CN105777457A - Method for coating energetic crystal surfaces - Google Patents
Method for coating energetic crystal surfaces Download PDFInfo
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- CN105777457A CN105777457A CN201610203737.2A CN201610203737A CN105777457A CN 105777457 A CN105777457 A CN 105777457A CN 201610203737 A CN201610203737 A CN 201610203737A CN 105777457 A CN105777457 A CN 105777457A
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- Prior art keywords
- dopamine
- crystal
- containing energy
- solution
- cladding
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Classifications
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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
-
- 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
-
- 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 method for coating energetic crystal surfaces. Coating of the energetic crystal surfaces is achieved through oxidation-self-polymerization of dopamine under the condition of a weakly alkaline aqueous solution and formation of poly-dopamine coatings powerfully adhering to material surfaces. The method comprises the following steps: dissolving Tris in a mixed solution of water and ethanol in a volume ratio of 9 to 1 and then dropwise adding hydrochloric acid to prepare a buffer solution with the pH value of 8.0-10.0; then dissolving dopamine in the buffer solution to prepare a dopamine solution with the concentration of 1-5g/L; then adding a proper amount of energetic crystal to the dopamine solution and stirring the materials at a stirring rate of 200-900rpm to form uniform suspension; and continuously stirring the suspension for a period of time and then carrying out suction filtration and vacuum drying. The method has the beneficial effects that coating of the energetic crystal surfaces is completed in the aqueous phase, so the method is green and safe; and especially, the method can achieve efficient coating aiming at the energetic crystal surfaces with different characteristics.
Description
Technical field
The present invention relates to a kind of energetic material field, be specifically related to the method containing energy plane of crystal cladding.
Background technology
Containing the organic molecule crystalline material that a class is important can be belonged to by crystal, containing blast official in its molecular structure
Can roll into a ball, can react rapidly and discharge substantial amounts of gas and heat.In civil and military field, this kind of material
It is widely used as the key component in explosive, propellant, pyrotechnic material.Owing to the crystal containing energy be pulverulence,
Cannot directly actual application.Therefore, it is necessary to containing carrying out cladding process by crystal.Polymer bonding explosive
It it is most common processing method.But owing to polymer bonding explosive containing Surface coating degree and the cladding of energy crystal
Intensity is relatively low, has a strong impact on the material combination property in processes such as preparation and uses.
Up to now, many methods have been developed for containing being coated with by plane of crystal.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], be spray-dried 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 use substantial amounts of
Organic solvent dissolves substrate or covering material.Such as document (Chemical Engineering Journal, 2015,
In 268,60-66), the method for report uses toluene to carry out in-situ polymerization cladding as medium.This gives operator
Adverse influence is all brought with environment.The patent of invention of Application No. 201510727192.0 describes a kind of base
Explosive crystal in Thermo-sensitive binding agent is coated with and the method for bonded pelleting.Its principle is according to a kind of water solublity
High polymer binder be dissolved in water when temperature is relatively low, be raised to during uniform temperature become hydrophobic, thus realize fried
Medicine crystal is coated with and induces micro-nano explosive particle to assemble.The crystal containing energy be insensitiveness in aqueous phase, the method
In aqueous phase, achieve the Surface coating containing energy crystal, be both provided that the cladding medium of a safety, green again
Environmental protection, will not produce poisonous solvent slop, and safety is high.But the cladding limited strength that the method reaches.Examine
Consider combination property such as energy, safety, mechanics etc. to energetic material, how to use the fewest cladding material
Material, and method for coating is safe and simple, and can adapt to multiple containing energy crystal system, it is still that this kind of material list
Bread covers facing challenges.
Therefore, novel development and the application containing energy crystalline material being had containing energy plane of crystal method for coating is developed
Important meaning.
Summary of the invention
[solving the technical problem that]
Present invention aim to address above-mentioned prior art problem, it is provided that a kind of pervasive containing can plane of crystal bag
Coating method.The method safe green, to crystal cladding entirely, can be containing energy crystal and to be correlated with containing energy complex
Application provides technical support.
[technical scheme]
In order to reach above-mentioned technique effect, the present invention takes techniques below scheme:
Effective adhesion member dopamine that the present invention utilizes in a kind of ocean in the byssus protein of Mussels is as bag
Cover material.Dopamine is 4-(2-amino-ethyl)-1,2-Benzodiazepines.The present invention utilizes dopaminergic at weak base
Property aqueous conditions under aoxidize-form strength from coalescence and attach to the poly-dopamine coating of material surface and come real
Now containing being coated with by plane of crystal.
A kind of method containing energy plane of crystal cladding, it is that the poly-dopamine formed with dopamine oxidation autohemagglutination is made
It is prepared for covering material.
The present invention further technical scheme, it comprises the following steps:
(1) Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, then dropping hydrochloric acid preparation
The buffer solution becoming pH value to be 8.0～10.0；
(2) dopamine is dissolved in buffer solution, is configured to the dopamine solution that concentration is 1～5g/L；
(3) will add in dopamine solution by the crystal containing energy in right amount, and under the stir speed (S.S.) of 200～900rpm
Stir into uniform suspension；
(4) after continuing stirring a period of time, sucking filtration, vacuum drying.
The present invention further technical scheme, described dopamine is dopamine hydrochloride.
The present invention further technical scheme, the described crystal containing energy be 1,3,5,7-tetranitro-1,3,5,7-tetra-azepines
Cyclooctane (HMX, HMX), 1,3,5-trinitro--1,3,5-Trianacyclohexanes (RDX, RDX),
1,3,5-triamido-1,3,5-trinitrobenzene (TATB), 1,1-diaminourea-2,2-dinitro ethylene (FOX-7), 2,6-
Diamino-3,5-dinitropyrazine-1-oxide (LLM-105) or Hexanitrohexaazaisowurtzitane (HNIW,
CL-20)。
The present invention further technical scheme, the addition of described Tris is the mixed solution after adding Tris
In, the concentration of Tris is 10mM.
The present invention further technical scheme, the described addition containing energy crystal is that step (4) is dried to be obtained
The 95%～99% of the material mass arrived.
The present invention further technical scheme, described stirring is mechanical agitation, its stir speed (S.S.) be 400～
800rpm。。
The present invention further technical scheme, the described mean diameter containing energy crystal is 5～100 μm.
The present invention further technical scheme, in step (4), described mixing time is 2～6h, stirs
Mixing temperature is room temperature.
In view of containing can the particularity such as crystalline material sensitivity, thermodynamic instability, this based on dopamine at water
The system that can realize polymerization cladding under phase solution, room temperature is especially suitable for containing energy crystalline material and other little molecule
The surface of organic crystal material processes.
Will be described in detail the present invention below.
The present invention selects dopamine hydrochloride to be to consider that dopamine hydrochloride easily preserves as dopamine raw material, source
Convenient.The present invention, when selective response condition, needs in view of the sensitivity containing energy crystal itself and thermodynamics
The characteristics such as instability.It is mainly reflected in: 1. aqueous phase is to containing the energy safest system of crystal.2. consider containing energy
Crystal is broken, is different from the process of other material, the therefore preferred mechanical agitation of alr mode, stir speed (S.S.)
Selection so that crystal grain is stirred, preferably 400～800rpm.3. extend along with mixing time,
Poly-dopamine covering amount increases, but the time oversize is unfavorable for simple flow, it is possible to produce crystal quality
Impact, the time is the shortest, and poly-dopamine cladding is the most complete.Therefore, the preferred mixing time of the present invention is 2h～6h.
4. less demanding to temperature of the present invention, along with temperature raises, poly-dopamine is containing can plane of crystal cladding speed
Spend the fastest, but in view of the simplicity and the most handling of operation, at room temperature can realize poly-dopamine and contain
Can plane of crystal cladding.
[beneficial effect]
The present invention compared with prior art, has a following beneficial effect:
With existing containing can be compared with crystal method for coating, characteristic and the creativeness of the present invention be: use dopamine
For containing plane of crystal cladding having no report at present；In the present invention, the plane of crystal cladding containing energy be in aqueous phase
Complete, green safety；In particular for different qualities containing can plane of crystal, the present invention can realize efficient packet
Cover.
Accompanying drawing explanation
Fig. 1 is HMX surface SEM figure；
Fig. 2 is the SEM figure of the HMX Surface coating effect that the embodiment of the present invention 1 obtains；
Fig. 3 is TATB surface SEM figure；
Fig. 4 is the SEM figure of the TATB Surface coating effect that the embodiment of the present invention 3 obtains；
Fig. 5 is CL-20 surface SEM figure；
Fig. 6 is the SEM figure of the CL-20 Surface coating effect that the embodiment of the present invention 4 obtains；
Fig. 7 is that the HMX crystal of the embodiment of the present invention 1 preparation is schemed by the SEM after acetone corrosion；
Fig. 8 is that the CL-20 crystal of the embodiment of the present invention 4 preparation is schemed by SEM after ethyl acetate corrosion.
Detailed description of the invention
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
A kind of HMX is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 8.0 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride solution that concentration is 1g/L；
Then, 10g HMX (mean diameter is 60 μm) is joined the hydrochloric acid DOPA that 200mL prepares
In amine aqueous solution, and under the stir speed (S.S.) of 500rpm, stir into uniform suspension；
After continuing stirring 6h, sucking filtration, vacuum drying.
HMX crystal Surface coating prepared by the present embodiment is complete.Through efficient liquid phase chromatographic analysis, HMX
The covering amount of plane of crystal dopamine is 0.5%.
As a comparison, Fig. 1 is the scanning electron microscope (SEM) photograph of untreated HMX crystal.Fig. 2 is the HMX after cladding
Crystal.As in figure 2 it is shown, the HMX crystal Surface coating of preparation is complete.
Embodiment 2:
A kind of HMX is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 8.5 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride solution that concentration is 2g/L；
Then, 10g HMX (mean diameter is 10 μm) is joined the hydrochloric acid DOPA that 200mL prepares
In amine aqueous solution, and under the stir speed (S.S.) of 600rpm, stir into uniform suspension；
After continuing stirring 6h, sucking filtration, vacuum drying.
HMX crystal Surface coating prepared by the present embodiment is complete.Through efficient liquid phase chromatographic analysis, HMX
The covering amount of plane of crystal dopamine is 2.0%.
Embodiment 3:
A kind of TATB is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 9.5 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride that concentration is 2.5g/L molten
Liquid；
Then, 10g TATB (mean diameter is 5 μm) is joined the hydrochloric acid DOPA that 200mL prepares
In amine aqueous solution, and under the stir speed (S.S.) of 800rpm, stir into uniform suspension；
After continuing stirring 3h, sucking filtration, vacuum drying.
As a comparison, Fig. 3 is the scanning electron microscope (SEM) photograph of untreated TATB crystal.Fig. 4 is the TATB after cladding
Crystal.As shown in Figure 4, the TATB plane of crystal cladding of preparation is complete, through efficient liquid phase chromatographic analysis,
The covering amount of TATB plane of crystal dopamine is 0.5%.
Embodiment 4:
A kind of CL-20 is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 9.0 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride solution that concentration is 2g/L；
Then, 10g CL-20 (mean diameter is 90 μm) is joined the hydrochloric acid DOPA that 200mL prepares
In amine aqueous solution, and under the stir speed (S.S.) of 500rpm, stir into uniform suspension；
After continuing stirring 4h, sucking filtration, 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 after cladding
Crystal.As shown in Figure 6, the CL-20 plane of crystal cladding of preparation is complete, through efficient liquid phase chromatographic analysis,
The covering amount of CL-20 plane of crystal dopamine is 0.5%.
Embodiment 5:
A kind of RDX is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 8.5 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride solution that concentration is 5g/L；
Then, 20g RDX (mean diameter is 100 μm) is joined the hydrochloric acid DOPA that 200mL prepares
In amine aqueous solution, and under the stir speed (S.S.) of 500rpm, stir into uniform suspension；
After continuing stirring 1h, sucking filtration, vacuum drying.
The RDX plane of crystal cladding of preparation is complete, through efficient liquid phase chromatographic analysis, RDX plane of crystal
The covering amount of dopamine is 0.4%.
Embodiment 6:
A kind of FOX-7 is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 8.5 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride solution that concentration is 2g/L；
Then, 10g FOX-7 (mean diameter is 20 μm) is joined the hydrochloric acid DOPA that 200mL prepares
In amine aqueous solution, and under the stir speed (S.S.) of 400rpm, stir into uniform suspension；
After continuing stirring 3h, sucking filtration, vacuum drying.
The FOX-7 plane of crystal cladding of preparation is complete, through efficient liquid phase chromatographic analysis, FOX-7 crystal table
The covering amount of face dopamine is 0.4%.
Embodiment 7:
A kind of LLM-105 is containing the method for coating of energy crystal, and it comprises the following steps:
At ambient temperature, Tris is dissolved in the mixed solution that water is 9:1 with ethanol volume ratio, makes
Tris concentration is the solution of 10mM；Then to be configured to the buffer solution that pH is 9.0 standby for dropping hydrochloric acid.
Then, dopamine hydrochloride is dissolved in buffer solution, makes the dopamine hydrochloride solution that concentration is 2g/L；
Then, 10g LLM-105 (mean diameter is 100 μm) is joined the hydrochloric acid that 200mL prepares
In dopamine solution, and under the stir speed (S.S.) of 500rpm, stir into uniform suspension；
After continuing stirring 6h, sucking filtration, vacuum drying.
Completely, through efficient liquid phase chromatographic analysis, LLM-105 is brilliant for the LLM-105 plane of crystal cladding of preparation
The covering amount of surface dopamine is 0.4%.
Embodiment 8:
In order to verify the covered effect in the present invention, the present embodiment is specifically designed for the HMX being easily dissolved by the solvent
Product after crystal cladding.Product after HMX crystal cladding 0.2g embodiment 1 obtained joins
In 100mL acetone, dissolving of fully vibrating, and with 5 insoluble matters of washing with acetone.Finally by insoluble matter with sweeping
Retouch electronic microscope photos.As it is shown in fig. 7, HMX crystal is by after acetone corrosion, the insoluble matter stayed is (for poly-DOPA
Amine clad) in hollow-core construction, still keep the shape of HMX crystal, this illustrates that poly-dopamine is at HMX
Defining the clad of densification outside crystal, cladding is completely.
Embodiment 9:
In order to verify the covered effect in the present invention, the present embodiment is specifically designed for the CL-20 being easily dissolved by the solvent
Product after crystal cladding.Product after CL-20 crystal cladding 0.2g embodiment 4 obtained joins
In 100mL ethyl acetate, dissolving of fully vibrating, and wash 5 insoluble matters by ethyl acetate.Finally will not
Molten thing scanning electron microscope analysis.As shown in Figure 8, CL-20 crystal is by after ethyl acetate corrosion, and stay is insoluble
Thing (for poly-DOPA amine layer) is film layer structure, and this illustrates that poly-dopamine defines outside CL-20 crystal
Fine and close clad, cladding is completely.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, and above-described embodiment is only
For the present invention preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, it should
Understanding, those skilled in the art can be designed that a lot of other amendments and embodiment, and these are revised and real
The mode of executing will fall within spirit disclosed in the present application and spirit.
Claims (9)
1. the method containing energy plane of crystal cladding, it is characterised in that it is formed with dopamine oxidation autohemagglutination
Poly-dopamine is prepared as covering material.
Method containing energy plane of crystal cladding the most according to claim 1, it is characterised in that it includes following
Step:
(1) being dissolved in by Tris in the mixed solution that water is 9:1 with ethanol volume ratio, then dropping hydrochloric acid is joined
Make the buffer solution that pH value is 8.0～10.0；
(2) dopamine is dissolved in buffer solution, is configured to the dopamine solution that concentration is 1～5g/L；
(3) will add in dopamine solution by the crystal containing energy in right amount, and under the stir speed (S.S.) of 200～900rpm
Stir into uniform suspension；
(4) after continuing stirring a period of time, sucking filtration, vacuum drying.
Method containing energy plane of crystal cladding the most according to claim 2, it is characterised in that described dopamine
For dopamine hydrochloride.
Method containing energy plane of crystal cladding the most according to claim 2, it is characterised in that described brilliant containing energy
Body is 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclododecane octane, 1,3,5-trinitro--1,3,5-three azepine hexamethylene
Alkane, 1,3,5-triamido-1,3,5-trinitrobenzene, 1,1-diaminourea-2,2-dinitro ethylene, 2,6-diaminourea
-3,5-dinitro pyrazine-1-oxide or Hexanitrohexaazaisowurtzitane.
Method containing energy plane of crystal cladding the most according to claim 2, it is characterised in that described Tris's
Addition is that in the mixed solution after adding Tris, the concentration of Tris is 10mM.
Method containing energy plane of crystal cladding the most according to claim 2, it is characterised in that described brilliant containing energy
The addition of body is the 95%～99% of the material mass that step (4) obtains after drying.
Method containing energy plane of crystal cladding the most according to claim 2, it is characterised in that described stirring is
Mechanical agitation, its stir speed (S.S.) is 400～800rpm.
Method containing energy plane of crystal cladding the most according to claim 4, it is characterised in that described brilliant containing energy
The mean diameter of body is 5～100 μm.
Method containing energy plane of crystal cladding the most according to claim 2, it is characterised in that in step (4)
In, described mixing time is 2～6h, whipping temp is room temperature.
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| CN106518582A (en) * | 2016-11-03 | 2017-03-22 | 中国工程物理研究院化工材料研究所 | Preparation method of energetic material with controllable interface infiltration performance |
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