A kind of synthetic method of dimethyl azobisisobutyrate
A technology of dimethyl azobisisobutyrate and a synthesis method, which is applied in the direction of organic chemistry and the like, can solve the problems of unsuitable industrial scale production, difficult to handle discharge, human body and environmental hazards, etc., and achieves thorough product separation and reaction. The effect of short time, environmentally friendly and non-toxic raw materials
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Embodiment 1
[0030] (1) Condensation: Add the measured azobisisobutyronitrile, methanol, and isophorone into the reaction vessel, start stirring, add phosphorus trichloride solution dropwise, and the reaction temperature is 25°C. After the dropwise addition, keep warm for reaction 8 hours; the feed liquid was centrifuged to obtain azoimine methyl ether hydrochloride solid material; the mass concentration of phosphorus trichloride solution was 95%; the molar ratio of raw materials was azobisisobutyronitrile:methanol:isophor Alone: phosphorus trichloride=1:2:3.2:2;
[0031] (2) Hydrolysis: Add the measured pure water into the hydrolysis container, add the solid material of azoimine methyl ether hydrochloride obtained in step (1) into the hydrolysis container under stirring, control the temperature at 30°C, and wait for the azo After adding iminomethyl ether hydrochloride, adjust the pH value of the system to 6 for hydrolysis; the weight ratio of azoiminomethyl ether hydrochloride solid mat...
Embodiment 2
[0037] (1) Condensation: Add the measured azobisisobutyronitrile, methanol, and isophorone into the reaction vessel, start stirring, add phosphorus trichloride solution dropwise, the reaction temperature is 10°C, and keep warm after the dropwise addition 15 hours; the feed liquid was centrifuged to obtain azoimine methyl ether hydrochloride solid material; the mass concentration of the phosphorus trichloride solution was 97%; the molar ratio of the raw materials was azobisisobutyronitrile:methanol: Isophorone: phosphorus trichloride=1:2:5.8:2.8;
[0038] (2) Hydrolysis: Add the measured pure water into the hydrolysis container, add the solid material of azoimine methyl ether hydrochloride obtained in step (1) into the hydrolysis container under stirring, control the temperature at 20°C, and wait for the azoimine methyl ether hydrochloride solid material to After adding iminomethyl ether hydrochloride, adjust the pH value of the system to 4 for hydrolysis; the weight ratio of a...
Embodiment 3
[0044] (1) Condensation: Add the measured azobisisobutyronitrile, methanol, and isophorone into the reaction vessel, start stirring, add phosphorus trichloride solution dropwise, the reaction temperature is 30°C, and keep warm after the dropwise addition 10 hours; the feed liquid was centrifuged to obtain azoimine methyl ether hydrochloride solid material; the mass concentration of the phosphorus trichloride solution was 95%; the molar ratio of the raw materials was azobisisobutyronitrile:methanol: Isophorone: phosphorus trichloride=1:3.5:5.8:2.8;
[0045] (2) Hydrolysis: Add the measured pure water into the hydrolysis container, add the solid material of azoimine methyl ether hydrochloride obtained in step (1) into the hydrolysis container under stirring, control the temperature at 10°C, and wait for the azoimine methyl ether hydrochloride solid material to After adding iminomethyl ether hydrochloride, adjust the pH value of the system to 7 for hydrolysis; the weight ratio of...
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