Preparation method of nitrification organic matter and prepared nitrification organic matter
A technology of organic matter and nitrating acid solution, which is applied in the preparation of nitro compounds, organic chemistry, chemical instruments and methods, etc. It can solve the problems of affecting the quality of chemical products, poor batch production stability, and high post-processing costs, and achieve large-scale industrial applications. value, improved production environment, and high production efficiency
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[0022] An embodiment of the present invention provides a method for preparing nitrated organic matter, which includes the following steps: pass the nitrated acid solution and the molten organic matter to be nitrated into a microchannel reactor for reaction; preferably, the reaction residence time is more than 10s to correct Take the cresol reaction as an example, the reaction principle is as follows:
[0023]
[0024] Wherein, the organic matter to be nitrated is solid at room temperature, and after the organic matter to be nitrated in a molten state is passed into the microchannel reactor, the organic matter to be nitrated will not be solidified and / or dissolved in the nitrating acid solution. In order to ensure the state of the organic substance to be nitrated in the microchannel reactor, the reaction temperature should not be too low. Preferably, the difference between the reaction temperature and the melting point temperature of the organic substance to be nitrated is X, X≥-30...
Example Embodiment
[0045] Example 1
[0046] This embodiment provides a method for preparing nitrated organic matter (o-nitro-p-cresol), which includes the following steps:
[0047] Connect two metal high-pressure constant flow pumps with the first two feed ports of the microchannel reactor, and wash them with solvent water. The sampling bottle is cleaned, dried, and then connected to the sixth discharge port of the microchannel reactor. After the microchannel reactor is rinsed with solvent, it is filled with 30% nitric acid solution.
[0048] The temperature of the microchannel reactor is set to 20℃, the p-cresol is heated to a molten state in a water bath or a thermostat, the molar ratio of p-cresol and nitric acid is set to 1:1.3, p-cresol and 30% nitric acid The flow rates of the solution were 18.5mL / min and 41.5mL / min, respectively, and they were mixed in the microchannel reactor with a residence time of 60s (effective holding capacity of 60.0mL). During the reaction, the temperature was contro...
Example Embodiment
[0049] Example 2
[0050] This embodiment provides a method for preparing nitrated organic matter (o-nitro-p-cresol), which includes the following steps:
[0051] Connect two metal high-pressure constant flow pumps with the first two feed ports of the microchannel reactor, and wash them with solvent water. The sampling bottle is cleaned, dried, and then connected to the sixth discharge port of the microchannel reactor. After the microchannel reactor is rinsed with solvent, it is filled with 30% nitric acid solution.
[0052] The temperature of the microchannel reactor is set to 30°C, the p-cresol is heated to 40°C in a water bath or in a constant temperature box, and the molar ratio of p-cresol to nitric acid is set to 1:1.3. The flow rates of the% nitric acid solution are 18.5 mL / min and 41.5 mL / min, respectively, and enter the microchannel reactor for mixing, and the residence time is 60 s (the effective holding capacity is 60.0 mL). During the reaction, the temperature was cont...
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