A kind of method for preparing o-chlorobenzaldehyde by continuous oxidation of o-chlorotoluene
A technology of o-chlorotoluene and an oxidizing agent, which is applied in the technical field of organic synthesis technology, can solve the problems of inapplicability for large-scale promotion, large amount of catalyst, high production cost, etc., and achieves avoiding the use of co-catalyst, short reaction time and high production efficiency. high effect
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Embodiment 1
[0044] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor, the pipeline type is: (3a+3b) direct flow channel + round cake pulse variable diameter rectangular flat pipeline, the inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time, and the heat exchange medium is heat conduction Oil.
[0045] (2) 3.03g cobalt acetate and 3.03g sodium molybdate were dissolved in 200ml o-chlorotoluene and 200ml acetic acid respectively to form a mixed solution. At this time, n (cobalt acetate):n (o-chlorotoluene)=0.0075:1, and 3.03g NaBr dissolved in 5% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this moment n (sodium bromide):n (o-chlorotoluene)=0.0075:1, o-chlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by the flow velocity of 8.33ml / min and 16.67ml / min respectively, at this moment n(H 2 o 2 ): n (o-chlorotolue...
Embodiment 2
[0047] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3c) direct flow channel + oblique square cake pulse variable diameter rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time. The heat exchange medium is heat transfer oil.
[0048] (2) Dissolve 6.06g cobalt acetate and 6.06g sodium molybdate in 200ml o-chlorotoluene and 200ml acetic acid respectively to form a mixed solution. At this time, n (cobalt acetate): n (o-chlorotoluene)=0.015:1, and 6.06g NaBr dissolved in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (o-chlorotoluene)=0.015:1, o-chlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by the flow velocity of 8.33ml / min and 16.67ml / min respectively, at this moment n(H 2 o 2 ): n (o-chlorotoluene)=2...
Embodiment 3
[0050] (1) Device: refer to figure 2 Determine the connection mode of the tubular reactor. The pipeline type is: (3a+3d) direct flow channel + enhanced mixed round cake type rectangular flat pipeline. The inner diameter and volume of the pipeline are determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil. .
[0051] (2) Dissolve 6.06g cobalt acetate and 6.06g sodium molybdate in 200ml o-chlorotoluene and 200ml acetic acid respectively to form a mixed solution. At this time, n (cobalt acetate): n (o-chlorotoluene)=0.015:1, and 6.06g NaBr dissolved in 15% H 2 o 2 form H 2 o 2 -Acetic acid solution, at this time n (sodium bromide):n (o-chlorotoluene)=0.015:1, o-chlorotoluene-acetic acid solution and H 2 o 2 -Acetic acid solution is injected in the tubular reactor of continuous heat exchange by the flow velocity of 8.33ml / min and 16.67ml / min respectively, at this moment n(H 2 o 2 ): n (o-chlorotoluene)=2:1, usi...
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