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Method for preparing nitroguanidine by nitration of guanidine sulfate in continuous flow microchannel reactor

A micro-channel reactor and channel reactor technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large reactor volume, occupying a large workshop, obvious amplification effect, etc., to avoid The effect of serious corrosion of equipment, reduction of waste acid production, and improvement of reaction efficiency

Active Publication Date: 2015-12-23
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] Process features: This method does not require high temperature or high pressure conditions, and the pollution is relatively small, but it has high requirements for temperature control, the amplification effect is obvious, and the accumulation of materials is likely to bring safety hazards; the second is the batch method of production, the feeding, unloading It takes a long time to process materials, etc., and the volume of the reactor is huge, which requires a large workshop, etc.
[0017] So far, there has been no research on the preparation of nitroguanidine by nitrating guanidine sulfate with Corning microchannel continuous flow

Method used

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  • Method for preparing nitroguanidine by nitration of guanidine sulfate in continuous flow microchannel reactor
  • Method for preparing nitroguanidine by nitration of guanidine sulfate in continuous flow microchannel reactor
  • Method for preparing nitroguanidine by nitration of guanidine sulfate in continuous flow microchannel reactor

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Experimental program
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Effect test

Embodiment 1

[0040] (1) Device used: continuous flow microchannel reactor (straight channel functional module + "heart-shaped" structural functional module), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0041](2) Raw material tanks 1 and 2 are equipped with guanidine sulfate with a mass concentration of sulfuric acid solution of 10% and a mass concentration of nitric acid of 30%. Set the flow control of each metering pump 3, pump 4 to change the sulfuric acid solution of guanidine sulfate: nitric acid mol ratio=1:0.9, control the sulfuric acid solution flow rate of guanidine sulfate: 0.25mL / min, control the nitric acid flow rate: 0.2mL / min, and The materials are injected into each straight channel preheating module respectively, and the reaction temperature is controlled to be 40°C; the sulfuric acid ...

Embodiment 2

[0044] (1) Device used: continuous flow microchannel reactor (straight channel functional module + droplet channel), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0045] (2) Raw material tanks 1 and 2 are configured with a mass concentration of sulfuric acid solution of guanidine sulfate to be 15%; and a mass concentration of nitric acid to be 35%. Set the flow control of each metering pump 3 and pump 4 to change the sulfuric acid solution of guanidine sulfate: nitric acid molar ratio=1:1, control the sulfuric acid solution flow rate of guanidine sulfate: 0.2mL / min, control the nitric acid flow rate: 0.2mL / min, and The materials are injected into the preheating modules of each straight channel respectively, and the reaction temperature is controlled to be 50°C; the sulfuric acid solution o...

Embodiment 3

[0048] (1) The device used: continuous flow microchannel reactor (straight channel functional module + spherical baffle plate channel), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0049] (2) Raw material tanks 1 and 2 are configured with a mass concentration of sulfuric acid solution of guanidine sulfate to be 20%; and a mass concentration of nitric acid to be 35%. Set the flow control of each metering pump 3 and pump 4 to change the sulfuric acid solution of guanidine sulfate: nitric acid molar ratio=1:2, control the sulfuric acid solution flow rate of guanidine sulfate: 0.2mL / min, control the nitric acid flow rate: 0.8mL / min, and The materials are injected into the preheating modules of each straight channel respectively, and the reaction temperature is controlled to be 80°C; the sulfu...

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Abstract

The method for preparing nitroguanidine through nitration of guanidine sulfate in a continuous-flow microchannel reactor of the present invention belongs to the technical field of organic synthesis application, and is a method in which a sulfuric acid solution of guanidine sulfate and nitric acid are used as raw materials in a continuous-flow microchannel reactor. A new process for the synthesis of nitroguanidine with a reaction time ranging from ten seconds to several minutes. After the material is fed into the continuous flow microchannel reactor through the metering pump, it is preheated, mixed, and reacted to obtain the nitrated product nitroguanidine. This method is easy and safe to operate, and it is possible to produce nitroguanidine in a high-yield continuous manner. Process environment pollution is small. The product yield of the present invention is 90-93%, and the melting point is 230-232°C.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis application, and specifically relates to a method for preparing nitroguanidine by nitrifying and dehydrating a sulfuric acid solution of guanidine sulfate as a raw material, more specifically, using nitric acid to nitrify in a high-flux continuous flow microchannel reactor A process for preparing nitroguanidine from sulfuric acid solution of guanidine sulfate. Background technique [0002] Nitroguanidine is a raw material for organic synthesis. It is used as an intermediate for imidacloprid and acetamiprid in pesticides, and is used to synthesize N-nitroiminoimidazolidine, an intermediate in the next step. In addition, it can be used to prepare aminoguanidine through reduction. It is used in the synthesis of angina pectoris drugs such as Rocoan, and can also be used in the preparation of explosives and smokeless water medicines. Used in organic synthesis, preparation of aminoguanidine, ...

Claims

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Application Information

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IPC IPC(8): C07C279/34C07C277/08
Inventor 张跃严生虎刘建武辜顺林何兆斌陈明珠黄亚飞冯兴洋王莉杨玫玫史佳一
Owner CHANGZHOU UNIV
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