Process of preparing dicamba by 3, 6-dichlorosalicylic acid
A technology of dichlorosalicylic acid and dicamba, which is applied in the field of preparation technology of dicamba and the preparation technology of herbicide dicamba, can solve the problems of low utilization rate of equipment, reduced waste water volume, long saponification time, etc., and achieves the utilization of equipment. Increased efficiency, reduced waste water, and automated effects
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Embodiment 1
[0039] A process for preparing dicamba using 3,6-dichlorosalicylic acid, comprising the following process steps:
[0040] A. Methylation reaction
[0041] Dissolve 3,6-dichlorosalicylic acid in lye, pump it into the methylation continuous reactor, fill it with methyl chloride gas, and add lye and methanol solution of the catalyst dropwise at the same time to carry out the methylation reaction. After the reaction is completed, the pressure is released to obtain a methylation reaction solution;
[0042] B. Saponification reaction
[0043] Put the methylation reaction solution obtained in step A into the saponification continuous reactor, add lye, keep the reaction temperature at 100°C, the pressure at 0.10MPa, and the time of 0.2h, after the reaction is complete, cool down to 30°C, release the pressure, and obtain the saponification reaction solution;
[0044] C. Recovery of methanol
[0045] The saponification reaction solution obtained in step B is entered into a distillati...
Embodiment 2
[0049] A process for preparing dicamba using 3,6-dichlorosalicylic acid, comprising the following process steps:
[0050] A. Methylation reaction
[0051] Dissolve 3,6-dichlorosalicylic acid in lye, pump it into the methylation continuous reactor, fill it with methyl chloride gas, and add lye and methanol solution of the catalyst dropwise at the same time to carry out the methylation reaction. After the reaction is completed, the pressure is released to obtain a methylation reaction solution;
[0052] B. Saponification reaction
[0053] Put the methylation reaction solution obtained in step A into the saponification continuous reactor, add lye, keep the reaction temperature at 140°C, the pressure at 0.50MPa, and the time for 1.5h, after the reaction is complete, cool down to 90°C, release the pressure, and obtain the saponification reaction solution;
[0054] C. Recovery of methanol
[0055] The saponification reaction solution obtained in step B is entered into a distillat...
Embodiment 3
[0059] A process for preparing dicamba using 3,6-dichlorosalicylic acid, comprising the following process steps:
[0060] A. Methylation reaction
[0061]Dissolve 3,6-dichlorosalicylic acid in lye, pump it into the methylation continuous reactor, fill it with methyl chloride gas, and add lye and methanol solution of the catalyst dropwise at the same time to carry out the methylation reaction. After the reaction is completed, the pressure is released to obtain a methylation reaction solution;
[0062] B. Saponification reaction
[0063] Put the methylation reaction solution obtained in step A into the saponification continuous reactor, add lye, keep the reaction temperature at 120°C, the pressure at 0.30MPa, and the time of 0.9h, after the reaction is complete, cool down to 60°C, release the pressure, and obtain the saponification reaction solution;
[0064] C. Recovery of methanol
[0065] The saponification reaction solution obtained in step B is entered into a distillatio...
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