Method for synthesizing isooctyl nitrate
A technology of isooctyl nitrate and a synthesis method, applied in the field of synthesis of isooctyl nitrate, can solve problems such as potential safety hazards, low yield of isooctyl nitrate, etc., so as to ensure production safety, reduce synthesis cost and nitration reaction smoothly. Effect
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Embodiment 1
[0018] Add 52ml of nitric acid with a concentration of 98% into the three-necked bottle, add 131ml of sulfuric acid with a concentration of 98% under water cooling and vigorous stirring to make a mixed acid, the temperature during the preparation of the mixed acid can be controlled below 35°C, and then add 90 79ml of petroleum ether at ~120°C, and then 157ml of isooctyl alcohol was added to the three-necked bottle, and the addition rate was controlled so that the reaction temperature was lower than 30°C, and the addition was completed in about 30 to 45 minutes. React for another half an hour. Static layering, separation of acid, ester and inert solvent mixed layer for water washing, alkali washing and washing to neutrality. After distillation, the purity of isooctyl nitrate reaches 99%, and the yield is 97%.
Embodiment 2
[0020] Process is the same as example 1, only change mixed acid proportioning and inert solvent: concentration is 82ml of 80% nitric acid, and concentration is 163ml of 98% sulfuric acid to make mixed acid, add No. 120 solvent naphtha 53ml, isooctyl alcohol 157ml in mixed acid. After distillation, the purity of 2-EHN reaches 99%, and the yield is 96.5%.
Embodiment 3
[0022] Process is the same as example 1, only change mixed acid proportioning and inert solvent: concentration is 65% nitric acid 105ml, and concentration is that 98% sulfuric acid 136ml makes mixed acid. Add 24ml of dichloroethane to the raw material isooctyl alcohol, and then add isooctyl alcohol (the amount of isooctyl alcohol is 157ml) with an inert solvent into the mixed acid. After distillation, the purity of 2-EHN reaches 98.3%, and the yield is 96%.
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