Method for synthesizing nitromethane
A technology of nitromethane and synthesis methods, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of nitromethane yield decline, easy generation of sparks, and influence on the distillation process, etc., to achieve beneficial Product purity and yield, avoiding the harm of Mars, and improving the effect of reaction yield
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[0045] Example 1
[0046] In a four-necked flask equipped with an electric stirrer, a reflux condenser, a constant pressure dropping funnel and a thermometer, add 69 grams (1 mol) of sodium nitrite and 30 milliliters of water, respectively, and add sodium carbonate to make the pH of the reaction solution between 11 Between -12, add 0.03mol phase transfer catalyst dodecyl trimethyl ammonium chloride, add 50 ml of diethyl ether as solvent, add 63 g (0.5mol) dimethyl sulfate dropwise under stirring, and control the dimethyl sulfate The dropping rate of the ester is controlled at 30°C-35°C, the dropwise addition is completed, and the reaction is completed after 3 hours of incubation. After-treatment: the reaction solution was cooled to minus 27.5°C under stirring, the water was in the form of crushed ice, water and solid by-products were precipitated, filtered, and the solid-liquid two phases were separated. The separated liquid phases were combined, and after the solvent was rec...
Example Embodiment
[0047] Example 2
[0048] In a four-necked flask equipped with an electric stirrer, a reflux condenser, a constant pressure dropping funnel and a thermometer, add 69 grams (1 mol) of sodium nitrite and 35 milliliters of water, respectively, and add sodium carbonate to make the pH of the reaction solution between 10 Between -11, add 0.03mol of phase transfer catalyst tetrabutylammonium chloride, add 30 ml of dichloromethane as a solvent, add 63 g (0.5mol) of dimethyl sulfate dropwise under stirring, by controlling the concentration of dimethyl sulfate The dropping speed was controlled to control the temperature at 35°C-40°C, the dropwise addition was completed, and the incubation reaction was completed after 3 hours. After-treatment: the reaction solution was cooled to minus 22°C under stirring, and the water was in the form of crushed ice, so that water and solid by-products were precipitated, filtered, and the solid-liquid two phases were separated, and the solid phase was wa...
Example Embodiment
[0049] Example 3
[0050] In a four-necked flask equipped with an electric stirrer, a reflux condenser, a constant pressure dropping funnel and a thermometer, add 69 grams (1 mol) of sodium nitrite and 30 milliliters of water, respectively, and add sodium carbonate to make the pH of the reaction solution between 11 Between -12, add 0.035mol phase transfer catalyst 18-crown-6, add 10 ml of diethyl ether and 20 ml of methyl propyl ether as solvent, add 63 g (0.5mol) dimethyl sulfate dropwise under stirring, by controlling the diethyl sulfate The rate of addition of methyl ester was controlled at 34°C-40°C, the dropwise addition was completed, and the reaction was completed after 4 hours of incubation. After-treatment: the reaction solution was cooled to minus 25°C under stirring, the water was in the form of crushed ice, water and solid by-products were precipitated, filtered, and the solid-liquid two phases were separated, and the solid phase was washed twice with 60 ml of ethy...
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