Nitroguanidine crystal and microchannel crystallization process and device of nitroguanidine

A crystallization device and micro-channel technology, applied in crystallization separation, oscillating crystallization, solution crystallization, etc., can solve the problems of inability to realize continuous production, a large amount of organic solvents, complicated processing procedures, etc., and achieve simple and controllable reaction conditions and easier washing. , the effect of high reaction safety

Active Publication Date: 2019-09-06
西安万德能源化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zheng Dan of Nanjing University of Science and Technology and others recrystallized in polyvinyl alcohol aqueous solution through recrystallization and mechanical methods, and mechanically pulverized the wet product after crystallization to obtain ultrafine, granular nitroguanidine crystals, but the The method has complex treatment procedures, a large amount of organic solvent is required in the crystallization process, and the processing cost is high. At the same time, mechanical equipment is used to apply external force to the nitroguanidine crystal, which has certain safety risks.
Liu Yunchuan and others selected needle-shaped nitroguanidine, used a mixture of methyl cellulose and polyacryl alcohol as an inhibitor of nitroguanidine extraction, and used water as a solvent to carry out recrystallization to obtain spherical nitroguanidine. , but this method is easy to introduce more impurities in the preparation process, and continuous production cannot be realized in actual production

Method used

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  • Nitroguanidine crystal and microchannel crystallization process and device of nitroguanidine
  • Nitroguanidine crystal and microchannel crystallization process and device of nitroguanidine
  • Nitroguanidine crystal and microchannel crystallization process and device of nitroguanidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] This experiment uses a stainless steel horizontal tubular microchannel crystallizer E with a length of 100m and an inner diameter of 2mm coated with anti-corrosion material. An ultrasonic probe F is added every 10m in the pipeline and placed in a constant temperature bath K at -5°C. Turn on the ultrasonic generator L, set the ultrasonic frequency at 20kHz, and the power at 1000W, and the nitroguanidine acid solution and water are respectively measured by the second metering pump D and the first metering pump D from the nitroguanidine acid solution storage tank B and the water storage tank A. The pump C is delivered to the reaction pipeline, the input flow rate of the nitroguanidine acid solution is 100mL / min, and the input flow rate of the water is 150mL / min. After the material is rapidly crystallized in the microchannel crystallizer, it is transported to the separator G, and the resulting The solid material is fully washed by the washing device H, and dehydrated in the ...

Embodiment 2

[0038] This experiment uses a stainless steel horizontal tubular microchannel crystallizer E with a length of 80m and an inner diameter of 4mm coated with anti-corrosion material. An ultrasonic probe F is added every 8m in the pipeline and placed in a constant temperature bath K at -5°C. Turn on the ultrasonic generator L, set the ultrasonic frequency at 22kHz, and the power at 1200W, and the nitroguanidine acid solution and water are respectively measured from the nitroguanidine acid solution storage tank B and the water storage tank A by the second metering pump D and the first metering pump. The pump C is delivered to the reaction pipeline, the input flow rate of the nitroguanidine acid solution is 150mL / min, and the input flow rate of the water is 180mL / min. After the material is rapidly crystallized in the microchannel crystallizer, it is transported to the separator G, and the resulting The solid material is fully washed by the washing device H, and dehydrated in the cont...

Embodiment 3

[0040] This experiment uses a stainless steel riser microchannel crystallizer E with a length of 50m and an inner diameter of 6mm coated with anti-corrosion material. An ultrasonic probe F is added every 4m in the pipeline and placed in a constant temperature bath at -3°C. Turn on the ultrasonic generator L, set the ultrasonic frequency at 30kHz, and the power at 1800W, and the nitroguanidine acid solution and water are respectively measured by the second metering pump D and the first metering pump D from the nitroguanidine acid solution storage tank B and the water storage tank A. The pump C is delivered to the reaction pipeline, the input flow rate of the nitroguanidine acid solution is 200mL / min, and the input flow rate of the water is 200mL / min. After the material is rapidly crystallized in the microchannel crystallizer, it is transported to the separator G, and the resulting The solid material is fully washed by the washing device H, and dehydrated in the continuous dryer ...

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Abstract

The invention discloses a nitroguanidine crystal and a nitroguanidine microchannel crystallization process and device. After water, concentrated nitric acid and guanidine nitrate react, a nitroguanidine acid solution is obtained and is respectively fed into a microchannel crystallizer in a continuous mode for crystallization, ultrasonic treatment is carried out in the crystallization process, anda crystallized product is separated, washed and dried to obtain the high-purity spherical nitroguanidine crystal, wherein the mass fraction of nitroguanidine in the nitroguanidine acid solution is 25%-50%, the input flow rate of the nitroguanidine acid solution is 100-300 mL / min, the input flow rate of water is 150-400 mL / min, and the ultrasonic power of ultrasonic treatment is 1000-1800 W. The nitroguanidine microchannel crystallization process and the nitroguanidine microchannel crystallization device have the advantages of continuous operation, simple and controllable reaction conditions, high reaction safety and the like, and can be directly applied to actual production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a nitroguanidine crystal and a microchannel crystallization process and device for nitroguanidine. Background technique [0002] Nitroguanidine is an important energetic material, which is mainly used in propellants and bullet charge components of rockets and missiles. Its explosive performance is higher than that of TNT, and it has the advantages of low explosion temperature and low sensitivity. The crystal unit of nitroguanidine belongs to the orthorhombic crystal system, and the crystal shape tends to grow in the direction of long needles. This long needle-like crystal form has an adverse effect on the mechanical properties and combustion properties of propellants, and nitroguanidine suitable for military use It must be a spherical crystal with a high packing density. Gao Sijing from Nanjing University of Science and Technology mentioned in the article "Spherific...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/08C07C279/34B01D9/02B01J19/10
CPCC07C277/08B01D9/0013B01D9/0081B01D2009/0086C07C279/34
Inventor 丁金皓王育斌汪希领李海斌刘平杨亚妮刘婉
Owner 西安万德能源化学股份有限公司
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