CN106946635B - The preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere - Google Patents
The preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere Download PDFInfo
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- CN106946635B CN106946635B CN201710272365.3A CN201710272365A CN106946635B CN 106946635 B CN106946635 B CN 106946635B CN 201710272365 A CN201710272365 A CN 201710272365A CN 106946635 B CN106946635 B CN 106946635B
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- hexanitrohexaazaisowurtzitane
- syringe needle
- hollow sphere
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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
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
Abstract
The invention discloses the preparation methods of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere, comprising the following steps: A. weighs a certain amount of Hexanitrohexaazaisowurtzitane, is added into organic solvent, and heating, stirring make it completely dissolved；It B. will be in the syringe of the solution suction belts flat-top syringe needle in step A, syringe is fixed on micromass culture pump, set parameter, regulate syringe needle to collector distance, regulate the voltage on syringe needle and collector, so that syringe needle is kept taylor cone, monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere can be obtained after a certain period of time.Product of the present invention granule-morphology is spherical shape, and particle size distribution is narrow, and microsphere particle is all made of nano particle, has important application prospect in fields such as primings.And present invention process process is simple, manufactured microsphere particle does not need further work-up, and experiment condition is mild, and safety is good.
Description
Technical field
The invention belongs to energetic material preparation technical fields, and in particular to a kind of monodispersed six azepine of hexanitro different 5 is hereby
The preparation method of alkane micrometre hollow sphere.
Background technique
Modern war proposes requirements at the higher level to improving weapon and injure power, and the high energy single chmical compound explosive that service performance is excellent
It is then explosive energetic, promotes the most fundamental way that weapon injures power.Hexanitrohexaazaisowurtzitane (CL-20) is now
The highest single chmical compound explosive of practical application energy, energy output is higher by 10~15% than octogen (HMX), and it is fried to be applied to fire
Medicine field can significantly improve weapons and ammunitions Kill capability.
Hollow and porous structure energetic material can significantly improve the burning speed of explosive wastewater due to there is high specific surface area
Rate, and spherical structure enables to loading to increase to improve the energy density of explosive wastewater.Wang Ping etc. (energetic material, 2015,
11,1107-1110) it is prepared for nitrocotton micropore ball using solvent leaching process, micropore ball surface obtained is smooth, and partial size is at 20 μm
Left and right, sphericity 0.89.Wang Jiang etc. (explosive wastewater journal, 2015,1,16-21) utilizes the technique study being spray-dried entrance
The influence of temperature, feed rate, nebulizing gas flow rate and solution concentration to RDX granule-morphology finally obtains 2.8 μm, surface light
Sliding spherical RDX particle, the impact sensitivity of spherical RDX are substantially reduced than raw material.Shen Jinpeng etc. (CN103044173B, 2012)
It is assisted using crystal morphology controlling agent, has invented a kind of preparation method of ordered porous crystalline material containing energy.Lin Xiangyang etc.
(CN201410029365.7,2014) solvent-nonsolvent method has invented a kind of continuous preparation method for preparing nitrocotton microballoon.
Chen Huaxiong etc. (CN200910090462.6,2010) is prepared for the spherical shape having a size of 20-500 μm using the method for crystal form adjuvant
Hexanitrohexaazaisowurtzitane, the method system that unliterary jasmine etc. (CN201511000272.2,2016) uses dilute solution crystallization
For the Hexanitrohexaazaisowurtzitane crystal of high-quality.These technologies to the preparation of the poroid sphere energetic material of micron and
The preparation of the Hexanitrohexaazaisowurtzitane of high-quality and spheroidization has certain reference.
From the point of view of existing open source information, there are some methods for preparing energetic material micron sphere, but existing side at present
There are complex process, bad dispersibility for method, and to the preparation of Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive description compared with
It is few.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, and it is hollow to provide monodispersed Hexanitrohexaazaisowurtzitane micron
The preparation method of ball, core of the invention content are to be atomized rapid crystallization using electrostatic spray, and the electrification formed using atomization is small
Drop is mutually exclusive, and the solvent in last drop volatilizees completely, so that it is micro- to form monodispersed Hexanitrohexaazaisowurtzitane
Rice hollow sphere explosive.In view of the above problem of the prior art, according to one aspect of the present disclosure, the present invention is using following
Technical solution:
The preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere, comprising the following steps:
A. a certain amount of Hexanitrohexaazaisowurtzitane is weighed, is added into organic solvent, heating, stirring keep it completely molten
Solution；
B. by the syringe of the solution suction belts flat-top syringe needle in step A, syringe is fixed on micromass culture pump, if
Parameter has been set, syringe needle has been regulated to the distance of collector, regulates the voltage on syringe needle and collector, syringe needle is made to keep Taylor
Cone, can be obtained monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere after a certain period of time.
Further, concentration is 5.5wt%~38.9wt% after Hexanitrohexaazaisowurtzitane dissolution；
Further, the organic solvent is in acetone, ethyl acetate, butyl acetate, butanone and dimethylformamide
One kind；
Further, described, mixing speed is 300rpm~700rpm, and stirring is until blasting explosive granules are completely dissolved；
Further, the syringe is 5mL injector for medical purpose, metal needle is 19G~27G flat-top syringe needle, band
The electrostatic atomizer of micromass culture pump and high voltage power supply, collector is aluminium foil；
Further, the propulsion flow rate pump is 0.05mm/s~0.2mm/s, and the distance of syringe needle to collector is 10cm
~25cm, negative voltage are -7kV~-10kV, and positive voltage is 5kV~8kV, and it is 25 DEG C~35 DEG C that temperature, which is arranged, in instrument internal environment；
Further, the monodisperse Hexanitrohexaazaisowurtzitane microballoon explosive diameter of preparation is 2 μm~8 μm, product
Purity is greater than 99%.
Compared with prior art, beneficial effects of the present invention first is that: product particle pattern is spherical shape, particle size point
Cloth is narrow, and microsphere particle is all made of nano particle, has important application prospect in fields such as primings.And present invention process process
Simply, manufactured microsphere particle does not need further work-up, and experiment condition is mild, and safety is good.
Detailed description of the invention
Illustrate present specification embodiment or technical solution in the prior art in order to clearer, it below will be to embodiment
Or attached drawing needed in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only
It is the reference to embodiments some in present specification, for those skilled in the art, what is do not made the creative labor
In the case of, other attached drawings can also be obtained according to these attached drawings.
Fig. 1 is to be scanned according to 2000 times of explosive of monodisperse Hexanitrohexaazaisowurtzitane microballoon of the embodiment of the present invention 1
Electron microscope；
Fig. 2 is to be scanned according to 5000 times of explosive of monodisperse Hexanitrohexaazaisowurtzitane microballoon of the embodiment of the present invention 1
Electron microscope；
Fig. 3 is to be scanned according to 1000 times of explosive of monodisperse Hexanitrohexaazaisowurtzitane microballoon of the embodiment of the present invention 2
Electron microscope；
Fig. 4 is to be scanned according to 2500 times of explosive of monodisperse Hexanitrohexaazaisowurtzitane microballoon of the embodiment of the present invention 3
Electron microscope；
Fig. 5 is to be swept again according to the monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive 1000 of the embodiment of the present invention 4
Retouch electron microscope；
Specific embodiment
The present invention is described in further detail below with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1
Hexanitrohexaazaisowurtzitane 0.5g is weighed at room temperature, measurement butyl acetate 9g mixing speed is 500rpm,
It makes it completely dissolved as clear solution.Resulting solution is quickly fitted into 5mL plastic injector, syringe is replaced into upper 27G
Flat-top metal needle, syringe, which is then mounted on environment temperature, is on propulsion pump in 30 DEG C of electrostatic atomizer, if
Setting and promoting the flow velocity of pump is 0.05mm/s, and positive high voltage is connected on metal flat-top syringe needle.Aluminium foil as collector is consolidated
It is scheduled on an insulating plate, and is connected on negative high voltage power source.The distance for adjusting flat-top syringe needle to collector is 20cm.Opening pushes away
Into the switch of pump, first adjusts negative electricity and be pressed onto -10kV, then adjust positive electricity and be pressed onto 6kV, taylor cone occurs in flat-top syringe needle at this time.Surely
Instrument is closed after determining a period of time, monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive can be obtained.Fig. 1 and
Fig. 2 is respectively 2000 times and 5000 times according to the resulting monodisperse Hexanitrohexaazaisowurtzitane microballoon explosive of the present embodiment
Scanning electron microscope (SEM) photograph.Blasting explosive granules size is about 2 μm -5 μm, product purity 99.1%.
Embodiment 2
Hexanitrohexaazaisowurtzitane 10g is weighed at room temperature, measures acetone 20mL, and mixing speed 300rpm makes
It is completely dissolved as clear solution.Resulting solution is quickly fitted into 5mL plastic injector, syringe is replaced upper 19G's
Then syringe is mounted on the propulsion pump in the electrostatic atomizer that environment temperature is 20 DEG C, setting by flat-top metal needle
The good flow velocity for promoting pump is 0.2mm/s, and positive high voltage is connected on metal flat-top syringe needle.Aluminium foil as collector is fixed on
On one insulating plate, and it is connected on negative high voltage power source.The distance for adjusting flat-top syringe needle to collector is 10cm.It opens and promotes pump
Switch, first adjust negative electricity be pressed onto -7kV, then adjust positive electricity be pressed onto 6kV, there is taylor cone in flat-top syringe needle at this time.Stablize one section
Instrument is closed after time, and monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive can be obtained.Fig. 3 is respectively root
According to 1000 times of scanning electron microscope (SEM) photographs of the resulting monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive of the present embodiment.Explosive
Particle size is about 3 μm -6 μm, product purity 99.0%.
Embodiment 3
Hexanitrohexaazaisowurtzitane 2g is weighed at room temperature, measures dimethylformamide 10mL, and mixing speed is
700rpm makes it completely dissolved as clear solution.Resulting solution is quickly fitted into 5mL plastic injector, syringe is set
The flat-top metal needle of 23G is changed, the propulsion then syringe being mounted in the electrostatic atomizer that environment temperature is 35 DEG C
On pump, setting and promoting the flow velocity of pump is 0.075mm/s, and positive high voltage is connected on metal flat-top syringe needle.Collector will be used as
Aluminium foil be fixed on an insulating plate, and be connected on negative high voltage power source.Adjust flat-top syringe needle to collector distance be
25cm.The switch for promoting pump is opened, negative electricity is first adjusted and is pressed onto -10kV, positive electricity is then adjusted and is pressed onto 8kV, flat-top syringe needle goes out at this time
Existing taylor cone.Instrument is closed after a period of stabilisation, and it is hollow that monodispersed Hexanitrohexaazaisowurtzitane micron can be obtained
Ball explosive.Fig. 4 is respectively according to the 2500 of the resulting monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive of the present embodiment
Times scanning electron microscope (SEM) photograph.Blasting explosive granules size is about 1 μm~6 μm, product purity 99.2%.
Embodiment 4
Hexanitrohexaazaisowurtzitane 3g is weighed at room temperature, measures ethyl acetate 10mL, mixing speed 400rpm,
It makes it completely dissolved as clear solution.Resulting solution is quickly fitted into 5mL plastic injector, syringe is replaced into upper 25G
Flat-top metal needle, syringe, which is then mounted on environment temperature, is on propulsion pump in 25 DEG C of electrostatic atomizer, if
Setting and promoting the flow velocity of pump is 0.1mm/s, and positive high voltage is connected on metal flat-top syringe needle.Aluminium foil as collector is fixed
On an insulating plate, and it is connected on negative high voltage power source.The distance for adjusting flat-top syringe needle to collector is 15cm.It opens and promotes
The switch of pump first adjusts negative electricity and is pressed onto -7kV, then adjusts positive electricity and be pressed onto 8kV, taylor cone occurs in flat-top syringe needle at this time.Stablize one
Instrument is closed after the section time, monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive can be obtained.Fig. 5 is respectively
According to 1000 times of scanning electron microscope (SEM) photographs of the resulting monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive of the present embodiment.Explosive
Particle size is about 4 μm~8 μm, product purity 99.3%.
Embodiment 5
Hexanitrohexaazaisowurtzitane 20g is weighed at room temperature, measures butanone 30mL, and mixing speed 600rpm makes
It is completely dissolved as clear solution.Resulting solution is quickly fitted into 5mL plastic injector, syringe is replaced upper 21G's
Then syringe is mounted on the propulsion pump in the electrostatic atomizer that environment temperature is 32 DEG C, setting by flat-top metal needle
The good flow velocity for promoting pump is 0.15mm/s, and positive high voltage is connected on metal flat-top syringe needle.Aluminium foil as collector is fixed
On an insulating plate, and it is connected on negative high voltage power source.The distance for adjusting flat-top syringe needle to collector is 22cm.It opens and promotes
The switch of pump first adjusts negative electricity and is pressed onto -10kV, then adjusts positive electricity and be pressed onto 6kV, taylor cone occurs in flat-top syringe needle at this time.Stablize
Instrument is closed after a period of time, and monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive can be obtained.Explosive
Particle size is about 2 μm~6 μm, product purity 99.1%.
" one embodiment " for being spoken of in the present specification, " another embodiment ", " embodiment " etc., refer to combining
Specific features, structure or the feature of embodiment description are included at least one embodiment generally described herein.
It is not centainly to refer to the same embodiment that statement of the same race, which occur, in multiple places in the description.Furthermore, it is understood that in conjunction with any
When a embodiment describes a specific features, structure or feature, to be advocated be realized in conjunction with other embodiments it is this
Feature, structure or feature are also fallen within the scope of the present invention.
Although reference be made herein to invention has been described for the multiple explanatory embodiments invented, however, it is to be understood that this
Field technical staff can be designed that a lot of other modification and implementations, these modifications and implementations will fall in the application
Within disclosed scope and spirit.More specifically, it is disclosed in the scope of the claims in the application, it can be to theme group
The building block and/or layout for closing layout carry out a variety of variations and modifications.In addition to the modification carried out to building block and/or layout
Outer with improving, to those skilled in the art, other purposes also will be apparent.
Claims (4)
1. the preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere, it is characterised in that the following steps are included:
A. a certain amount of Hexanitrohexaazaisowurtzitane is weighed, is added into organic solvent, heating, stirring make it completely dissolved,
The solution that concentration is 5.5wt%~38.9wt% is obtained, the organic solvent is acetone, butyl acetate, butanone and dimethyl
One of formamide；
B. by the syringe of the solution suction belts flat-top syringe needle in step A, syringe is fixed on micromass culture pump, is set
Parameter regulates syringe needle to the distance of collector, regulates the voltage on syringe needle and collector, make syringe needle keep taylor cone, one
Monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere can be obtained after fixing time；The parameter of setting includes: micromass culture
Flow rate pump is 0.05mm/s~0.2mm/s, and the distance of syringe needle to collector is 10cm~25cm, and negative voltage is -7kV~-10kV,
Positive voltage is 5kV~8kV, and it is 25 DEG C~35 DEG C that temperature, which is arranged, in electrostatic atomizer instrument internal environment.
2. the preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere according to claim 1, feature
It is:
The speed of the stirring is 300rpm~700rpm, and stirring is until Hexanitrohexaazaisowurtzitane is completely dissolved.
3. the preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere according to claim 2, feature
It is:
The metal flat-top syringe needle that the syringe is 5mL injector for medical purpose, flat-top syringe needle is 19G~27G.
4. the preparation method of monodisperse Hexanitrohexaazaisowurtzitane micrometre hollow sphere according to claim 3, feature
It is:
In step B, micromass culture pump is in electrostatic atomizer, and electrostatic atomizer further includes high voltage power supply, and collector is aluminium
Foil.
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| CN108164378A (en) * | 2018-01-11 | 2018-06-15 | 中国工程物理研究院化工材料研究所 | A kind of nanometer of cocrystallized explosive and preparation method thereof |
| CN109485531A (en) * | 2018-12-13 | 2019-03-19 | 南京理工大学 | Superfine spherical CL-20 Composite Energetic Materials and preparation method thereof |
| CN110143843B (en) * | 2019-06-04 | 2021-06-29 | 中国工程物理研究院化工材料研究所 | Nano aluminum-based porous microspheres and preparation method thereof |
| CN110218134B (en) * | 2019-06-27 | 2021-05-14 | 南京理工大学 | TKX-50 nanocrystallization preparation method |
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| CN103172476A (en) * | 2013-04-08 | 2013-06-26 | 中国工程物理研究院化工材料研究所 | Preparation method of submicron particle 1-oxo-diamino-3, 5-dinitropyrazine explosive |
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