CN104591936B - Composite material containing energy based on three-dimensional ordered macroporous carbon skeleton and preparation method thereof - Google Patents
Composite material containing energy based on three-dimensional ordered macroporous carbon skeleton and preparation method thereof Download PDFInfo
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- CN104591936B CN104591936B CN201510048316.2A CN201510048316A CN104591936B CN 104591936 B CN104591936 B CN 104591936B CN 201510048316 A CN201510048316 A CN 201510048316A CN 104591936 B CN104591936 B CN 104591936B
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Abstract
The invention discloses a kind of composite material containing energy in three-dimensional ordered macroporous carbon skeleton and preparation method thereof, belong to energetic material field, said method comprising the steps of: have in volatile organic solvent by being dissolved under energetic material room temperature, select three-dimensional ordered macroporous carbon skeleton material room temperature immersion in above-mentioned solution, after solvent volatilizees completely, energetic material is loaded in three-dimensional ordered macroporous carbon skeleton with nanocrystalline form, obtains the adjustable Nanocomposite Energetic Materials of performance.The present invention can provide a kind of new approaches by stable for energetic material at nanoscale for the high-energy-density energetic material that design performance is controlled.The Energetic Nano-composites of gained in hot property be improved significantly, thermal decomposition peak temperature significantly reduces, energy release rapidly, at energetic material nanorize, realizing controlled-release energy and micro-containing being with a wide range of applications in device.
Description
Technical field
Embodiments of the present invention relate to energetic material field, more specifically, embodiments of the present invention relate to
A kind of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton and preparation method thereof.
Background technology
Energetic material, mainly includes explosive, propellant and pyrotechnic compound etc., is that one obtains on military and civilian
Multifunctional material to large-scale application.Owing to its reactivity is all had clearly by the great majority application of energetic material
Requirement, the energetic material that therefore design performance is controlled is always the study hotspot in this field.Grinding in early days
In studying carefully, can only reach, by mixing different types of chemical substance, the purpose that energetic material is reactive.
Development along with nanotechnology, it has been found that due to energetic material typically by organic point containing high-energy-density
Son composition, the release of its energy is dynamic control process, is therefore in 10～30nm when material granule particle diameter
During nanoscale, the reactivity of energetic material can occur to change greatly, can be real by controlling grain diameter
The design that existing energetic material is reactive.But the particle surface energy of nanoscale is very big, easily reunites, it is difficult to all
Even it is scattered among other compositions.How to make energetic material can become design at stable existence under nanoscale
The difficult problem that the controlled energetic material of performance must solve.A kind of effective method is to be born by energetic material
It is loaded in the stephanoporate framework material with micro-nano structure, obtains Nanocomposite Energetic Materials.Utilize the limit in duct
Territory effect can make energetic material crystallize on nanoscale, grow, it is also possible to accurately controls composite
Composition, thus reach the purpose that controlled material is reactive, as reduced the sensitivity of high explosive and obtaining higher
Energy density and energy output.In conventional research, the molecular sieve of small-bore and ordered mesoporous material quilt
Being chosen for use as framework material to prepare Energetic Nano-composites, the aperture size in these skeletons typically only has
Several nanometers, too small aperture significantly limit energetic material and enters skeleton and diffusion wherein.
Nano-carbon material refers to the most one-dimensional material with carbon element less than 100nm of dispersion phase yardstick, and dispersion phase both may be used
To be made up of carbon atom, it is also possible to be made up of the xenogenesis atom of non-carbon, it might even be possible to be nano-pore,
It mainly includes three types: CNT, carbon nano-fiber and nano carbon microsphere.Three-dimensional ordered macroporous carbon bone
Frame is the class aperture new macroporous material with carbon element more than 50nm.The aperture size of material is big and is evenly distributed, hole
Road is neat and orderly, is interconnected by wicket between macropore, constitutes the three-dimensional large-meshed net of internal crosslinking
Network.There is presently no the report preparing Energetic Nano-composites with three-dimensional ordered macroporous carbon skeleton for carrier.
Summary of the invention
Instant invention overcomes the deficiency that the load capacity of Energetic Nanomaterials is restricted by existing framework material, carry
For a kind of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton and preparation method thereof, can obtain with expectation
Obtain a kind of high performance composite material containing energy.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
The invention provides a kind of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton, it is with three-dimensional
Ordered big hole carbon skeleton is the composite material containing energy that carrier loaded energetic material is formed.
Further technical scheme is: contain in described composite material containing energy based on three-dimensional ordered macroporous carbon skeleton
The mass fraction of energy material is 33.3～62.9%.The consumption of energetic material can directly affect nanometer containing energy composite wood
The performance of material, under the conditions of this mass fraction, the three-dimensional ordered macroporous carbon skeleton load effect to energetic material
Best.
Further technical scheme is: described energetic material is in CL-20, RDX, FOX-7, PETN, AP
The mixture of one or more.Containing nitro and the energetic material of amino, it is easier to and macropore carbon skeleton duct
Interior Surface oxygen-containing groups produces and interacts, and strengthens load effect.
Further technical scheme is: the aperture of described three-dimensional ordered macroporous carbon skeleton is 180～430nm.
The macropore diameter of three-dimensional ordered macroporous carbon skeleton is homogeneous, and pore structure is ordered arrangement in three dimensions, macropore it
Between be interconnected by wicket, beneficially energetic material enters inside macropore from all directions, thus reduces
The resistance of material diffusion, the transmission for material provides higher efficiency with diffusion.And each macropore space
Being construed as the reaction compartment of a nanoscale, energetic material can crystallize wherein and be grown to serve as
Nanocrystalline, make energetic material can at stable existence under nanoscale so that performance be improved significantly.Cause
This, three-dimensional ordered macroporous carbon skeleton is a kind of ideal carrier material preparing Energetic Nano-composites, can have
Effect overcome small-bore molecular sieve and mesoporous material make it difficult for energetic material enter cavity and in skeleton diffusion lack
Fall into, obtain the adjustable Energetic Nano-composites of performance.
Present invention also offers the preparation side of a kind of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton
Method, it comprises the following steps:
(1) energetic material is at room temperature dissolved completely in have in right amount in volatile organic solvent obtain contain
Can material solution；
(2) three-dimensional ordered macroporous carbon skeleton is added mix homogeneously in energetic material solution and obtain mixed liquor；
(3) at room temperature being stood by mixed liquor, part organic solvent is removed in volatilization, and residue organic solvent is with just
Pentane removes, and during this, energetic material loads to inside three-dimensional ordered macroporous carbon skeleton with brilliant form；
(4) material that step (3) obtains i.e. is obtained based on three-dimensional ordered macroporous carbon skeleton through dried
Composite material containing energy.
Further technical scheme is: described composite material containing energy based on three-dimensional ordered macroporous carbon skeleton
In preparation method, described organic solvent is the mixed liquor of acetone or acetone and dimethyl sulfoxide.Good solvent can
With the upper active force reduced between energetic material molecule largely, along with solvent volatilizees, energetic material molecule
Three-dimensional ordered macroporous carbon skeleton is entered, it is achieved load under capillary force action.
Further technical scheme is: described composite material containing energy based on three-dimensional ordered macroporous carbon skeleton
Preparation method in, the mass ratio of acetone and dimethyl sulfoxide in the mixed liquor of described acetone and dimethyl sulfoxide
It is 4～8:1.
Further technical scheme is: described composite material containing energy based on three-dimensional ordered macroporous carbon skeleton
Preparation method in, described dry temperature is 50～80 DEG C.
Compared with prior art, one of beneficial effects of the present invention is: the present invention have chosen three-dimensional ordered macroporous
Carbon skeleton is carrier material, effectively overcomes small-bore molecular sieve and mesoporous material makes it difficult for energetic material and enters
Cavity and the defect spread in skeleton；The preparation method flow process of the present invention is simple, and reaction condition is gentle, suitable
For multiple energetic material；Energetic Nano-composites prepared by the present invention is substantially changed in hot property
Kind, with containing can compared with block materials and physical mixture, the thermal decomposition peak temperature of complex typically can reduce by 17 DEG C～
71 DEG C, and thermal discharge increases, energy release is rapidly.
Accompanying drawing explanation
Fig. 1 is the SEM photograph of the three-dimensional ordered macroporous carbon skeleton material of the embodiment of the present invention 1 aperture 300nm.
Fig. 2 is the TEM photo of the three-dimensional ordered macroporous carbon skeleton material of the embodiment of the present invention 2 aperture 300nm.
Fig. 3 is that the three-dimensional ordered macroporous carbon skeleton of embodiment of the present invention 3CL-20 and aperture 300nm obtains
The SEM photograph of Nanocomposite Energetic Materials, CL-20 content is 62.9%.
Fig. 4 be the three-dimensional ordered macroporous carbon skeleton of CL-20 of the present invention and aperture 300nm obtain nano combined
The XRD spectra of energetic material.
Fig. 5 be the three-dimensional ordered macroporous carbon skeleton of CL-20 of the present invention and aperture 300nm obtain nano combined
The DSC spectrogram of energetic material and respective physical mixture.
Fig. 6 be the three-dimensional ordered macroporous carbon skeleton of CL-20 of the present invention and aperture 300nm obtain nano combined
The TG spectrogram of energetic material and respective physical mixture.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and reality
Execute example, the present invention is further elaborated.Only should be appreciated that specific embodiment described herein
Only in order to explain the present invention, it is not intended to limit the present invention.
Embodiment 1
The Nanocomposite Energetic Materials of the three-dimensional ordered macroporous carbon skeleton composition of CL-20 and aperture 300nm, CL-20
Content is 33.3%, and the SEM photograph of the three-dimensional ordered macroporous carbon skeleton material of aperture 300nm is as shown in Figure 1.
The CL-20 at room temperature taking 0.05g is dissolved in 4.0g under the conditions of the magnetic agitation that rotating speed is 300 revs/min
In acetone, stirring to CL-20 is completely dissolved.Take the three-dimensional ordered macroporous carbon skeleton material that 0.1g aperture is 300nm
Material adds in solution, stirs 5 minutes to mix homogeneously under the conditions of the magnetic agitation that rotating speed is 100 revs/min.Mixed
Compound stands at room temperature, after solvent all volatilizees, obtains blackish green solid.One is entered in 65 DEG C of air
Step is dried, and obtains Energetic Nano-composites, and CL-20 content is 33.3%.Its XRD spectra is as shown in Figure 4.
The temperature of initial decomposition of the dsc analysis display Energetic Nano-composites of Fig. 5 is 144 DEG C, and exothermic peak temperature is
169 DEG C, reduce by 76 DEG C and 71 DEG C than pure CL-20 block materials respectively.The TG curve display nanometer of Fig. 6 contains can be multiple
Condensation material has faster weight loss rate.
Embodiment 2
The Nanocomposite Energetic Materials of the three-dimensional ordered macroporous carbon skeleton composition of CL-20 and aperture 300nm, CL-20
Content is 52.4%, and the TEM photo of the three-dimensional ordered macroporous carbon skeleton material of aperture 300nm is as shown in Figure 2.
The CL-20 at room temperature taking 0.11g is dissolved in 4.0g under the conditions of the magnetic agitation that rotating speed is 300 revs/min
In acetone, stirring to CL-20 is completely dissolved.Take the three-dimensional ordered macroporous carbon skeleton material that 0.1g aperture is 300nm
Material adds in solution, stirs 5 minutes to mix homogeneously under the conditions of the magnetic agitation that rotating speed is 100 revs/min.Mixed
Compound stands at room temperature, after solvent all volatilizees, obtains blackish green solid.One is entered in 65 DEG C of air
Step is dried, and obtains Energetic Nano-composites, and CL-20 content is 52.4%.Its XRD spectra is as shown in Figure 4.
The temperature of initial decomposition of the dsc analysis display Energetic Nano-composites of Fig. 5 is 146 DEG C, and Exotherm peak temperature is
172 DEG C, reduce by 74 DEG C and 68 DEG C than pure CL-20 block materials respectively.The TG curve display nanometer of Fig. 6 contains can be multiple
Condensation material has faster weight loss rate.
Embodiment 3
The Nanocomposite Energetic Materials of the three-dimensional ordered macroporous carbon skeleton composition of CL-20 and aperture 300nm, its
SEM photograph is as it is shown on figure 3, CL-20 content is 62.9%.
The CL-20 at room temperature taking 0.17g is dissolved under the conditions of the magnetic agitation that rotating speed is 300 revs/min
In 4.0g acetone, stirring to CL-20 is completely dissolved.Take the three-dimensional ordered macroporous carbon that 0.1g aperture is 300nm
Framework material adds in solution, stirs 5 minutes to mixing under the conditions of the magnetic agitation that rotating speed is 100 revs/min
Uniformly.Mixture stands at room temperature, after solvent all volatilizees, obtains blackish green solid.At 65 DEG C of skies
Being further dried in gas, obtain Energetic Nano-composites, CL-20 content is 62.9%.Its XRD spectra is shown in
Shown in Fig. 4.The temperature of initial decomposition of the dsc analysis display Energetic Nano-composites of Fig. 5 is 147 DEG C, low
Temperature exothermic peak temperature is 175 DEG C, reduces by 73 DEG C and 65 DEG C than pure CL-20 block materials respectively, than same proportioning
Physical mixture reduces by 90 DEG C and 70 DEG C；The generation heat of Energetic Nano-composites is 1607J/g, and pure
CL-20 block materials and the generation heat with the physical mixture of proportioning are respectively 1494J/g and 1428J/g, put
Heat improves a lot.The TG curve display Energetic Nano-composites of Fig. 6 has faster weight loss rate.
Physical mixture in Fig. 5 is big with the three-dimensional order that 0.1g aperture is 300nm by the CL-20 block of 0.17g
Hole carbon skeleton material mixed grinding forms.
Embodiment 4
The Nanocomposite Energetic Materials of the three-dimensional ordered macroporous carbon skeleton composition of CL-20 and aperture 180nm, CL-20
Content is 62.9%.
The CL-20 at room temperature taking 0.17g is dissolved in 4.0g under the conditions of the magnetic agitation that rotating speed is 300 revs/min
In acetone, stirring to CL-20 is completely dissolved.Take the three-dimensional ordered macroporous carbon skeleton material that 0.1g aperture is 180nm
Material adds in solution, stirs 5 minutes to mix homogeneously under the conditions of the magnetic agitation that rotating speed is 100 revs/min.Mixed
Compound stands at room temperature, after solvent all volatilizees, obtains black solid.In 65 DEG C of air further
Being dried, obtain Energetic Nano-composites, CL-20 content is 62.9%.Dsc analysis display nanometer is containing being combined
The temperature of initial decomposition of material is 156 DEG C, and exothermic peak temperature is 205 DEG C, reduces than pure CL-20 block materials respectively
64 DEG C and 35 DEG C.
Embodiment 5
The Nanocomposite Energetic Materials of the three-dimensional ordered macroporous carbon skeleton composition of CL-20 and aperture 430nm, CL-20
Content is 62.9%.
The CL-20 at room temperature taking 0.17g is dissolved in 4.0g under the conditions of the magnetic agitation that rotating speed is 300 revs/min
In acetone, stirring to CL-20 is completely dissolved.Take the three-dimensional ordered macroporous carbon skeleton material that 0.1g aperture is 430nm
Material adds in solution, stirs 5 minutes to mix homogeneously under the conditions of the magnetic agitation that rotating speed is 100 revs/min.Mixed
Compound stands at room temperature, after solvent all volatilizees, obtains red solid.One is entered in 80 DEG C of air
Step is dried, and obtains Energetic Nano-composites, and CL-20 content is 62.9%.Dsc analysis display nanometer contains can be multiple
The temperature of initial decomposition of condensation material is 151 DEG C, and exothermic peak temperature is 214 DEG C, drops than pure CL-20 block materials respectively
Low 69 DEG C and 26 DEG C.
Embodiment 6
What CL-20/FOX-7 mixture and the three-dimensional ordered macroporous carbon skeleton of aperture 300nm formed nano combined contains
Energy material, CL-20/FOX-7 mixture content is 62.9%.
At room temperature take the FOX-7 of CL-20 and 0.085g of 0.085g in the magnetic agitation that rotating speed is 300 revs/min
Under the conditions of be dissolved in the mixed solvent of 3.5g acetone and 0.5g dimethyl sulfoxide, stir to CL-20 and FOX-7
It is completely dissolved.Take the three-dimensional ordered macroporous carbon skeleton material that 0.1g aperture is 300nm and add in solution, at rotating speed
It is to stir 5 minutes under the conditions of the magnetic agitation of 100 revs/min to mix homogeneously.Mixture stands at room temperature, treats
After acetone all volatilizees, wash away residue dimethyl sulfoxide with pentane, obtain blackish green solid.At 70 DEG C of skies
Being further dried in gas, obtain Energetic Nano-composites, the content of energetic material is 62.9%.Dsc analysis
The temperature of initial decomposition of display Energetic Nano-composites is 190 DEG C, and Exotherm peak temperature is 208 DEG C, respectively
Reduce by 30 DEG C and 32 DEG C than pure CL-20 block materials, reduce than the Exotherm peak value of pure FOX-7 block materials
17℃。
Embodiment 7
CL-20/RDX mixture is nano combined containing energy with the three-dimensional ordered macroporous carbon skeleton of aperture 300nm composition
Material, CL-20/RDX mixture content is 62.9%.
At room temperature take the RDX of CL-20 and 0.085g of 0.085g at the magnetic agitation bar that rotating speed is 300 revs/min
Being dissolved under part in 4.0g acetone, stirring to CL-20 and RDX is completely dissolved.Take that 0.1g aperture is 300nm three
Dimension ordered big hole carbon skeleton material adds in solution, stirs 5 under the conditions of the magnetic agitation that rotating speed is 100 revs/min
Minute to mix homogeneously.Mixture stands at room temperature, after solvent all volatilizees, obtains blackish green solid.
Being further dried in 60 DEG C of air, obtain Energetic Nano-composites, energetic material content is 62.9%.DSC
The temperature of initial decomposition analyzing display Energetic Nano-composites is 162 DEG C, and Exotherm peak temperature is 184 DEG C,
Respectively ratio pure CL-20 block materials reduce by 58 DEG C and 56 DEG C, respectively than pure RDX block materials reduce by 58 DEG C with
59℃。
Although reference be made herein to invention has been described for the multiple explanatory embodiment of the present invention, but, should
This understanding, those skilled in the art can be designed that a lot of other amendments and embodiment, these amendment and
Embodiment will fall within spirit disclosed in the present application and spirit.More specifically, public in the application
Open, in the range of drawings and claims, the building block of theme composite configuration and/or layout can be carried out
Multiple modification and improvement.In addition to the modification that building block and/or layout are carried out and improvement, for this area
For technical staff, other purposes also will be apparent from.
Claims (4)
1. the preparation method of a composite material containing energy based on three-dimensional ordered macroporous carbon skeleton, it is characterised in that it
Comprise the following steps:
(1) energetic material is at room temperature dissolved completely in have in right amount in volatile organic solvent obtain contain
Can material solution；Described energetic material be the one in CL-20, RDX, FOX-7, PETN, AP or
Multiple mixture；
(2) the three-dimensional ordered macroporous carbon skeleton that aperture is 180～430nm is added in energetic material solution mixed
Close and uniformly obtain mixed liquor；
(3) at room temperature being stood by mixed liquor, part organic solvent is removed in volatilization, and residue organic solvent is with just
Pentane removes, and during this, energetic material loads to inside three-dimensional ordered macroporous carbon skeleton with brilliant form；
(4) material that step (3) obtains i.e. is obtained based on three-dimensional ordered macroporous carbon skeleton through dried
Composite material containing energy.
The preparation side of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton the most according to claim 1
Method, it is characterised in that described organic solvent is the mixed liquor of acetone or acetone and dimethyl sulfoxide.
The preparation side of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton the most according to claim 2
Method, it is characterised in that described acetone and acetone in the mixed liquor of dimethyl sulfoxide and the matter of dimethyl sulfoxide
Amount ratio is 4～8:1.
The preparation side of composite material containing energy based on three-dimensional ordered macroporous carbon skeleton the most according to claim 1
Method, it is characterised in that described dry temperature is 50～80 DEG C.
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| CN106886615B (en) * | 2015-12-10 | 2020-06-05 | 南京理工大学 | Simulation method of RDX-based multi-component energetic compound |
| CN106892789B (en) * | 2017-03-28 | 2018-10-26 | 中国工程物理研究院化工材料研究所 | Three-dimensional ordered macroporous-mesoporous carbon/ammonium perchlorate composite material and preparation method |
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| CN101440008A (en) * | 2007-11-23 | 2009-05-27 | 深圳大学 | Lead oxide / carbon nano-tube composite powder and preparation thereof |
| CN202328355U (en) * | 2011-08-12 | 2012-07-11 | 南京理工大学 | Igniter embedded with conductive energetic material in pores |
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