CN110937960B - Preparation method of host-guest explosive for in-situ self-assembly of ozone molecules - Google Patents
Preparation method of host-guest explosive for in-situ self-assembly of ozone molecules Download PDFInfo
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- 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
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/10—Preparation of ozone
- C01B13/11—Preparation of ozone by electric discharge
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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
The invention discloses a method for preparing a host-guest explosive by in-situ self-assembly of ozone molecules, which comprises the steps of cooperatively filling oxygen molecules and HNIW into a cavity of a pressurizing device, preparing the ozone molecules in situ by utilizing pulse point discharge, and embedding the ozone molecules into HNIW unit cells by pressurizing, thereby obtaining the host-guest explosive by self-assembly of HNIW and ozone molecules. The method of the invention enables oxygen molecules to generate ozone molecules in situ in a pressurizing device through the point discharge of the pulse electrode, and enables the ozone molecules to be embedded into HNIW explosive unit cells in situ through pressurization, thereby effectively solving the problem of short half-life period of the ozone molecules, enabling the ozone molecules to be embedded into the explosive unit cells after in situ synthesis, realizing the high-efficiency and high-content embedding of the ozone molecules, and obtaining HNIW and O in the host-guest explosive3The molar ratio of the molecules reaches 2: 1.
Description
Technical Field
The invention relates to the technical field of preparation methods of high-energy explosives, in particular to a preparation method of a host-guest explosive for in-situ self-assembly of ozone molecules.
Background
The energy and safety of energetic materials directly determine the performance level of weapons. Hexanitrohexaazaisowurtzitane (HNIW or CL-20) has been put to practical useThe molecular formula of the elementary explosive with the highest energy is C6H6N12O12The epsilon-HNIW detonation velocity with the highest density and energy reaches 9450 m.s-1The explosion velocity of alpha-HNIW is also close to 9280 m.s-1. HNIW not only has very high energy, also has good detonating and detonating properties. Therefore, the HNIW is used as a base for carrying out structure optimization and performance improvement, and the performance of the explosive can be greatly improved.
Scholars at home and abroad have developed various technical means for regulating and controlling the performance of HNIW, such as crystal quality improvement, explosive crystal surface modification and coating, energetic eutectic preparation and the like, and the methods can reduce the sensitivity of HNIW to a certain extent, but also obviously reduce the energy density of HNIW. For example, HNIW is capable of forming energetic eutectics with a variety of solvents or explosives, but due to the introduction of non-energetic components or lower energy components and the induced cell re-packing during the formation of eutectics with HNIW, the crystal packing density is reduced, which in turn leads to a significant reduction in the detonation performance of the modified HNIW explosive. For this reason, new technical means are needed to realize further improvement of HNIW energy density.
The pressure, one of the external variables with the greatest range of variation, can become the "catalyst" for new chemical and bonding reactions that do not exist at normal pressure, thus opening a new door for the discovery of new energetic materials and the creation of new synthetic methods. The high pressure can change the atom distance to cause the change of the physical property of the explosive, and simultaneously can change the bonding property of atoms through regulating and controlling the atomic energy level to generate a brand new chemical reaction mode to generate a novel explosive which can not be synthesized under normal pressure. For example, hydrogen helium reaction, CO and N2The reaction to form high-energy compounds cannot be carried out under the conventional conditions, but the high-pressure confinement effect is a material which can cross the reaction energy barrier to synthesize a novel structure. The preparation of novel energetic materials under extreme conditions is carried out by utilizing a high-pressure means, active oxygen-enriched micromolecules are embedded into the explosive unit cells in a self-assembly manner to form host-guest explosive crystals, the space complementarity and the charge complementation characteristics between the host and the guest are fully utilized, the dense accumulation of molecules is realized, and thus, the high density and the specificity are obtainedThe energetic host-guest explosive crystal can realize the performance regulation and control of the explosive while keeping high energy density.
Patent CN106810409B discloses a method for preparing an embedded host-guest explosive crystal based on a gas replacement technology, which comprises using CL-20-based solvate as an initial template, purging the solvate crystal with gas molecules, inducing the replacement of the gas molecules with the solvent guest molecules in the solvate, and performing molecular stacking rearrangement to obtain the host-guest explosive crystal with the gas molecules embedded in the unit cell. Although this method allows the insertion of a variety of small gas molecules into the explosive cell under mild experimental conditions, the gas purge time in this method is typically several hours or more, whereas ozone molecules suffer from the short half-life and decompose to form O before insertion2Molecule, resulting in no HNIW/O available3The amount of crystal or intercalation of the host-guest explosive is small, and therefore, a technology for preparing the host-guest explosive capable of efficiently intercalating ozone molecules into the interior of unit cells in situ needs to be explored.
Disclosure of Invention
The invention overcomes the defects of the prior art, provides the preparation method of the host-guest explosive with in-situ self-assembled ozone molecules, obtains the host-guest explosive crystals with compact crystal stacking structures and excellent safety performance, effectively solves the preparation problem that the self-assembly of the ozone molecules is difficult to embed into explosive unit cells due to short half-life period of the ozone molecules, is beneficial to batch preparation, and is convenient for subsequent product processing, forming and use.
In order to achieve the technical effects, the invention provides a method for preparing a host-guest explosive by in-situ self-assembly of ozone molecules, which is characterized in that oxygen molecules and HNIW are cooperatively arranged in a cavity of a pressurizing device, ozone molecules are prepared in situ by pulse point discharge, and then the ozone molecules are embedded into HNIW unit cells through pressurization, so that the host-guest explosive by self-assembly of HNIW and ozone molecules is obtained.
The more specific technical scheme of the invention is as follows:
the preparation method of the host-guest explosive for in-situ self-assembly of ozone molecules comprises the following steps:
the method comprises the following steps: filling HNIW and oxygen into the cavity of the pressurizing device simultaneously;
step two: adding a tip electrode into the cavity of the pressurizing device, accessing electric field pulse, instantaneously forming an electric field enough for ionizing oxygen molecules at the tip, and preparing ozone molecules in situ through oxygen molecule ionization;
step three: continuously applying pressure to HNIW and ozone in the cavity of the pressurizing device, so that ozone molecules are embedded into HNIW unit cells under the driving of high pressure, and the host-guest explosive self-assembled by HNIW and ozone molecules can be obtained.
In the above method for preparing the host-guest explosive of in-situ self-assembled ozone molecules, the pressurizing device is selected from one of a diamond anvil cell and a large press, but is not limited to the listed devices.
In the preparation method of the host-guest explosive of in-situ self-assembled ozone molecules, the HNIW and the oxygen are filled in the cavity of the pressurizing device simultaneously, and the packaging mode is that liquid helium or liquid nitrogen is adopted to liquefy the oxygen in the corrosion-resistant tank body, then the pressurizing device filled with the HNIW is placed in the tank body, the liquefied oxygen in the tank body flows into the cavity of the pressurizing device through a gap reserved between a sleeve and a plunger in the pressurizing device, then a screw of the pressurizing device is fastened in situ in a low-temperature environment, and the oxygen and the HNIW are filled in the cavity after being pressurized to a certain pressure; the certain pressure is 0.3 GPa-1.5 GPa.
In the preparation method of the host-guest explosive of in-situ self-assembled ozone molecules, the electric field voltage of the point discharge is between 0.5eV and 10 eV.
In the preparation method of the host-guest explosive of in-situ self-assembled ozone molecules, a laser auxiliary loading mode is adopted in the second step, wherein a laser beam generated by a laser is transmitted into the cavity through the diamond position of the pressurizing device to perform a laser auxiliary effect on the oxygen molecules in the cavity, so that the preparation efficiency of ozone is further improved, and the laser power is controlled to be between 1mW and 50 mW.
In the preparation method of the host-guest explosive of the in-situ self-assembled ozone molecules, the pressure applied to HNIW and ozone in the cavity of the pressurizing device in the third step is between 0.5GPa and 15 GPa.
In the preparation method of the host-guest explosive of in-situ self-assembled ozone molecules, HNIW and ozone in the cavity of the pressurizing device are heated while applying pressure, and the heating temperature is controlled to be between 40 and 80 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method of the invention enables oxygen molecules to generate ozone molecules in situ in a pressurizing device through the point discharge of the pulse electrode, and enables the ozone molecules to be embedded into HNIW explosive unit cells in situ through pressurization, thereby effectively solving the problem of short half-life period of the ozone molecules, enabling the ozone molecules to be embedded into the explosive unit cells after in situ synthesis, realizing the high-efficiency and high-content embedding of the ozone molecules, and obtaining HNIW and O in the host-guest explosive3The molar ratio of the molecules reaches 2: 1.
(2) the host-guest explosive prepared by the method has a compact unit cell stacking structure, and the crystal density is as high as 2.039g.cm at room temperature-3The energy density loss of HNIW is effectively reduced; the effective active oxygen atoms provided by the ozone molecules greatly improve the oxygen balance of the HNIW explosive, and the oxygen balance is increased from-10.96% to-5.48%, so that the HNIW explosive is more completely oxidized, the released energy and gas content are increased, and the detonation performance of the explosive is effectively improved; in addition, compared with the raw material HNIW, the HNIW and the ozone molecule self-assembled host-guest explosive have the characteristic of high H50The HNIW is improved from 20.3cm to 35.2cm, and the high-efficiency reduction of the HNIW is realized. The method can provide a new technical approach for the performance regulation of HNIW-based explosive and the preparation of high-energy low-sensitivity explosive.
Drawings
FIG. 1 is HNIW/O3A flow chart of a preparation method of the host-guest explosive.
FIG. 2 is a pulsed electric field in situ synthesis of O3Schematic representation of (a).
FIG. 3 is HNIW/O3The structure diagram of the unit cell stack of the host-guest explosive.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Example 1
FIG. 1 is a HNIW/O of the present invention3A flow chart of a preparation method of the host-guest explosive.
(1) Weighing 1g of HNIW explosive powder, filling the HNIW explosive powder into a sample cavity of a large press, combining a plunger and a sleeve of the large press together, simultaneously leaving a small amount of gaps, and then putting the HNIW explosive powder into a copper tank body and covering a cover of the copper tank;
(2) putting the tank body into liquid nitrogen, introducing oxygen into the tank body by using an air inlet above a cover, gradually liquefying the oxygen at low temperature, closing an oxygen valve after the liquid oxygen is over a large press, then opening the cover of the tank body, screwing a pressurizing screw on the large press, packaging the liquid oxygen flowing into the large press in a sample cavity containing HNIW explosive, characterizing the anvil cell pressure value by using a laser pressing instrument, and displaying the pressure at the moment to be 0.8 GPa;
(3) turning on a power supply of a tip electrode laid in a sample cavity of a large press in advance, starting electric field pulse, instantly discharging at the tip to form an electric field, controlling the voltage of the electric field to be 0.5eV, starting for 120 seconds, and irradiating a laser beam of a solid laser aiming at a sample while starting the electric field with the irradiation power of 50 mW;
(4) and (3) continuing symmetrically screwing the pressure screws on the large press until the pressure value of the large press reaches 5GPa, standing for 50min, unscrewing the pressure screws, and taking out the sample to obtain the HNIW and ozone molecule self-assembled host-guest explosive.
FIG. 2 shows the in-situ synthesis of O by pulsed electric field3Schematic representation of (a). Adopts differential scanning calorimetry-thermal weight loss combined instrument (DSC-TG) to HNIW/O3Analyzing the thermal performance of the explosive of the host and the object, and obtaining HNIW and O according to the weight loss calculation3In a molar ratio of 2: 1. Subject-object explosive by density gradient methodThe density of the explosive can reach 2.039g.cm-3. Performing structure refinement on the crystal structure of the host-guest explosive to obtain HNIW/O3The unit cell stacking structure of the host-guest explosive is shown in fig. 3. The impact sensitivity of the host-guest explosive crystal is characterized by utilizing an H3.5-10W type spherical drop hammer instrument (with the weight of 2kg), and the result shows that the characteristic drop height H of the raw material HNIW5020.3cm, and the characteristic falling height H of the subject-guest explosive50The height is increased to 35.2cm, the safety performance is better, and the HNIW is effectively reduced.
Example 2
(1) Weighing 1g of HNIW explosive powder, filling the HNIW explosive powder into a sample cavity of a large press, combining a plunger and a sleeve of the large press together, simultaneously leaving a small amount of gaps, and then putting the HNIW explosive powder into a copper tank body and covering a cover of the copper tank;
(2) putting the tank body into liquid helium, introducing oxygen into the tank body by using an air inlet above a cover, gradually liquefying the oxygen at low temperature, closing an oxygen valve after the liquid oxygen submerges the large press, then opening the cover of the tank body, screwing a pressurizing screw on the large press, so that the liquid oxygen flowing into the large press is encapsulated in a sample cavity containing explosive, characterizing the anvil pressure value by using a laser pressing instrument, and displaying the pressure at the moment as 1 GPa;
(3) turning on a power supply of a tip electrode laid in a sample cavity of a large press in advance, starting electric field pulse, instantly discharging at the tip to form an electric field, controlling the voltage of the electric field to be 10eV, and starting the electric field for 20 seconds, and irradiating a laser beam of a solid laser aiming at a sample while starting the electric field with the irradiation power of 1 mW; the laser auxiliary loading mode is adopted, and the laser beam generated by the laser enters the cavity through the transmission of the diamond position of the pressurizing device, so that the oxygen molecules in the cavity are subjected to laser auxiliary action, and the ozone preparation efficiency is further improved.
(4) And then heating a sample chamber of the large press by using a heating sleeve, controlling the temperature at 50 ℃, continuously and symmetrically screwing the pressurizing screws on the large press until the pressure value of the large press reaches 10GPa, standing for 40min, unscrewing the pressurizing screws, and taking out the sample to obtain the HNIW and ozone molecule self-assembled host-guest explosive.
Example 3
(1) Weighing 0.2g of HNIW explosive powder, filling the HNIW explosive powder into a sample cavity of a diamond anvil cell, combining a plunger of the anvil cell and a sleeve together, leaving a small amount of gaps, and then putting the HNIW explosive powder into a copper tank body and covering a cover of the copper tank;
(2) putting the tank body into liquid nitrogen, introducing oxygen into the tank body by using an air inlet above a cover, gradually liquefying the oxygen at low temperature, closing an oxygen valve after the liquid oxygen passes through the anvil cell, then opening the cover of the tank body, screwing a pressurizing screw on the anvil cell, so that the liquid oxygen flowing into the anvil cell is encapsulated in a sample cavity containing explosive, characterizing the pressure value of the anvil cell by using a laser pressure instrument, and displaying the pressure at the moment as 1.5 GPa;
(3) turning on a power supply of a tip electrode laid in a counter anvil sample cavity in advance, starting electric field pulse, instantly discharging at the tip to form an electric field, controlling the voltage of the electric field to be 5eV, starting for 30 seconds, and irradiating a laser beam of a solid laser aiming at a sample while starting the electric field with the irradiation power of 20 mW; the laser auxiliary loading mode is adopted, and the laser beam generated by the laser enters the cavity through the transmission of the diamond position of the pressurizing device, so that the oxygen molecules in the cavity are subjected to laser auxiliary action, and the ozone preparation efficiency is further improved.
(4) And then heating a sample chamber of the large press by using a heating sleeve, controlling the temperature at 40 ℃, continuously and symmetrically screwing the pressure screws on the anvil until the pressure value of the anvil reaches 15GPa, standing for 30min, unscrewing the pressure screws, and taking out the sample to obtain the HNIW and ozone molecule self-assembled host-guest explosive.
Example 4
(1) Weighing 1g of HNIW explosive powder, filling the HNIW explosive powder into a sample cavity of a large press, combining a plunger and a sleeve of the large press together, simultaneously leaving a small amount of gaps, and then putting the HNIW explosive powder into a copper tank body and covering a cover of the copper tank;
(2) putting the tank body into liquid nitrogen, introducing oxygen into the tank body by using an air inlet above a cover, gradually liquefying the oxygen at low temperature, closing an oxygen valve after the liquid oxygen submerges the large press, then opening the cover of the tank body, screwing a pressurizing screw on the large press, packaging the liquid oxygen flowing into the large press in a sample cavity containing explosive, characterizing a anvil pressure value by using a laser pressing instrument, and displaying the pressure at the moment to be 0.3 GPa;
(3) turning on a power supply of a tip electrode laid in a sample cavity of a large press in advance, starting electric field pulse, instantly discharging at the tip to form an electric field, controlling the voltage of the electric field to be 5eV, starting for 30 seconds, and irradiating a laser beam of a solid laser aiming at a sample while starting the electric field with the irradiation power of 20 mW;
(4) and then heating a sample chamber of the large press by using a heating sleeve, controlling the temperature at 80 ℃, continuously and symmetrically screwing the pressurizing screws on the large press until the pressure value of the large press reaches 0.5GPa, standing for 60min, unscrewing the pressurizing screws, and taking out the sample to obtain the HNIW and ozone molecule self-assembled host-guest explosive.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (6)
1. A method for preparing a host-guest explosive of in-situ self-assembled ozone molecules is characterized in that oxygen molecules and HNIW are cooperatively arranged in a cavity of a pressurizing device, ozone molecules are prepared in situ by utilizing pulse point discharge, and then the ozone molecules are embedded into HNIW unit cells through pressurization, so that the host-guest explosive of the HNIW and the ozone molecules self-assembled is obtained.
2. The method for preparing a host-guest explosive for in-situ self-assembly of ozone molecules according to claim 1, characterized in that it comprises the following steps:
the method comprises the following steps: filling HNIW and oxygen into the cavity of the pressurizing device simultaneously;
step two: adding a tip electrode into the cavity of the pressurizing device, accessing electric field pulse, instantaneously forming an electric field enough for ionizing oxygen molecules at the tip, and preparing ozone molecules in situ through oxygen molecule ionization;
step three: continuously applying pressure to HNIW and ozone in the cavity of the pressurizing device, and embedding ozone molecules into HNIW unit cells under the driving of the pressure of 0.5GPa-15GPa, thus obtaining the host-guest explosive self-assembled by HNIW and ozone molecules.
3. The method for preparing a host-guest explosive for in-situ self-assembly of ozone molecules as claimed in claim 2, wherein the pressurizing device is selected from one of a diamond anvil cell and a large press.
4. The method for preparing a host-guest explosive containing self-assembled ozone molecules in situ according to claim 2, wherein the HNIW and the oxygen are simultaneously filled in the cavity of the pressurizing device and simultaneously packaged in a way that liquid helium or liquid nitrogen is adopted to liquefy the oxygen in a corrosion-resistant tank, then the pressurizing device filled with the HNIW is placed in the tank, the liquefied oxygen in the tank flows into the cavity of the pressurizing device through a gap reserved between a sleeve and a plunger in the pressurizing device, then a screw of the pressurizing device is fastened in situ in a low-temperature environment, and the oxygen and the HNIW are filled in the cavity after being pressurized to a certain pressure; the certain pressure is 0.3 GPa-1.5 GPa.
5. The method for preparing a host-guest explosive of in-situ self-assembled ozone molecules according to claim 2, wherein the electric field voltage of the point discharge is between 0.5eV and 10 eV.
6. The method for preparing a host-guest explosive for in-situ self-assembly of ozone molecules according to claim 2, wherein the HNIW and the ozone in the cavity of the pressurizing device are heated at the same time with the pressure applied in the step three, and the heating temperature is controlled to be between 40 ℃ and 80 ℃.
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