CN103980075B - The preparation method with micro-nano multi-level structure explosive - Google Patents
The preparation method with micro-nano multi-level structure explosive Download PDFInfo
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Abstract
The invention discloses a kind of preparation method with micro-nano multi-level structure explosive, comprise the following steps: step one: the preparation of the explosive of micro-nano primary structure, prepared the solvent adduct of explosive and solvent by the mode of solvation, make solvent adduct decompose again through external forces and remove the explosive that solvent obtains having micro-nano primary structure; Step 2: utilize heated solvent mode to form the solvent vapo(u)r explosive to micro-nano primary structure and carry out the solvent adduct that secondary solvent obtains having micro-nano structure, make the solvent adduct secondary desolvation with micro-nano structure obtain the explosive with micro-nano secondary structure again through external forces; Step 3: namely the operation of repetition step 2 obtains the explosive with micro-nano multi-level structure. This method adopts repeatedly solvation-desolvation method that explosive molecules recurring structure is recombinated, and then obtains the explosive crystal structure with multi-layer micro-nano structure, hence it is evident that improve the explosion transfer performance that detonates of explosive.
Description
Technical field
The invention belongs to the design of explosive material micro structure and regulation and control method, be specifically related to a kind of preparation method with micro-nano multi-level structure explosive, the method adopts repeatedly solvation-desolvated method acquisition to have micro-nano multi-level structure explosive.
Background technology
Material microstructure is closely related with its macro property. As special energetic material, the micro structure of explosive is also determine the most important factor of its physicochemical characteristics. Research shows, the microstructure features such as blasting explosive granules size and distribution, specific surface area, exterior appearance, pore-size, reunion state and crystalline structure, not only affects its macro-mechanical property, has an effect on its response sensitivity to particular stimulation. Change such as pore-size and distribution may make explosive initiation sensitivity change, and granularity change can cause the performances such as the output of shock sensitivity, mechanical sensitivity, energy, detonation energy and thermostability to produce to change. Therefore, by changing explosive microstructure, it is achieved the improvement of some particular characteristic or the lifting of combination property become the focus of current explosive area research.
In the means of existing explosive regulating microstructure, mainly there is two ways, one is reduce crystalline mi defect, obtain high-quality explosive crystal, feel HMX (HMX) as Kr �� ber etc. utilizes recrystallization method to obtain dropping of different micro structure, and confirm that its shock sensitivity and detonation energy tool improve significantly.But, though high-quality explosive reduces shock sensitivity to a certain extent, but mechanical sensitivity is not well improved, and does not also have bigger lifting in the explosion transfer performance that detonates. Another kind is then by reducing grain graininess, increases explosive specific surface area so that it is structure micro-nano. Research shows, has the explosive crystal of micro-nano structure, and the difference of its micro structure stimulates the response of (such as the mechanical stimulus under thermostimulation, low pressure long pulse, shock wave stimulation etc. under high pressure-burst pulse) significantly different to external world. Schoenitz etc. confirm explosive structure micro-nanos such as HMX, and its total specific surface area enlarges markedly, surface activity atom and group increase, and is more beneficial for the propagation of explosion that detonates. It is improve the explosive important channel to particular stimulation response sensitivity that visible acquisition has the explosive crystal of micro-nano structure. And micro-nano multi-level structure is a kind of with low dimensional nano-particle for construction unit, self assembly or artificially assemble the multi-layer three-dimensional composite micro-nano structure with special appearance and structure obtained. Owing to the energetic material of this structure has the hole of wider distribution, the granule of different scale, specific surface area is bigger, has a very important role for detonating of explosive and propagation of explosion stability. Therefore, for realizing the reliable initiation of explosive and stable propagation of explosion, the regulation and control of explosive microstructure are realized by diverse ways, it is thus achieved that micro-nano multi-level structure is crucial.
The present invention aims at the design to explosive micro structure and regulation and control just, utilizes the solvation effect of explosive and solvent, utilizes repeatedly solvation-desolvation method, it is thus achieved that have the explosive crystal material of micro-nano multi-level structure. This method can design the multilevel hierarchy of different dimensions according to actual needs, and by the multilevel hierarchy explosive of relevant desolvation processing mode acquisition variable grain yardstick, this micro-nano multi-level structure can realize the improvement of explosive property.
Summary of the invention
It is an object of the invention to provide a kind of preparation method with micro-nano multi-level structure explosive, this preparation method adopts repeatedly the micro structure of solvation-desolvated method regulation and control explosive, hence it is evident that improve the micro structure of explosive.
In order to reach above-mentioned technique effect, the present invention takes techniques below scheme:
A kind of preparation method with micro-nano multi-level structure explosive, comprises the following steps:
Step one: the preparation of the explosive of micro-nano primary structure, prepares the solvent adduct of explosive and solvent by the mode of solvation, makes solvent adduct decompose again through external forces and removes the explosive that solvent obtains having micro-nano primary structure; The solvent adduct crystal that will obtain in this step, take the mode such as heat, chemical force separately or cooperatively to act on and bring it about decomposition, remove part or all of solvent molecule, the explosive molecules generation crystal structure in solvent adduct is promoted to reset, when solid-phase crystallization, the limited growth of crystal obtains the explosive micro-nano primary structure with certain mode of appearance.
Step 2: utilize heated solvent mode to form the solvent vapo(u)r explosive to micro-nano primary structure and carry out the solvent adduct that secondary solvent obtains having micro-nano primary structure, make the solvent adduct secondary desolvation with micro-nano structure obtain the explosive with micro-nano secondary structure again through external forces; Again assemble under the solvation of solvent vapo(u)r and form the solvent adduct with micro-nano primary structure, the solvent adduct with micro-nano primary structure occurs desolvation to decompose again under the action conditions such as heat, chemical force, remove solvent molecule therein, limited by growing environment, explosive molecules in micro-nano primary structure will be reset by recurring structure again, forms the micro-nano secondary structure of explosive.
Step 3: namely the operation of repetition step 2 obtains the explosive with micro-nano multi-level structure.
In above-mentioned preparation method, described solvent adduct is the co-crystallization compound that explosive molecules is formed when weak interaction force with solvent molecule.
In above-mentioned preparation method, described weak interaction force is one or more in hydrogen bond, electrostatic force, Van der Waals force.
In above-mentioned preparation method, described external forces is the one in heat, pressure and chemical force.
In above-mentioned preparation method, described solvent vapo(u)r is the solvent molecule of gaseous form.
In above-mentioned preparation method, described heated solvent mode is the one in water-bath, oil bath and electrical heating.
The present invention compared with prior art, has following beneficial effect:
This method adopts repeatedly solvation-desolvation method that explosive molecules recurring structure is recombinated, and then obtains the explosive crystal structure with multi-layer micro-nano structure, hence it is evident that improve the explosion transfer performance that detonates of explosive.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of HNS explosive in embodiment 1, and wherein a represents HNS explosive crystal; B represents the solvent adduct crystal of HNS and dioxane (Dioxane); C is HNS micro-nano primary structure; D represents HNS and the Dioxane solvent adduct with micro-nano primary structure; E is HNS micro-nano secondary structure; F is HNS and the Dioxane solvent adduct with micro-nano secondary structure; G is HNS micro-nano tertiary structure.
Fig. 2 is the XRD figure of HNS explosive in embodiment 1, and a represents HNS former state XRD figure; B represents the XRD figure of HNS and Dioxane solvent adduct; C represents the XRD figure with micro-nano primary structure HNS; D represents the XRD figure of HNS and the Dioxane solvent adduct with micro-nano primary structure; E represents the XRD figure with micro-nano secondary structure HNS; F represents the XRD figure of HNS and the Dioxane solvent adduct with micro-nano secondary structure; G represents the XRD figure of the HNS with micro-nano multi-level structure.
Fig. 3 is the shape appearance figure of HMX explosive in embodiment 2, and wherein a represents the solvent adduct crystal of HMX and DMF (DMF); B is HMX micro-nano primary structure; C is the HMX with one-level micro-nano structure and DMF solvent adduct; D is HMX micro-nano secondary structure; E is the HMX with micro-nano secondary structure and DMF solvent adduct; F is HMX micro-nano tertiary structure.
Fig. 4 is the XRD figure of HMX explosive in embodiment 2, and a represents HMX former state XRD figure; B represents the XRD figure of HMX and DMF solvent adduct; C represents the XRD figure with micro-nano primary structure HMX; D represents the XRD figure of HMX and the DMF solvent adduct with micro-nano primary structure; E represents the XRD figure with micro-nano secondary structure HMX; F represents the XRD figure of HMX and the DMF solvent adduct with micro-nano secondary structure; G represents the XRD figure of the HMX with micro-nano multi-level structure.
Detailed description of the invention
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
(1) HNS of 1.25g is weighed, it is dissolved in the there-necked flask of dioxane (Dioxane) of 250mL, it is completely dissolved under 70 DEG C��85 DEG C stirred in water bath states, after stablizing 1h, water-bath is carried out cooling recrystallization by opening program temperature control, precipitate out solvent adduct crystal gradually, when continuing stirring 2h after near 15 DEG C��20 DEG C of temperature, until crystal precipitates out completely; It is then passed through vacuum filtration and obtains solvent adduct crystal.
(2) the solvent adduct crystal that step (1) obtains is placed in the vacuum drying oven of 75 DEG C��100 DEG C, heat resolve removes the solvent molecule in solvent adduct, unlatching vacuum pump is bled, and can obtain the HNS explosive with micro-nano primary structure after heat treatment 2h.
(3) the HNS explosive with micro-nano primary structure step (2) obtained is evenly laid out in the nylon wire that size of mesh opening is 200 ��m (60 order��80 order) left and right, it is placed in, just on the Dioxane solution of 80 DEG C��95 DEG C heating, utilizing Dioxane solvent vapo(u)r to carry out again the HNS solvent adduct that solvation obtains having micro-nano primary structure.
(4) the HNS solvent adduct with micro-nano primary structure that step (3) obtains is again placed in the vacuum drying oven of 75 DEG C��100 DEG C, open vacuum suction and be heated desolvation, after 2h, obtain the HNS explosive with micro-nano secondary structure.
(5) solvation-go solvent can obtain the micro-nano multi-level structure of HNS is carried out repeatedly according to step (3), step (4).
(6) sample that step (2), step (3), step (4), step (5) obtain carries out structure and exterior appearance analysis, and HNS shape appearance figure and XRD figure refer to Fig. 1 and Fig. 2.
Embodiment 2:
(1) HMX of 5g is weighed, it is dissolved in the there-necked flask of DMF of 45ml, in 65 DEG C��85 DEG C water-baths, it is completely dissolved under stirring, dissolve and after completely, stablize opening program temperature control after 1h, water-bath is carried out cooling recrystallization, progressively the solvent adduct crystal of precipitation HMX and DMF, after temperature constant 2h, vacuum cycle pump sucking filtration is utilized to obtain solvent adduct crystal.
(2) the solvent adduct crystal that step (1) obtains it is placed in the vacuum drying oven of 80 DEG C��120 DEG C and opens vacuum suction, solvent adduct is carried out pyrolysis desolvation, after heat treatment 2h��4h, obtains the HMX explosive with micro-nano primary structure.
(3) the HMX explosive with micro-nano primary structure step (2) obtained is evenly laid out in the nylon wire that size of mesh opening is 200 ��m (60 order��80 order) left and right, it is placed in just utilizing water-bath on the DMF solution of 110 DEG C��140 DEG C heating, utilizes DMF solvent steam to carry out again solvation and assemble the HMX solvent adduct obtaining there is micro-nano primary structure.
(4) the HMX solvent adduct with micro-nano primary structure that step (3) obtains it is again placed in the vacuum drying oven of 80 DEG C��120 DEG C and opens vacuum suction, solvent adduct is carried out pyrolysis desolvation, obtains the HMX explosive with micro-nano secondary structure through Overheating Treatment 2h��3h.
(5) according to step (3), step (4), HMX explosive is carried out repeatedly solvation-desolvation and can obtain the micro-nano multi-level structure of HMX.
(6) sample that step (2), step (3), step (4), step (5) obtain carries out structure and exterior appearance analysis, and HMX shape appearance figure (SEM) and XRD figure refer to Fig. 3 and Fig. 4.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, above-described embodiment is only the present invention preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, should be appreciated that, those skilled in the art can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (6)
1. a preparation method with micro-nano multi-level structure explosive, it is characterised in that comprise the following steps:
Step one: the preparation of the explosive of micro-nano primary structure, prepares the solvent adduct of explosive and solvent by the mode of solvation, makes solvent adduct decompose again through external forces and removes the explosive that solvent obtains having micro-nano primary structure;
Step 2: utilize heated solvent mode to form the solvent vapo(u)r explosive to micro-nano primary structure and carry out the solvent adduct that secondary solvent obtains having micro-nano structure, make the solvent adduct secondary desolvation with micro-nano structure obtain the explosive with micro-nano secondary structure again through external forces;
Step 3: namely the operation of repetition step 2 obtains the explosive with micro-nano multi-level structure.
2. the preparation method with micro-nano multi-level structure explosive according to claim 1, it is characterised in that described solvent adduct is the co-crystallization compound that explosive molecules is formed when weak interaction force with solvent molecule.
3. the preparation method with micro-nano multi-level structure explosive according to claim 2, it is characterised in that described weak interaction force is one or more in hydrogen bond, electrostatic force, Van der Waals force.
4. the preparation method with micro-nano multi-level structure explosive according to claim 1, it is characterised in that described external forces is the one in heat, pressure and chemical force.
5. the preparation method with micro-nano multi-level structure explosive according to claim 1, it is characterised in that described solvent vapo(u)r is the solvent molecule of gaseous form.
6. the preparation method with micro-nano multi-level structure explosive according to claim 1, it is characterised in that described heated solvent mode is the one in water-bath, oil bath and electrical heating.
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| CN106966841B (en) * | 2017-03-29 | 2018-07-31 | 西安近代化学研究所 | A kind of press fitting powder column circumferential crack method for prefabricating |
| CN107827835B (en) * | 2017-11-22 | 2021-09-28 | 中国工程物理研究院化工材料研究所 | Simple preparation method of explosive solvate |
| CN111908990B (en) * | 2020-07-17 | 2021-07-09 | 中北大学 | Energetic material filled layered framework composite structure and preparation method thereof |
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