Morphology improvement method of LLM-105 explosives on basis of crystal-form modifying agent

A technology for modifiers and explosives, applied in the field of improving the morphology of LLM-105 explosives based on crystal modifiers, can solve problems such as poor solubility, achieve mild reaction conditions, improve crystal morphology, and have good safety effects

Active Publication Date: 2015-05-13
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, due to the poor solubility of LLM-105 (2,6-diamino-3,5-dinitropyrazine-1-oxide) explosives, there is only some solubility in polar aprotic solvents, with Most of the LLM-105 crystals obtained

Method used

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  • Morphology improvement method of LLM-105 explosives on basis of crystal-form modifying agent
  • Morphology improvement method of LLM-105 explosives on basis of crystal-form modifying agent
  • Morphology improvement method of LLM-105 explosives on basis of crystal-form modifying agent

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Experimental program
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Effect test

Embodiment 1

[0034] At room temperature, add 100g of dimethyl sulfoxide into the crystallizer, then add 6g of raw material LLM-105 explosive under stirring, raise the temperature to 80°C to obtain a saturated solution of LLM-105 explosive; then add 0.06g Add urea in the saturated solution of LLM-105 explosive, stir evenly, then adopt the dissolution crystallization method, drop ethyl acetate 300g with the speed of 2ml / min at this temperature, filter, wash, dry to obtain such as figure 1 The needle-like LLM-105 crystal shown is 5.16 g, and the yield is 86%.

Embodiment 2

[0036] At room temperature, add 300g of dimethylformamide into the crystallizer, then add 6g of raw material LLM-105 explosive under stirring, raise the temperature to 65°C to obtain a saturated solution of LLM-105 explosive; then add 0.1g Cyclohexanone was added to the saturated solution of LLM-105 explosives, stirred evenly, and then using the dissolution crystallization method, 600g of absolute ethanol was added dropwise at a speed of 2ml / min at this temperature, filtered, washed, and dried to obtain needle-shaped LLM- 4.62 g of 105 crystals, yield 77%.

Embodiment 3

[0038] At room temperature, add 100g of dimethyl sulfoxide into the crystallizer, then add 6g of raw material LLM-105 explosive under stirring, raise the temperature to 90°C to obtain a saturated solution of LLM-105 explosive; then add 0.06g Glycine is added in the saturated solution of LLM-105 explosive, stirs evenly, adopts elution crystallization method then, drops anhydrous methanol 300g with the speed of 1ml / min at this temperature, filters, washes, dries to obtain such as figure 2 The shown rod-shaped LLM-105 crystals were 5.34 g, and the yield was 89%.

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Abstract

The invention discloses a morphology improvement method of LLM-105 explosives on the basis of a crystal-form modifying agent. The morphology improvement method comprises the following steps of: firstly adding the LLM-105 explosives into a recrystallization solvent to obtain saturated solution of the LLM-105 explosives under the temperature of 20-150 DEG C, then adding one or more in a ketone-type crystal-form modifying agent, an acid-type crystal-form modifying agent, an amide-type crystal-form modifying agent, a polymer-type crystal-form modifying agent and an ion-liquid-type crystal-form modifying agent into the saturated solution of the LLM-105 explosives and stirring to be uniform; and finally, adopting a solvent-out crystallization method to obtain LLM-105 crystals. The morphology improvement method disclosed by the invention has the advantages that the crystal morphology of the LLM-105 explosives can be effectively improved; the prepared crystal of the LLM-105 explosives with regular morphology such as a rod shape, a needle shape and a block shape is prepared and obtained; the preparation method is simple in process route, is moderate in reaction condition and good in safety; and all the solvents can be recovered, so that environmental pollution can not be caused and the suitability for batch production is achieved.

Description

technical field [0001] Embodiments of the present invention relate to the field of energetic materials, more specifically, embodiments of the present invention relate to a method for improving the morphology of LLM-105 explosives based on crystal modifiers, which has good application prospects in insensitive ammunition . Background technique [0002] At present, the morphology control of general explosives mainly uses conventional crystallization conditions such as different types of crystallization solvents, changing crystallization temperature, and stirring speed. However, due to the poor solubility of LLM-105 (2,6-diamino-3,5-dinitropyrazine-1-oxide) explosives, there is only some solubility in polar aprotic solvents, with Most of the LLM-105 crystals obtained by solvent crystallization are cross-shaped rod-shaped twins. Moreover, due to the molecular structure of LLM-105 explosive itself, it is difficult to improve its morphology by conventional methods. [0003] Crys...

Claims

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Application Information

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IPC IPC(8): C07D241/20
CPCC07D241/20
Inventor 周小清张祺李洪珍陈东徐容廖龙渝杨宗伟程碧波卢欢畅
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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