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Method for preparing nitroguanidine by adopting micro-channel reactor

A micro-channel reactor, nitroguanidine technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large reactor volume, occupying large workshops, and high temperature control requirements, avoiding the need for Severely corroded equipment, reduced waste acid production, and excellent corrosion resistance

Active 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

[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 adopting micro-channel reactor
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  • Method for preparing nitroguanidine by adopting micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0043] (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 respectively injected into the preheating modules of each straight channel, and the reaction temperature is controlled to be 40°C; the sulfuric...

Embodiment 2

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

[0047] (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 respectively injected into the preheating modules of each straight channel, and the reaction temperature is controlled to be 50°C; the...

Embodiment 3

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

[0051] (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 poured into the preheating modules of each straight channel respectively, and the reaction temperature is controlled to be 80°C; the s...

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Abstract

The invention relates to a method for preparing nitroguanidine by adopting a micro-channel reactor, belonging to the technical field of organic synthesis applications. The mehtod is a new process for synthesizing nitroguanidine by taking a sulfuric acid solution of guanidine sulfate and nitric acid as raw materials and performing nitrification and 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 90-93%, 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 nitrifying and dehydrating a sulfuric acid solution of guanidine sulfate as a raw material, more specifically, a Corning microchannel continuously flowing in a high-flux microchannel In the reactor, the process of preparing nitroguanidine by using the sulfuric acid solution of nitric acid to nitrate 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 syn...

Claims

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Application Information

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