Method for preparing spherical 1,1-diamino-2,2-dinitroethylene crystal assisted by ultrasonic assistance

A technology of dinitroethylene and diamino is applied in the direction of purification/separation of amino compounds, nitration of acyclic/alicyclic/heterocyclic amine explosive compositions, organic chemistry, etc., and can solve the problems of rough surface and uneven particle size, etc. Achieve narrow particle size distribution, good dispersion and high reproducibility

Inactive Publication Date: 2020-01-17
ZHONGBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the particle size of the obtained product is uneven, most of them are irregular long rods or flakes, and the surface is rough (Teipel U, FuhrI, Hanlieb K, et al. Crystallization of 1,1-diamino-2,2-dinitroethylene (FOX-7)[C] / / 35 th International Annual Conference of ICT. Karlsruhe: ICT, 2004.)

Method used

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  • Method for preparing spherical 1,1-diamino-2,2-dinitroethylene crystal assisted by ultrasonic assistance
  • Method for preparing spherical 1,1-diamino-2,2-dinitroethylene crystal assisted by ultrasonic assistance
  • Method for preparing spherical 1,1-diamino-2,2-dinitroethylene crystal assisted by ultrasonic assistance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Measure 20 mL of dimethyl sulfoxide and 10 mL of acetone, weigh 0.05% of the initial amount of FOX-7 additive polyethylene glycol 600, and add it to the crystallization kettle, which is in a constant temperature water bath at 25°C; 9.2 g Powdered FOX-7 raw materials were added into the organic solvent, and the stirrer was turned on at a stirring rate of 500 r / min to completely dissolve FOX-7. Start the dropping device to add ethyl acetate dropwise to the crystallization kettle, and add dropwise while stirring. The stirring rate is 500 r / min, the dropping rate is 0.6mL / min, and the total amount of ethyl acetate is 100mL. After all the drops are completed, the crystals are ultrasonically treated in the mother liquor, and ultrasonically treated while stirring. The stirring rate is 500 r / min, the ultrasonic frequency is 50KHz, and the ultrasonic time is 2h; after filtering, washing and drying, it can be obtained Spherical FOX-7 crystals.

[0034] figure 1 It is the optica...

Embodiment 2

[0037] Measure 30 mL of dimethyl sulfoxide, weigh the additive polyethylene glycol 4000 whose weight is 1% of the initial amount of FOX-7, and add it to the crystallization kettle, which is placed in a constant temperature water bath at 23 °C. Add 8.5 g of powdered FOX-7 raw materials into the organic solvent, start the stirrer, and stir at a rate of 300 r / min to completely dissolve FOX-7. Start the dropping device to add acetone dropwise to the crystallization kettle, and add dropwise while stirring. The stirring rate is 300 r / min, the dropping rate is 3mL / min, and the total consumption of acetone is 150mL. After all the addition was completed, the crystals were ultrasonically treated in the mother liquor, and the ultrasonic treatment was performed while stirring. The stirring rate was 300 r / min, the ultrasonic frequency was 30KHz, and the ultrasonic time was 2.5h. Spherical FOX-7 crystals can be obtained after filtering, washing and drying.

Embodiment 3

[0039] Measure 35 mL of N-methylpyrrolidone and 15 mL of water, weigh 0.01% of the initial amount of FOX-7 additive polyethylene glycol 400, and add it to the crystallization kettle, which is placed in a constant temperature water bath at 35 °C. Add 15.6 g of powdered FOX-7 raw materials into the organic solvent, start the stirrer, and stir at a rate of 100 r / min to completely dissolve FOX-7. Start the dropping device to add water dropwise to the crystallization kettle, and add dropwise while stirring. The stirring rate is 100 r / min, the dropping rate is 2mL / min, and the total amount of water is 180mL. After all the addition was completed, the crystals were ultrasonically treated in the mother liquor, and ultrasonically treated while stirring. The stirring rate was 100 r / min, the ultrasonic frequency was 45KHz, and the ultrasonic time was 2h. Spherical FOX-7 crystals can be obtained after filtering, washing and drying.

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Abstract

The invention discloses a method for preparing spherical 1,1-diamino-2,2-dinitroethylene crystals by ultrasonic assistance, and the method comprises the following steps of: 1) adding Fox-7, an organicsolvent and an additive into a crystallization kettle to be fully dissolved to prepare a saturated solution, wherein the water temperature of the crystallization kettle is controlled at 20-40 DEG C;(2) adding an antisolvent dropwise to the saturated solution while stirring to form a supersaturated solution and then performing crystal nuclei generating and crystal growth; 3) after the crystal iscompletely separated out, performing ultrasonic treatment on the crystal in mother liquor while stirring, wherein the ultrasonic treatment time is 1-3 hours, and the ultrasonic frequency is 30-70 khz;and 4) filtering, washing and drying to obtain a spherical FOX-7 crystal. The spherical FOX-7 crystal prepared by the method has smooth surface, few transparent defects in the crystal and good fluidity; the process is simple and easy to control, the anti-solvent consumption is small and recyclable, the reaction conditions are mild, safe and reliable, green and efficient, and industrialization iseasy to realize.

Description

technical field [0001] The invention relates to the technical field of energetic crystal materials, in particular to a method for ultrasonically assisted preparation of spherical 1,1-diamino-2,2-dinitroethylene crystals. Background technique [0002] In recent years, countries around the world are actively developing solid propellants based on new energetic materials that theoretically have high efficacy and potentially meet the requirements of low vulnerability, thus promoting the research and development of high-energy, low-sensitivity energetic materials (Ren Xiaoting, Ye Danyang, Ding Ning, et al. Molecular dynamics simulation study on the influence of solvent effect on the crystal morphology of FOX-7. Acta Armamentae Sinica, 2015, 36(2):272-278.). 1,1-diamino-2,2-dinitroethylene, the molecular formula is C 2 h 4 N 4 o 4 , the structural formula is , commonly known as FOX-7, is a new type of high-energy insensitive energetic material, which has the characteristics ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/86C07C211/24C06B25/34
CPCC07C209/86C06B25/34
Inventor 陈丽珍赵鑫华王建龙周诚周群刘立媛
Owner ZHONGBEI UNIV
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