CN108129247B - Method for modifying surface defects of FOX-7 crystal - Google Patents
Method for modifying surface defects of FOX-7 crystal Download PDFInfo
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- CN108129247B CN108129247B CN201711322110.XA CN201711322110A CN108129247B CN 108129247 B CN108129247 B CN 108129247B CN 201711322110 A CN201711322110 A CN 201711322110A CN 108129247 B CN108129247 B CN 108129247B
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- fox
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- bonding agent
- fluororubber
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/36—Compositions containing a nitrated organic compound the compound being a nitroparaffin
Abstract
The invention discloses a method for modifying surface defects of an FOX-7 crystal, which comprises the following steps: step A: preparing a bonding agent solution; and B: adding the FOX-7 crystal particles into a bonding agent solution to pretreat the FOX-7, and stirring and drying; and C: preparing a fluororubber solution; step D: surface filling of FOX-7 particles: and D, adding the FOX-7 crystal particles obtained in the step B into the fluororubber filling liquid, stirring, and performing vacuum evaporation in a rotary evaporator. Step F: surface cleaning of FOX-7 particles: and D, adding the FOX-7 particles obtained in the step D into a butyl acetate solvent to prepare a butyl acetate suspension, stirring, filtering and drying. The FOX-7 crystal particles with the finished surface modification are obtained. According to the invention, the surface of the FOX-7 crystal is modified by adopting the bonding agent HX-878 and the fluororubber F2311, so that the roughness of the surface of the FOX-7 crystal can be effectively reduced, and the technological performance of the FOX-7-based PBX is improved.
Description
Technical Field
The invention belongs to the technical field of energetic materials, and particularly relates to a method for modifying surface defects of a FOX-7 crystal.
Background
1, 1-diamino-2, 2-dinitroethane (FOX-7) is a novel high-energy low-sensitivity elementary explosive, the energy of which is equivalent to that of common explosive hexogen (RDX), but the mechanical sensitivity of which is far lower than that of RDX. The FOX-7-based high polymer bonded explosive (PBX) also has the characteristics of high energy and low sensitivity, and has a good application prospect in penetration and carrier-borne weapon systems.
In the FOX-7 crystal, FOX-7 molecules are arranged in a layered wave shape, and different layers of molecules are mainly acted by hydrogen bonds, so that the crystal surface of the FOX-7 is generally high in roughness and has defects such as pits, and the like, which shows that the defects greatly increase the viscosity of the FOX-7-based PBX material and reduce the process forming performance of the FOX-7-based PBX material.
Disclosure of Invention
The invention aims to provide a method for modifying surface defects of FOX-7 crystals to obtain FOX-7 crystal particles with lower surface roughness.
In order to achieve the technical effects, the invention adopts the following technical scheme:
a method for modifying surface defects of FOX-7 crystals comprises the following steps:
step A: preparing a bonding agent solution: dissolving a bonding agent in ethanol to prepare a bonding agent solution with the mass fraction of 5-8%;
and B: pretreatment of FOX-7: adding the FOX-7 crystal particles into a bonding agent solution, mechanically stirring at normal temperature to enable the FOX-7 to be suspended in the bonding agent solution, stirring for 30-40 min, filtering to obtain FOX-7 particles after stirring is finished, and drying the particles for 2h at 50-60 ℃;
and C: preparing a fluororubber filling liquid: dissolving fluororubber in ethyl acetate to prepare a fluororubber solution with the mass content of 6-10%;
step D: surface filling of FOX-7 particles: and D, adding the FOX-7 crystal particles obtained in the step B into a fluororubber filling liquid, mechanically stirring for 1-1.5 h at normal temperature, adding the suspension of the FOX-7 into a rotary evaporator, and performing rotary evaporation for 20-25 min under a vacuum condition. The ethyl acetate solution in the fluororubber solution was evaporated completely by evaporation. The purpose of adopting rotary evaporation is to improve the coating effect of the fluororubber on the surface of the FOX-7 particles.
Step F: surface cleaning of FOX-7 particles: and D, adding the FOX-7 particles obtained in the step D into a butyl acetate solvent to prepare a 10-15 mass percent butyl acetate suspension, and mechanically stirring at normal temperature for 10 min. Filtering to obtain FOX-7 crystal particles, and drying the particles for 2-3 h at the temperature of 60-70 ℃. Thus obtaining the FOX-7 crystal particles after the surface modification is finished.
The further technical proposal is that the bonding agent is HX-878.
The further technical scheme is that the fluororubber is F2311.
In the invention, FOX-7 is pretreated by adopting a bonding agent HX-878, on one hand, HX-878 can form weak molecular bond interaction with nitro in FOX-7 molecules, so that HX-878 and FOX-7 crystals form stronger interface bonding force; on the other hand, the fluororubber has better wetting performance on the surface of HX-878, and the fluororubber treated by HX-878 can more fully enter pores on the surface of the FOX-7 crystal.
The fluorine rubber F2311 is adopted to modify the FOX-7 crystal particles, on one hand, the F2311 has higher mechanical strength and density, and the density of the particles can be increased while the surface smoothness of the crystal particles is improved after the FOX-7 crystal particles are modified, on the other hand, the F2311 has better compatibility with other components in a PBX explosive formula, and the introduction of the F2311 can improve the physical and chemical stability of the PBX based on FOX-7.
The butyl acetate is used for cleaning the surface of the treated FOX-7 particles, the solubility of the butyl acetate to F2311 is weaker than that of ethyl acetate in the fluororubber filling liquid to F2311, and the butyl acetate is used as the cleaning liquid to prevent the F2311 entering the surface defects of the FOX-7 crystal particles from being dissolved.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the surface of the FOX-7 crystal is modified by adopting the bonding agent HX-878 and the fluororubber F2311, so that the roughness of the surface of the FOX-7 crystal can be effectively reduced, and the technological performance of the FOX-7-based PBX is improved.
Detailed Description
The invention will be further elucidated and described with reference to the embodiments of the invention described hereinafter.
Example 1:
step A: preparing a bonding agent solution: dissolving a bonding agent HX-878 in ethanol to prepare a bonding agent solution with the mass fraction of 6%;
and B: pretreatment of FOX-7: adding the FOX-7 crystal particles into a bonding agent solution, mechanically stirring at normal temperature to enable the FOX-7 to be suspended in the bonding agent solution, stirring for 30min, filtering to obtain FOX-7 particles after stirring is finished, and drying the particles for 2h at 55 ℃;
and C: preparing a fluororubber filling liquid: dissolving fluororubber in ethyl acetate to prepare a fluororubber solution with the mass content of 6%;
step D: surface filling of FOX-7 particles: the FOX-7 crystal particles are added into the fluororubber filling liquid, mechanically stirred for 1.5h at normal temperature, and then the suspension of the FOX-7 is added into a rotary evaporator and rotary evaporated for 25min under vacuum condition.
Step F: surface cleaning of FOX-7 particles: and D, adding the FOX-7 particles obtained in the step D into a butyl acetate solvent to prepare a 10 mass percent butyl acetate suspension, and mechanically stirring at normal temperature for 10 min. Filtering to obtain FOX-7 crystal particles, and drying the particles at 60 ℃ for 2 h. Thus obtaining the FOX-7 crystal particles after the surface modification is finished.
The quality indexes of the obtained FOX-7 crystal particles after surface modification are as follows:
(1) density 1.873g/cm3；
(2) Specific surface area 1.23m2/g；
(3) Initial Secant Modulus (ISM) (compressive stiffness method) 50 MPa.
The FOX-7 crystal particles without surface modification have the following quality indexes:
(1) density 1.875g/cm3；
(2) Specific surface area 1.63m2/g；
(3) Initial Secant Modulus (ISM) (compressive stiffness method) 42 MPa.
The surface roughness of the modified FOX-7 crystal is reduced, and defects such as pits are reduced, so that the specific surface area is reduced. After the modification, since the defects of the surface of FOX-7 were filled with fluororubber and were less likely to be broken, the Initial Secant Modulus (ISM) (compressive stiffness method) was increased.
Example 2:
step A: preparing a bonding agent solution: dissolving a bonding agent HX-878 in ethanol to prepare a bonding agent solution with the mass fraction of 8%;
and B: pretreatment of FOX-7: adding the FOX-7 crystal particles into a bonding agent solution, mechanically stirring at normal temperature to enable the FOX-7 to be suspended in the bonding agent solution, stirring for 40min, filtering to obtain FOX-7 particles after stirring is finished, and drying the particles for 2h at 58 ℃;
and C: preparing a fluororubber filling liquid: dissolving fluororubber in ethyl acetate to prepare a fluororubber solution with the mass content of 9%;
step D: surface filling of FOX-7 particles: adding the FOX-7 crystal particles into the fluororubber filling liquid, mechanically stirring for 1h at normal temperature, adding the suspension of the FOX-7 into a rotary evaporator, and performing rotary evaporation for 25min under a vacuum condition.
Step F: surface cleaning of FOX-7 particles: and D, adding the FOX-7 particles obtained in the step D into a butyl acetate solvent to prepare a butyl acetate suspension with the mass content of 15%, and mechanically stirring for 10min at normal temperature. Filtering to obtain FOX-7 crystal particles, and drying the particles at 70 ℃ for 3 h. Thus obtaining the FOX-7 crystal particles after the surface modification is finished.
The quality indexes of the obtained FOX-7 crystal particles after surface modification are as follows:
(1) density 1.875g/cm3；
(2) Specific surface area 1.38m2/g；
(3) Initial Secant Modulus (ISM) (compressive stiffness method) 54MPa
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (1)
1. A method for modifying surface defects of FOX-7 crystals is characterized by comprising the following steps: the method comprises the following steps:
step A: preparing a bonding agent solution: dissolving a bonding agent HX-878 in ethanol to prepare a bonding agent solution with the mass fraction of 5-8%;
and B: pretreatment of FOX-7: adding the FOX-7 crystal particles into a bonding agent solution, mechanically stirring at normal temperature to enable the FOX-7 to be suspended in the bonding agent solution, stirring for 30-40 min, filtering to obtain FOX-7 particles after stirring is finished, and drying the particles for 2h at 50-60 ℃;
and C: preparing a fluororubber filling liquid: dissolving fluororubber F2311 in ethyl acetate to prepare a fluororubber solution with the mass content of 6-10%;
step D: surface filling of FOX-7 particles: adding the FOX-7 crystal particles obtained in the step B into a fluororubber filling liquid, mechanically stirring at normal temperature for 1-1.5 h, then adding the suspension of the FOX-7 into a rotary evaporator, and rotationally evaporating for 20-25 min under a vacuum condition;
step F: surface cleaning of FOX-7 particles: and D, adding the FOX-7 particles obtained in the step D into a butyl acetate solvent to prepare a butyl acetate suspension with the mass content of 10-15%, mechanically stirring for 10min at normal temperature, filtering to obtain FOX-7 crystal particles, and drying the particles for 2-3 h at the temperature of 60-70 ℃ to obtain the FOX-7 crystal particles with the finished surface modification.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711322110.XA CN108129247B (en) | 2017-12-12 | 2017-12-12 | Method for modifying surface defects of FOX-7 crystal |
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| CN201711322110.XA CN108129247B (en) | 2017-12-12 | 2017-12-12 | Method for modifying surface defects of FOX-7 crystal |
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| CN108129247B true CN108129247B (en) | 2020-04-28 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1869392A2 (en) * | 2005-04-12 | 2007-12-26 | Rafael-Armament Development Authority Ltd. | Extremely insensitive detonating substance and method for its manufacture |
| CN104649850A (en) * | 2015-02-09 | 2015-05-27 | 中国工程物理研究院化工材料研究所 | High polymer bonded explosive enhancing mechanical properties with nanoparticles and preparation method of high polymer bonded explosive |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1869392A2 (en) * | 2005-04-12 | 2007-12-26 | Rafael-Armament Development Authority Ltd. | Extremely insensitive detonating substance and method for its manufacture |
| CN104649850A (en) * | 2015-02-09 | 2015-05-27 | 中国工程物理研究院化工材料研究所 | High polymer bonded explosive enhancing mechanical properties with nanoparticles and preparation method of high polymer bonded explosive |
Non-Patent Citations (1)
| Title |
|---|
| 偶联剂对TATB造型粉表面性质及力学性能的影响;刘学涌等;《合成化学》;20031030(第5期);第413-416页 * |
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