Diquat synthesizing and refining technology
A diquat and refining technology, applied in herbicides and algaecides, chemicals for biological control, animal repellents, etc., can solve the problem of high consumption of dibromoethane raw materials, affecting the synthesis of diquat efficiency, increase the difficulty of exhaust gas treatment, etc., to achieve the effect of reducing material consumption, shortening reaction time, and reducing toluene consumption
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Embodiment 1
[0023] Diquat synthesis and refining process described in the present embodiment comprises the following steps:
[0024] (1) Precipitation: Take the bipyridyl toluene liquid and remove the solvent toluene through a two-stage thin-film evaporator under reduced pressure to obtain 2.2-bipyridine, and control the temperature during vacuum distillation to be 120-150°C for subsequent use;
[0025] (2) Synthesis: Take 600kg of 2.2-bipyridine obtained in the above step (1) and 6000kg of 1,2-dibromoethane, add them to the reaction kettle in turn, heat up to 140-160°C for heat preservation reaction, and take samples during the reaction Analysis, when the content of 2.2-bipyridine≦2% (compared with the initial amount), the reaction is terminated, and the total reaction time is 11 hours;
[0026] (3) Layering: after the reaction, add 1000 kg of water to the reaction kettle to mix evenly, and let the reaction solution stand still for 2 hours before layering, and separate the lower layer of...
Embodiment 2
[0032] Diquat synthesis and refining process described in the present embodiment comprises the following steps:
[0033] (1) Precipitation: Take the bipyridyl toluene liquid and remove the solvent toluene through a two-stage thin-film evaporator under reduced pressure to obtain 2.2-bipyridine, and control the temperature during vacuum distillation to be 120-150°C for subsequent use;
[0034] (2) Synthesis: Take 600kg of 2.2-bipyridine obtained in the above step (1) and 6300kg of 1,2-dibromoethane, add them to the reaction kettle in turn, heat up to 140-160°C, and carry out insulation reaction. Sampling analysis, when the content of 2.2-bipyridine≦2% (compared with the initial amount), the reaction is terminated, and the total reaction time is 12 hours;
[0035] (3) Layering: after the reaction, add 13300 kg of water to the reaction kettle to mix evenly, and separate the reaction liquid for 3 hours to separate the lower layer of 1,2-dibromoethane to obtain a reaction liquid con...
Embodiment 3
[0041] Diquat synthesis and refining process described in the present embodiment comprises the following steps:
[0042] (1) Precipitation: Take the bipyridyl toluene liquid and remove the solvent toluene through a two-stage thin-film evaporator under reduced pressure to obtain 2.2-bipyridine, and control the temperature during vacuum distillation to be 120-150°C for subsequent use;
[0043] (2) Synthesis: Take 630kg of 2.2-bipyridine obtained in the above step (1) and 6000kg of 1,2-dibromoethane, add them to the reaction kettle in turn, heat up to 140-160°C, and carry out insulation reaction. Sampling analysis, when the content of 2.2-bipyridine≦2% (compared with the initial amount), the reaction is terminated, and the total reaction time is 12 hours;
[0044] (3) Layering: after the reaction, add 1500 kg of water to the reaction kettle to mix evenly, and separate the reaction liquid for 4 hours to separate the lower layer of 1,2-dibromoethane to obtain a reaction liquid cont...
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