Method for synthesizing plasticizer 3-nitro furazan-4-methyl ether

A technology of nitrofurazan and synthesis method, which is applied in the synthesis of plasticizer 3-nitrofurazan-4-methyl ether, and in the field of plasticizer synthesis, which can solve problems such as delayed detonation

Inactive Publication Date: 2012-10-03
太仓市新星轻工助剂厂
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  • Summary
  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Nitrate is one of the plasticizers with the highest energy density at present, but this type of compound is sensitive to heat, mechanical action and chemical substances. The currently developed nitrate solid propellants are all Class I and Class II dangerous goods, and there are Delayed detonation and other dangerous phenomena whose mechanism is not fully understood

Method used

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Embodiment Construction

[0007] The raw materials ethyl cyanoacetate, hydroxylamine hydrochloride, sodium nitrite, sodium hydroxide, sodium borohydride, zinc chloride, concentrated sulfuric acid, hydrogen peroxide, thionyl chloride, pyridine, sodium methoxide, acetonitrile etc. used in the present invention are analysis Pure reagents.

[0008] (1) Synthesis of AFCA

[0009] Take 138g (2mol) sodium nitrite and 1600ml distilled water to make a solution, 226.4g (2mol) ethyl cyanoacetate and 140ml EtOH to make a solution, pour it into a 2L flask. Take 80ml85%H 3 PO 4 Add dropwise and stir at room temperature for 1h. Lower to 10°C and stir overnight. Add 16Og (4mol) NaOH, 278g (4mol) NH 2 OH·HCI and 336 g (6 mol) KOH, stirred for 1 h. Heated to reflux for 2h. Cool in an ice bath to ambient temperature and adjust the pH to 6 with concentrated hydrochloric acid, and filter off the white solid. Continue to adjust the pH until a white solid precipitates, filter with suction, and recrystallize the filte...

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Abstract

The invention discloses a method for synthesizing plasticizer 3-nitro furazan-4-methyl ether. The method comprises the following steps: adding hydroxylamine under the alkaline condition by taking ethyl cyanoacetate as a starting material to form a ring, so as to obtain 3-amino furazan-4-carboxylic acid; then, reducing carboxyl group on the furazan ring to an alcoholic extract hydroxyl group by using a sodium borohydride/zinc chloride system, so as to obtain 3-amino furazan-4-methanol; then, oxidizing an amino group on the furazan ring to a nitro group by using a hydrogen peroxide/concentrated sulphuric acid system, so as to obtain 3-nitro furazan-4-methanol; in the presence of pyridine, carrying out chloride substituent on the alcoholic extract hydroxyl group by using thionyl chloride, so as to obtain 3-nitro-4-chloromethyl methyl ether furazan; and finally, reacting 3-nitro-4-chloromethyl methyl ether furazan with sodium methoxide in acetonitrile to remove NaCl so as to obtain the target compound. Compared with the traditional nitrate plasticizer, the plasticizer synthesized by using the method has higher positive enthalpies of formation and thermal stability, lower sensitivity and melting point, and has potential application prospect in the field of solid propellants.

Description

technical field [0001] The invention belongs to the technical field of plastic additives, and relates to the synthesis of a plasticizer, in particular to a method for synthesizing the plasticizer 3-nitrofurazan-4-methyl ether. Background technique [0002] The main components that determine the energy of solid propellants are oxidizers, binders, plasticizers and fuels. The binder system composed of binders and plasticizers is the basis for solid propellants to have mechanical and processing properties. Nitrate is one of the plasticizers with the highest energy density at present, but this type of compound is sensitive to heat, mechanical action and chemical substances. The currently developed nitrate solid propellants are all Class I and Class II dangerous goods, and there are Delayed detonation and other dangerous phenomena whose mechanism is not fully understood. [0003] Furazan compounds are a popular research object in the field of energetic materials in recent years. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D271/08C06D5/00
Inventor 李树叶
Owner 太仓市新星轻工助剂厂
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