Tetra-azido alkane and preparation method thereof

A technology of tetraazide-based alkanes and nitrogen-based alkanes, which is applied in the field of tetraazide-based alkanes and their preparation, can solve the problems that the preparation technology cannot be widely popularized and applied, and the burning speed is slow, and the synthesis process is simple and stable, and the burning speed is fast. , good speed-up performance

Inactive Publication Date: 2012-07-25
XINXIANG UNIV
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Problems solved by technology

At present, the tetraazide alkanes that have been synthesized mainly include azide derivatives of pentaerythritol, which can provide more energy for energetic materials because of their four azide groups, but because of their slow burning speed, making its preparation technology can not be widely applied
In view of this, the synthesis of new tetraazido derivatives with fast burning speed has become a research hotspot, and 2,6-diazido-1,7-diazidoheptane has not yet seen relevant information on its synthesis and performance. to report

Method used

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  • Tetra-azido alkane and preparation method thereof
  • Tetra-azido alkane and preparation method thereof
  • Tetra-azido alkane and preparation method thereof

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Embodiment Construction

[0010] The principle of the synthesis method of the tetraazide alkane of the present invention is that the optional alkali metal azide compounds include lithium azide, potassium azide and sodium azide, among which sodium azide is preferred. The separation of the product is carried out by column chromatography on a silica gel column to obtain the azide product.

[0011] Concrete synthetic route is as follows:

[0012]

[0013]

[0014]

[0015]

[0016]

[0017]

[0018]

[0019]

[0020] where n=2, 3, 4, 5 or 6.

[0021] Synthetic method of the present invention has the following steps:

[0022] 1 Preparation and characterization of tetraethyl 1,1,5,5-pentane tetracarboxylate

[0023] Under nitrogen protection, add 3.45g of sodium block into 75mL of absolute ethanol and dissolve at low temperature (-10°C-10°C). Reflux until the reaction is complete, and finally add 5.1 mL of 1,3-dibromopropane dropwise to the mixed solution. After the dropwise additi...

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Abstract

The invention discloses a tetra-azido alkane and a preparation method thereof. A structural formula of the tetra-azido alkane is (N3CH2)2CH(CH2)3CH(CH2N3)2. The preparation method comprises the following steps of: under the protection of nitrogen, reacting diethyl malonate and 1,3-dibromopropane at a low temperature to obtain tetracthyl-1,1,5,5-pentanctetracarboxylate; under the protection of the nitrogen, carrying out ice bath at below 5 DEG C, and reacting the tetracthyl-1,1,5,5-pentanctetracarboxylate and a tetrahydroaluminate diethyl ether solution to obtain 2,6-dihydromethyl-1,7-heptandiol; carrying out the ice bath at below 5 DEG C, reacting paratoluensulfonyl chloride and a pyridine solution of the 2,6-dihydromethyl-1,7-heptandiol for 10h, and carrying out chloroform recrystallization to obtain 2,6-p-ditoluenosulfonate methyl-1,7-p-ditoluenosulfonate methyl heptaester; and adding an aqueous solution of sodium azide to a dimethylformamide solution of the 2,6-p-ditoluenosulfonate methyl-1,7-p-ditoluenosulfonate methyl heptaester to react for 15h at 80 DEG C to obtain a 2,6-biazido-1,7-di-azido heptane product.

Description

Technical field: [0001] The present invention relates to a kind of high heat energy compound, especially a kind of tetraazide alkanes and its preparation method. Background technique: [0002] The use of azide-based binders, plasticizers, oxidants and other additives in energetic materials such as propellants, propellants and high-energy explosives can not only increase the energy level (each azide group can provide 356kJ / mol Formation enthalpy), can also endow it with many other excellent properties: increase the nitrogen content of the system without affecting its carbon-hydrogen ratio, increase the exhaust volume of the system during combustion; increase the burning speed of propellant or propellant without increasing Flame temperature; reduces the target signature produced by various propulsion systems, thereby increasing the stealth of the weapon. The azide compounds that have been synthesized are generally divided into azide polyethers, azide nitroamines, azide nitro ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C247/04
Inventor 刘冰周勇梁宇李丽
Owner XINXIANG UNIV
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