CN110467581A - A kind of anhydrous nonmetallic pentazole ion salt and preparation method thereof - Google Patents
A kind of anhydrous nonmetallic pentazole ion salt and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of anhydrous nonmetallic pentazole ion salt and preparation method thereof, the chemical structural formulas of affiliated non-metal salt are as follows: Cat (N5) n, when Cat is positive the nonmetallic ammonium of monovalence, guanidine, hydrazine, azanol, guanidine radicals urea or oxalyl hydrazine cation, n=1；When Cat is positive divalent non-metal carbon hydrazides, 4,4 ', 5,5 '-tetramino -3,3 ' -1,2,4- triazoles or 6, when four azepine -3,9- diamines (575) of 7- dihydro-bis- ([1,2,4] triazol) [1,2,4,5] is cationic, n=2.This kind of anhydrous nonmetallic pentazole ion salt is with pentazole sodium-salt hydrate [Na (H2O)(N5)]∙2H2O and the hydrochloride of non-metal cations are raw material, are taken water as a solvent, then ultrasonic dissolution is evaporated, recrystallize preparation repeatedly with methanol.Simple process of the present invention is efficient；Pentazole ion salt interaction of hydrogen bond obtained is obvious, and structural stability is higher, a kind of good high nitrogen stell of comprehensive performance.
Description
Technical field
The present invention relates to a kind of anhydrous nonmetallic pentazole ion salts and preparation method thereof, belong to energetic material technology neck
Domain.
Background technique
High Energy Density Materials refer to energy density be higher than best standard energetic material (such as RDX, HMX) 15%~20% with
On the novel energetic material technology of one kind, be the essential power of land, sea, air all kinds of weapon systems of all services and power source
Material technology mainly includes CL-20, diamide ammonium (ADN), trinitroazetidine (TNAZ), otanitrocubane, complete
MOLECULE DESIGN, synthesis and technology of preparing of the high energy density compounds such as nitrogen material etc..Pentazole anion is a kind of full nitrogen material,
Its research has been approached a century.Compared to other full nitrogen materials, cause researchers' because it is with preferable stability
Broad interest.2016, Bazanov etc. five oxazolinium ions are detected in tetrahydrofuran solution and prove this ion-
40 DEG C are stabilized, pentazole anion cause again special attention [Angew.Chem.Int.Ed.2016,55,13233-
13235].Subsequent Steele etc. reports first solid-state pentazole metal salt CsN5High pressure (60GPa) synthesis, but the compound
It cannot be stabilized under normal temperature and pressure [Chem.Mater.2017,29,735-741].2017, the stable non-gold of normal temperature and pressure
Belong to pentazole complex salt (N5)6(H3O)3(NH4)4Cl is reported [Science 2017,355,374-376].This complex salt be with
Aryl pentazole is raw material, using ferrous bisglycinate chelate and metachloroperbenzoic acid as auxiliary agent and cutting reagent, cuts off rear pillar by oxidation
Chromatographic isolation obtains.Then similar method is used to synthesis pentazole metal salt [Na (H2O)(N5)]·2H2O[Nature
2017,549,78-81] and three-dimensional porous pentazole sodium frame structure MPF-1 [Angew.Chem.Int.Ed.2018,57,2592-
2595].To so far, manganese, iron, cobalt, zinc, the magnesium salts hydrate of five oxazolinium ions have been reported, but in these material molecules all
It is not energetic material truly containing the crystallization water, water of coordination and metal ion.Therefore, energetic material is answered to develop
Demand, preparing for anhydrous nonmetallic pentazole ion salt are imperative.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of anhydrous nonmetallic pentazole ion salt, with pentazole sodium-salt hydrate
[Na(H2O)(N5)]·2H2O and the hydrochloride of non-metal cations are raw material, are taken water as a solvent, then ultrasonic dissolution is evaporated,
It is recrystallizing repeatedly so as to obtain with methanol.
Realize the technical solution of the object of the invention:
A kind of anhydrous nonmetallic pentazole ion salt, chemical structural formula are as follows: Cat (N5) n, Cat represents non-metal cations,
When Cat is positive the nonmetallic ammonium of monovalence, guanidine, hydrazine, azanol, guanidine radicals urea or oxalyl hydrazine cation, n=1；When the Cat divalent that is positive is non-
Metal Cabonyls hydrazine, 4,4 ', 5,5 '--1,2,4- of tetramino -3,3 ' triazoles or 6,7- dihydro-bis- ([1,2,4] triazols) [1,2,
4,5] when four azepine -3,9- diamines (referred to as 575) cation, n=2.
Wherein, when Cat is guanidine radicals urea, i.e., when nonmetallic pentazole salt is pentazole guanidine radicals urea, the crystalline substance of the monocrystalline of the ion salt
Volume data is as follows:
Molecular formula: C2H7N9O；
Molecular weight: 173.17；
Crystallographic system: monoclinic system；
Point group: P21/c；
Cell parameter:α=γ=90 °, β=94.130
(6)°；
Unit cell volume:
Z=4；
Density: 1.596g cm-3(173K)。
Wherein, when Cat is oxalyl hydrazine, i.e., when nonmetallic pentazole salt is pentazole oxalyl hydrazine, the crystalline substance of the monocrystalline of the ion salt
Volume data is as follows:
Molecular formula: C2H7N9O2；
Molecular weight: 189.17；
Crystallographic system: monoclinic system；
Point group: P21/c；
Cell parameter:α=γ=90 °, β=119.324
(19)°；
Unit cell volume:
Z=8；
Density: 1.681g cm-3(173K)。
Wherein, when Cat ([1,2,4] triazol) [1,2,4,5] four azepine -3,9- diamines bis- for 6,7- dihydro -, that is, work as
When nonmetallic pentazole salt is 575 salt of pentazole, the crystal data of the monocrystalline of the ion salt is as follows:
Molecular formula: C5H10N20；
Molecular weight: 350.33；
Crystallographic system: monoclinic system；
Point group: C2/c；
Cell parameter:α=γ=90 °, β=100.519
(16)°；
Unit cell volume:
Z=4；
Density: 1.660g cm-3(173K)。
The preparation method of above-mentioned nonmetallic pentazole ion salt, by with pentazole sodium-salt hydrate [Na (H2O)(N5)]·2H2O
Hydrochloride with non-metal cations is raw material, is taken water as a solvent, ultrasonic dissolution is stirred to react, and is then evaporated, repeatedly with methanol
It is recrystallized to give.
Further, in preparation method, the material ratio of reactant is [Na (H2O)(N5)]·2H2O and it is nonmetallic sun from
The molar ratio of the hydrochloride of son is 1:1~2:1.
Further, in preparation method, reaction temperature is 15~25 DEG C, and the reaction time is 1~5.5 hour.
Further, in preparation method, methanol concentration is 75~95wt%.
Further, in preparation method, recrystallization number is 3~5 times.
Compared with prior art, the present invention the beneficial effect is that:
(1) preparation method of inorganic non-metallic pentazole ion salt of the invention is simple and efficient, and effectively removes intramolecular
The crystallization water and water of coordination, be successfully prepared the really ionic energetic material containing pentazole, which has biggish application
Value.
(2) pillar layer separation is not necessarily in preparation process, technique is simpler efficiently.
(3) anhydrous nonmetallic pentazole ion salt good thermal stability of the invention, wherein pentazole guanidine radicals urea, pentazole oxalyl hydrazine
110 DEG C, 95 DEG C and 100 DEG C are up to the thermal decomposition temperature of 575 salt of pentazole.
Detailed description of the invention
Fig. 1 is the crystal structure figure of pentazole guanidine radicals urea of the present invention.
Fig. 2 is the structure cell accumulation graph of pentazole guanidine radicals urea of the present invention.
Fig. 3 is the crystal structure figure of pentazole oxalyl hydrazine of the present invention.
Fig. 4 is the structure cell accumulation graph of pentazole oxalyl hydrazine of the present invention.
Fig. 5 is the crystal structure figure of 575 salt of pentazole of the present invention.
Fig. 6 is the structure cell accumulation graph of 575 salt of pentazole of the present invention.
Fig. 7 is the differential scanning calorimetric thermogram of pentazole guanidine radicals urea of the present invention, 575 salt of pentazole oxalyl hydrazine and pentazole.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully appreciated, but not limit in any way
The system present invention.The present invention includes but are not limited to following several nonmetallic pentazole ion salts.
Embodiment 1:1mmol guanidine radicals urea hydrochloride and 1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 1h at 15 DEG C, is then evaporated, with recrystallizing methanol 3 times that concentration is 75%, mother liquor
Slowly volatilization obtains anhydrous pentazole guanidine radicals urea crystal, yield 70%.
Embodiment 2:1mmol guanidine radicals urea hydrochloride and 1.2mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 3h at 20 DEG C, is then evaporated, with recrystallizing methanol 5 times that concentration is 85%, mother liquor
Slowly volatilization obtains anhydrous pentazole guanidine radicals urea crystal, yield 75%.
Embodiment 3:1mmol oxalyl hydrazine hydrochloride and 1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 5.5h at 25 DEG C, is then evaporated, female with recrystallizing methanol 5 times that concentration is 95%
Liquid, which slowly volatilizees, obtains anhydrous pentazole oxalyl hydrazine crystal, yield 62%.
Embodiment 4:1mmol oxalyl hydrazine hydrochloride and 1.1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 3h at 20 DEG C, is then evaporated, with recrystallizing methanol 4 times that concentration is 90%, mother liquor
Slowly volatilization obtains anhydrous pentazole oxalyl hydrazine crystal, yield 58%.
Embodiment 5:1mmol ammonium chloride and 1.1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added 20ml and steams
In distilled water, ultrasonic dissolution stirs 5h at 25 DEG C, is then evaporated, and with recrystallizing methanol 3 times that concentration is 75%, mother liquor is slowly waved
Hair obtains anhydrous pentazole ammonium salt crystal, yield 38%.
Embodiment 6:1mmol ammonium chloride and 1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H220ml distillation is added in O
In water, ultrasonic dissolution stirs 3h at 20 DEG C, is then evaporated, and with recrystallizing methanol 5 times that concentration is 75%, mother liquor slowly volatilizees
Obtain anhydrous pentazole ammonium salt crystal, yield 42%.
Embodiment 7:1mmol guanidine hydrochloride and 1.2mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added 20ml and steams
In distilled water, ultrasonic dissolution stirs 1h at 25 DEG C, is then evaporated, and with recrystallizing methanol 3 times that concentration is 90%, mother liquor is slowly waved
Hair obtains anhydrous pentazole guanidine salt crystal, yield 35%.
Embodiment 8:1mmol guanidine hydrochloride and 1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H220ml distillation is added in O
In water, ultrasonic dissolution stirs 5h at 15 DEG C, is then evaporated, and with recrystallizing methanol 4 times that concentration is 95%, mother liquor slowly volatilizees
Obtain anhydrous pentazole guanidine salt crystal, yield 32%.
Embodiment 9:1mmol hydrazine monohydrochloride and 1.1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H220ml is added in O
In distilled water, ultrasonic dissolution stirs 1h at 25 DEG C, is then evaporated, and with recrystallizing methanol 4 times that concentration is 70%, mother liquor is slow
Volatilization obtains anhydrous pentazole hydrazonium salt crystal, yield 28%.
Embodiment 10:1mmol hydrazine monohydrochloride and 1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added 20ml and steams
In distilled water, ultrasonic dissolution stirs 1.5h at 20 DEG C, is then evaporated, and with recrystallizing methanol 3 times that concentration is 75%, mother liquor is slow
Volatilization obtains anhydrous pentazole hydrazonium salt crystal, yield 33%.
Embodiment 11:1mmol hydroxylamine hydrochloride and 1.1mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H220ml is added in O
In distilled water, ultrasonic dissolution stirs 1h at 15 DEG C, is then evaporated, and with recrystallizing methanol 3 times that concentration is 95%, mother liquor is slow
Volatilization obtains anhydrous pentazole azanol salt crystal, yield 36%.
Embodiment 12:1mmol hydroxylamine hydrochloride and 1.2mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H220ml is added in O
In distilled water, ultrasonic dissolution stirs 2h at 15 DEG C, is then evaporated, and with recrystallizing methanol 3 times that concentration is 92%, mother liquor is slow
Volatilization obtains anhydrous pentazole azanol salt crystal, yield 38%.
Embodiment 13:1mmol carbohydrazide dihydrochloride and 1.9mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O adds
Enter in 20ml distilled water, ultrasonic dissolution, 4h is stirred at 25 DEG C, is then evaporated, it is female with recrystallizing methanol 4 times that concentration is 70%
Liquid, which slowly volatilizees, obtains anhydrous pentazole carbohydrazide salt crystal, yield 42%.
Embodiment 14:1mmol carbohydrazide dihydrochloride and 2mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 5h at 15 DEG C, is then evaporated, with recrystallizing methanol 3 times that concentration is 75%, mother liquor
Slowly volatilization obtains anhydrous pentazole carbohydrazide salt crystal, yield 45%.
Embodiment 15:1mmol 4,4 ', 5,5 '-tetramino -3,3 ' -1,2,4- triazole dihydrochloride and 2mmol pentazole sodium
Hydrate [Na (H2O)(N5)]·2H2O is added in 20ml distilled water, ultrasonic dissolution, stirs 4h at 25 DEG C, is then evaporated, use is dense
Degree is recrystallizing methanol 3 times of 70%, and mother liquor, which slowly volatilizees, obtains anhydrous 4,4 ', 5,5 '-tetramino -3 of pentazole, 3 ' -1,2,4-
Triazole crystal, yield 51%.
Embodiment 16:1mmol 4,4 ', 5,5 '-tetramino -3,3 ' -1,2,4- triazole dihydrochloride and 1.8mmol pentazole
Sodium hydrate [Na (H2O)(N5)]·2H2O is added in 20ml distilled water, ultrasonic dissolution, stirs 4.5h at 20 DEG C, is then evaporated,
With recrystallizing methanol 4 times that concentration is 75%, mother liquor, which slowly volatilizees, obtains anhydrous 4,4 ', 5,5 '-tetramino -3 of pentazole, and 3 ' -1,
2,4- triazole crystal, yield 56%.
575 dihydrochloride of embodiment 17:1mmol and 2mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 2.5h at 25 DEG C, is then evaporated, female with recrystallizing methanol 4 times that concentration is 80%
Liquid, which slowly volatilizees, obtains anhydrous 575 crystal of pentazole, yield 55%.
575 dihydrochloride of embodiment 18:1mmol and 1.9mmol pentazole sodium hydrate [Na (H2O)(N5)]·2H2O is added
In 20ml distilled water, ultrasonic dissolution stirs 1h at 25 DEG C, is then evaporated, with recrystallizing methanol 3 times that concentration is 75%, mother liquor
Slowly volatilization obtains anhydrous 575 crystal of pentazole, yield 60%.
Embodiment 1-4 and embodiment 17-18 obtains the anhydrous pentazole guanidine radicals with rock-steady structure by metathesis reaction
575 salt of urea, pentazole oxalyl hydrazine and pentazole, reaction equation are as follows:
Anhydrous pentazole guanidine radicals urea, pentazole oxalyl hydrazine and 575 salt of pentazole pass through X-ray single crystal diffraction, infrared spectroscopy, nuclear-magnetism
Resonance confirms its structure.The crystal structure of pentazole guanidine radicals urea is as shown in Figure 1, the stratiform structure cell of pentazole guanidine radicals urea is accumulated such as Fig. 2 institute
Show；The crystal structure of pentazole oxalyl hydrazine is as shown in figure 3, the structure cell accumulation of pentazole oxalyl hydrazine is as shown in Figure 4；The crystalline substance of 575 salt of pentazole
Body structure is as shown in figure 5, the structure cell accumulation of 575 salt of pentazole is as shown in Figure 6.It can be seen that ion salt from Fig. 2, Fig. 4 and Fig. 6
N-H ... N hydrogen bond is intensive between pentazole anion and more azonias.Intensive hydrogen bond is to itself and unstable pentazole anion
Play good stabilization.Hydrogen bond plays an important role to the sensitivity of ion salt and the improvement of thermal stability, and especially five
Azoles guanidine radicals urea salt is accumulated in stratiform, and thermostabilization is up to 110 DEG C, and impact sensitivity compares favourably with TNT.
Differential scanning calorimetry is carried out to anhydrous nonmetallic pentazole ion salt obtained by embodiment 1-4 and embodiment 17-18
Analysis, analysis result are shown in Fig. 7.The good thermal stability of anhydrous non-metal salt, decomposition temperature obtained by the method are above 100 DEG C.
The theoretical detonation property of anhydrous pentazole oxalyl hydrazine crystal synthesized by embodiment 3 and embodiment 4 is as shown in table 1, compares
It was found that its detonation property is similar with ionic energetic material FOX-12, significantly larger than traditional energetic material TNT.Especially pentazole
The generation heat and nitrogen content of oxalyl hydrazine are high, and explosion product more cleans, and can be used as the candidate materials of green explosive.
Table 1
Combustion product is carried out to three kinds obtained by embodiment 1-4 and embodiment 17-18 anhydrous nonmetallic pentazole ion salts
Analysis, combustion reaction equation are as follows:
C5H10N20(s)+7.5O2(g)→5CO2(g)+5H2O(1)+10N2(g)
C2H7N9O(s)+3.25O2(g)→2CO2(g)+3.5H2O(1)+4.5N2(g)
C2H7N9O2(s)+2.75O2(g)→2CO2(g)+3.5H2O(1)+4.5N2(g)
1 mole of pentazole guanidine radicals urea, pentazole oxalyl hydrazine and the burning of 575 salt of pentazole can produce 7.5 moles respectively, 3.25 rub
You, 3.75 moles of gas, no solid product, and all carbon dioxide of gas component and nitrogen, it is green non-poisonous pollution-free.It can be with
As supplementary energy for various purposes on guided missile --- the candidate material of gas-forming agent solves the combustion gas of current gas-forming agent
Existing ablative, corrosivity and contain a small amount of solia particle the disadvantages of.Nonmetallic pentazole ion salt anhydrous in the future may conduct
The powder charge of various gas generators, apply aircraft, guided missile related component in, provide the necessary energy for them.
Claims (9)
1. a kind of anhydrous nonmetallic pentazole ion salt, which is characterized in that its chemical structural formula are as follows: Cat (N5) n, Cat represents Fei Jin
Belong to cation, when Cat is positive the nonmetallic ammonium of monovalence, guanidine, hydrazine, azanol, guanidine radicals urea or oxalyl hydrazine cation, n=1；Work as Cat
The divalent that is positive non-metal carbon hydrazides, 4,4 ', 5,5 '--1,2,4- of tetramino -3,3 ' triazoles or 6,7- dihydro-bis- ([1,2,4] three
Azoles is simultaneously) [1,2,4,5] four bis- amine cation of azepine -3,9- when, n=2.
2. anhydrous nonmetallic pentazole ion salt as described in claim 1, which is characterized in that when Cat is guanidine radicals urea, the ion
The crystal characterization of the monocrystalline of salt is as follows:
Molecular formula: C2H7N9O；
Molecular weight: 173.17；
Crystallographic system: monoclinic system；
Point group: P21/c；
Cell parameter:
Unit cell volume:
Z=4；
Density: 1.596g cm-3(173K)。
3. anhydrous nonmetallic pentazole ion salt as described in claim 1, which is characterized in that when Cat is oxalyl hydrazine, the ion
The crystal characterization of the monocrystalline of salt is as follows:
Molecular formula: C2H7N9O2；
Molecular weight: 189.17；
Crystallographic system: monoclinic system；
Point group: P21/c；
Cell parameter:
Unit cell volume:
Z=8；
Density: 1.681g cm-3(173K)。
4. anhydrous nonmetallic pentazole ion salt as described in claim 1, which is characterized in that when Cat be 6,7- dihydro-it is bis- ([1,
2,4] triazol) [1,2,4,5] four azepine -3,9- diamines when, the crystal characterization of the monocrystalline of the ion salt is as follows:
Molecular formula: C5H10N20；
Molecular weight: 350.33；
Crystallographic system: monoclinic system；
Point group: C2/c；
Cell parameter:
Unit cell volume:
Z=4；
Density: 1.660g cm-3(173K)。
5. the preparation method of nonmetallic pentazole ion salt as described in claim 1, which is characterized in that by with pentazole natrium brine
Close object [Na (H2O)(N5)]·2H2O and the hydrochloride of non-metal cations are raw material, are taken water as a solvent, ultrasonic dissolution, and stirring is anti-
It answers, is then evaporated, be recrystallizing repeatedly so as to obtain with methanol.
6. preparation method as claimed in claim 5, which is characterized in that the material ratio of reactant is [Na (H2O)(N5)]·2H2O
Molar ratio with the hydrochloride of non-metal cations is 1:1~2:1.
7. preparation method as claimed in claim 5, which is characterized in that reaction temperature be 15~25 DEG C, the reaction time be 1~
5.5 hour.
8. preparation method as claimed in claim 5, which is characterized in that methanol concentration is 75~95wt%.
9. preparation method as claimed in claim 5, which is characterized in that recrystallization number is 3~5 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125858A (en) * | 2020-09-11 | 2020-12-25 | 南京理工大学 | Gemini energetic ion compound and preparation method thereof |
| CN113387901A (en) * | 2020-01-17 | 2021-09-14 | 吉林大学 | Limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN5High pressure preparation method of |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387901A (en) * | 2020-01-17 | 2021-09-14 | 吉林大学 | Limited-area high-density anhydrous alkali metal polymeric nitrogen Cm-NaN5High pressure preparation method of |
| CN113387902A (en) * | 2020-01-17 | 2021-09-14 | 吉林大学 | High-temperature high-pressure preparation method of limited-area high-density anhydrous alkali metal polymeric nitrogen Pmn21-NaN5 |
| CN113387902B (en) * | 2020-01-17 | 2023-02-24 | 吉林大学 | High-temperature high-pressure preparation method of limited-area high-density anhydrous alkali metal polymeric nitrogen Pmn21-NaN5 |
| CN112125858A (en) * | 2020-09-11 | 2020-12-25 | 南京理工大学 | Gemini energetic ion compound and preparation method thereof |
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Application publication date: 20191119 |