Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF7 Cites 17 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing nitroguanidine through micro-channel reactor
  • Method for preparing nitroguanidine through micro-channel reactor
  • Method for preparing nitroguanidine through 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 configured with a mass concentration of 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, and control nitric acid The flow rate of guanidine aqueous solution: 0.25mL / min, control the flow rate of concentrated sulfuric acid: 0.2mL / min, put the materials into the preheating modules of each straight channel respectively, and control the reaction temperature to 40°C; 3 and 4 are poured into the h...

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 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 to be 50°C; the guanidine nitrate aqueous solution and the concentrated sulfuric ...

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 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: concentrated sulfuric acid molar ratio = 1:2, control the flow rate of the guanidine nitrate aqueous solution: 0.2mL / min, control the concentrated sulfuric acid flow rate: 0.8mL / min, and separate the materials Pour into each straight channel preheating module, and control the reaction temperature to be 90°C; the guanidine nitrate aqueous solution and the concentrated sulfuric ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Features
  • Generate Ideas
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com