CN113717119A - Pentazole compound material and preparation method thereof - Google Patents
Pentazole compound material and preparation method thereof Download PDFInfo
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- CN113717119A CN113717119A CN202110305490.6A CN202110305490A CN113717119A CN 113717119 A CN113717119 A CN 113717119A CN 202110305490 A CN202110305490 A CN 202110305490A CN 113717119 A CN113717119 A CN 113717119A
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- pentazole
- nitrogen
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- -1 Pentazole compound Chemical class 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000004093 laser heating Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000010432 diamond Substances 0.000 claims description 11
- 229910003460 diamond Inorganic materials 0.000 claims description 11
- 239000010437 gem Substances 0.000 claims 2
- 229910001751 gemstone Inorganic materials 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 46
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 23
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000010979 ruby Substances 0.000 description 8
- 229910001750 ruby Inorganic materials 0.000 description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 5
- 229910052702 rhenium Inorganic materials 0.000 description 5
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 5
- 238000003825 pressing Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IVRMZWNICZWHMI-UHFFFAOYSA-N Azide Chemical compound [N-]=[N+]=[N-] IVRMZWNICZWHMI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001540 azides Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- AYTVLULEEPNWAX-UHFFFAOYSA-N cesium;azide Chemical compound [Cs+].[N-]=[N+]=[N-] AYTVLULEEPNWAX-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- WUHLVXDDBHWHLQ-UHFFFAOYSA-N pentazole Chemical compound N=1N=NNN=1 WUHLVXDDBHWHLQ-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D259/00—Heterocyclic compounds containing rings having more than four nitrogen atoms as the only ring hetero atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to a pentazole compound material and a preparation method thereof, belonging to the technical field of nitrogen-rich material preparation, and comprising the following steps: and (2) placing sodium azide powder in a pressurizing device, pressurizing to 38GPa, performing reciprocating rotation by taking 45 degrees as a rotation period, applying shear stress, stopping rotation when the total reciprocating rotation angle is 90 degrees, and performing laser heating to 2000K for 10 seconds to obtain the pentazole compound. The method of the invention does not need to introduce other impurities in the preparation process, has low synthesis pressure, simple process, low cost, no environmental pollution, safety and reliability.
Description
Technical Field
The invention belongs to the technical field of nitrogen-rich material preparation, and particularly relates to a pentazole compound material and a preparation method thereof.
Background
At normal pressure, nitrogen molecules are diatomic molecules in which the nitrogen atoms are strongly covalently bonded by triple bonds, while the nitrogen molecules have relatively weak van der waals forces. Under the action of pressure, the interaction between nitrogen molecules is gradually enhanced, and when the covalent bond between the nitrogen molecules and the covalent bond in the molecule is comparable, the nitrogen-nitrogen triple bond is opened to form non-molecular nitrogen bonded by the nitrogen-nitrogen single bond, namely polymeric nitrogen. Because of huge energy difference between the nitrogen-nitrogen single bond and the nitrogen-nitrogen triple bond, huge energy can be released when the nitrogen-nitrogen single bond in the polymerized nitrogen is converted into the nitrogen with the triple bond, and the product only contains nitrogen which does not pollute the environment in the process of releasing the energy, so that the material is a green and environment-friendly high-energy density material. Therefore, the polymeric nitrogen has important application prospect in the fields of national defense, aerospace, new energy and the like.
Numerous theoretical studies have predicted that nitrogen-rich compounds are potential High Energy Density Materials (HEDMs). Since the theoretical possibility of synthesizing polymeric nitrogen structures of different morphologies has been obtained, there has been extensive interest in finding new polymeric nitrogen structures by various experimental techniques. However, since the conditions for synthesizing these polymeric nitrogens are severe, only four polymeric nitrogen structures (three-dimensional reticulated polymeric nitrogen cubic structural (cg-N), layered polymeric nitrogen lamellar structural (LP-N), hexagonal layered polymeric nitrogen lamellar polymeric structural (HLP-N) and black phosphorus structure polymeric nitrogen black phosphorus structural (bp-N)) have been successfully synthesized. Alkali metal azides have advantages in designing new polymeric nitrogen structures because metal-nitrogen interactions may stabilize more forms of nitrogen-rich structures relative to structures composed of pure nitrogen. The skilled person has predicted a number of novel nitrogen-rich structural groups, e.g. caged N10Chain form N8And cyclic N5、N6And the like, among which five-membered cyclic N5-is attracting attention due to its unique aromaticity.
Sodium azide (NaN)3) Is a typical metal azide, is a white hexagonal crystal, is a colorless and tasteless solid granular crystal, and is toxic; dissolving in water (39% at 0 deg.C, 40.16% at 10 deg.C, and 55% at 100 deg.C) and liquid ammonia (50.7% at 0 deg.C), slightly soluble in ethanol (0.3% at 25 deg.C), and insoluble in diethyl ether; when heated to 400 ℃, the sodium hydroxide can be decomposed into metallic sodium and nitrogen and emit a large amount of heat; sodium azide is explosive, has no risk of ignition, and is thermally stable as compared with other metal azides. Due to itDue to the special physical and chemical properties, sodium azide is widely applied to the fields of medicines, explosives, photo preparations, synthetic resins, pesticides, chemical synthesis, biology and the like.
The high temperature, high pressure and shearing technology can effectively regulate the structure and properties of the material, and is a new method for preparing the material with new structure and new properties. Currently, researchers have begun to explore NaN by means of high pressure3New structures may appear in (1). NaN3As the alkali metal azide having the highest stability, the ordinary temperature and high pressure behavior thereof has been studied intensively by Raman spectroscopy and X-ray diffraction techniques. In 2004, Eremets et al (Eremets, M.I.el., Polymerization of nitrogen in sodium azide.J.chem.Phys.2004, 120, 10618-10623) reported that NaN was present at room temperature under 120GPa3Middle 1600cm-1The azide ion tensile vibration v1 disappeared, completely disappeared only at 160GPa, and it was interpreted that sodium azide was completely converted into the pentazole compound. In 2017, Chinese scientists firstly prepare stable pentatomic ring N5-containing ionic salt (N5)6(H3O)3 (NH) by an oxidation cutting method under the low-temperature condition4)4Cl, however, does not satisfy the requirements as a high energy density material in terms of the density of the material and the like due to its complex non-energetic stoichiometry. In the same year, Oleynik et al successfully obtained a metal salt of pentazole (CsN) at a high pressure of 60GPa by theoretical prediction in combination with experiments5) The crystal of (4). The method is to mix cesium azide (CsN)3) And liquid nitrogen is put into a diamond pressure cavity, a new substance with a new structure and new properties is obtained by adopting high pressure and laser heating, and the new substance is CsN proved by X-ray diffraction spectrum and Raman spectrum analysis5. Up to now, high temperature and high pressure synthesis is a synthesis of N containing five-membered cyclic rings5The compound is extremely effective.
Disclosure of Invention
The invention aims to provide a pentazole compound material and a preparation method thereof, and the prepared pentazole compound material is a pure phase and does not contain a sodium azide phase.
In order to achieve the above object, the present invention provides the following technical solutions:
a pentazole compound material and a preparation method thereof comprise the following steps:
and (2) placing sodium azide powder in a pressurizing device, pressurizing to 38GPa, performing reciprocating rotation by taking 45 degrees as a rotation period, applying shear stress, stopping rotation when the total reciprocating rotation angle is 90 degrees, and performing laser heating to 2000K for 10 seconds to obtain the pentazole compound.
Preferably, the pressing device is a non-balanced load diamond anvil cell press.
Preferably, the pressurizing rate to 38GPa is 4-5 GPa/min.
Preferably, the rate of reciprocal rotation is 45 °/10 s.
Preferably, in the pressurizing process, the ruby ball is used as a pressure mark, and the diameter of the ruby ball is 3 μm.
The invention provides a pentazole compound material prepared by the preparation method in the technical scheme.
According to the method, sodium azide powder is used as a raw material, a pentazole compound is synthesized by utilizing shear stress generated by high temperature, high pressure and reciprocating rotation, the phase change pressure is remarkably reduced by the rotary shear stress generated in the reciprocating rotation process, and then laser heating is carried out, so that a new phase is generated, and the pentazole compound material is obtained.
The method of the invention does not need to introduce other impurities in the preparation process, has low synthesis pressure, simple process, low cost, no environmental pollution, safety and reliability, and the existing experimental method is that the pentazole compound appears after the pressure is increased to 80GPa and the laser heating is carried out (or the pentazole compound is rotated and applied with shear stress along one direction when the pressure is 67 GPa).
Drawings
FIG. 1 is a Raman scattering spectrum of a pentazole compound material prepared in example 1.
Detailed Description
The invention provides a preparation method of a pentazole compound material, which comprises the following steps:
and (2) placing sodium azide powder in a pressurizing device, pressurizing to 38GPa, performing reciprocating rotation by taking 45 degrees as a rotation period, applying shear stress, stopping rotation when the total reciprocating rotation angle is 90 degrees, and performing laser heating to 2000K for 10 seconds to obtain the pentazole compound.
In the present invention, unless otherwise specified, all the required starting materials or apparatus for the preparation are commercially available products well known to those skilled in the art.
In the invention, the pressurizing device is preferably a non-balanced load diamond anvil cell press; the invention is not particularly limited to the non-equilibrium loading diamond anvil cell press, which has an anvil surface of 200 μm diamond, and corresponding devices well known in the art.
In the present invention, to prevent laser heating from damaging the anvil surface and the pad material, a thin layer of magnesium oxide is laminated on the upper anvil surface of the unbalanced load diamond anvil, and a magnesium oxide film is used as the heat insulating layer.
In the invention, the process of placing the sodium azide powder in a pressurizing device is preferably to pre-press a rhenium sheet by adopting a diamond anvil cell press, drill a hole in the center of the obtained indentation, and use the round hole obtained by drilling as a sample cavity for filling the sodium azide powder raw material; and filling excessive sodium azide powder into a round hole of the rhenium sheet, and pressurizing by taking the ruby ball as a pressure mark and taking no other medium as a pressure transmission medium. The rhenium sheet is not particularly limited in the present invention, and a rhenium sheet known in the art may be used.
In the present invention, the diameter of the circular hole drilled is preferably 66 μm; the number of the ruby balls is preferably one or two, and the diameter of the ruby ball is preferably 3 mu m; the invention utilizes the pressure mark
Measuring the pressure value in a diamond pressing cavity formed in the non-equilibrium load diamond anvil cell pressing machine, and determining the magnitude of the pressure value according to the peak position change of an R1 fluorescence line of the ruby ball, wherein the precision is 0.1 GPa; the process of determining the magnitude of the pressure value by using the R1 fluorescence line of the ruby ball is not particularly limited in the invention, and the process can be carried out according to a labeling method and a labeling process which are well known in the field.
In the invention, the pressurizing speed is preferably 4-5 GPa/min; the rate of reciprocating rotation is preferably 45 °/10 s. The present invention is not particularly limited to the specific process of the reciprocating rotation, and the process may be performed according to a process well known in the art.
The invention provides a pentazole compound material prepared by the preparation method in the technical scheme.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Pre-pressing a rhenium sheet by using a diamond anvil press with the anvil surface of 200 mu m, drilling a round hole with the diameter of 66 mu m in the center of an indentation, wherein the round hole is used as a sample cavity filled with a raw material, filling excessive sodium azide powder into the sample cavity, adding two ruby balls with the diameter of 3 mu m as a pressure mark, not adding any other medium as a pressure transmission medium, pressurizing at the rate of 4GPa/min, rotating 90 degrees at the rate of 45 degrees of rotation every 10s when the pressure is pressurized to 38GPa, stopping rotating, and then performing laser heating to 2000K for 10 seconds to obtain the pentazole compound.
The pentazole compound material prepared in this example was subjected to Raman scattering test, and the results are shown in fig. 1; as is clear from FIG. 1, the azide ion stretching vibration v1 disappeared, and the sodium azide decomposed and disappeared at 770cm-1A new peak appears at the position, which indicates that the phase of the sodium azide is changed into a pentazole compound.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A pentazole compound material and a preparation method thereof comprise the following steps: and (2) placing sodium azide powder in a pressurizing device, pressurizing to 38GPa, performing reciprocating rotation by taking 45 degrees as a rotation period, applying shear stress, stopping rotation when the total reciprocating rotation angle is 90 degrees, and performing laser heating to 2000K for 10 seconds to obtain the pentazole compound.
2. The pentazole compound material and the preparation method thereof as claimed in claim 1, wherein the press device is a non-equilibrium load diamond anvil press.
3. The pentazole compound material and the preparation method thereof as claimed in claim 1, wherein the rate of pressurizing to 38GPa is 4-5 GPa/min.
4. The pentazole compound material and the preparation method thereof according to claim 1, wherein the reciprocating rotation speed is 45 °/10 s.
5. The pentazole compound material and the preparation method thereof as claimed in claim 1, wherein the red precious stone ball is used as a pressure mark during the pressurizing process, and the diameter of the red precious stone ball is 3 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110305490.6A CN113717119A (en) | 2021-03-19 | 2021-03-19 | Pentazole compound material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110305490.6A CN113717119A (en) | 2021-03-19 | 2021-03-19 | Pentazole compound material and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518797A (en) * | 2016-08-18 | 2017-03-22 | 南京理工大学 | Pentazole composite salt and preparation method thereof |
| CN111233778A (en) * | 2020-01-17 | 2020-06-05 | 吉林大学 | High-temperature high-pressure preparation and normal-pressure capture method of limited-area high-density anhydrous alkali metal polymeric nitrogen NaN5 |
-
2021
- 2021-03-19 CN CN202110305490.6A patent/CN113717119A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518797A (en) * | 2016-08-18 | 2017-03-22 | 南京理工大学 | Pentazole composite salt and preparation method thereof |
| CN111233778A (en) * | 2020-01-17 | 2020-06-05 | 吉林大学 | High-temperature high-pressure preparation and normal-pressure capture method of limited-area high-density anhydrous alkali metal polymeric nitrogen NaN5 |
Non-Patent Citations (2)
| Title |
|---|
| MIAO ZHOU，等: "High-Pressure-Induced Structural and Chemical Transformations in NaN3", 《J. PHYS. CHEM. C》 * |
| 周淼: "碱金属富氮化合物的高压研究", 《吉林大学硕士学位论文》 * |
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Application publication date: 20211130 |