CN108840834B - Two (1,5- dinitro aminotetrazoles)-four are hydrated zinc impregnation potassium compound - Google Patents
Two (1,5- dinitro aminotetrazoles)-four are hydrated zinc impregnation potassium compound Download PDFInfo
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- CN108840834B CN108840834B CN201810815669.4A CN201810815669A CN108840834B CN 108840834 B CN108840834 B CN 108840834B CN 201810815669 A CN201810815669 A CN 201810815669A CN 108840834 B CN108840834 B CN 108840834B
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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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Abstract
The invention discloses a kind of two (1,5- dinitro aminotetrazoles)-four to be hydrated zinc impregnation 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- dinitro aminotetrazoles)-four hydration zinc 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, and quick-fried heat is 3929J/g, quick-fried to hold for 506L/kg.But the compound it is quick-fried hold compared with
It is small, energy 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,
Energy higher two (1,5- dinitro aminotetrazole)-four is hydrated zinc impregnation potassium compound.
The synthetic route of two (1,5- dinitro aminotetrazoles)-four hydration zinc impregnation 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 zinc chloride and generates two (1,5- dinitro aminotetrazoles)-four hydration zinc potassium.
Two (1,5- dinitro aminotetrazoles)-four of the invention are hydrated zinc impregnation potassium compound, and structural formula is such as shown in (I):
The synthetic method of two (1,5- dinitro aminotetrazoles)-four hydration zinc 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- dinitro aminotetrazoles)-four hydration zinc potassium
At room temperature, 1,5- dinitro aminotetrazole sylvite, water are added in reaction flask, after stirring and dissolving, zinc chloride are added, adds
Heat is to 50 DEG C of reaction 2h, cooling, filtering, and filtrate, cooling, filtering, dry clear crystal is concentrated under reduced pressure;Wherein bis- nitramine of 1,5-
The molar ratio of base tetrazolium sylvite and zinc chloride is 1:1~2.
Advantages of the present invention:
The quick-fried appearance of two (1,5- dinitro aminotetrazoles)-four hydration zinc impregnation potassium compound of the invention is larger, quick-fried to hold for 568L/
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
Dinitro aminotetrazole)-four hydration zinc impregnation potassium compound energy are higher, and explosion velocity 7673m/s, quick-fried heat is 4051J/g, and comparison is literary
The explosion velocity that four (5- nitro tetrazolium) two hydrated irons (II) of part change sodium is 5550m/s, and quick-fried heat is 3929J/g.
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- dinitro aminotetrazoles)-four hydration zinc potassium
At room temperature, 0.133g (0.5mmol) 1,5- dinitro aminotetrazole sylvite, 3.0mL water are added in reaction flask, stirring
After dissolution, 0.075g (0.55mmol) zinc chloride is added, is heated to 50 DEG C of reaction 2h, cooling, filtering is reduced pressure filtrate, cold
But, filtering, dry 0.061g clear crystal, yield 41.5%.
Structural Identification:
Infrared spectroscopy: IR (KBr, cm-1), υ: 3511,3441,1530,1444,1418,1356,1291,1107,1041,
919,859
Elemental analysis: molecular formula C2H8N16O12ZnK2
Theoretical value: C 4.06, H 1.36, N 37.87
Measured value: C 4.13, H 1.30, N 37.96
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=104.281 (2) °, γ=90 °,Z=2, μ=1.891mm-1, F (000)=592.
Above structure appraising datum confirms to obtain substance to be strictly two (1,5- dinitro aminotetrazoles)-four hydration zinc potassium.
The performance of two (1,5- dinitro aminotetrazoles)-four hydration zinc potassium of the invention
(1) physical and chemical performance
Appearance: clear crystal
Solubility: dimethyl sulfoxide, water etc. are soluble in;Insoluble in petroleum ether, n-hexane, ether, ethyl acetate, acetonitrile etc.
Density: 2.138g/cm3X-ray single crystal diffractometer
(2) detonation property
Explosion velocity: density 2.138g/cm3, calculating explosion velocity is 7673m/s K-J equation
Quick-fried heat: density 2.138g/cm3, calculating detonation pressure is 28.9GPa K-J equation
Quick-fried appearance: density 2.138g/cm3, calculate quick-fried hold for 568L/kg K-J equation
The purposes of two (1,5- dinitro aminotetrazoles)-four hydration zinc potassium of the invention
Two (1,5- dinitro aminotetrazoles)-four hydration zinc potassium of the invention has the characteristics that quick-fried appearance is larger, energy is higher,
It is expected to as novel environment friendly priming.
Claims (1)
1. one kind two (1,5- dinitro aminotetrazole)-four is hydrated zinc impregnation potassium compound, structural formula is such as shown in (I):
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