Method for preparing nickel hydrazine azide

A technology of nickel salt and sodium nitride, which is applied in the direction of azide/azide/halogen azide, etc., can solve the problems affecting the feasibility and rationality of the process, environmental and personnel pollution, inconsistent drug quality, etc., and achieve Effects of reduced mechanical sensitivity, increased detonation ability, and stable pH

Inactive Publication Date: 2010-01-06
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the above preparation process, the main problems that exist are: (1) nickel nitrate and sodium nitride are mixed, and HN is easily released due to high acidity. 3 Toxic gas, causing pollution and injury to the environment and personnel; (2) The mixed solution of nickel nitrate and sodium nitride will form a gelatinous substance when left for a long time, thus affecting the feasibility and rationality of the process , and it is easy to cause pipeline blockage; (3) The pH value of the compounding process is unstable, resulting in inconsistent pharmaceutical quality

Method used

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  • Method for preparing nickel hydrazine azide
  • Method for preparing nickel hydrazine azide
  • Method for preparing nickel hydrazine azide

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Embodiment 1: in conjunction with Fig. 1, raw material specification and requirement: hydrazine hydrate (N 2 h 4 ·H 2 O)AR, nickel acetate (NiAc 2 4H 2 O)CP, sodium nitride (NaN 3 ) CP, graphite 1000 mesh, acetic acid (HAc) CP, ethanol (C 2 h 5 OH)CP, main instruments and equipment: electric mixer; voltage regulating transformer; super constant temperature water bath; tall beaker (combiner) 400mL, metering pump, Buchner funnel Φ65mm; filter bottle 1000mL, water bath oven, water circulation vacuum pump.

[0014] According to the raw material feeding ratio (mass ratio): Ni(Ac) 2 4H 2 O:NaN 3 :N 2 h 4 ·H 2 O=1.76:1:0.80, weigh 12.3g of nickel acetate, dissolve it with 160mL of pure water, filter it and transfer it to a combiner, then add 4.0mL of acetic acid and 100mg of graphite; then weigh 7.0g of sodium nitride and measure Dissolve and dilute 6.0mL of hydrazine hydrate with 30mL of pure water, put them into small beakers after filtering, and set aside. Inst...

Embodiment 2

[0023] Embodiment 2: by raw material charging ratio (mass ratio): Ni(Ac) 2 4H 2 O:NaN 3 :N 2 h 4 ·H 2 O=1.76:1:0.80, weigh 14g of nickel acetate, dissolve it with 120mL of pure water, filter it and transfer it to the compounder, then add 3.5mL of acetic acid and 100mg of graphite; then weigh 7.0g of sodium nitride and measure 6.0 mL of hydrazine hydrate was dissolved and diluted with 90mL and 60mL of pure water respectively, filtered and put into small beakers respectively for later use. Install the reaction device and calibrate the metering pump. Heat in a constant temperature water bath to raise the temperature of the bottom liquid to 70°C, and at the same time start the stirrer and adjust the voltage to an appropriate stirring state. Slowly, uniformly and accurately add the sodium nitride and hydrazine hydrate solution dropwise through the metering pump, controlling the feeding time of sodium nitride to be 30min±5min, and the feeding time of hydrazine hydrate to be 45...

Embodiment 3

[0024] Embodiment 3: according to raw material charging ratio (mass ratio): Ni(Ac) 2 4H 2 O:NaN 3 :N 2 h 4 ·H 2 O=1.76:1:0.80, weigh 12.3g of nickel acetate, dissolve it with 120mL of pure water, filter it and transfer it to a combiner, then add 3.5mL of acetic acid and 100mg of graphite; then weigh 7.0g of sodium nitride and measure Dissolve and dilute 5.6mL of hydrazine hydrate with 30mL and 30mL of pure water respectively, put them into small beakers after filtering, and set aside. Install the reaction device and calibrate the metering pump. Heat in a constant temperature water bath to raise the temperature of the bottom solution to 65°C, and at the same time start the stirrer and adjust the voltage to an appropriate stirring state. Slowly, uniformly and accurately add the sodium nitride and hydrazine hydrate solution dropwise through the metering pump, controlling the feeding time of sodium nitride to be 30min±2min, and the feeding time of hydrazine hydrate to be 45m...

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Abstract

The invention discloses a method for preparing nickel hydrazine azide. The method comprises: taking soluble nickel salts as base solution; using acetic acid to adjust the pH of the formed base solution; using graphite as modified additives of medicaments; adding sodium nitride solution and hydrazine hydrate solution to the base solution dropwise to perform chemical combination; preserving heat, cooling, leaching, washing, dehydrating and drying; and obtaining a finished product of nickel hydrazine azide. The method is simple in pH control, and buffer solution consisting of weak acid and weak-acid salts ensures stable pH, longer effectiveness and the unicity of medicament composition, and significantly improves explosion initiation capacity, so the buffer solution is more suitable to be used as a primary explosive. By adopting nickel acetate as raw material, a small quantity of nickel hydrazine nitrate substances which are formed by use of nitrates and result in worse or unstable pharmaceutical performance can be avoided. Dropping and time difference ensure the complete reaction of sodium nitride and high yield of nickel hydrazine azide.

Description

technical field [0001] The invention relates to a preparation method of a primary explosive, in particular to a preparation method of a nickel hydrazine compound. Background technique [0002] Currently, agents used as primers include lead azide (LA), lead styphenate (LTNR), dinitrodiazophenol (DDNP), cadmium perchlorate carbohydrazide (GTG) and nickel hydrazine nitrate (NHN ). The latter two agents, together with nickel azide, belong to energetic complexes. The order of their power is: LA>GTG>NHN>DDNP>LTNR, and the order of flame sensitivity is just the opposite. Lead azide, cadmium perchlorate carbohydrazide, and lead styphate at both ends, in practical applications, either need to be filled with igniting powder because the flame sensitivity is too low, or cannot be used alone because of the low power. At the same time, there are problems such as high mechanical sensitivity of lead azide, high electrostatic spark sensitivity of lead styphate, weak detonation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/08
Inventor 朱顺官李燕张琳牟景艳
Owner NANJING UNIV OF SCI & TECH
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