CN108863968B - Two (1,5- nitre aminotetrazoles)-four are hydrated ferrous ironization potassium compound - Google Patents
Two (1,5- nitre aminotetrazoles)-four are hydrated ferrous ironization potassium compound Download PDFInfo
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- CN108863968B CN108863968B CN201810815670.7A CN201810815670A CN108863968B CN 108863968 B CN108863968 B CN 108863968B CN 201810815670 A CN201810815670 A CN 201810815670A CN 108863968 B CN108863968 B CN 108863968B
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- ironization
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D257/00—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms
- C07D257/02—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms not condensed with other rings
- C07D257/04—Five-membered rings
- C07D257/06—Five-membered rings with nitrogen atoms directly attached to the ring carbon atom
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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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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of two (1,5- nitre aminotetrazoles)-four to be hydrated ferrous ironization potassium compound, and structural formula is such as shown in (I):
Description
Technical field
The present invention relates to a kind of energetic materials, and in particular to a kind of two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium
Compound.
Background technique
Priming is most sensitive chemical energy source, has the characteristics that high sensitivity, high-voltage instant, high-power, when by the external world compared with
When small initial punching can be such as shock, friction, needle thorn, flame equal excitation, detonation can be generated and cause secondary charging explosion.Currently,
In dual-use field, widely used priming is lead azide and lead styphnate, is had since both primings contain
Malicious heavy metal element --- lead causes to cause seriously to pollute to personnel and environment using such priming, as people are to weapon
The performance deficiency of the raising of ammumtion safety and environmental quality requirement, lead azide and lead styphnate leads to priming system and medicament
Major accident occurs in duties processing and use, also counteracts the development of priming system, therefore, various countries' researcher is all positive
Carry out the research work of Novel detonating medicine, desired design goes out to prepare safety, sensitivity is suitable for rising with a new generation of high energy output, environment-friendly type
Quick-fried drug kind.High nitrogen tetrazole derivatives structure contains a large amount of N-N and C-N key, with aromatic structure stability, have compared with
The features such as good thermal stability, higher positive generation heat and biggish gas production, and its decomposition product is predominantly cleaned without dirt
The nitrogen of dye has bright prospects in terms of constructing novel environment-friendly priming.5- nitro tetrazolium has chemical potential height, energy
The features such as density is big, high nitrogen, low-carbon hydrogen content are easy to reach oxygen balance, are a kind of potential energetic material ligands of tool, wherein
It is a kind of novel green, environment-friendly type that preparation is designed based on 5- nitro tetrazolium that four (5- nitro tetrazolium) two hydrated irons (II), which change sodium,
Priming.
Zhu Yahong etc. " synthesis and characteristic that environmentally friendly four (5- nitro tetrazolium) two hydrated irons (II) of priming change sodium ", contains energy
Material, 2012,20 (6), 726-730 disclose the molecular structure that four (5- nitro tetrazolium) two hydrated irons (II) change sodium compound
And detonation property, the compound structure are as follows:
The compound explosion velocity is 5550m/s, quick-fried to hold for 506L/kg.But the quick-fried appearance of the compound is smaller, explosion velocity is lower.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of background technique and defect, provide it is a kind of it is quick-fried hold it is larger,
Explosion velocity higher two (1,5- nitre aminotetrazole)-four is hydrated ferrous ironization potassium compound.
The synthetic route of two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium compound of the invention is as follows:
With 1,5- dinitro aminotetrazole for raw material, is reacted with potassium hydroxide generate 1,5- dinitro aminotetrazole sylvite first,
Then metathesis reaction occurs with green vitriol and generates two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium.
Two (1,5- nitre aminotetrazoles)-four of the invention are hydrated ferrous ironization potassium compound, and structural formula is such as shown in (I):
The synthetic method of two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium of the invention, comprising the following steps:
(1) synthesis of 1,5- dinitro aminotetrazole sylvite
At room temperature, successively 1,5- dinitro aminotetrazole, methanol are added in reaction flask, ice-water bath is cooled to 0~5 DEG C, drop
The methanol solution for adding potassium hydroxide, the reaction was continued at 0~5 DEG C 0.5h, filtering, methanol are washed, are dried in vacuo to obtain white solid；Wherein
The molar ratio of 1,5- dinitro aminotetrazole and potassium hydroxide is 1:2~3.
The synthesis of (2) two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium
At room temperature, 1,5- dinitro aminotetrazole sylvite, water are added in reaction flask, after stirring and dissolving, seven hydration sulphur is added
It is sour ferrous, it is heated to 55 DEG C of reaction 2h, cooling, filtering, reduced pressure filtrate, cooling, filtering, dry yellowish-brown crystal；Its
The molar ratio of middle 1,5- dinitro aminotetrazole sylvite and green vitriol is 1:1~2.
Advantages of the present invention:
The quick-fried appearance of two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium compound of the invention is larger, quick-fried to hold for 577L/
Kg, the quick-fried appearance that four (5- nitro tetrazolium) two hydrated irons (II) of documents change sodium is 506L/kg；Two (1,5- of the invention
Nitre aminotetrazole)-four hydration ferrous ironization potassium compound energy it is higher, explosion velocity 7630m/s, four (5- nitros of documents
Tetrazolium) two hydrated irons (II) change sodium explosion velocity be 5550m/s.
Specific embodiment
Invention is further described in detail with reference to embodiments.
Embodiment 1
(1) synthesis of 1,5- dinitro aminotetrazole sylvite
At room temperature, successively 0.17g (0.89mmol) 1,5- dinitro aminotetrazole, 3.0mL methanol are added in reaction flask, ice
To 0~5 DEG C the methanol solution that 3.0mL contains 0.112g (2mmol) potassium hydroxide is added dropwise, the reaction was continued at 0~5 DEG C in water-bath cooling
0.5h, filtering, methanol are washed, are dried in vacuo to obtain 0.19g white solid, yield 79.8%.
Structural Identification:
Infrared spectroscopy: IR (KBr, cm-1), υ: 1510,1439,1412,1367,1291,1236,1228,1099,1034,
912,856
Nuclear magnetic spectrum:13C NMR(DMSO-d6, 125MHz), δ: 154.42
Elemental analysis: molecular formula CK2N8O4
Theoretical value: C 4.51, N 42.08
Measured value: C 4.62, N 42.03.
Above structure appraising datum confirms to obtain substance to be strictly 1,5- dinitro aminotetrazole sylvite.
The synthesis of (2) two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium
At room temperature, 0.133g (0.5mmol) 1,5- dinitro aminotetrazole sylvite, 3.0mL water are added in reaction flask, stirring
After dissolution, 0.209g (0.75mmol) green vitriol is added, is heated to 55 DEG C of reaction 2h, cooling, filtering is concentrated under reduced pressure
Filtrate, cooling, filtering, dry 0.045g yellowish-brown crystal, yield 30.9%.
Structural Identification:
Infrared spectroscopy: IR (KBr, cm-1), υ: 3546,3433,1528,1438,1422,1350,1290,1112,1029,
920
Elemental analysis: molecular formula C2H8N16O12FeK2
Theoretical value: C 4.13, H 1.38, N 38.49
Measured value: C 4.21, H 1.47, N 38.36
Mono-crystalline structures parameter: the compound crystal is monoclinic system, and space group is P2 (1)/c, crystallographic parameter are as follows: α=90 °, β=103.726 (2) °, γ=90 °,Z=2, μ=1.370mm-1, F (000)=584.
Above structure appraising datum confirms to obtain substance to be strictly two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium.
The performance of two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium of the invention
(1) physical and chemical performance
Appearance: yellowish-brown crystal
Solubility: soluble easily in water；Insoluble in petroleum ether, n-hexane, ether, ethyl acetate, acetonitrile etc.
Density: 2.095g/cm3X-ray single crystal diffractometer
(2) detonation property
Explosion velocity: density 2.095g/cm3, calculating explosion velocity is 7630m/s K-J equation
Quick-fried heat: density 2.095g/cm3, calculating detonation pressure is 28.4GPa K-J equation
Quick-fried appearance: density 2.095g/cm3, calculate quick-fried hold for 577L/kg K-J equation
The purposes of two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium of the invention
Two (1,5- nitre aminotetrazoles)-four hydration ferrous ironization potassium of the invention is larger with quick-fried appearance, energy is higher, does not contain
The features such as malicious heavy metal element, is expected to as novel environment friendly priming.
Claims (1)
1. one kind two (1,5- nitre aminotetrazole)-four is hydrated ferrous ironization potassium compound, structural formula is such as shown in (I):
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434617A (en) * | 2008-08-20 | 2009-05-20 | 西北大学 | Energetic coordination complex based on azo tetrazole azotetrazole and use thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434617A (en) * | 2008-08-20 | 2009-05-20 | 西北大学 | Energetic coordination complex based on azo tetrazole azotetrazole and use thereof |
Non-Patent Citations (3)
| Title |
|---|
| Metal perchlorate complexes with 1,5-diaminotetrazole;Lavrenova, L. G.，等;《Zhurnal Neorganicheskoi Khimii》;19881231;第33卷(第10期);第2583-2586页 * |
| 含能配合物研究新进展;张同来，等;《含能材料》;20130430;第21卷(第2期);摘要，第138页表I * |
| 绿色四唑类起爆药研究的最新进展;张光全;《含能材料》;20110831;第19卷(第4期);第474页Scheme 5 * |
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