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Nitroguanidine production process

A production process and technology for nitroguanidine, applied in the field of nitroguanidine production technology, can solve the problems of environmental pollution, waste of resources, poor mechanical properties and the like, and achieve the effects of simple process and low requirements for process conditions

Pending Publication Date: 2021-01-08
西安万德能源化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But adopt the concentrated sulfuric acid as solvent when carrying out the preparation of nitroguanidine in the prior art, react with guanidine sulfate as raw material, perhaps adopted guanidine nitrate as raw material, the concentrated sulfuric acid reacts as dehydrating agent; The nitro that above-mentioned two kinds of synthetic methods obtain All guanidines are needle-shaped and tend to grow in the direction of long needles during the crystallization process. When the needle-shaped nitroguanidine is applied to explosives or gunpowder, it will have defects such as poor fluidity and poor mechanical properties.
[0004] The existing nitroguanidine preparation process has the following disadvantages: a large amount of waste liquid, waste gas or other solid waste will be discharged during the production process, which will pollute the environment, and the by-products produced during the production of nitroguanidine cannot be reused, resulting in Resource waste is serious, therefore, it needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Nitroguanidine synthesis

[0044] Pump concentrated nitric acid from the nitric acid storage tank into the mixing kettle through the metering pump, start stirring, and open the refrigerant inlet and outlet valves of the jacket of the mixing kettle at the same time; wait for the concentrated nitric acid in the kettle to cool down to 2°C, start the solid feeder and measure through the electronic scale , slowly add the guanidine nitrate in the hopper into the mixing tank, and control the temperature of the material in the mixing tank to 5°C; use a metering pump to pass the mixed solution into the microtube impingement flow reactor, react at 45°C for 10 minutes, and cool down through the microtube to 5°C for crystallization;

[0045] (2) Dilute crystallization and centrifugation

[0046] The crystallization tank is prepared to measure 45% dilute nitric acid in advance, and the reaction solution and a certain volume of washing liquid are slowly added to the crystallizat...

Embodiment 2

[0057] (1) Nitroguanidine synthesis

[0058] Pump concentrated nitric acid from the nitric acid storage tank into the mixing kettle through the metering pump, start stirring, and open the refrigerant inlet and outlet valves of the jacket of the mixing kettle at the same time; wait for the concentrated nitric acid in the kettle to cool down to 1°C, start the solid feeder and measure through the electronic scale , slowly add the guanidine nitrate in the hopper into the mixing tank, and control the temperature of the material in the mixing tank at 7°C; use a metering pump to pass the mixed solution into the microtube impingement flow reactor, react at 47°C for 15 minutes, and cool down through the microtube to 7°C for crystallization;

[0059] (2) Dilute crystallization and centrifugation

[0060] The crystallization tank is prepared to measure 50% dilute nitric acid in advance, and the reaction solution and a certain volume of washing liquid are slowly added to the crystallizat...

Embodiment 3

[0071] (1) Nitroguanidine synthesis

[0072] Pump concentrated nitric acid from the nitric acid storage tank into the mixing kettle through the metering pump, start stirring, and open the refrigerant inlet and outlet valves of the jacket of the mixing kettle at the same time; wait for the concentrated nitric acid in the kettle to cool down to 0°C, start the solid feeder and measure through the electronic scale , slowly add guanidine nitrate in the hopper into the mixing tank, and control the temperature of the material in the mixing tank at 3°C; use a metering pump to pass the mixed solution into the microtube impingement flow reactor, react at 43°C for 20min, and cool down to 3°C for crystallization;

[0073] (2) Dilute crystallization and centrifugation

[0074] The crystallization tank is prepared to measure 55% dilute nitric acid in advance, slowly add the mixed material of the reactor and a certain volume of washing liquid into the crystallization tank in sequence, and e...

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Abstract

The invention belongs to the technical field of organic synthesis. The invention provides a nitroguanidine production process. The nitroguanidine production process comprises the following steps of S1, synthesizing nitroguanidine, and S2, conducting dilution crystallization and centrifugal treatment. According to the method, guanidine nitrate and concentrated nitric acid are mixed, concentrated nitric acid serves as a dehydrating agent, a crude nitroguanidine acid solution is prepared through a semi-continuous reaction, crystallization and multi-stage washing treatment are conducted through dilute nitric acid, centrifugal dehydration is conducted, and finally high-purity nitroguanidine with the high stacking density, by-product dilute nitric acid and a washing solution are obtained; the byproduct dilute nitric acid is repeatedly used as a raw material after being concentrated, and the process is free of waste liquid, waste gas and solid waste.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a nitroguanidine production process. 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 can be used in the synthesis of angina pectoris drug Lekoan, etc. It can also be used in the preparation of explosives and smokeless gunpowder. It is an important component of nitrocellulose gunpowder, nitroglycerin gunpowder, admixture of diethylene glycol dinitrate, and solid rocket propellant. [0003] But adopt the concentrated sulfuric acid as solvent when carrying out the preparation of nitroguanidine in the prior art, react with guanidine sulfate as raw material, perhaps adopted guanidine nitrate as raw ma...

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/34C01B21/46
CPCC07C277/08C01B21/46
Inventor 王育斌汪希领丁金皓刘平李海斌杨亚妮刘婉赵笑男
Owner 西安万德能源化学股份有限公司
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