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Method for preparing nitrourea by utilizing microchannel reactor

A microchannel reactor, nitrourea technology, applied in chemical instruments and methods, preparation of urea derivatives, preparation of organic compounds, etc., can solve the problem of low impact sensitivity and friction sensitivity, nitrourea has not yet been seen, and increase safety. hidden dangers and other problems to achieve the effect of avoiding explosion, fast mass transfer rate, and reducing potential safety hazards

Active Publication Date: 2015-12-02
HANGZHOU HI TECH FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Since the current industrial preparation methods of nitrourea are all kettle-type reactions, and nitrourea is an explosive with very small impact sensitivity and friction sensitivity, and a large amount of heat is released during the reaction process, if the process control is not good, it is easy to A security incident occurred
If the amount of material held in the reactor is large, the potential safety hazard is greatly increased, and the highest yield of the traditional method is only 88%.
[0009] So far, there has been no research on the preparation of nitrourea by nitration of urea and acid in a microchannel reactor

Method used

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Embodiment 1

[0030] (1) A high-throughput microchannel reactor (straight channel module + spherical structure module) is used, connected according to the drawings in the manual. The number of modules is determined by the flow rate and reaction residence time. The material is injected into the heat exchange module through a metering pump, and the heat exchange The medium is heat transfer oil.

[0031] (2) Prepare a suspension of urea-concentrated sulfuric acid, design the molar ratio of urea:sulfuric acid to be 1:5, the reaction temperature is 15°C, and the reaction residence time is 60s. Control the flow rate of the sulfuric acid solution of urea sulfate to 2.0mL / min, control the flow rate of nitric acid to 0.4mL / min, the reaction temperature is 5°C, and the reaction residence time is 60s. After the sulfuric acid solution of urea sulfate passes through the mixing module, it enters the next mixing module and continues Mixing reaction, after the mixing is completed, the mixed product is cool...

Embodiment 2

[0034] (1) High-throughput microchannel reactor (straight channel module + Baguayang fish-shaped structure module), connected according to the drawings in the manual, the number of modules is determined by the flow rate and reaction residence time, and the material is injected into the heat exchange module through a metering pump , the heat transfer medium is heat transfer oil.

[0035] (2) Prepare a suspension of urea-concentrated sulfuric acid, design the molar ratio of urea:sulfuric acid to be 1:2, the reaction temperature is 10°C, and the reaction residence time is 100s. Control the flow rate of the sulfuric acid solution of urea sulfate to 2.0mL / min, control the flow rate of nitric acid to 0.4mL / min, the reaction temperature is 5°C, and the reaction residence time is 100s. After the sulfuric acid solution of urea sulfate passes through the mixing module, it enters the next mixing module and continues Mixing reaction, after the mixing is completed, the mixed product is coo...

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Abstract

The invention discloses a method for preparing nitrourea by utilizing a microchannel reactor and belongs to the technical field of organic synthesis application. In the microchannel reactor with a special internal structure, urea, concentrated sulphuric acid and concentrated nitric acid serve as raw materials, and nitrourea is synthesized in reaction time of tens of seconds to several minutes through the novel method. The materials enter the microchannel reactor through a metering pump and then undergo preheating, mixing, reaction and aftertreatment to obtain the nitrourea product. The method has the advantages that the microchannel reactor has excellent heat and mass transport effects and is simple and safe to operate, the product yield is high, and the emission of waste acid is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of organic synthesis application, in particular to a method for preparing nitrourea in a microchannel reactor. Background technique [0002] Nitrourea is a widely used organic chemical raw material and organic synthesis intermediate. Due to its specific electronic structure, it is capable of many forms of chemical reactions. Therefore, it has important applications in the preparation of medicines, explosives, foaming agents and various additives. [0003] At present, the main production process of nitrourea is divided into two categories: [0004] ① From the reverse process of the hydrolysis reaction of nitrourea, nitrourea is synthesized by the reaction of nitroamide and isocyanic acid. [0005] HNCO+H 2 NNO 2 =H 2 NCONHNO 2 [0006] Because this reaction is a reversible reaction, the product yield is not high, and nitroamide is extremely unstable, and the raw material is expensive, so it is not sui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/66C07C273/18
Inventor 陈海贤徐智锋
Owner HANGZHOU HI TECH FINE CHEM
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