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A method for preparing large and round ε-hniw crystals with different concentrations

A technology of large particles and crystals, which is applied in the field of preparing large particles and smooth ε-HNIW crystals, which can solve the problems of poor morphology and achieve the effects of smooth crystals, easy industrialization, and simple operation

Active Publication Date: 2019-02-12
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The anti-solvent is chloroform and xylene, and the process of adding seed crystals is also considered. After many experiments, the samples after recrystallization are reunited without adding seeds. Although they do not reunite after adding seeds, their morphology is very Difference

Method used

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  • A method for preparing large and round ε-hniw crystals with different concentrations
  • A method for preparing large and round ε-hniw crystals with different concentrations
  • A method for preparing large and round ε-hniw crystals with different concentrations

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 7g of HNIW in 20mL of industrial ethyl acetate, filter the solution for use as filtrate A, dissolve 40g of HNIW in 100mL of industrial ethyl acetate, filter the solution for use as filtrate B; first wash the crystallization kettle with industrial ethyl acetate, and then use industrial Rinse with n-octane, then add 50ml of industrial n-octane to the crystallization kettle, place the crystallization kettle in a constant temperature water bath at 40°C; turn on the agitator, preheat and keep warm at a low speed of 100rpm until the temperature of the anti-solvent is the same as the water temperature in the jacket; Then the stirring speed is adjusted to 350rpm, and the constant flow pump is started to drip the filtrate A in the crystallization tank at a rate of 40mL / min; after all the addition is completed, continue to stir for 35min; Add the filtrate B dropwise to the crystallization kettle with the constant flow pump, stir for 2 minutes after all the addition is com...

Embodiment 2

[0028] Dissolve 12g of HNIW in 40mL of industrial ethyl acetate, filter the solution for use as filtrate A, dissolve 80g of HNIW in 200mL of industrial ethyl acetate, filter the solution for use as filtrate B; first wash the crystallization kettle with industrial ethyl acetate, and then use industrial Rinse with n-octane, then add 120ml of industrial n-octane to the crystallization kettle, place the crystallization kettle in a 40°C constant temperature water bath; turn on the stirrer, preheat and keep warm at a low speed of 100rpm until the temperature of the anti-solvent is the same as the water temperature in the jacket, Then the stirrer speed was adjusted to 350rpm, and the constant flow pump was turned on to drip the filtrate A into the crystallization tank at a rate of 50mL / min; Add the filtrate B dropwise to the crystallization kettle with the pump, and stir for 2 minutes after all the addition is completed, then turn on the constant flow pump and add 400ml of n-octane dr...

Embodiment 3

[0031] Dissolve 160g of HNIW in 500mL of industrial ethyl acetate, filter the solution for use as filtrate A, dissolve 1kg of HNIW in 2.5L of industrial ethyl acetate, filter the solution for use as filtrate B; wash the crystallization kettle with industrial ethyl acetate first, and then use Rinse with industrial n-octane, then add 1.5L industrial n-octane to the crystallization kettle, place the crystallization kettle in a constant temperature water bath at 38°C; turn on the stirrer, preheat and keep warm at a low speed of 100rpm until the temperature of the anti-solvent is the same as the water temperature in the jacket The same, then adjust the stirrer speed to 300rpm, turn on the constant flow pump to drip the filtrate A into the crystallization tank at a rate of 35mL / min; Add the filtrate B dropwise to the crystallization kettle with the constant flow pump, stir for 5 minutes after all the addition is completed, then turn on the constant flow pump and add 6L n-octane dropw...

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Abstract

The invention relates to a method for preparing large-grain smooth epsilon-HNIW crystals by a different-concentration process, belonging to the field of energetic materials. The method comprises the following steps: adding low-concentration HNIW into a counter solvent, and continuously stirring to precipitate crystals; adding high-concentration HNIW, stirring uniformly, and adding a large amount of counter solvent to precipitate the crystals from the solution; and filtering, washing and drying to obtain the large-grain smooth epsilon-HNIW crystals. The different-concentration process is utilized to prepare the large-grain smooth epsilon-HNIW crystals. The technique is simple to operate, has the advantages of low counter solvent consumption, recoverable counter solvent, mild reaction conditions, high safety and reliability, environment protection, high efficiency and the like, and can easily implement industrialization.

Description

technical field [0001] The invention relates to a method for preparing large-particle smooth ε-HNIW crystals with different concentration methods, and belongs to the field of energetic materials. Background technique [0002] Hexanitrohexaazaisowurtzitane (HNIW or CL-20) is a cage polynitroamine high-energy compound and one of the best single-substance explosives in the world today. HNIW has a variety of crystal forms, and there are four crystal forms (α, β, γ and ε) under normal temperature and pressure, among which the theoretical density of the ε crystal form is as high as 2.044g / cm 3 , the detonation velocity can reach 9.5km / s-9.6km / s, the detonation pressure can reach 42GPa-43GP, and the energy output is 10-14% higher than that of HMX. Can components. [0003] So far, among the high energy density materials synthesized, HNIW is the most promising to replace HMX. However, due to factors such as high sensitivity, irregular crystal shape, and wide particle size distribut...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07B2200/13C07D487/22
Inventor 郭学永张洪垒焦清介黄阳飞崔超任慧
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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