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Preparation method of amino-containing energetic material graded microspheres

A technology of microspheres and amino groups, applied in the field of micro-nano materials, can solve the problems that the preparation method cannot be directly introduced into use, and the hierarchical structure is difficult to be prepared, and achieves the effects of easy control of size and shape, low cost, and uniform size

Inactive Publication Date: 2012-06-20
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For most elemental energetic materials, they can be classified as organic small molecules. The particularity of this type of materials prevents many preparation methods in the field of organic small molecules from being directly introduced and used, and the hierarchical structure is even more difficult to prepare.

Method used

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  • Preparation method of amino-containing energetic material graded microspheres
  • Preparation method of amino-containing energetic material graded microspheres
  • Preparation method of amino-containing energetic material graded microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 2,6-diamino-3,5-dinitropyrazine (ANPZ, C 4 h 4 o 4 N 6 ) preparation of graded microspheres, the specific steps are:

[0032] 1) Dissolve 0.48g (8mmol) urea in 50mL absolute ethanol at room temperature, then add 0.222g (monomer molarity is 2mmol) surfactant PVP-K30, stir to obtain a light yellow solution;

[0033] 2) 0.046g (0.2mmol) precursor 2,6-dimethyl-3,5-dinitropyrazine (DMDP, C 6 h 6 o 6 N 4 ) into the solution obtained in step 1), and stirred at 35°C until the DMDP was completely dissolved to obtain a yellow transparent solution, which was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and then the autoclave was sealed and placed in a blast Oven, the temperature of the oven is 120°C, the ammonia gas produced by the alcoholysis of urea reacts with DMDP, and the reaction time is 9 hours. After the reaction is completed, the solid product is naturally precipitated and separated, and washed alternately with ultrapure water and ...

Embodiment 2

[0035]Same as Example 1, except that the autoclave is sealed and placed in an oil bath, and kept warm for 9 hours under stirring conditions to obtain ANPZ graded microspheres with a size of about 10 μm, which is smaller than the microspheres in Example 1. The SEM image Such as figure 1 Shown in c and d.

Embodiment 3

[0037] 1,3-Diamino-2,4,6-trinitrobenzene (DATB, C 6 h 5 o 6 N 5 ) preparation of graded microspheres, the specific steps are:

[0038] 1) Dissolve 0.48g (8mmol) of urea in 50mL of absolute ethanol at room temperature, then add 0.222g (monomer molarity is 2mmol) of surfactant PVP-K30, stir to obtain a yellow solution;

[0039] 2) 0.055g (0.2mmol) precursor 2,3,4,6-tetranitroaniline (TNA, C 6 h 3 o 8 N 5 ) was added to the solution obtained in step 1), stirred at 40°C until TNA was completely dissolved, and a yellow transparent solution was obtained, which was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and then the autoclave was sealed and placed in a blast Oven, the temperature of the oven is 100°C, the ammonia gas produced by the alcoholysis of urea reacts with TNA, and the reaction time is 9 hours. After the reaction is completed, the solid product is naturally precipitated and separated, and washed alternately with ultrapure water a...

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Abstract

The invention relates to a preparation method of amino-containing energetic material graded microspheres, belonging to the technical field of micro-nanomaterials. The preparation method comprises the steps of: dissolving urea in absolute ethanol at room temperature, then adding a surfactant, and stirring to obtain a solution; adding a precursor to the solution, stirring, transferring to a stainless steel autoclave, then sealing the autoclave, placing in a blast oven, carrying out an amination reaction between ammonia gas generated in the reaction between urea and ethanol and the precursor, after the reaction is finished, naturally precipitating, separating out a solid product, repeatedly and alternately washing the solid product with ultrapure water and absolute ethanol for multiple times, and drying to obtain amino-containing energetic material graded microspheres. The prepared graded microspheres are uniform in size and single in morphology and have the diameter of 10-150 mu m; the product yield generally reaches more than 70%; and the method has the advantages of mild reaction conditions, high yield, easiness in industrialization, low cost and easiness in product size and morphology control, and is suitable for organic low-molecular-weight substances.

Description

technical field [0001] The invention relates to a preparation method of classified microspheres of energy-containing materials with amino groups, and belongs to the technical field of micro-nano materials. Background technique [0002] Three-dimensional hierarchical micro / nanosphere structures assembled from nanoscale building blocks have attracted much attention due to their interesting geometric configurations, unique physical and chemical properties, and potential applications in catalysis, optics, electronics, and magnetism. Widespread concern. Therefore, the three-dimensional hierarchical micro / nanosphere structure of many inorganic materials, such as Fe 2 o 3 , CaCO 3 , BaCO 3 , BaSO 4 , Ni(OH) 2 etc. (Angew.Chem, Int.Ed., 2003, 42, 980; J.Am.Chem.Soc., 2005, 127, 3596; J.Am.Chem.Soc., 2006, 128, 15714), all available obtained by means of various methods and exhibit good properties in terms of magnetic and electrochemical properties. For organic small molecular...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02B82Y40/00C07D241/20C07C211/52C07C209/22C07C209/18
Inventor 胡长文黄兵曹敏花
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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