchange membrane electrolysis to prepare silver nitrate as oxidant for the sake of reducing costs and pollution.The thesis focused and studied on the following aspects:1 Optimized the synthesis process of 2-nitropropanol and investigated the materials ratio, reaction temperature and the conditions of experimental post-treatment. The optimal reaction conditions:the materials ratio is 1.01:1:1.03; reaction temperature is 0℃; the optimal conditions of experimental post-treatment is adjusting the pH with a 1:3 solution of phosphoric acid, and ethyl acetate as extraction solvent. The compounds were characterized by FT-IR and 1H-NMR. The product purity is determined by gas chromatography.2 On the best experimental conditions which has been determined in the first step, the second step nitrification oxidation was conducted by using silver nitrate of different concentrations including 8.0mol/L,6.0 mol/L,4.0 mol/L,2.0 mol/L,1.0 mol/L and 0.5 mol/L. The products were characterized by FT-IR and 1H-NMR. The product purity is determined by gas chromatography confirming that the product quality and yield can be satisfactory by using silver nitrate of low concentrations in the synthesis.3 Established a new technics to electrolyte recover silver into silver nitrate. The optimal reaction conditions determined through a series of condition experiment, which is applied voltage of 5V, anode electrolyte employed distilled water with a little of potassium nitrate, cathode electrolyte employed the mixed solution of KNO3-HNO3(1:1), and the optimal amount and concentration is 140ml&1.4mol/L. In this electrolysis conditions, the actual cell voltage is 2.31V, average current is 0.601A, working electrode potential is 1.925V, the concentration of silver nitrate solution electrolysised is 0.866mol/L, recovery radio is 81.6%, current efficiency reach to 92.7%.4 The synthesis was conducted with the recovery silver nitrate at low concentrations, investigated the key factors of synthesis at the same time. Orthogonal tests determined the optimal reaction conditions:after the first step reaction, the reacted solution and sodium nitrite solution were mixed, then the above mixture was add to the silver nitrate solution, the reaction temperature is 20℃, extracted by ethyl acetate. The product purity is determined by gas chromatography. The results show that the yield and purity of synthesized product achieved satisfactory confirming that the ion-exchange membrane electrolysis technics to recover silver is possible.5 Established the method of gas chromatography external standard and internal standard, to determinate the purity of 2-nitropropanol and 2,2-dinitropropanol synthesized respectively.