Method for acidizing and dewatering guanidine nitrate to prepare nitroguanidine in continuous flow micro-channel reactor

A technology of microchannel reactor and channel reactor, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of bulky reaction kettle, occupying a large factory building, and high temperature control requirements, so as to avoid Severely corroded equipment, reduced generation of waste acid, and excellent corrosion resistance

Active Publication Date: 2013-07-10
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 dehydration of concentrated sulfuric acid to acidify guanidine nitrate to prepare nitroguanidine by means of Corning microchannel continuous flow

Method used

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  • Method for acidizing and dewatering guanidine nitrate to prepare nitroguanidine in continuous flow micro-channel reactor
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  • Method for acidizing and dewatering guanidine nitrate to prepare nitroguanidine in continuous flow micro-channel reactor

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Effect test

Embodiment 1

[0043] (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.

[0044](2) Raw material tanks 1 and 2 are equipped with 10% 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: concentrated sulfuric acid molar ratio = 1:0.9, control the flow rate of the guanidine nitrate aqueous solution: 0.25mL / min, control the concentrated sulfuric acid flow rate: 0.2mL / min, and separate the materials Pour into each straight channel preheating module, and control the reaction temperature to be 40°C; the guanidine nitrate aqueous solution and the concentrated sulf...

Embodiment 2

[0047] (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.

[0048] (2) Raw material tanks 1 and 2 are equipped with 15% 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: concentrated sulfuric acid molar ratio = 1:1, control the flow rate of the guanidine nitrate aqueous solution: 0.2mL / min, control the concentrated sulfuric acid flow rate: 0.2mL / min, and separate the materials Pour into each straight channel preheating module, and control the reaction temperature at 50°C; the guanidine nitrate aqueous solution and the concentrated sulfuric acid are respectively inject...

Embodiment 3

[0051] (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.

[0052] (2) Raw material tanks 1 and 2 are equipped with 40% guanidine nitrate aqueous solution and concentrated sulfuric acid. Set the flow control of each metering pump 3, pump 4 to change the aqueous solution of guanidine nitrate: concentrated sulfuric acid mol ratio=1:2, control the aqueous solution flow rate of guanidine nitrate: 0.2mL / min, control the concentrated sulfuric acid flow rate: 0.8mL / min, the The materials are injected into the preheating modules of each straight channel respectively, and the reaction temperature is controlled to be 90°C; the aqueous solution of concentrated guanidine sulfate an...

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Abstract

The invention discloses a method for acidizing and dewatering guanidine nitrate to prepare nitroguanidine in a continuous flow micro-channel reactor, belongs to the technical field of organic synthesis application, and is a new technology of taking guanidine nitrate water solution and concentrated sulfuric acid as materials in the continuous flow micro-channel reactor, and synthesizing the nitroguanidine within the reaction time from dozens of seconds to a few minutes. The materials are led to the continuous flow micro-channel reactor through a metering pump, and the dewatered product nitroguanidine is finally obtained by pre-heating, mixing, and reacting. The method is simple and safe to operate; high-yield continuous production of the nitroguanidine becomes possible; the technology is small in environmental pollution; the yield of the product disclosed by the invention is 80-85%; and the melting point is 230-232 DEG C.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis applications, 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, using concentrated sulfuric acid to acidify nitric acid in a high-throughput continuous flow microchannel reactor A process for preparing nitroguanidine from an aqueous solution of guanidine. 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 o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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