CN105777457B - The method of the cladding of the plane of crystal containing energy - Google Patents
The method of the cladding of the plane of crystal containing energy Download PDFInfo
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- CN105777457B CN105777457B CN201610203737.2A CN201610203737A CN105777457B CN 105777457 B CN105777457 B CN 105777457B CN 201610203737 A CN201610203737 A CN 201610203737A CN 105777457 B CN105777457 B CN 105777457B
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- cladding
- containing energy
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/009—Wetting agents, hydrophobing agents, dehydrating agents, antistatic additives, viscosity improvers, antiagglomerating agents, grinding agents and other additives for working up
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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
Abstract
The invention discloses a kind of method of the cladding of the plane of crystal containing energy.Oxidation occur under the conditions of weak alkaline aqueous solution using dopaminergic for the present invention form strength from coalescence to attach to the poly-dopamine coating of material surface to realize that containing energy plane of crystal coats.It comprises the following steps：It is 9 that Tris is dissolved in into water with ethanol volume ratio：In 1 mixed solution, hydrochloric acid is then added dropwise and is configured to the cushioning liquid that pH value is 8.0~10.0；Then, dopamine is dissolved in cushioning liquid, is configured to the dopamine solution that concentration is 1~5g/L；Then it the crystal containing energy will add in right amount in dopamine solution, and uniform suspension is stirred under 200~900rpm stir speed (S.S.)；Continue after stirring a period of time, filter, vacuum drying.The cladding of the plane of crystal containing energy is completed in aqueous phase in the present invention, green safe；In particular for different qualities plane of crystal containing energy, efficiently cladding can be achieved in the present invention.
Description
Technical field
The present invention relates to a kind of energetic material field, and in particular to the method for the cladding of the plane of crystal containing energy.
Background technology
The crystal containing energy belongs to a kind of important organic molecule crystalline material, and blast functional group is contained in its molecular structure,
It can rapidly react and discharge substantial amounts of gas and heat.In civil and military field, this kind of material is widely used as explosive, pushed away
The key component entered in agent, pyrotechnic material., can not direct practical application because the crystal containing energy is pulverulence.Therefore, it is necessary to
Cladding processing is carried out to the crystal containing energy.Polymer bonding explosive is most common processing method.But due to polymer bonding explosive
In containing can crystal Surface coating degree and cladding intensity it is relatively low, have a strong impact on that material such as is preparing and used at the comprehensive of process
Energy.
Up to now, develop many methods and be used for the cladding of the plane of crystal containing energy.Such as crystallize cladding [Jung J W, Kim K
J.Effect of supersaturation on the morphology of coated surface in coating by
solution crystallization[J].Industrial&Engineering Chemistry Research,2011,50
(6):3475-3482], spray drying cladding [Qiu H, Stepanov V, Chou T, et al.Single-step
production and formulation of HMX nanocrystals[J].Powder technology,2012,226:
235-238；Ma Z,Gao B,Wu P,et al.Facile,continuous and large-scale production of
core–shell HMX@TATB composites with superior mechanical properties by a
spray-drying process[J].RSC Advances,2015,5(27):21042-21049], in-situ polymerization cladding
[Zhijian Yang,Ling Ding,Peng Wu,Yonggang Liu,Fude Nie,Fenglei Huang,
Fabrication of RDX,HMX and CL-20based microcapsules via in situ
polymerization of melamine–formaldehyde resins with reduced sensitivity,
Chemical Engineering Journal, 2015,268,60-66] etc..The plane of crystal method for coating containing energy of existing report
All substrate or covering material are dissolved using substantial amounts of organic solvent.Such as document (Chemical Engineering
Journal, 2015,268,60-66) in report method use toluene as medium progress in-situ polymerization cladding.This is to operation
Personnel and environment all bring detrimental effect.The patent of invention of Application No. 201510727192.0 describes a kind of based on temperature sensitive
Property binding agent explosive crystal cladding and bonded pelleting method.Its principle is existed according to a kind of water miscible high polymer binder
Water is dissolved in when temperature is relatively low, becomes hydrophobic when being raised to certain temperature, so as to realize that explosive crystal coats and induces micro-nano explosive
Particle buildup.The crystal containing energy is insensitiveness in aqueous phase, and this method realizes the Surface coating of the crystal containing energy in aqueous phase, can
The cladding medium of one safety is provided, but it is green, poisonous solvent slop will not be produced, it is safe.But this method reaches
Cladding limited strength.In view of combination property such as energy, safety, mechanics etc. of energetic material, how using as few as possible
Covering material, and method for coating is safe and simple, and a variety of crystal systems containing energy are can adapt to, it is still this kind of material surface cladding
Facing challenges.
Therefore, develop it is new containing can plane of crystal method for coating to containing can crystalline material development and application have it is important
Meaning.
The content of the invention
[technical problems to be solved]
Present invention aim to address above-mentioned prior art problem, there is provided a kind of pervasive cladding side of the plane of crystal containing energy
Method.This method safe green, crystal is coated entirely, technology branch can be provided for the application of the crystal containing energy and the related compound containing energy
Support.
[technical scheme]
In order to reach above-mentioned technique effect, the present invention takes following technical scheme：
The present invention is used as cladding material by the use of effective adhesion member dopamine in a kind of byssus protein of Mussels in ocean
Material.Dopamine is 4- (2- amino-ethyls) -1,2- benzenediols.The present invention is issued using dopaminergic in weak alkaline aqueous solution condition
Raw oxidation-form strength from coalescence attaches to the poly-dopamine coating of material surface to realize that contain can plane of crystal cladding.
A kind of method of the cladding of the plane of crystal containing energy, it is that the poly-dopamine formed by the use of dopamine oxidation autohemagglutination is used as cladding
Prepared by material.
The further technical scheme of the present invention, it comprises the following steps：
(1) it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, hydrochloric acid is then added dropwise and is configured to pH value and is
8.0~10.0 cushioning liquid；
(2) dopamine is dissolved in cushioning liquid, is configured to the dopamine solution that concentration is 1~5g/L；
(3) it the crystal containing energy will add in dopamine solution, and be stirred under 200~900rpm stir speed (S.S.) in right amount
Even suspension；
(4) continue after stirring a period of time, filter, vacuum drying.
The further technical scheme of the present invention, the dopamine is Dopamine hydrochloride.
The further technical scheme of the present invention, it is described containing can crystal be 1,3,5,7- tetranitros -1,3,5,7- tetra- azepines
Cyclooctane (HMX, HMX), 1,3,5- trinitro-s -1,3,5- Trianacyclohexanes (RDX, RDX), 1,3,5- tri- ammonia
Base -1,3,5- trinitrobenzens (TATB), 1,1- diaminourea -2,2- dinitros ethene (FOX-7), 2,6- diaminourea -3,5- dinitros
Base pyrazine -1- oxides (LLM-105) or Hexanitrohexaazaisowurtzitane (HNIW, CL-20).
The further technical scheme of the present invention, the addition of the Tris to add in the mixed solution after Tris,
Tris concentration is 10mM.
The further technical scheme of the present invention, the addition of the crystal containing energy are the thing obtained after step (4) is dried
The 95%~99% of matter quality.
The further technical scheme of the present invention, the stirring is mechanical agitation, and its stir speed (S.S.) is 400~800rpm..
The further technical scheme of the present invention, the average grain diameter of the crystal containing energy is 5~100 μm.
The further technical scheme of the present invention, in step (4), the mixing time is 2~6h, whipping temp is room
Temperature.
In view of containing can the particularity such as crystalline material sensitivity, thermodynamic instability, it is this be based on dopamine aqueous phase solution,
It is the table of the especially suitable crystalline material containing energy of system and other small molecule organic crystal materials that polymerization cladding can be achieved at room temperature
Face is handled.
The present invention is will be described in detail below.
Present invention selection Dopamine hydrochloride is to consider that Dopamine hydrochloride easily preserves as dopamine raw material, convenient sources.
The present invention is when select reaction condition, it is necessary in view of containing can the characteristic such as the sensitive and thermodynamic instability of crystal in itself.It is main
It is embodied in：1. aqueous phase is to the safest system of crystal containing energy.2. consider that the crystal containing energy is broken, different from other materials
Processing, therefore the preferred mechanical agitation of agitating mode, the selection of stir speed (S.S.) is so that crystal grain to be stirred, and preferably 400
~800rpm.3. as mixing time extends, poly-dopamine covering amount increase, but the time it is oversize be unfavorable for simple flow, have
Crystal quality may be had an impact, the time is too short, and poly-dopamine cladding is not complete.Therefore, the present invention preferably mixing time is 2h
~6h.4. the present invention is to the less demanding of temperature, as temperature raises, poly-dopamine is got in the cladding speed of the plane of crystal containing energy
Hurry up, but in view of operation simplicity and easily it is handling, at room temperature i.e. can be achieved poly-dopamine containing can plane of crystal cladding.
[beneficial effect]
The present invention compared with prior art, has following beneficial effect：
Compared with the existing crystal method for coating containing energy, characteristic of the invention and creativeness are：It is used to contain using dopamine
Energy plane of crystal cladding has no report at present；The cladding of the plane of crystal containing energy is completed in aqueous phase in the present invention, green safe；Especially
It is for different qualities plane of crystal containing energy, and efficiently cladding can be achieved in the present invention.
Brief description of the drawings
Fig. 1 schemes for HMX surfaces SEM；
Fig. 2 is the SEM figures for the HMX Surface coating effects that the embodiment of the present invention 1 obtains；
Fig. 3 schemes for TATB surfaces SEM；
Fig. 4 is the SEM figures for the TATB Surface coating effects that the embodiment of the present invention 3 obtains；
Fig. 5 schemes for CL-20 surfaces SEM；
Fig. 6 is the SEM figures for the CL-20 Surface coating effects that the embodiment of the present invention 4 obtains；
Fig. 7 is that HMX crystal prepared by the embodiment of the present invention 1 is schemed by the SEM after acetone corrosion；
Fig. 8 is that CL-20 crystal prepared by the embodiment of the present invention 4 is schemed by SEM after ethyl acetate corrosion.
Embodiment
With reference to embodiments of the invention, the invention will be further elaborated.
Embodiment 1：
A kind of method for coating of HMX crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 8.0 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 1g/L is made；
Then, 10g HMX (average grain diameter is 60 μm) are added in the Dopamine hydrochloride solution that 200mL is prepared, and
Uniform suspension is stirred under 500rpm stir speed (S.S.)；
Continue after stirring 6h, filter, vacuum drying.
HMX crystal Surface coating manufactured in the present embodiment is complete.By efficient liquid phase chromatographic analysis, HMX crystal surface is more
The covering amount of bar amine is 0.5%.
As a comparison, Fig. 1 is the scanning electron microscope (SEM) photograph of untreated HMX crystal.Fig. 2 is the HMX crystal after cladding.Such as Fig. 2
Shown, the HMX crystal Surface coating of preparation is complete.
Embodiment 2：
A kind of method for coating of HMX crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 8.5 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 2g/L is made；
Then, 10g HMX (average grain diameter is 10 μm) are added in the Dopamine hydrochloride solution that 200mL is prepared, and
Uniform suspension is stirred under 600rpm stir speed (S.S.)；
Continue after stirring 6h, filter, vacuum drying.
HMX crystal Surface coating manufactured in the present embodiment is complete.By efficient liquid phase chromatographic analysis, HMX crystal surface is more
The covering amount of bar amine is 2.0%.
Embodiment 3：
A kind of method for coating of TATB crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 9.5 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 2.5g/L is made；
Then, 10g TATB (average grain diameter is 5 μm) are added in the Dopamine hydrochloride solution that 200mL is prepared, and
Uniform suspension is stirred under 800rpm stir speed (S.S.)；
Continue after stirring 3h, filter, vacuum drying.
As a comparison, Fig. 3 is the scanning electron microscope (SEM) photograph of untreated TATB crystal.Fig. 4 is the TATB crystal after cladding.Such as figure
Shown in 4, the TATB planes of crystal cladding of preparation is complete, by efficient liquid phase chromatographic analysis, the bag of TATB plane of crystal dopamines
The amount of covering is 0.5%.
Embodiment 4：
A kind of method for coating of CL-20 crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 9.0 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 2g/L is made；
Then, 10g CL-20 (average grain diameter is 90 μm) are added in the Dopamine hydrochloride solution that 200mL is prepared,
And uniform suspension is stirred under 500rpm stir speed (S.S.)；
Continue after stirring 4h, filter, vacuum drying.
As a comparison, Fig. 5 is the scanning electron microscope (SEM) photograph of untreated CL-20 crystal.Fig. 6 is the CL-20 crystal after cladding.Such as
Shown in Fig. 6, the CL-20 planes of crystal cladding of preparation is complete, by efficient liquid phase chromatographic analysis, CL-20 plane of crystal dopamines
Covering amount be 0.5%.
Embodiment 5：
A kind of method for coating of RDX crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 8.5 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 5g/L is made；
Then, 20g RDX (average grain diameter is 100 μm) are added in the Dopamine hydrochloride solution that 200mL is prepared, and
Uniform suspension is stirred under 500rpm stir speed (S.S.)；
Continue after stirring 1h, filter, vacuum drying.
The RDX planes of crystal cladding of preparation is complete, by efficient liquid phase chromatographic analysis, the bag of RDX plane of crystal dopamines
The amount of covering is 0.4%.
Embodiment 6：
A kind of method for coating of FOX-7 crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 8.5 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 2g/L is made；
Then, 10g FOX-7 (average grain diameter is 20 μm) are added in the Dopamine hydrochloride solution that 200mL is prepared,
And uniform suspension is stirred under 400rpm stir speed (S.S.)；
Continue after stirring 3h, filter, vacuum drying.
The FOX-7 planes of crystal cladding of preparation is complete, by efficient liquid phase chromatographic analysis, FOX-7 plane of crystal dopamines
Covering amount be 0.4%.
Embodiment 7：
A kind of method for coating of LLM-105 crystal containing energy, it comprises the following steps：
At ambient temperature, it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, Tris concentration, which is made, is
10mM solution；Then it is standby to be configured to the cushioning liquid that pH is 9.0 for dropwise addition hydrochloric acid.
Then, Dopamine hydrochloride is dissolved in cushioning liquid, the Dopamine hydrochloride solution that concentration is 2g/L is made；
Then, 10g LLM-105 (average grain diameter be 100 μm) are added to the Dopamine hydrochloride solution that 200mL prepares
In, and uniform suspension is stirred under 500rpm stir speed (S.S.)；
Continue after stirring 6h, filter, vacuum drying.
The LLM-105 planes of crystal cladding of preparation is complete, and by efficient liquid phase chromatographic analysis, LLM-105 planes of crystal are more
The covering amount of bar amine is 0.4%.
Embodiment 8：
In order to verify the covered effect in the present invention, the present embodiment is specifically for the HMX crystal bag being easily dissolved by the solvent
Product after covering.Product after the HMX crystal that 0.2g embodiments 1 are obtained is coated is added in 100mL acetone, fully vibration
Dissolving, and wash 5 insoluble matters with acetone.Finally by insoluble matter scanning electron microscope analysis.As shown in fig. 7, HMX crystal is by acetone
After corrosion, the insoluble matter that leaves is in hollow-core construction (for poly-dopamine clad), still keeps the shape of HMX crystal, this explanation
Poly-dopamine forms the clad of densification outside HMX crystal, and cladding is complete.
Embodiment 9：
In order to verify the covered effect in the present invention, the present embodiment is specifically for the CL-20 crystal being easily dissolved by the solvent
Product after cladding.Product after the CL-20 crystal that 0.2g embodiments 4 are obtained is coated is added in 100mL ethyl acetate,
Fully vibration dissolving, and wash 5 insoluble matters with ethyl acetate.Finally by insoluble matter scanning electron microscope analysis.As shown in figure 8,
The insoluble matter that CL-20 crystal after ethyl acetate corrosion, is left is thin layer membrane structure (for poly-dopamine layer), and this illustrates poly- DOPA
Amine forms the clad of densification outside CL-20 crystal, and cladding is complete.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modifications and embodiment, and these modifications and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (8)
- A kind of 1. method of the cladding of the plane of crystal containing energy, it is characterised in that it is the poly-dopamine formed with dopamine oxidation autohemagglutination Prepared as covering material；It comprises the following steps：(1) it is 9 Tris to be dissolved in into water with ethanol volume ratio：In 1 mixed solution, hydrochloric acid is then added dropwise and is configured to pH value as 8.0 ~10.0 cushioning liquid；(2) dopamine is dissolved in cushioning liquid, is configured to the dopamine solution that concentration is 1~5g/L；(3) it the crystal containing energy will add in dopamine solution, and be stirred into uniformly under 200~900rpm stir speed (S.S.) in right amount Suspension；(4) continue after stirring a period of time, filter, vacuum drying.
- 2. the method for the cladding of the plane of crystal containing energy according to claim 1, it is characterised in that the dopamine is that hydrochloric acid is more Bar amine.
- 3. the method for the cladding of the plane of crystal containing energy according to claim 1, it is characterised in that the crystal containing energy is 1,3, 5,7- tetranitro -1,3,5,7- tetraazacyclododecanes octane, 1,3,5- trinitro- -1,3,5- Trianacyclohexanes, 1,3,5- triamidos - 1,3,5- trinitrobenzens, 1,1- diaminourea -2,2- dinitros ethene, 2,6- diaminourea -3,5- dinitros pyrazine -1- oxides or Hexanitrohexaazaisowurtzitane.
- 4. it is according to claim 1 containing can plane of crystal cladding method, it is characterised in that the addition of the Tris is Add in the mixed solution after Tris, Tris concentration is 10mM.
- 5. the method for the cladding of the plane of crystal containing energy according to claim 1, it is characterised in that the addition of the crystal containing energy Measure the 95%~99% of the material mass obtained after being dried for step (4).
- 6. the method for the cladding of the plane of crystal containing energy according to claim 1, it is characterised in that the stirring is mechanical agitation, Its stir speed (S.S.) is 400~800rpm.
- 7. the method for the cladding of the plane of crystal containing energy according to claim 3, it is characterised in that the crystal containing energy is averaged Particle diameter is 5~100 μm.
- 8. the method for the cladding of the plane of crystal containing energy according to claim 1, it is characterised in that described to stir in step (4) Mix the time be 2~6h, whipping temp be room temperature.
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| CN102153426A (en) * | 2010-11-09 | 2011-08-17 | 中北大学 | Coating method for in-situ generating energy-containing deterrent ANPZ on surface of 1,3,5-trinitro-1,3,5-triaza-cyclohexane (RDX) |
| CN103086812A (en) * | 2013-02-04 | 2013-05-08 | 中国工程物理研究院化工材料研究所 | Preparation method of bicomponent energetic material core-shell structure |
| CN105126810A (en) * | 2015-07-28 | 2015-12-09 | 西安近代化学研究所 | Preparation method of SnO2@C nanometer combustion catalyst with octahedral structure |
| CN105399341A (en) * | 2015-11-24 | 2016-03-16 | 中国工程物理研究院化工材料研究所 | Single-layer fluorene conjugated polymer film based on polydopamine modified inorganic substrate as well as preparation method and application of single-layer fluorene conjugated polymer film |
| CN105440583A (en) * | 2015-12-04 | 2016-03-30 | 武汉理工大学 | Dopamine compound modified or coated nano particle modified polymer composite material and preparation method thereof |
| CN105801324A (en) * | 2016-03-04 | 2016-07-27 | 中国工程物理研究院化工材料研究所 | Preparation method for reducing mechanical sensitivity of HMX |
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