CN103044173A - Method for preparing ordered porous energetic crystal material - Google Patents
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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 the energetic material field, be specifically related to a kind of ordered porous preparation method who contains the energy crystalline material.
Background technology
Ordered porous material is the novel nano structured material that rises rapidly the nineties in 20th century, and it obtains the great attention of international physics, chemistry and material educational circles once being born, and develops rapidly and become one of study hotspot interdisciplinary.Ordered porous material have duct size evenly, arrange in order, the characteristic such as can be regulated within the specific limits continuously in the aperture, has broad application prospects at aspects such as optical material, electronics and electro-optical assembly, vertical magnetism record material, biosensor, photocatalyst, sorbing material and medicine controlled releasings.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 that obtains large-scale application in fields such as civilian, military and space.Along with the development of nanotechnology, many new ideas are incorporated in the energetic material field, and its research work has been produced profound influence.Because the nano-porous structure of nano-porous materials has affected the physical and chemical process of material, such as mass transfer, heat transfer etc., so new vitality has been injected in the research that is combined into energetic material of nano-porous materials and energetic material.At first, people adopt the unordered gac of porous to come Treatment of TNT (2，4，6-trinitrotoluene) as sorbent material, waste water or the waste gas such as AP (perchloric acid is pressed), but research contents is confined to unordered porous material.Until the nineties in 20th century, the in a large number appearance of novel ordered porous material.Ordered porous material is applied to the energetic material field.2006, the selections such as Majano have the straight hole road, and ((the pure silicon MFI type molecular sieve of 0.51nm * 0.55nm) is material of main part for 0.53nm * 0.56nm) and Z-type duct, be used for adsorbing high energy density compound FOX-7 (1,1-diamino-2,2-dinitrobenzene ethene).The DSC test shows, compares (225 ℃ and 275 ℃ of exothermic peaks) with body phase material, and the thermostability of nano-scale FOX-7 strengthens (264 ℃ and 377 ℃ of exothermic peaks) in the duct.Fu etc. make supported catalyst with CuO nano particle high dispersing at the SBA-15 carrier, and when the interpolation quality was 1% catalyzer in the AP system, 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 the duct, preparation CL-20/SBA-15 Composite Energetic Materials.The DSC test result shows: the thermolysis peak value of CL-20 is at 240 ℃, and the CL-20/SBA-15 nano-complex is compared CL-20 and the mechanical mixture decomposition peak shifts to an earlier date, occur in 229 ℃, because it is little to be filled in the CL-20 granularity of SBA-15, the atomicity relative proportion on surface is larger, Surface atomic mobility is higher, under the same temperature condition, and easier generation decomposition reaction.
But above-mentioned research only is that porous structure material is applied to energetic material, compound as solid support material and energetic material the ordered porous structural material, porous material itself is not energetic material, skeleton is a kind of ordered porous Composite Energetic Materials with what obtain in experiment and use procedure, does not obtain the ordered porous energetic material that is made of energetic material self.So on the basis of ordered porous Composite Energetic Materials, if can in the situation that does not affect vesicular structure, deviate from not contain the solid support material of energy, just can obtain the energetic material of ordered porous structural.
The present invention under the induction regulating controlling effect of special tensio-active agent, prepares a kind of ordered porous energetic material that is made of energetic material self from the angle thinking of numerator self-assembly technique and crystal engineering.Ordered porous be conducive to energetic material the burning or the blast process in combustion wave and pressure propagation.
Summary of the invention
The object of the invention provides a kind of ordered porous preparation method who contains the energy crystalline material.Core content of the present invention is to add a kind of crystal morphology control agent in energetic material solvent-nonsolvent crystallisation process, and energetic material and crystal morphology control agent cocrystallization are removed the crystal morphology control agent again, have just formed ordered porous energetic material.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of ordered porous preparation method who contains the energy crystalline material is characterized in that may further comprise the steps:
A. a certain amount of energetic material at room temperature is dissolved in the optimum solvent of energetic material, makes energetic material can be dissolved in the optimum solvent fully;
B. add a certain amount of crystal morphology control agent in the solution of steps A, stirring and dissolving so that crystal morphology control agent and energetic material fully act on, is regulated and control the crystal morphology of energetic material;
C. the solution with step B joins under the condition of magnetic agitation in the poor solvent of energetic material and crystal morphology control agent slowly so that energetic material and crystal morphology control agent can be in bad solution crystallization obtain the mixture of energetic material and crystal morphology control agent;
D. the solution continuation of step C is stirred after the certain hour, filter, obtain the mixture of energetic material and crystal morphology control agent;
E. join in the solvent in the mixture with gained among the step D, described solvent is the poor solvent of energetic material, the optimum solvent of crystal morphology control agent, so that the crystal morphology control agent in the mixture of energetic material and crystal morphology control agent is dissolved in the solvent, energetic material is crystallization in solvent; Repeatedly washing so that can remove the crystal morphology control agent, obtains the high ordered porous energy crystalline material that contains of purity;
F. the step e gained is filtered, drying, 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.Because calixarene, crown ether, cyclodextrin all has unique void structure, easily organic with it energetic material molecule forms non covalent bond, thereby form supramolecular complex system in order complicated and that have specific function, thus calixarene, crown ether, cyclodextrin can be used as the crystal morphology control agent of energetic material, and the crystal morphology of energetic material is regulated and control into ordered porous containing can crystalline material.
Further, the quality percentage composition of described crystal morphology control agent is 1%-50%.
Further, the rotating speed of described magnetic agitation is 100 rev/mins-1000 rev/mins.
Further, among the described step C in poor solvent and the steps A volume ratio of optimum solvent greater than 5, with guarantee energetic material can and the crystal morphology control agent from step C, crystallize out completely the mixture of formation energetic material and crystal morphology control agent.
Further, adopting the ordered porous aperture that contains the energy crystalline material of described preparation method's preparation is 10-500nm.
The present invention is ordered porous contain can crystalline material preparation method's technical process simple, reaction conditions is gentle, reaction conditions is easy to control, is applicable to multiple energetic material, preparation ordered porous contain can crystalline material purity greater than 99.5%.
Description of drawings
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:
At room temperature get 0.1gCL-20 and under rotating speed is 500 rev/mins magnetic agitation condition, be dissolved in the 5ml nitrogen dimethylformamide, be stirred to CL-20 and dissolve fully.
Get 0.05g cup [4] aromatic hydrocarbons and add in the solution, continue to stir, until cup [4] aromatic hydrocarbons dissolves fully.
Under the condition that stirs, solution is added dropwise in the 50ml redistilled water, CL-20/ cup [4] aromatic hydrocarbons mixture is slowly separated out.Continue to stir 30 minutes, filter, at 50 ℃ of lower vacuum-drying 12h, obtain CL-20/ cup [4] aromatic hydrocarbons mixture.
Get 0.1gCL-20/ cup [4] aromatic hydrocarbons mixture and put into the 100ml redistilled water, under 100 rev/mins of magnetic agitation, wash, cup [4] aromatic hydrocarbons in the mixture is slowly dissolved, repeated washing repeatedly, remove cup [4] aromatic hydrocarbons in CL-20/ cup [4] the aromatic hydrocarbons mixture, filter, drying obtains ordered porous CL-20.
Fig. 1 is 2000 times of SEM figure of ordered porous CL-20, and Fig. 2 is 6000 times of SEM figure of ordered porous CL-20, 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:
At room temperature get 0.1g CL-20 and under rotating speed is 500 rev/mins magnetic agitation condition, be dissolved in the 5ml nitrogen dimethylformamide, be stirred to CL-20 and dissolve fully.
Get the 0.05g beta-cyclodextrin and add in the solution, continue to stir, until beta-cyclodextrin dissolves fully.
Under the condition that stirs, solution is added dropwise in the 50ml redistilled water, CL-20/ beta-cyclodextrin mixture is slowly separated out, and continues to stir 30 minutes, filters, and at 50 ℃ of lower vacuum-drying 12h, obtains CL-20/ beta-cyclodextrin mixture.
Get 0.1gCL-20/ beta-cyclodextrin mixture and put into the 100ml redistilled water, under 100 rev/mins of magnetic agitation, wash, beta-cyclodextrin in the mixture is slowly dissolved, repeated washing repeatedly, remove the beta-cyclodextrin in the 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:
At room temperature get 0.1gHMX and under rotating speed is 500 rev/mins magnetic agitation condition, be dissolved in the 5ml nitrogen dimethylformamide, be stirred to HMX and dissolve fully.
Get 0.05g cup [8] aromatic hydrocarbons and add in the solution, continue to stir, until cup [8] aromatic hydrocarbons dissolves fully.
Under the condition that stirs, solution is added dropwise in the 50ml redistilled water, CL-20/ cup [8] aromatic hydrocarbons mixture is slowly separated out, and continues to stir 30 minutes, filters, and at 50 ℃ of lower vacuum-drying 12h, obtains HMX/ cup [8] aromatic hydrocarbons mixture.
Get 0.1g HMX/ cup [8] aromatic hydrocarbons mixture and put into the 100ml redistilled water, under 100 rev/mins of magnetic agitation, wash, cup [8] aromatic hydrocarbons in the mixture is slowly dissolved, repeated washing repeatedly, remove cup [8] aromatic hydrocarbons in HMX/ cup [8] the aromatic hydrocarbons mixture, filter, drying obtains ordered porous HMX.
Embodiment 4:
Preparation method's step of ordered porous RDX is as follows:
At room temperature get 0.1gRDX and under rotating speed is 500 rev/mins magnetic agitation condition, be dissolved in the 5ml nitrogen dimethylformamide, be stirred to RDX and dissolve fully.
Get the 0.05g alpha-cylodextrin and add in the solution, continue to stir, until alpha-cylodextrin dissolves fully.
Under the condition that stirs, solution is added dropwise in the 50ml redistilled water, RDX/ alpha-cylodextrin mixture is slowly separated out, and continues to stir 30 minutes, filters, and at 50 ℃ of lower vacuum-drying 12h, obtains RDX/ alpha-cylodextrin mixture.
Get 0.1gRDX/ alpha-cylodextrin mixture and put into the 100ml redistilled water, under 100 rev/mins of magnetic agitation, wash, the alpha-cylodextrin in the mixture is slowly dissolved, repeated washing repeatedly, remove the alpha-cylodextrin in the RDX/ alpha-cylodextrin mixture, filter, drying obtains ordered porous RDX.
Embodiment 5:
Preparation method's step of ordered porous PETN is as follows:
At room temperature get 0.1gPETN and under rotating speed is 500 rev/mins magnetic agitation condition, be dissolved in the 5ml nitrogen dimethylformamide, be stirred to PETN and dissolve fully.
Get the 0.05g beta-cyclodextrin and add in the solution, continue to stir, until beta-cyclodextrin dissolves fully.
Under the condition that stirs, solution is added dropwise in the 50ml redistilled water, PETN/ beta-cyclodextrin mixture is slowly separated out, and continues to stir 30 minutes, filters, and at 50 ℃ of lower vacuum-drying 12h, obtains PETN/ beta-cyclodextrin mixture.
Get 0.1g PETN/ beta-cyclodextrin mixture and put into the 100ml redistilled water, under 100 rev/mins of magnetic agitation, wash, beta-cyclodextrin in the mixture is slowly dissolved, repeated washing repeatedly, remove the beta-cyclodextrin in the PETN/ beta-cyclodextrin mixture, filter, drying obtains ordered porous PETN.
Although invention has been described with reference to explanatory embodiment of the present invention here, above-described embodiment only is the better embodiment of the present invention, 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 modification and embodiments, and these are revised and embodiment will drop within the disclosed principle scope and spirit of the application.
Claims (7)
- One kind ordered porous contain can crystalline material the preparation method, it is characterized in that may further comprise the steps:A. a certain amount of energetic material at room temperature is dissolved in the optimum solvent of energetic material;B. in the solution of steps A, add a certain amount of crystal morphology control agent, stirring and dissolving;C. the solution of step B is joined slowly the poor solvent of energetic material and crystal morphology control agent under the condition of magnetic agitation;D. the solution continuation of step C is stirred after the certain hour, filter, obtain the mixture of energetic material and crystal morphology control agent;E. join in the solvent in the mixture with gained among the step D, described solvent is the poor solvent of energetic material, the optimum solvent of crystal morphology control agent; Repeatedly the crystal morphology control agent is removed in washing;F. the step e gained is filtered, drying, obtaining pure ordered porous containing can crystalline material.
- According to claim 1 a kind of ordered porous contain can crystalline material the preparation method, it is characterized in that described energetic material is a kind of among CL-20, HMX, RDX, PETN, FOX-7, the AP.
- 3. a kind of ordered porous preparation method who contains the energy crystalline material according to claim 1 is characterized in that described crystal morphology control agent is cup [a 4] aromatic hydrocarbons, cup [6] aromatic hydrocarbons, cup [8] aromatic hydrocarbons, dibenzo-18-crown-6 (DB18C6), alpha-cylodextrin, beta-cyclodextrin, a kind of in the γ-cyclodextrin.
- According to claim 1 a kind of ordered porous contain can crystalline material the preparation method, the quality percentage composition that it is characterized in that described crystal morphology control agent is 1%-50%.
- According to claim 1 a kind of ordered porous contain can crystalline material the preparation method, the rotating speed that it is characterized in that described magnetic agitation is 100 rev/mins-1000 rev/mins.
- According to claim 1 a kind of ordered porous contain can crystalline material the preparation method, it is characterized in that among the described step C that the volume ratio of optimum solvent is greater than 5 in the poor solvent and steps A.
- 7. the described a kind of ordered porous preparation method who contains the energy crystalline material of any one is characterized in that adopting the ordered porous aperture that contains the energy crystalline material of described preparation method's preparation is 10-500nm according to claim 1-6.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104591936A (en) * | 2015-01-29 | 2015-05-06 | 中国工程物理研究院化工材料研究所 | Energetic composite material based on three-dimensional ordered macroporous carbon skeleton and preparation method of energetic composite material |
| CN105503487A (en) * | 2016-01-26 | 2016-04-20 | 中国工程物理研究院化工材料研究所 | Nanometer flaky 1,1-diamido-2,2-binitro ethylene explosive and preparation method thereof |
| CN107353417A (en) * | 2017-06-08 | 2017-11-17 | 西安交通大学 | The preparation method of polymer nano material |
| CN110590565A (en) * | 2019-09-25 | 2019-12-20 | 中北大学 | Method for preparing highly-sphericized 1,1-diamino-2,2-dinitroethylene crystals |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104591936A (en) * | 2015-01-29 | 2015-05-06 | 中国工程物理研究院化工材料研究所 | Energetic composite material based on three-dimensional ordered macroporous carbon skeleton and preparation method of energetic composite material |
| CN105503487A (en) * | 2016-01-26 | 2016-04-20 | 中国工程物理研究院化工材料研究所 | Nanometer flaky 1,1-diamido-2,2-binitro ethylene explosive and preparation method thereof |
| CN107353417A (en) * | 2017-06-08 | 2017-11-17 | 西安交通大学 | The preparation method of polymer nano material |
| CN107353417B (en) * | 2017-06-08 | 2020-03-13 | 西安交通大学 | Preparation method of polymer nano material |
| CN110590565A (en) * | 2019-09-25 | 2019-12-20 | 中北大学 | Method for preparing highly-sphericized 1,1-diamino-2,2-dinitroethylene crystals |
| 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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