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Aqueous metal ion pentazole salts and preparation method thereof

A technology of metal ions and pentazolium salts, which is applied in the field of pentazolium anion salts and their synthesis, can solve the problems of no progress and achieve the effect of wide application

Active Publication Date: 2017-11-21
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since then about N 5 ˉThe report did not make any progress, only some theoretical calculations were reported. Until 2016, Haas et al. reported that the C in the aryl pentazole molecule was selectively cut off by reduction cleavage at low temperature using metal sodium as the cutting reagent. -N bond, N was first detected in a mass spectrometer 5 The signal of ˉ confirms that N 5 ˉIons can exist in solution at low temperature (≤-40°C)[ Angew Chem Int Ed, 2016, 55(42), 13233-13235]

Method used

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  • Aqueous metal ion pentazole salts and preparation method thereof
  • Aqueous metal ion pentazole salts and preparation method thereof
  • Aqueous metal ion pentazole salts and preparation method thereof

Examples

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Embodiment example 1

[0037] Example 1: Dissolve 3,5-dimethyl-4-hydroxyphenylpentazole (3 mmol) in a mixed solvent of methanol and acetonitrile in a single-necked flask, and add ferrous glycinate under the reaction condition of -45 °C (6 mmol) in methanol aqueous solution (pre-cooled to -45 °C), stirred for 30 min, then added m-chloroperoxybenzoic acid (Wt85%) (12 mmol) in methanol solution (pre-cooled to -45 °C), and reacted for 36 h. Filtrate, remove most of the solvent by rotary evaporation, extract by separation, combine the aqueous phases, then add cobalt chloride hexahydrate (3 mmol), stir and react at 25 °C for 3 h, and spin through the column to obtain 58.4 mg pentazole metal salt Co(N 5 )2 (H 2 O) 8 , yield 11.35%.

Embodiment example 2

[0038] Example 2: Dissolve 3,5-dimethyl-4-hydroxyphenylpentazole (3 mmol) in a mixed solvent of methanol and acetonitrile in a single-necked flask, and add ferrous glycinate under the reaction condition of -45 °C (6 mmol) in methanol aqueous solution (pre-cooled to -45 °C), stirred for 30 min, then added m-chloroperoxybenzoic acid (Wt85%) (12 mmol) in methanol solution (pre-cooled to -45 °C), and reacted for 36 h. Filtration, rotary evaporation to remove most of the solvent, liquid separation extraction, combined water phase, then added cobalt nitrate hexahydrate (6 mmol), stirred at 25 °C for 6 h, rotary evaporation through the column to obtain 63.1 mg pentazole metal salt Co(N 5 ) 2 (H 2 O) 8 , yield 12.26%.

Embodiment example 3

[0039] Example 3: Dissolve 3,5-dimethyl-4-hydroxyphenylpentazole (3 mmol) in a mixed solvent of methanol and acetonitrile in a single-necked flask, and add ferrous glycinate under the reaction condition of -45 °C (6 mmol) in methanol aqueous solution (pre-cooled to -45 °C), stirred for 30 min, then added m-chloroperoxybenzoic acid (Wt85%) (12 mmol) in methanol solution (pre-cooled to -45 °C), and reacted for 36 h. Filtration, rotary evaporation to remove most of the solvent, liquid separation extraction, combined water phase, then added cobalt sulfate heptahydrate (9 mmol), stirred at 30 °C for 6 h, rotary evaporation through the column to obtain 56.4 mg pentazole metal salt Co(N 5 ) 2 (H 2 O) 8 , yield 10.96%.

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Abstract

The invention discloses aqueous metal ion pentazole salts and a preparation method thereof. The metal salts have a chemical structural formula of M(N5)x(H2O)y. When M represents a monovalent metal Li, Na, K or Ag, x is 1 and y is 4. When M represents a divalent metal Fe, Co, Ni, Mg, Ca, Ba, Cu, Zn or Pb, x is 2 and y is 8 or 10. The preparation method utilizes metachloroperbenzoic acid and ferrous glycinate as a cleavage reagent and an aid acting with aryl pentazole. Through an oxidative cleavage method, the C-N bond of the aryl pentazol molecule is selectively cut and a metal ion-containing salt is used as a capture reagent in preparation of the aqueous metal ion pentazole salts. The preparation method successfully prepares the metal pentazole salts. The metal pentazole salts can be widely used in the field of energetic materials.

Description

technical field [0001] The invention relates to a class of pentazole anion salts containing metal ions and a synthesis method thereof, belonging to the research field of high-energy energetic materials. Background technique [0002] The chemical structural formula of the pentazolium anion is as follows: [0003] [0004] New ultra-high-energy energetic materials are the focus of the development of various military powers in the world today, and they are also an important symbol of the country's core military capabilities and commanding heights of military technology in the future. Total nitrogen substances have high density, high enthalpy of formation, ultra-high energy and explosive The detonation product is clean and pollution-free and has become a typical representative of a new generation of ultra-high-energy energetic materials. It is expected to be used as a new generation of ultra-high-energy energetic materials in the fields of explosives, propellants and propella...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D259/00C06B43/00
CPCC06B43/00C07D259/00
Inventor 胡炳成章冲孙呈郭杨陈郑占胜
Owner NANJING UNIV OF SCI & TECH
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