Method for preparing nitroguanidine through micro-channel reactor

A micro-channel reactor, nitroguanidine technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as nitroguanidine that have not yet been seen, and avoid serious corrosion of equipment, avoid leakage, temperature Precisely controlled effects

Inactive Publication Date: 2013-06-26
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] So far, there has been no research on the dehydration of concentrated sulfuric acid to aci

Method used

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  • Method for preparing nitroguanidine through micro-channel reactor
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  • Method for preparing nitroguanidine through micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 1

[0042] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning cardioid channel 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 the reaction residence time, and the heat exchange medium is heat transfer oil.

[0043] (2) Raw material tanks 1 and 2 are equipped with 10% guanidine nitrate aqueous solution and concentrated sulfuric acid, and set the flow control of each metering pump 3 and pump 4 to change the guanidine nitrate aqueous solution: the molar ratio of concentrated sulfuric acid = 1:0.9 to control nitric acid Guanidine aqueous solution flow rate: 0.25mL / min, control concentrated sulfuric acid flow rate: 0.2mL / min, feed the materials into each straight channel preheating module, and control the reaction temperature to 40℃; use metering pumps for guanidine nitrate aqueous solution and conce...

Example Embodiment

[0045] Example 2

[0046] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning cardioid channel 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 the reaction residence time, and the heat exchange medium is heat transfer oil.

[0047] (2) Raw material tanks 1 and 2 are equipped with a mass concentration of 15% guanidine nitrate aqueous solution and concentrated sulfuric acid. Set the flow control of each metering pump 3 and pump 4 to change the molar ratio of guanidine nitrate aqueous solution: concentrated sulfuric acid = 1:1, control the flow rate of guanidine nitrate aqueous solution: 0.2mL / min, control the flow rate of concentrated sulfuric acid: 0.2mL / min, separate the materials Into each straight channel preheating module, control the reaction temperature to 50℃; the guanidine nitrate aqueous solution and co...

Example Embodiment

[0049] Example 3

[0050] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning cardioid channel 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 the reaction residence time, and the heat exchange medium is heat transfer oil.

[0051] (2) Raw material tanks 1 and 2 are equipped with 20% guanidine nitrate aqueous solution and concentrated sulfuric acid. Set the flow control of each metering pump 3 and pump 4 to change the guanidine nitrate aqueous solution: the molar ratio of concentrated sulfuric acid = 1:2, control the flow rate of the guanidine nitrate aqueous solution: 0.2mL / min, control the flow rate of concentrated sulfuric acid: 0.8mL / min, separate the materials Into each straight channel preheating module, the reaction temperature is controlled to 90℃; the guanidine nitrate aqueous solution and concentrated...

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Abstract

The invention relates to a method for preparing nitroguanidine through a micro-channel reactor, belonging to the technical field of organic synthesis applications. The method is a new process for synthesizing nitroguanidine by taking a water solution of guanidine nitrate and concentrated sulfuric acid as raw materials and performing acid dehydration in the Corning micro-channel reactor within a short reaction time from tens of seconds to a few minutes. Materials are introduced into the Corning micro-channel reactor through a metering pump, a nitroguanidine product is obtained by preheating, mixing, reaction and post-treatment, and the method has the advantages of simplicity, convenience and safety in operation, high yield and continuous production of the nitroguanidine product; and in addition, by adopting the process, the environmental pollution can be greatly reduced. The yield of the product according to the method disclosed by the invention is 80-85%, and the melting point of the product is 230-232 DEG 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 acidifying and dehydrating an aqueous solution of guanidine nitrate as a raw material, more specifically, a Corning microchannel reactor continuously flowing in a high-flux microchannel In the process of preparing nitroguanidine by acidifying aqueous solution of guanidine nitrate with sulfuric acid. 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...

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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