Method for nitration synthesis of acifluorfen in microreactor
A technology of acifluorfen and microreactors, which is applied in the preparation of nitro compounds, chemical instruments and methods, chemical/physical/physical chemical reactors, etc., can solve the harsh and safe synthesis conditions of acifluorfen Low problems, to achieve the effect of fast mass transfer rate and reaction rate, increased heat transfer efficiency, and easy to scale up
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[0027]Example 1
[0028]Use 98 wt% fuming nitric acid and 20 wt% fuming sulfuric acid to prepare mixed acid with a nitric acid:sulfuric acid molar ratio of 0.55:1. The temperature of the mixed acid configuration process is controlled at 15-20 ℃. The mass fractions of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid, acetic anhydride, and dichloroethane in the organic phase were 15.8%, 5.3%, and 78.9%, respectively.
[0029]Under the condition of 15 ℃, the mixed acid and organic phase are pumped into the micro-mixer by a high-pressure syringe pump through a pipeline. The micro-mixers adopt T-type mixing mode and pass into the micro-channel reactor with a diameter of 500 μm; nitric acid and 3-(2 The molar ratio of -chloro-4-trifluoromethylphenoxy)benzoic acid is 1.4:1, the reaction residence time is 540 s, the reaction product flows out of the reactor, and the product is obtained by phase separation, drying, and water washing. The reaction conversion rate reaches 99.19 %, selectivity 81.08...
Example Embodiment
[0042]Example 2
[0043]The process is the same as in Example 1, the molar ratio of mixed acid nitric acid: sulfuric acid remains unchanged, and the mass fraction of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid in the organic phase is 8%. At 10 ℃, the molar ratio of nitric acid to 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid is 0.96:1, the reaction residence time is 30 s, the reaction conversion rate is 53.13%, and the selectivity is 80.32 %.
Example Embodiment
[0044]Example 3
[0045]The process is the same as in Example 1, the molar ratio of mixed acid nitric acid: sulfuric acid remains unchanged, and the mass fraction of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid in the organic phase is 30%. At 35 ℃, the molar ratio of nitric acid to 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid is 1.8:1, the reaction residence time is 780 s, the reaction conversion rate is 99.98%, and the selectivity is 69.21 %.
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