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Preparation method of glycidyl azide polymer modified micro-nano zirconium composite particles

A technology of glycidyl ether and composite particles, which is applied in the generation of compressed gas and attacking equipment, etc., can solve the problems of high electrostatic spark sensitivity, reduced electrostatic spark sensitivity, and unsafety, so as to improve the use safety performance and reduce the electrostatic spark sensitivity , the effect of high nitrogen content

Active Publication Date: 2015-01-28
XIAN MODERN CHEM RES INST
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Problems solved by technology

[0003] Although zirconium powder has good ignition performance and combustion performance, the electrostatic spark sensitivity of ultra-fine zirconium powder is relatively high, about 0.3-0.5mJ, and it is easy to ignite and burn under the stimulation of environmental static electricity. In severe cases, it will cause dust explosion. Accidents, so that there are certain safety hazards in production, transportation, storage and use
In addition to being unsafe, due to the large specific surface area of ​​micro-nano-sized zirconium powder, there are also problems such as difficulty in dispersion and poor rheology in use.
A zirconium composite particle coated with hydroxyl-terminated polybutadiene (HTPB) was disclosed in Nanjing University of Science and Technology Liang Jiyuan's master thesis "Preparation of Zirconium Composite Particles and Research on Electrostatic Sensitivity and Thermal Properties", Nanjing University of Science and Technology, 2010) , the electrostatic spark sensitivity is lower than that of the raw material zirconium powder before coating. Under the experimental conditions, the average explosion probability of Zr / HTPB composite particles is 50%, and the 50% ignition energy is 3.12×10 -3 J, but there is still a certain risk, and the coating agent HTPB itself does not contain energy and has a low density, which will reduce the density and specific impulse of the propellant, affecting the use effect, and still needs further improvement

Method used

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  • Preparation method of glycidyl azide polymer modified micro-nano zirconium composite particles
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  • Preparation method of glycidyl azide polymer modified micro-nano zirconium composite particles

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Experimental program
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Effect test

Embodiment 1

[0031] Weigh 5.0g of zirconium powder with an average particle size of 20μm, add 90mL of absolute ethanol and 10mL of water, ultrasonically disperse for 30min to disperse the zirconium powder evenly, then add 0.25g of silane coupling agent γ-aminopropyltriethoxysilane into the system, disperse and stir at 60°C for 2 hours, let stand, centrifuge, wash and dry in a vacuum oven for 12 hours to obtain pretreated zirconium powder.

[0032] Weigh 1.0 g of glycidyl azide (GAP) in 500 mL of acetone solution and dissolve it completely with ultrasonic waves to prepare a 2.0 g / L GAP solution.

[0033] Weigh 1.0g of pretreated zirconium powder and 125mL of cyclohexane into a three-necked flask, stir ultrasonically for 20min, and after the dispersion is even, slowly drop in 25mL of the above-mentioned GAP with a constant pressure dropping funnel at a rate of 1-2 drops / s. The solution was stirred for 4 hours after the dropwise addition, and the temperature of the reaction process was contro...

Embodiment 2

[0036] Weigh 5.0g of zirconium powder with an average particle size of 80nm, add 90mL of absolute ethanol and 10mL of water, ultrasonically disperse for 30min to disperse the zirconium powder evenly, then add 0.25g of silane coupling agent γ-glycidyl etheroxypropyl trimethoxy Add silane to the system, disperse and stir at 60°C for 2 hours, let stand, centrifuge, wash and dry in a vacuum oven for 12 hours to obtain pretreated zirconium powder.

[0037] Weigh 2.5g polyazide glycidyl ether (GAP) in 500mL acetone solution and dissolve it completely with ultrasonic waves to prepare 5.0g / L GAP solution.

[0038]Weigh 1.0g of pretreated zirconium powder and 75mL of cyclohexane into a three-necked flask, and stir ultrasonically for 20min until they are evenly dispersed, then slowly drop in 15mL of the above-mentioned GAP with a constant pressure dropping funnel at a rate of 1-2 drops / s. The solution was stirred for 6 hours after the dropwise addition, and the temperature of the reacti...

Embodiment 3

[0040] Weigh 5.0g of zirconium powder with an average particle size of 40nm, add 90mL of absolute ethanol and 10mL of water, and ultrasonically disperse for 30min to disperse the zirconium powder evenly, then add 0.25g of silane coupling agent γ-(methacryloyloxy)propane Add trimethoxysilane to the system, disperse and stir at 60°C for 2 hours, let stand, centrifuge, wash and dry in a vacuum oven for 12 hours to obtain pretreated zirconium powder.

[0041] Weigh 1.5g polyazide glycidyl ether (GAP) in 500mL acetone solution and dissolve it completely with ultrasonic wave to prepare 3.0g / L GAP solution.

[0042] Weigh 1.0g of pretreated zirconium powder and 45mL of cyclohexane into a three-necked flask, and stir ultrasonically for 20min until uniform dispersion, then slowly drop in 15mL of the above-mentioned GAP with a constant pressure dropping funnel at a rate of 1-2 drops / s. The solution was stirred for 6 hours after the dropwise addition, and the temperature of the reaction ...

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Abstract

The invention provides a preparation method of glycidyl azide polymer modified micro-nano zirconium composite particles. The preparation method comprises the following steps: (1) pretreatment of zirconium powder; and (2) preparation of the zirconium composite particles. According to the preparation method, the electrostatic spark sensitivity of the prepared zirconium composite particles is obviously reduced relative to the uncoated zirconium powder, so that the safety performance of the zirconium powder is improved to a great extent; the selected coating material glycidyl azide polymer which is used as an energetic adhesive is capable of providing energy during the combustion and has favorable consistency with the components of propellants, so that the practical application of the zirconium powder as a composite propellant fuel to ramjets and volume-limited solid rocket engines is promoted.

Description

technical field [0001] The invention relates to a chemical coating method, in particular to a preparation method for coating modified zirconium composite particles with polyazide glycidyl ether. Background technique [0002] Modern warfare requires missiles to be as small as possible while ensuring the range, so that on the one hand, it can reduce the chance of being discovered by the enemy and increase the survival rate of the missile; On weapon platforms that have strict restrictions on engine size, such as systems, the smaller the engine size, the smaller the air resistance it will suffer. Therefore, high-density specific impulse propellant has become an important direction of research and development. At present, high-density propellants are mainly achieved by adding high-density metal powder and high-energy-density materials. With the emergence of some explosives with special requirements for density, zirconium has more application advantages than other metals due to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C06D5/00
Inventor 姜菡雨赵凤起徐司雨姚二岗裴庆郝海霞胥会祥樊学忠谭艺
Owner XIAN MODERN CHEM RES INST
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