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Continuous synthetic method of nitroguanidine

A technology of nitroguanidine and chemical synthesis, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of short residence time, potential safety hazards, and large workshop occupation, so as to increase the content and yield , The effect of reducing the operating intensity and improving production efficiency

Inactive Publication Date: 2015-12-16
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Method features: This method does not require high temperature or high pressure conditions, and the pollution is relatively small, but it requires high 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.
[0005] At present, nitroguanidine is prepared by continuously flowing into the microchannel to concentrated sulfuric acid and guanidine nitrate, but because the flow rate of the material and the residence time of the reaction are too small, the final comprehensive yield can only be maintained at 80-85%, which cannot make The comprehensive yield reaches more than 85%, and the finished product content does not reach more than 98%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 500ml primary synthesis kettle equipped with a thermometer, a stirring, and an addition funnel, add 240g of guanidine nitrate (1.8mol) and 360g of concentrated sulfuric acid (3.6mol) respectively, and keep warm at 50°C for 1 hour. After the heat preservation finishes, start to carry out continuous reaction. Through a small screw feeder, control the feed rate of guanidine nitrate 240g / h, through a small metering pump, control the concentrated sulfuric acid flow rate of 340g / h to smoothly and evenly add to the primary synthesis kettle, and control the temperature in the 500ml primary synthesis kettle. 50±5°C. The residence time of the materials in the primary synthesis kettle is controlled to be 2 hours, and the dissolved material overflows from the opening on the side of the primary synthesis kettle into the 500m secondary reaction kettle, and the temperature of the secondary reaction kettle is controlled to be 50±2°C. Control the residence time of the material in t...

Embodiment 2

[0023] In a 500ml primary synthesis kettle equipped with a thermometer, a stirring, and an addition funnel, add 240g of guanidine nitrate (1.8mol) and 360g of concentrated sulfuric acid (3.6mol) respectively, and keep warm at 50°C for 1 hour. After the heat preservation finishes, start to carry out continuous reaction. Through a small screw feeder, control the feed rate of guanidine nitrate 240g / h, through a small metering pump, control the concentrated sulfuric acid flow rate of 396g / h to smoothly and evenly add to the primary synthesis kettle, and control the temperature in the 500ml primary synthesis kettle. 50±5°C. The residence time of the materials in the primary synthesis kettle is controlled to be 2 hours, and the dissolved material overflows from the opening on the side of the primary synthesis kettle into the 500m secondary reaction kettle, and the temperature of the secondary reaction kettle is controlled to be 50±2°C. Control the residence time of the material in t...

Embodiment 3

[0025] In a 500ml primary synthesis kettle equipped with a thermometer, a stirring, and an addition funnel, add 240g of guanidine nitrate (1.8mol) and 360g of concentrated sulfuric acid (3.6mol) respectively, and keep warm at 50°C for 1 hour. After the heat preservation finishes, start to carry out continuous reaction. Through a small screw feeder, control the feed rate of guanidine nitrate 120g / h, through a small metering pump, control the flow of concentrated sulfuric acid at 180g / h to smoothly and evenly add to the primary synthesis kettle, and control the temperature in the 500ml primary synthesis kettle. 50±5°C. The residence time of the materials in the primary synthesis kettle is controlled to be 2 hours, and the dissolved material overflows from the opening on the side of the primary synthesis kettle into the 500m secondary reaction kettle, and the temperature of the secondary reaction kettle is controlled to be 50±2°C. Control the residence time of the material in the...

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Abstract

The invention relates to a continuous synthetic method of nitroguanidine. The method comprises the steps that guanidine nitrate and concentrated sulfuric acid are used as raw materials to respectively flow into a reaction kettle formed by serially connecting three reaction kettles with openings formed in the side surfaces according to a molar ratio of 1: 2, by controlling the material flow rate, the temperature of each synthetic kettle and the material reaction retention time, and feeding reaction is continuously carried out by virtue of the overflow of materials after the reaction, wherein the content of a finished product is 98.0 percent to 98.5 percent, and the comprehensive yield is 85 percent to 95 percent. By adopting the method for continuously synthesizing the nitroguanidine, the content and yield of the product are remarkably increased, the problems that an additional device is needed in a conventional intermittent reaction and leakage appears in a transferring process can be avoided, the operation intensity is greatly alleviated, and the production efficiency is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for synthesizing nitroguanidine, in particular to a method for continuously synthesizing nitroguanidine. 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, drug Lekoan, etc. It can also be used in the preparation of explosives and smokeless gunpowder, and is an important component of nitrocellulose gunpowder, nitroglycerin gunpowder, admixture of diethylene glycol dinitrate, and solid ro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/34C07C277/08
Inventor 谭建平金永华
Owner NANTONG TENDENCI CHEM
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