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Kilogram-grade preparation method of 3,3'-diamino-4,4'-azoxyfurazan

A technology of azofurazan oxide and diamino, which is applied in organic chemistry, offensive equipment, explosives processing equipment and other directions, can solve the problems of a large amount of acidic waste liquid, unsuitable process amplification, long reaction time, etc., and achieves optimized preparation process, reaction The effect of short time and simple preparation method

Inactive Publication Date: 2019-01-18
SOUTHWEAT UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, the synthetic technique of DAOAF mainly contains two kinds: (1) with suitable oxidizing agent, as potassium persulfate compound salt (Oxone), H 2 o 2 / HNO 3 -H 2 SO 4 Synthesis of DAOAF by oxidation of 3,4-diaminofurazan, in which H 2 o 2 / HNO 3 -H 2 SO 4 When it is an oxidizing agent, the yield of DAOAF is 96.8%, and the purity is 99.2%, but the reaction time is longer (20h), and it is easy to produce a large amount of acidic waste liquid, which is not suitable for process amplification; (2) with 3,4-diaminofurazan As a raw material, first formylate in formic acid solution to obtain intermediates 3-amino-4-formylaminofurazan and 3,4-diformylaminofurazan, and then undergo H 2 o 2 Oxidation to obtain DAOAF, the process has problems such as many reaction steps, long time and high cost, which is contrary to the preparation requirements of explosives

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  • Kilogram-grade preparation method of 3,3'-diamino-4,4'-azoxyfurazan

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Embodiment 1

[0041] The kilogram-level preparation method of 3,3'-diamino-4,4'-azofurazan, the steps are:

[0042] a. Efficient preparation of intermediate 3,4-diaminofurazan:

[0043] Under ice-bath temperature and stirring, add 1.0mol glyoxal into the reactor (three-necked flask), add 6.5mol hydroxylamine hydrochloride, and then slowly dropwise add 7.0mol sodium hydroxide solution in 600mL water to the reaction vessel. Add sodium hydroxide aqueous solution dropwise at a temperature <10°C; after dropping, raise the temperature to 100-108°C, reflux for 7 hours, add 5.8mol urea, and heat up to 100-110°C for reflux After reacting for 14 hours, after the reaction, the material was cooled (placed in a refrigerator) and kept in a refrigerator at 0-6°C, and white needle-like crystals were precipitated, namely the prepared 3,4-diaminofurazan, with a yield of 44% and a purity of 99.6% (HPLC area normalization method);

[0044] b. Efficient preparation of high-purity DAOAF:

[0045] Add 10.0 mol...

Embodiment 2

[0049] The kilogram-level preparation method of 3,3'-diamino-4,4'-azofurazan, the steps are:

[0050] a. Efficient preparation of intermediate 3,4-diaminofurazan:

[0051] Under ice-bath temperature and stirring, 115mL volume percent content is that 40% glyoxal aqueous solution is added in the reactor (three-necked flask), adds 450g hydroxylamine hydrochloride, then 280g sodium hydroxide is dissolved in the sodium hydroxide aqueous solution of 600mL water (Slowly) dropwise into the reactor (three-necked flask), and keep the temperature <10°C and dropwise add sodium hydroxide aqueous solution; after dropping, raise the temperature to 100-108°C, and reflux for 7h. Add 350g of urea, raise the temperature to 100-110°C for reflux reaction for 20 hours; after the reaction, the material is cooled (placed in the refrigerator) and refrigerated at 0-6°C, white needle-like crystals are precipitated, that is, the prepared 3,4-di Aminofurazan, yield 50%, purity 99.8% (HPLC area normalizat...

Embodiment 3

[0056] The kilogram-level preparation method of 3,3'-diamino-4,4'-azofurazan, the steps are:

[0057] a. Efficient preparation of intermediate 3,4-diaminofurazan:

[0058] Under ice-bath temperature and stirring, 115mL volume percent content is that 40% glyoxal aqueous solution is added in the reactor (three-necked flask), adds 450g hydroxylamine hydrochloride, then 280g sodium hydroxide is dissolved in the sodium hydroxide aqueous solution of 600mL water (Slowly) dropwise into the reactor (three-necked flask), and keep the temperature <10°C and dropwise add sodium hydroxide aqueous solution; after dropping, raise the temperature to 100-108°C, and reflux for 7h. 350g of urea was added, and the temperature was raised to 100-110°C for reflux reaction for 24h. After the reaction solution was cooled (placed in the refrigerator), it was refrigerated and left standing at 0-6°C, and white needle-like crystals were precipitated, namely the prepared 3,4-diaminofurazan, with a yield of...

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Abstract

The invention discloses a kilogram-grade preparation method of 3,3'-diamino-4,4'-azoxyfurazan. The kilogram-grade preparation method is characterized by comprising the following steps: taking glyoxaland the like as raw materials; enabling the raw materials and hydroxylamine hydrochloride to react under an alkaline condition to synthesize an intermediate 3,4-diaminofurazan; then oxidizing the 3,4-diaminofurazan in a sodium bicarbonate solution through potassium bisulfate to obtain a crude product; recrystallizing the crude product to remove impurities, so as to obtain the high-purity 3,3'-diamino-4,4'-azoxyfurazan with the purity of 99.6 percent. The preparation method disclosed by the invention has the advantages of simplicity, short reaction time and stable technology; the prepared 3,3'-diamino-4,4'-azoxyfurazan is especially applicable as initiating explosive for a slapper plate detonator.

Description

technical field [0001] The present invention belongs to the preparation of organic compounds, and relates to the kilogram-level preparation method of 3,3'-diamino-4,4'-azofurazan. The 3,3'-diamino-4,4'- Azofurazan oxide is suitable as the primary explosive for various engineering detonators, especially for (high-safety) primary explosives for shock-disc detonators. Background technique [0002] As a new type of detonating agent, it should at least have sufficient detonating ability, appropriate sensitivity, high stability, fluidity and compressibility and many other stringent requirements. In terms of preparation, it requires easy access to raw materials, simple production process, and safe operation. Good process stability and less "three wastes" or easy treatment and no pollution. Therefore, exploring and preparing new primers suitable for various engineering detonators has become one of the hotspots in the research of energetic materials. [0003] 3,3′-Diamino-4,4′-Azof...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D271/08C06B21/00C06B43/00
CPCC06B21/00C06B43/00C07D271/08
Inventor 李鸿波王小旭黄明张勇吴金婷陈明龙孟俞富
Owner SOUTHWEAT UNIV OF SCI & TECH
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