CN106946635A - The preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere - Google Patents
The preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere Download PDFInfo
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- CN106946635A CN106946635A CN201710272365.3A CN201710272365A CN106946635A CN 106946635 A CN106946635 A CN 106946635A CN 201710272365 A CN201710272365 A CN 201710272365A CN 106946635 A CN106946635 A CN 106946635A
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- hexanitrohexaazaisowurtzitane
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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
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- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
Abstract
The invention discloses the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, comprise the following steps：A. a certain amount of Hexanitrohexaazaisowurtzitane is weighed, is added into organic solvent, heating, stirring are completely dissolved it；B. by the syringe of the solution suction belts flat-top syringe needle in step A, syringe is fixed on micromass culture pump, set parameter, syringe needle is regulated to the distance of collector, regulate the voltage on syringe needle and collector, syringe needle is kept taylor cone, monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere is can obtain after certain time.Product particle pattern of the present invention is spherical, and particle size distribution is narrow, and microsphere particle is all made up of nano particle, has important application prospect in fields such as primings.And present invention process flow is simple, the microsphere particle being made does not need further work-up, and experiment condition is gentle, and security is good.
Description
Technical field
The invention belongs to energetic material preparing technical field, and in particular to a kind of monodispersed azepine of hexanitro six different 5 is hereby
The preparation method of alkane micrometre hollow sphere.
Background technology
Modern war injures power to improving weapon and proposes requirements at the higher level, and the excellent high energy single chmical compound explosive of performance
It is then explosive energetic, lifts the most fundamental way that weapon injures power.Hexanitrohexaazaisowurtzitane (CL-20) is now
Practical application energy highest single chmical compound explosive, its energy output is higher by 10~15% than HMX (HMX), is applied to fire fried
Medicine field can significantly improve weapons and ammunitions Kill capability.
The hollow and loose structure energetic material specific surface area high due to having, can significantly improve the burning speed of explosive wastewater
Rate, and spherical structure enables to loading increase to improve the energy density of explosive wastewater.Wang Ping etc. (energetic material, 2015,
11,1107-1110) nitrocotton micropore ball is prepared for using solvent leaching process, obtained micropore ball surface is smooth, and particle diameter is at 20 μm
Left and right, sphericity is 0.89.Wang Jiang etc. (explosive wastewater journal, 2015,1,16-21) utilizes the technique study of spray drying entrance
The influence of temperature, feed rate, nebulizing gas flow rate and solution concentration to RDX granule-morphologies, finally gives 2.8 μm, surface light
Sliding spherical RDX particles, spherical RDX impact sensitivity reduction more obvious than raw material.Shen Jinpeng etc. (CN103044173B, 2012)
Aided in using crystal morphology controlling agent, invented a kind of preparation method of the 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.
It is spherical for 20-500 μm that Chen Huaxiong etc. (CN200910090462.6,2010) uses the method for crystal formation adjuvant to be prepared for size
Hexanitrohexaazaisowurtzitane, the method system that text jasmine etc. (CN201511000272.2,2016) is not crystallized using dilute solution
For the Hexanitrohexaazaisowurtzitane crystal of high-quality.These technologies to the preparation of the poroid spheroid 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 spheroid, but existing side at present
There is complex process, bad dispersibility in method, and to the preparation description of Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive compared with
It is few.
The content of the invention
Instant invention overcomes the deficiencies in the prior art, there is provided monodispersed Hexanitrohexaazaisowurtzitane micron is hollow
The preparation method of ball, core content of the invention is to be atomized rapid crystallization using electrostatic spray, utilizes the powered small of atomization formation
Drop is mutually exclusive, and the solvent in last drop volatilizees completely, so that it is micro- to form monodispersed Hexanitrohexaazaisowurtzitane
Rice hollow ball explosive.In view of the above mentioned problem of prior art, according to one side disclosed by the invention, the present invention is using following
Technical scheme：
The preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, comprises the following steps：
A. a certain amount of Hexanitrohexaazaisowurtzitane is weighed, is added into organic solvent, heating, stirring make 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 put, syringe needle has been regulated to the distance of collector, regulates the voltage on syringe needle and collector, syringe needle is kept Taylor
Monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere is can obtain after cone, certain time.
Further, concentration is 5.5wt%~38.9wt% after the dissolving of described Hexanitrohexaazaisowurtzitane；
Further, described organic solvent is in acetone, ethyl acetate, butyl acetate, butanone and dimethylformamide
One kind；
Further, described, mixing speed is 300rpm~700rpm, stirring until blasting explosive granules are completely dissolved；
Further, described syringe be 5mL injector for medical purpose, metal needle be 19G~27G flat-top syringe needle, band
The electrostatic atomizer of micromass culture pump and high voltage power supply, collector is aluminium foil；
Further, described propulsion flow rate pump is 0.05mm/s~0.2mm/s, and the distance of syringe needle to collector is 10cm
~25cm, negative voltage is -7kV~-10kV, and positive voltage is 5kV~8kV, and instrument internal ambient As temperature is 25 DEG C~35 DEG C；
Further, a diameter of 2 μm of the single dispersing Hexanitrohexaazaisowurtzitane microballoon explosive of preparation~8 μm, product
Purity is more than 99%.
Compared with prior art, one of beneficial effects of the present invention are：Product particle pattern is spherical, particle size point
Cloth is narrow, and microsphere particle is all made up of nano particle, has important application prospect in fields such as primings.And present invention process flow
Simply, the microsphere particle being made does not need further work-up, and experiment condition is gentle, and security is good.
Brief description of the drawings
, below will be to embodiment for clearer explanation present specification embodiment or technical scheme of the prior art
Or the accompanying drawing to be used needed for the description of prior art is briefly described, it should be apparent that, drawings in the following description are only
It is the reference to the embodiment of some in present specification, for those skilled in the art, is not paying creative work
In the case of, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is 2000 times of scannings of single dispersing Hexanitrohexaazaisowurtzitane microballoon explosive according to the embodiment of the present invention 1
Electron microscope；
Fig. 2 is 5000 times of scannings of single dispersing Hexanitrohexaazaisowurtzitane microballoon explosive according to the embodiment of the present invention 1
Electron microscope；
Fig. 3 is 1000 times of scannings of single dispersing Hexanitrohexaazaisowurtzitane microballoon explosive according to the embodiment of the present invention 2
Electron microscope；
Fig. 4 is 2500 times of scannings of single dispersing Hexanitrohexaazaisowurtzitane microballoon explosive according to 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；
Embodiment
The present invention is described in further detail with reference to embodiment, but embodiments of the present invention not limited to this.
Embodiment 1
Hexanitrohexaazaisowurtzitane 0.5g is weighed at room temperature, measures butyl acetate 9g mixing speeds for 500rpm,
It is completely dissolved for settled solution.The solution of gained is quickly fitted into 5mL plastic injectors, syringe is replaced into upper 27G
Flat-top metal needle, syringe is then arranged on environment temperature on the propulsion pump in 30 DEG C of electrostatic atomizer, if
Set and promote the flow velocity of pump for 0.05mm/s, 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 is pushed away
Enter the switch of pump, first adjust negative electricity and be pressed onto -10kV, then adjust positive electricity and be pressed onto 6kV, now taylor cone occurs in flat-top syringe needle.Surely
Determine to close instrument after a period of time, you can obtain monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive.Fig. 1 and
Fig. 2 is respectively 2000 times and 5000 times of the single dispersing Hexanitrohexaazaisowurtzitane microballoon explosive according to obtained by the present embodiment
Scanning electron microscope (SEM) photograph.Blasting explosive granules size is about 2 μm -5 μm, and product purity is 99.1%.
Embodiment 2
Hexanitrohexaazaisowurtzitane 10g is weighed at room temperature, acetone 20mL is measured, and mixing speed is 300rpm, is made
It is completely dissolved as settled solution.The solution of gained is quickly fitted into 5mL plastic injectors, syringe is replaced upper 19G's
Flat-top metal needle, syringe then be arranged on environment temperature on the propulsion pump in 20 DEG C of electrostatic atomizer, to set
The flow velocity for promoting pump well 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.Open and promote pump
Switch, first adjust negative electricity be pressed onto -7kV, then adjust positive electricity be pressed onto 6kV, now there is taylor cone in flat-top syringe needle.Stablize one section
Instrument is closed after time, you can obtain monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive.Fig. 3 is respectively root
According to 1000 times of scanning electron microscope (SEM) photographs of the monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive obtained by the present embodiment.Explosive
Particle size is about 3 μm -6 μm, and product purity is 99.0%.
Embodiment 3
Hexanitrohexaazaisowurtzitane 2g is weighed at room temperature, dimethylformamide 10mL is measured, and mixing speed is
700rpm, is completely dissolved it for settled solution.The solution of gained is quickly fitted into 5mL plastic injectors, syringe is put
23G flat-top metal needle is changed, it is the propulsion in 35 DEG C of electrostatic atomizer that syringe then is arranged on into environment temperature
On pump, set and promote the flow velocity of pump for 0.075mm/s, 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.Regulation 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, now flat-top syringe needle goes out
Existing taylor cone.Instrument is closed after a period of stabilisation, you can obtain monodispersed Hexanitrohexaazaisowurtzitane micron hollow
Ball explosive.Fig. 4 is respectively 2500 of the monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive according to obtained by the present embodiment
Times scanning electron microscope (SEM) photograph.Blasting explosive granules size is about 1 μm~6 μm, and product purity is 99.2%.
Embodiment 4
Hexanitrohexaazaisowurtzitane 3g is weighed at room temperature, ethyl acetate 10mL is measured, and mixing speed is 400rpm,
It is completely dissolved for settled solution.The solution of gained is quickly fitted into 5mL plastic injectors, syringe is replaced into upper 25G
Flat-top metal needle, syringe is then arranged on environment temperature on the propulsion pump in 25 DEG C of electrostatic atomizer, if
Set and promote the flow velocity of pump for 0.1mm/s, 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.Open and promote
The switch of pump, first adjusts negative electricity and is pressed onto -7kV, then adjust positive electricity and be pressed onto 8kV, now taylor cone occurs in flat-top syringe needle.Stablize one
Instrument is closed after the section time, you can obtain monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive.Fig. 5 is respectively
1000 times of scanning electron microscope (SEM) photographs of the monodispersed Hexanitrohexaazaisowurtzitane microballoon explosive according to obtained by the present embodiment.Explosive
Particle size is about 4 μm~8 μm, and product purity is 99.3%.
Embodiment 5
Hexanitrohexaazaisowurtzitane 20g is weighed at room temperature, butanone 30mL is measured, and mixing speed is 600rpm, is made
It is completely dissolved as settled solution.The solution of gained is quickly fitted into 5mL plastic injectors, syringe is replaced upper 21G's
Flat-top metal needle, syringe then be arranged on environment temperature on the propulsion pump in 32 DEG C of electrostatic atomizer, to set
The flow velocity for promoting pump well 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.Open and promote
The switch of pump, first adjusts negative electricity and is pressed onto -10kV, then adjust positive electricity and be pressed onto 6kV, now taylor cone occurs in flat-top syringe needle.It is stable
Instrument is closed after a period of time, you can obtain monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere explosive.Explosive
Particle size is about 2 μm~6 μm, and product purity is 99.1%.
" one embodiment ", " another embodiment ", " embodiment " for being spoken of in this manual etc., refers to combining
Specific features, structure or the feature of embodiment description are included at least one embodiment of the application generality description.
It is not necessarily to refer to same embodiment that statement of the same race, which occur, in multiple places in the description.Furthermore, it is understood that with reference to any
When individual embodiment describes a specific features, structure or feature, what is advocated is this to realize with reference to other embodiment
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
Art personnel can be designed that a lot of other modification and embodiment, and these modifications and embodiment will fall in the application
Within disclosed spirit and spirit.More specifically, can be to theme group in the range of disclosure claim
The building block and/or layout for closing layout carry out a variety of variations and modifications.Except 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 (8)
1. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, it is characterised in that comprise the following steps：
A. a certain amount of Hexanitrohexaazaisowurtzitane is weighed, is added into organic solvent, heating, stirring are completely dissolved it；
B. by the syringe of the solution suction belts flat-top syringe needle in step A, syringe is fixed on micromass culture pump, set
Parameter, regulates syringe needle to the distance of collector, regulates the voltage on syringe needle and collector, syringe needle is kept taylor cone, one
Monodispersed Hexanitrohexaazaisowurtzitane micrometre hollow sphere is can obtain after fixing time.
2. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, its feature according to claim 1
It is：
Concentration is 5.5wt%~38.9wt% after described Hexanitrohexaazaisowurtzitane dissolving.
3. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere according to claim 1 or claim 2, it is special
Levy and be：
Described organic solvent is one kind in acetone, ethyl acetate, butyl acetate, butanone and dimethylformamide.
4. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, its feature according to claim 3
It is：
The speed of the stirring is 300rpm~700rpm, stirring until Hexanitrohexaazaisowurtzitane is completely dissolved.
5. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, its feature according to claim 4
It is：
Described syringe is the metal flat-top syringe needle that 5mL injector for medical purpose, flat-top syringe needle are 19G~27G.
6. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, its feature according to claim 5
It is：
In step B, during micromass culture pump is electrostatic atomizer, electrostatic atomizer also includes high voltage power supply, and collector is aluminium
Paper tinsel.
7. the preparation method of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere, its feature according to claim 6
It is：
Described micromass culture flow rate pump is 0.05mm/s~0.2mm/s, and the distance of syringe needle to collector is 10cm~25cm, negative electricity
Press as -7kV~-10kV, positive voltage is 5kV~8kV, electrostatic atomizer instrument internal ambient As temperature is 25 DEG C~35
℃。
8. the preparation of single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere described in claim 1 to 7 any claim
The single dispersing Hexanitrohexaazaisowurtzitane micrometre hollow sphere that method is prepared, a diameter of 2 μm~8 μm, product purity is big
In 99%.
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Cited By (4)
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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 |
| CN110143843A (en) * | 2019-06-04 | 2019-08-20 | 中国工程物理研究院化工材料研究所 | A kind of aluminium-based porous microballoon of nanometer and preparation method thereof |
| CN110218134A (en) * | 2019-06-27 | 2019-09-10 | 南京理工大学 | A kind of preparation method of TKX-50 nanosizing |
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| CN110143843A (en) * | 2019-06-04 | 2019-08-20 | 中国工程物理研究院化工材料研究所 | A kind of aluminium-based porous microballoon of nanometer and preparation method thereof |
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| CN110218134A (en) * | 2019-06-27 | 2019-09-10 | 南京理工大学 | A kind of preparation method of TKX-50 nanosizing |
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| CN106946635B (en) | 2019-07-19 |
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