Continuous coupling reaction integrated device and application thereof
A coupling reaction, integrated device technology, applied in chemical/physical/physical-chemical reactors, azo dyes, monoazo dyes, etc., can solve the problems of matching flow adjustment, high purity and yield, and good dispersion. , to achieve the effect of good dispersion, high purity yield and small product particles
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Embodiment 1
[0054] (1) 500g red base-3GL, 831.1g industrial hydrochloric acid (32%), and 4.41L water are made into amino matter slurry, and 207.0g sodium nitrite is dissolved in 5L water to prepare a solution, and the above slurry and solution are mixed in heavy The diazonium salt solution is obtained in the nitrogen salt storage tank 101.
[0055](2) 436g industrial product N-ethyl-3-cyano-4-methyl-6-hydroxyl-2-pyridone (purity 58.88%) was dissolved in 10L lye containing 87g NaOH, and the coupling solution was placed in Coupling component storage tank 301.
[0056] (3) The diazonium salt solution and the coupling component were continuously pumped into the layered partition microchannel reaction unit 8 through the heat exchanger at 50 mL / min for coupling reaction, and the temperature of the material at the outlet of the heat exchanger was controlled to be 15°C.
[0057] (4) The online ultraviolet detector automatically detects the color light of excess raw materials, automatically compa...
Embodiment 2
[0062] (1) Mix 30g of o-chloro-p-nitroaniline (DCB, 74%), 16mL of analytical hydrochloric acid (37.5%), 0.05g of EDTA, and 500mL of water for 30 minutes to make amino slurry, and dissolve 8g of sodium nitrite in 500mL of water to prepare To form a solution, the above slurry is mixed with the solution, and placed in the diazonium salt storage tank 101 to obtain the diazonium salt solution.
[0063] (2) 22.35g industrial product o-methyl acetoacetanilide (purity 58.88%) is dissolved in the 1L lye that contains 5.4g NaOH, adds 0.05g of EDTA, drips glacial acetic acid, makes the pH of the solution after acid precipitation at 5.5- 6.0, the obtained coupling solution is placed in the coupling component storage tank 301 .
[0064] (3) The diazonium salt solution and the coupling component are continuously pumped into the collision flow microchannel reactor through the heat exchanger at 10mL / min ( figure 2 ) to carry out the coupling reaction, and control the temperature of the mate...
Embodiment 3
[0070] (1) 30g o-chloro-p-nitroaniline, 5g industrial hydrochloric acid (32%), and 0.5L water are made into amino substance slurry, and 12.5g sodium nitrite is dissolved in 0.5L water to prepare a solution, and the above slurry is mixed with the solution Place in the diazonium salt storage tank 101 to obtain the diazonium salt solution.
[0071] (2) Add 95.8g of 3-(N,N-diacetoxyethyl)aminoacetanilide (purity: 58.88%) into 1L of water, add 4.8g of emulsifier system to form an emulsion, and the obtained coupling emulsion is placed in the coupling unit In the storage tank 301.
[0072] (3) The diazonium salt solution and the coupling emulsion are continuously pumped into the layered partition type microchannel reactor through the heat exchanger at 10mL / min ( Figure 4 ) to carry out the coupling reaction, and the temperature of the material at the outlet of the heat exchanger is controlled to be 18°C.
[0073] (4) The online ultraviolet detector automatically detects the color ...
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