CN103044173B - Method for preparing ordered porous energetic crystal material - Google Patents
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract
The invention discloses a method for preparing an ordered porous energetic crystal material. The method comprises the following steps of: dissolving a certain amount of energetic materials in a good solvent at room temperature; adding a certain amount of crystal morphology control agents into the solution in the previous step, stirring, dissolving, and slowly adding the solution in the previous step into a poor solvent of the energetic materials and the crystal morphology control agents under the magnetic stirring conditions; continuously stirring the solution in the previous step for a certain time, filtering, and obtaining a composite material of the energetic materials and the crystal morphology control agents; adding the obtained composite material into the solvent, wherein the solvent is a poor solvent of the energetic materials and a good solvent of the crystal morphology control agents; repeatedly washing and removing the crystal morphology control agents; and drying to obtain pure ordered porous energetic crystal material. The preparation method is simple in process flow and mild in reaction conditions and suitable for various energetic materials, the reaction conditions are easy to control, and the prepared ordered porous energetic crystal material has the purity of over 99.5 percent.
Description
Technical field
The invention belongs to energetic material field, be specifically related to a kind of ordered porous preparation method containing energy crystalline material.
Background technology
Highly ordered porous materials is the novel nano structure material risen rapidly the nineties in 20th century, and it obtains international physics, chemistry and the great attention of material educational circles once being born, and develops rapidly and become one of study hotspot interdisciplinary.Highly ordered porous materials have duct size evenly, arrangement in order, the characteristics such as aperture can regulate within the specific limits continuously, have broad application prospects in optical material, electronics and electro-optical assembly, vertical magnetism record material, biosensor, photocatalyst, sorbing material and medicine controlled releasing etc.Therefore, porous material is applied to the research that energetic material will be expanded and deepen to energetic material research.
Energetic material, mainly comprises explosive, propelling agent and pyrotechnics composition etc., is a kind of multifunctional material obtaining large-scale application in fields such as civilian, military and space.Along with the development of nanotechnology, many new ideas are incorporated in energetic material field, create profound influence to its research work.Nano-porous structure due to nano-porous materials have impact on the physical and chemical process of material, as mass transfer, heat transfer etc., so the research being combined into energetic material of nano-porous materials and energetic material is filled with new vitality.Waste water or the waste gas such as at first, the gac that people adopt porous unordered carrys out Treatment of TNT (2，4，6-trinitrotoluene) as sorbent material, AP (perchloric acid is pressed), but research contents is confined to unordered porous material.Until the nineties in 20th century, the appearance of highly ordered porous materials novel in a large number.Highly ordered porous materials is applied to energetic material field.2006, Majano etc. select the pure silicon MFI-type molecular sieve with straight hole road (0.53nm × 0.56nm) and Z-type duct (0.51nm × 0.55nm) to be material of main part, be used for adsorbing high energy density compound FOX-7 (1,1-diamino-2,2-dinitrobenzene ethene).DSC test shows, compared with body phase material (exothermic peak 225 DEG C and 275 DEG C), and the thermostability enhancing (exothermic peak 264 DEG C and 377 DEG C) of nano-scale FOX-7 in duct.CuO nano particle is highly dispersed on SBA-15 carrier and makes supported catalyst by Fu etc., and when to add quality in AP system be the catalyzer of 1%, combustion speed can increase by 9.5%, and Pressure Exponent can reduce by 17.3%.2011, Cai etc. utilized SBA-15, filled nanometer CL-20 explosive in duct, preparation CL-20/SBA-15 Composite Energetic Materials.DSC test result shows: the thermolysis peak value of CL-20 is at 240 DEG C, and CL-20/SBA-15 nano-complex compares CL-20 and mechanical mixture decomposition peak shifts to an earlier date, occur in 229 DEG C, because the CL-20 granularity being filled in SBA-15 is little, the atomicity relative proportion on surface is larger, Surface atomic mobility is higher, under same temperature condition, more easily decomposition reaction occurs.
But above-mentioned research is only that porous structure material is applied to energetic material, using ordered porous structural material as solid support material and energetic material compound, porous material itself is not energetic material, in experiment and use procedure, skeleton is a kind of ordered porous Composite Energetic Materials with what obtain, does not obtain the ordered porous energetic material be made up of energetic material self.So on the basis of ordered porous Composite Energetic Materials, if when not affecting vesicular structure, deviate from not containing the solid support material of energy, just can obtain the energetic material of ordered porous structural.
The present invention thinks deeply from the angle of numerator self-assembly technique and crystal engineering, under the induction regulating controlling effect of special tensio-active agent, prepares a kind of ordered porous energetic material be made up of energetic material self.Ordered porous be conducive to energetic material burning or blast process in combustion wave and pressure propagation.
Summary of the invention
The object of the invention is to provide a kind of ordered porous preparation method containing energy crystalline material.Core content of the present invention adds a kind of crystal morphology control agent in energetic material solvent-nonsolvent crystallisation process, energetic material and crystal morphology control agent cocrystallization, then remove crystal morphology control agent, just defines ordered porous energetic material.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
An ordered porous preparation method containing energy crystalline material, is characterized in that comprising the following steps:
A. a certain amount of energetic material is at room temperature dissolved in the good solvent of energetic material, makes energetic material be dissolved in good solvent completely;
B. in the solution of steps A, add a certain amount of crystal morphology control agent, stirring and dissolving, to make crystal morphology control agent and energetic material fully act on, the crystal morphology of energetic material is regulated and controled;
C. the solution of step B is joined slowly in the poor solvent of energetic material and crystal morphology control agent under the condition of magnetic agitation, in bad solution, crystallization can obtain the mixture of energetic material and crystal morphology control agent to make energetic material and crystal morphology control agent;
D., after the solution of step C being continued to stir certain hour, filter, obtain the mixture of energetic material and crystal morphology control agent;
E. join in solvent by the mixture of gained in step D, described solvent is the poor solvent of energetic material, the good solvent of crystal morphology control agent, to make the crystal morphology control agent in the mixture of energetic material and crystal morphology control agent be dissolved in solvent, energetic material is crystallization in a solvent; Repeatedly wash, to make to remove crystal morphology control agent, obtain high ordered porous containing can crystalline material of purity;
F. filtered by step e gained, dry, obtaining pure ordered porous containing can crystalline material.
Further, described energetic material can be the energetic materials such as CL-20, HMX, RDX, PETN, FOX-7, AP.
Further, described crystal morphology control agent can be cup [4] aromatic hydrocarbons, cup [6] aromatic hydrocarbons, cup [8] aromatic hydrocarbons, dibenzo-18-crown-6 (DB18C6), alpha-cylodextrin, beta-cyclodextrin, γ-cyclodextrin.Due to calixarene, crown ether, cyclodextrin all has unique void structure, easily energetic material molecule organic with it forms non covalent bond, thus formed complicated in order and there is the supramolecular complex system of specific function, therefore calixarene, crown ether, cyclodextrin can be used as the crystal morphology control agent of energetic material, regulates and controls into ordered porous containing can crystalline material to the crystal morphology of energetic material.
Further, the mass percentage of described crystal morphology control agent is 1%-50%.
Further, the rotating speed of described magnetic agitation is 100 revs/min-1000 revs/min.
Further, in described step C, in poor solvent and steps A, the volume ratio of good solvent is greater than 5, with ensure energetic material can and crystal morphology control agent from step C, crystallize out the mixture of formation energetic material and crystal morphology control agent completely.
Further, the ordered porous aperture containing energy crystalline material adopting described preparation method to prepare is 10-500nm.
The ordered porous preparation method's technical process containing energy crystalline material of the present invention is simple, and reaction conditions is gentle, and reaction conditions is easy to control, and is applicable to multiple energetic material, and the ordered porous purity containing energy crystalline material of preparation is greater than 99.5%.
Accompanying drawing explanation
Fig. 1 is 2000 times of SEM figure of ordered porous CL-20.
Fig. 2 is 6000 times of SEM figure of ordered porous CL-20.
Fig. 3 is the XRD figure of ordered porous CL-20.
Embodiment
Embodiment 1:
Preparation method's step of ordered porous CL-20 is as follows:
Be dissolved in 5ml nitrogen dimethylformamide under at room temperature getting the magnetic agitation condition that 0.1gCL-20 is 500 revs/min at rotating speed, be stirred to CL-20 and dissolve completely.
Getting 0.05g cup [4] aromatic hydrocarbons adds in solution, continues to stir, until cup [4] aromatic hydrocarbons dissolves completely.
Under the condition stirred, solution is added dropwise in 50ml redistilled water, and CL-20/ cup [4] aromatic hydrocarbons mixture is slowly separated out.Continue stirring 30 minutes, filter, vacuum-drying 12h at 50 DEG C, obtains CL-20/ cup [4] aromatic hydrocarbons mixture.
Get 0.1gCL-20/ cup [4] aromatic hydrocarbons mixture and put into 100ml redistilled water, wash under 100 revs/min of magnetic agitation, cup in mixture [4] aromatic hydrocarbons is slowly dissolved, repeatedly repeated washing, cup [4] aromatic hydrocarbons in removing CL-20/ cup [4] aromatic hydrocarbons mixture, filter, drying obtains ordered porous CL-20.
Fig. 1 is 2000 times of SEM figure of ordered porous CL-20, Fig. 2 is that 6000 times of SEM of ordered porous CL-20 scheme, and Fig. 3 is the XRD figure of ordered porous CL-20.
Embodiment 2:
Preparation method's step of ordered porous CL-20 is as follows:
Be dissolved in 5ml nitrogen dimethylformamide under at room temperature getting the magnetic agitation condition that 0.1g CL-20 is 500 revs/min at rotating speed, be stirred to CL-20 and dissolve completely.
Getting 0.05g beta-cyclodextrin adds in solution, continues to stir, until beta-cyclodextrin dissolves completely.
Under the condition stirred, solution is added dropwise in 50ml redistilled water, and CL-20/ beta-cyclodextrin mixture is slowly separated out, and continues stirring 30 minutes, and filter, vacuum-drying 12h at 50 DEG C, obtains CL-20/ beta-cyclodextrin mixture.
Get 0.1gCL-20/ beta-cyclodextrin mixture and put into 100ml redistilled water, wash under 100 revs/min of magnetic agitation, beta-cyclodextrin in mixture is slowly dissolved, repeatedly repeated washing, beta-cyclodextrin in removing CL-20/ beta-cyclodextrin mixture, filter, drying obtains ordered porous CL-20.
Embodiment 3:
Preparation method's step of ordered porous HMX is as follows:
Be dissolved in 5ml nitrogen dimethylformamide under at room temperature getting the magnetic agitation condition that 0.1gHMX is 500 revs/min at rotating speed, be stirred to HMX and dissolve completely.
Getting 0.05g cup [8] aromatic hydrocarbons adds in solution, continues to stir, until cup [8] aromatic hydrocarbons dissolves completely.
Under the condition stirred, solution is added dropwise in 50ml redistilled water, and CL-20/ cup [8] aromatic hydrocarbons mixture is slowly separated out, and continues stirring 30 minutes, and filter, vacuum-drying 12h at 50 DEG C, obtains HMX/ cup [8] aromatic hydrocarbons mixture.
Get 0.1g HMX/ cup [8] aromatic hydrocarbons mixture and put into 100ml redistilled water, wash under 100 revs/min of magnetic agitation, cup in mixture [8] aromatic hydrocarbons is slowly dissolved, repeatedly repeated washing, cup [8] aromatic hydrocarbons in removing HMX/ cup [8] aromatic hydrocarbons mixture, filter, drying obtains ordered porous HMX.
Embodiment 4:
Preparation method's step of ordered porous RDX is as follows:
Be dissolved in 5ml nitrogen dimethylformamide under at room temperature getting the magnetic agitation condition that 0.1gRDX is 500 revs/min at rotating speed, be stirred to RDX and dissolve completely.
Getting 0.05g alpha-cylodextrin adds in solution, continues to stir, until alpha-cylodextrin dissolves completely.
Under the condition stirred, solution is added dropwise in 50ml redistilled water, and RDX/ alpha-cylodextrin mixture is slowly separated out, and continues stirring 30 minutes, and filter, vacuum-drying 12h at 50 DEG C, obtains RDX/ alpha-cylodextrin mixture.
Get 0.1gRDX/ alpha-cylodextrin mixture and put into 100ml redistilled water, wash under 100 revs/min of magnetic agitation, the alpha-cylodextrin in mixture is slowly dissolved, repeatedly repeated washing, alpha-cylodextrin in removing RDX/ alpha-cylodextrin mixture, filter, drying obtains ordered porous RDX.
Embodiment 5:
Preparation method's step of ordered porous PETN is as follows:
Be dissolved in 5ml nitrogen dimethylformamide under at room temperature getting the magnetic agitation condition that 0.1gPETN is 500 revs/min at rotating speed, be stirred to PETN and dissolve completely.
Getting 0.05g beta-cyclodextrin adds in solution, continues to stir, until beta-cyclodextrin dissolves completely.
Under the condition stirred, solution is added dropwise in 50ml redistilled water, and PETN/ beta-cyclodextrin mixture is slowly separated out, and continues stirring 30 minutes, and filter, vacuum-drying 12h at 50 DEG C, obtains PETN/ beta-cyclodextrin mixture.
Get 0.1g PETN/ beta-cyclodextrin mixture and put into 100ml redistilled water, wash under 100 revs/min of magnetic agitation, beta-cyclodextrin in mixture is slowly dissolved, repeatedly repeated washing, beta-cyclodextrin in removing PETN/ beta-cyclodextrin mixture, filter, drying obtains ordered porous PETN.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only the present invention's preferably embodiment, embodiments of the present invention are not restricted to the described embodiments, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (6)
1. an ordered porous preparation method containing energy crystalline material, is characterized in that comprising the following steps:
A. a certain amount of energetic material is at room temperature dissolved in the good solvent of energetic material;
B. in the solution of steps A, a certain amount of crystal morphology control agent is added, stirring and dissolving;
C. the solution of step B is joined slowly in redistilled water under the condition of magnetic agitation;
D., after the solution of step C being continued to stir certain hour, filter, obtain the mixture of energetic material and crystal morphology control agent;
E. join in redistilled water by the mixture of gained in step D; Repeatedly wash, removing crystal morphology control agent;
F. step e gained is filtered, dry, obtain pure ordered porous containing can crystalline material;
Described energetic material is the one in CL-20, HMX, RDX, PETN, FOX-7, AP.
2. a kind of ordered porous preparation method containing energy crystalline material according to claim 1, it is characterized in that described crystal morphology control agent is cup [4] aromatic hydrocarbons, cup [6] aromatic hydrocarbons, cup [8] aromatic hydrocarbons, dibenzo-18-crown-6 (DB18C6), alpha-cylodextrin, beta-cyclodextrin, the one in γ-cyclodextrin.
3. a kind of ordered porous preparation method containing energy crystalline material according to claim 1, is characterized in that the mass percentage of described crystal morphology control agent is 1%-50%.
4. a kind of ordered porous preparation method containing energy crystalline material according to claim 1, is characterized in that the rotating speed of described magnetic agitation is 100 revs/min-1000 revs/min.
5. according to claim 1 a kind of ordered porous containing can the preparation method of crystalline material, it is characterized in that the volume ratio of good solvent in poor solvent and steps A in described step C is greater than 5.
6. a kind of ordered porous preparation method containing energy crystalline material according to claim 1-5 any one, is characterized in that the ordered porous aperture containing energy crystalline material adopting described preparation method to prepare is 10-500nm.
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| CN104591936B (en) * | 2015-01-29 | 2016-09-21 | 中国工程物理研究院化工材料研究所 | Composite material containing energy based on three-dimensional ordered macroporous carbon skeleton and preparation method thereof |
| CN105503487B (en) * | 2016-01-26 | 2018-06-12 | 中国工程物理研究院化工材料研究所 | Nano-sheet 1,1- diamino -2,2- dinitro ethylene explosives and preparation method thereof |
| CN107353417B (en) * | 2017-06-08 | 2020-03-13 | 西安交通大学 | Preparation method of polymer nano material |
| CN110590565B (en) * | 2019-09-25 | 2023-03-10 | 中北大学 | Preparation method of highly-spheroidized 1,1-diamino-2,2-dinitroethylene crystal |
| CN113831300A (en) * | 2021-11-04 | 2021-12-24 | 中国兵器工业第二一三研究所 | Preparation method of initiating explosive 5-nitrotetrazole cuprous |
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| US6666935B1 (en) * | 1997-09-09 | 2003-12-23 | The Regents Of The University Of California | Sol-gel manufactured energetic materials |
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| US20100024933A1 (en) * | 2003-02-28 | 2010-02-04 | Stec Iii Daniel | Methods for making and using high explosive fills for very small volume applications |
| US8585840B2 (en) * | 2003-08-29 | 2013-11-19 | G.D.O., Inc. | Recovery of the energetic component from plastic bonded explosives |
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