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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

Pending Publication Date: 2019-07-12
SHANDONG HIMILE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional process, which adopts intermittent flask or kettle production, has the following defects: (1) the heat release of p-cresol nitration reaction is large, and the phenomenon of "flying temperature" is easy to occur; (2) the condition is not well controlled, and tar-like oxidation By-products, and the solvent used needs to be further separated, which makes the separation and purification of the product difficult and the post-processing cost is high; (3) The stability of batch production is poor, which affects the quality of subsequent chemical products

Method used

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  • Preparation method of nitrification organic matter and prepared nitrification organic matter
  • Preparation method of nitrification organic matter and prepared nitrification organic matter
  • Preparation method of nitrification organic matter and prepared nitrification organic matter

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preparation example Construction

[0022] A kind of preparation method of nitrification organic matter provided by the embodiment of the present invention, it comprises the following steps: pass nitrification acid liquid and molten state to be nitrified organic matter into microchannel reactor to react; Preferably, reaction residence time is more than 10s, in order to Taking the cresol reaction as an example, the reaction principle is as follows:

[0023]

[0024] Wherein, the organic matter to be nitrated is solid at normal temperature, and after the organic matter to be nitrated in molten state is passed into the microchannel reactor, the organic matter to be nitrated will not solidify and / or dissolve in the nitrifying acid solution. In order to ensure the state of the organic matter 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 matter to be nitrated is X...

Embodiment 1

[0046] The present embodiment provides a kind of preparation method of nitrated organic matter (o-nitro-p-cresol), comprising the steps:

[0047] Connect two metal high-pressure constant-flow pumps to the first two feeding ports of the microchannel reactor, and wash them with solvent water. After the sampling bottle is cleaned and dried, it is connected to the outlet of the sixth piece of the microchannel reactor. After the microchannel reactor was rinsed with solvent, it was filled with 30% nitric acid solution.

[0048] The temperature of the microchannel reactor is set at 20°C, and the p-cresol is heated in a water bath or an incubator until it is molten, and the molar ratio of p-cresol and nitric acid is set to 1:1.3, and p-cresol and 30% nitric acid The flow rates of the solutions were 18.5mL / min and 41.5mL / min respectively, and they were mixed in the microchannel reactor, and the residence time was 60s (the effective liquid holding capacity was 60.0mL). During the reac...

Embodiment 2

[0050] The present embodiment provides a kind of preparation method of nitrated organic matter (o-nitro-p-cresol), comprising the steps:

[0051] Connect two metal high-pressure constant-flow pumps to the first two feeding ports of the microchannel reactor, and wash them with solvent water. After the sampling bottle is cleaned and dried, it is connected to the outlet of the sixth piece of the microchannel reactor. After the microchannel reactor was rinsed with solvent, it was filled with 30% nitric acid solution.

[0052] Set the temperature of the microchannel reactor to 30°C, place p-cresol in a water bath or incubator and heat it to 40°C to be in a molten state, set the molar ratio of p-cresol and nitric acid to 1:1.3, p-cresol and 30 The flow rate of % nitric acid solution is 18.5mL / min and 41.5mL / min respectively, enters the microchannel reactor and mixes, and the residence time is 60s (effective liquid holding capacity is 60.0mL). During the reaction process, the tempe...

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Abstract

The invention discloses a preparation method of nitrification organic matter and the prepared nitrification organic matter, and relates to the technical field of organic synthesis. The preparation method of the nitrification organic substance comprises the following steps: introducing a nitrification acid liquid and molten-state organic matter to be nitrified into a microchannel reactor, and performing a reaction, wherein the organic matter to be nitrified is solid at normal temperature, and solidification and / or dissolution in the nitrification acid liquid does not occur in the organic matterto be nitrified after the organic matter to be nitrified is introduced into the microchannel reactor. According to the preparation method of the nitrification organic matter provided by the invention, the nitrification organic matter prepared by the method has a very good yield and purity without a solvent removal post-treatment process; in the whole process, no solvent participates in the reaction, so that the post-treatment process of solvent removal is avoided; and the method has high safety in the whole reaction process, adopts automation control, has high production efficiency and a greatly-improved production environment, and has larger industrial application value.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and in particular to a method for preparing nitrated organic matter and the prepared nitrated organic matter. Background technique [0002] O-nitro-p-cresol is a widely used intermediate in organic synthesis, which can be used in the synthesis of o-amino-p-cresol, which is an intermediate for the production of fluorescent whitening agent DT. Therefore, it is of great significance to study the preparation methods of nitrifying organic compounds. In industry, it is prepared by relatively simple and economical p-cresol nitration method, that is, benzene is used as solvent, p-cresol is used as raw material, and about 20% of dilute nitric acid is used for direct nitration, and the yield is generally less than 80%. It is also reported in the literature that the less toxic dichloromethane is used as a solvent, and the steam distillation and purification are replaced by vacuum distillation and...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/22B01J19/00
CPCC07C201/08C07C205/22B01J19/0093
Inventor 肖淑焕郭敏李丛香任苗苗
Owner SHANDONG HIMILE CHEM TECH
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