CN109761730B - Preparation method of HMX explosive with snowflake-shaped structure - Google Patents
Preparation method of HMX explosive with snowflake-shaped structure Download PDFInfo
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- CN109761730B CN109761730B CN201910222729.6A CN201910222729A CN109761730B CN 109761730 B CN109761730 B CN 109761730B CN 201910222729 A CN201910222729 A CN 201910222729A CN 109761730 B CN109761730 B CN 109761730B
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Abstract
The invention discloses a preparation method of an HMX explosive with a snowflake-shaped structure, belonging to the technical field of energetic materials. The method comprises the following steps: the method comprises the following steps: under the room temperature environment, adding HMX crystals into a first organic solvent, and completely dissolving the HMX crystals in a mechanical stirring manner to obtain a clear and transparent HMX solution; step two: and (3) sucking the HMX solution obtained in the step one by using an injector, injecting the HMX solution into a second organic solvent under the stirring condition, maintaining stirring for a period of time, filtering, washing with deionized water, and drying to obtain the HMX explosive with the snowflake-shaped structure. The HMX explosive prepared by the method has a unique fractal structure, and has important significance in national defense fields such as initiation and detonation sequences of weapon charging, micro initiation devices, initiating explosive device technology and the like. The preparation method has the advantages of simple process, short period, mild reaction conditions, easy amplification, low cost and the like, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of energetic materials, and particularly relates to a preparation method of an HMX explosive with a snowflake-shaped structure.
Background
1,3,5, 7-tetranitro-tetraazacyclooctane (HMX) is the high-energy single-substance explosive with the best comprehensive performance at present, has high energy density characteristic and excellent physical and chemical properties, and has wide application prospect in the fields of high-efficiency damage warheads, high-energy propellants, engineering blasting and the like. In order to further widen the application range of the HMX explosive in the field of energetic materials, explosive crystals with a multilevel structure (such as a snowflake structure) can be prepared. The structure can meet the requirement of high-energy output of explosives, simultaneously, the initiation and safety performance of HMX are more excellent, and the structure has important significance in national defense fields such as weapon explosive-charging initiation and detonation transfer sequences, micro initiation devices, initiating explosive technology and the like.
Due to the unique structure of different explosive crystal morphologies, especially crystals with multilevel structures, the performance of the explosive can be further improved to a great extent and the application range of the explosive can be expanded. The solvent/anti-solvent method is adopted by Guo university of Beijing Physician and the like to invent a preparation method (CN105732531A, 2016) for repairing/modifying the appearance of HMX crystals, so that the sensitivity of HMX is reduced to a certain extent, but the structure of the HMX is relatively single. Corbin et al invented a method (CN102503905B, 2012) for preparing ultrafine porous octogen, which is more favorable for explosive initiation, but the problem of easy agglomeration of crystal particles is still not effectively overcome. Chenya et al invented a method for preparing nano-grid octogen (CN103626711A, 2014), and nano-grid octogen powder with different microstructures can be obtained. Zhou Xiao Qing and the like invent a preparation method (CN109180397A, 2019) of sea urchin type 1-oxygen-diamino-3, 5-dinitropyrazine (LLM-105) explosive crystal particles, and the method can effectively improve the specific surface area and the fluidity of the LLM-105 explosive. Cheng et al (Crystal Research and Technology,2018,53,1700226) invented a flower-like HMX preparation method, but with relatively severe control of conditions. The new technologies have certain reference significance for the preparation of micron and nanometer explosives, but the HMX explosives with snowflake-shaped structures cannot be prepared. From the existing published information, some methods exist for preparing HMX fractal structures at present, but the problems of complex process flow, overhigh cost, environmentally-friendly preparation process and the like still exist.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a preparation method of an HMX explosive with a snowflake flake structure. The process flow of the snowflake-shaped HMX explosive manufactured by the method is simple, the process can be carried out at normal temperature, a reaction kettle is not used, the cost is low, and the preparation process is more environment-friendly.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an HMX explosive with a snowflake flake-shaped structure comprises the following steps:
the method comprises the following steps: under the room temperature environment, adding HMX crystals into a first organic solvent, and completely dissolving the HMX crystals in a mechanical stirring manner to obtain a clear and transparent HMX solution;
step two: and (3) sucking the HMX solution obtained in the step one by using a syringe, injecting the HMX solution into a second organic solvent under a stirring condition, maintaining stirring for a period of time, filtering, washing with deionized water, and drying to obtain the HMX explosive with a snowflake flake structure, wherein the HMX explosive has a typical fractal structure.
According to an embodiment of the present invention, in the first step of the preparation method, the first organic solvent is one of N, N-dimethylformamide, dimethyl sulfoxide, γ -butyrolactone, and N-methylpyrrolidone.
According to the embodiment of the invention, in the HMX solution obtained in the first step of the preparation method, the mass percentage concentration of the dissolved HMX crystals is 1% to 10%.
According to an embodiment of the present invention, in the second step of the preparation method, the second organic solvent is one of ethanol, methanol, isopropanol, and petroleum ether.
According to an embodiment of the present invention, in the second step of the above preparation method, the mass ratio of the HMX solution sucked in the syringe to the second organic solvent is 1: 1-1: 20.
according to the embodiment of the present invention, in the second step of the preparation method, the size of the pinhole aperture of the syringe used is 0.4mm to 1.6 mm.
According to an embodiment of the present invention, in the second step of the above preparation method, the injection rate of the HMX solution obtained in the first step into the second organic solvent under stirring is 1mL/s to 10mL/s by sucking with a syringe.
According to an embodiment of the present invention, in the second step of the above-mentioned preparation method, the stirring speed under the stirring condition is 100rpm to 300 rpm.
According to an embodiment of the present invention, in the second step of the preparation method, after the injection of the HMX solution obtained in the first step into the second organic solvent under stirring is completed, stirring is maintained, and the stirring time is maintained to be 2min to 20 min.
According to the embodiment of the invention, in the second step of the preparation method, the prepared HMX explosive with snowflake flake-shaped structure has the particle size of 80-200 μm, the thickness of the flake layer of 1-3 μm and the purity of the product is more than 99%.
Compared with the prior art, the invention has the beneficial effects that:
the product has a unique snowflake fractal structure, uniform particle appearance and good dispersion, and has wide application prospect in the fields of weapon charge and detonation transfer sequences, micro detonation devices and the like. The invention has simple preparation process, does not need large-scale complex equipment and can be realized by an injector; short period, mild reaction condition, easy amplification, low cost and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a snowflake flake-structured HMX explosive prepared according to example 1 of the invention by a factor of 200;
FIG. 2 is a 1000-fold scanning electron microscope image of a snowflake flake-shaped structure HMX explosive prepared according to example 1 of the invention;
FIG. 3 is an optical microscope photograph of snowflake flake structured HMX explosives prepared in accordance with example 1 of the present invention;
FIG. 4 is a 1000-fold scanning electron microscope image of a snowflake flake-shaped structure HMX explosive prepared according to example 2 of the invention;
FIG. 5 is an optical microscope photograph of snowflake flake structured HMX explosive prepared according to example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Example 1
Weighing 2.5g of HMX crystals at room temperature, adding the HMX crystals into 47.5g N, N-dimethylformamide, and completely dissolving the HMX crystals by means of mechanical stirring to obtain a clear and transparent HMX solution with the mass concentration of 5%. 20g of the dissolved HMX solution was aspirated by a syringe with a pore size of 0.4mm and injected into 40g of absolute ethanol under stirring at 200r/min at an injection rate of 1 mL/s. And (3) after stirring is maintained for 2min, filtering the material, washing the material with deionized water, and drying to obtain the HMX explosive with the snowflake-shaped structure. FIGS. 1 and 2 are respectively the 200-fold and 1000-fold scanning electron micrographs of the HMX explosive with snowflake lamellar structure obtained according to this example, and FIG. 3 is an optical microscope photograph. The explosive has a flake particle size of about 100 μm, a thickness of about 2 μm and a product purity of 99.3%.
Example 2
Weighing 2.5g of HMX crystals at room temperature, adding the HMX crystals into 22.5g of gamma-butyrolactone, and completely dissolving the HMX crystals by means of mechanical stirring to obtain a clear and transparent HMX solution with the mass concentration of 10%. 20g of the dissolved HMX solution was aspirated by a syringe with a pore size of 1.2mm and injected into 20g of methanol at 300r/min at an injection rate of 2 mL/s. And (3) after stirring is maintained for 5min, filtering the material, washing the material with deionized water, and drying to obtain the HMX explosive with the snowflake-shaped structure. FIG. 4 is a 1000-fold scanning electron micrograph of a snowflake lamellar structured HMX explosive obtained according to the example, and FIG. 5 is an optical micrograph. The explosive has a flake particle size of about 120 μm, a thickness of about 1.5 μm and a product purity of 99.5%.
Example 3
Weighing 2.5g of HMX crystals at room temperature, adding the HMX crystals into 247.5g of dimethyl sulfoxide, and completely dissolving the HMX crystals by means of mechanical stirring to obtain a clear and transparent HMX solution with the mass concentration of 1%. 20g of the dissolved HMX solution was aspirated by a syringe with a pore size of 1.0mm and injected into 400g of isopropanol at 300r/min at an injection rate of 5 mL/s. And (3) after stirring is maintained for 15min, filtering the material, washing the material with deionized water, and drying to obtain the HMX explosive with the snowflake-shaped structure. The explosive has a flake particle size of about 150 μm, a thickness of about 2 μm and a product purity of 99.2%.
Example 4
Weighing 2.5g of HMX crystals at room temperature, adding the HMX crystals into 22.5g of N-methyl pyrrolidone, and completely dissolving the HMX crystals by a mechanical stirring mode to obtain a clear and transparent HMX solution with the mass concentration of 10%. 20g of the dissolved HMX solution was aspirated by a syringe with a bore size of 0.8mm and injected into 200g of petroleum ether at 100r/min at an injection rate of 2 mL/s. And (3) after stirring is maintained for 5min, filtering the material, washing the material with deionized water, and drying to obtain the HMX explosive with the snowflake-shaped structure. The explosive has a flake particle size of about 110 μm, a thickness of about 2.5 μm and a product purity of 99.6%.
Example 5
Weighing 50g of HMX at room temperature, adding the HMX into 750g of N, N-dimethylformamide, and completely dissolving HMX crystals in a mechanical stirring manner to obtain a clear and transparent HMX solution with the mass concentration of 6.25%. 500g of the dissolved HMX solution was aspirated by a syringe having a bore size of 1.6mm and injected into 1000g of methanol at 300r/min at an injection rate of 10 mL/s. And (3) after stirring is maintained for 20min, filtering the material, washing the material with deionized water, and drying to obtain the HMX explosive with the snowflake-shaped structure. The explosive has a flake particle size of about 180 μm, a thickness of about 1 μm and a product purity of 99.2%.
The embodiments are described in a progressive manner in the specification, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. A preparation method of an HMX explosive with a snowflake-shaped structure is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: under the room temperature environment, adding HMX crystals into a first organic solvent, and completely dissolving the HMX crystals in a mechanical stirring manner to obtain a clear and transparent HMX solution; the first organic solvent is one of N, N-dimethylformamide, dimethyl sulfoxide, gamma-butyrolactone and N-methyl pyrrolidone;
step two: absorbing the HMX solution obtained in the step one by using an injector, injecting the HMX solution into a second organic solvent under the stirring condition of 100-300 rpm, maintaining stirring for a period of time, filtering, washing with deionized water, and drying to obtain the HMX explosive with a snowflake-shaped structure; the second organic solvent is one of ethanol, methanol, isopropanol and petroleum ether;
the mass ratio of the HMX solution sucked in the syringe to the second organic solvent is 1: 1-1: 20; the size of the pinhole aperture of the used syringe is 0.4 mm-1.6 mm; and (3) sucking the HMX solution obtained in the step one by using a syringe, and injecting the HMX solution into the second organic solvent under the stirring condition at an injection speed of 1-10 mL/s.
2. The method for preparing the HMX explosive with the snowflake flake-shaped structure according to claim 1, wherein the method comprises the following steps: in the HMX solution obtained in the first step, the mass percentage concentration of the dissolved HMX crystals is 1-10%.
3. The method for preparing the HMX explosive with the snowflake flake-shaped structure according to claim 1, wherein the method comprises the following steps: in the second step, after the HMX solution obtained in the first step is absorbed by an injector and injected into the second organic solvent under the stirring condition, stirring is maintained, and the stirring time is maintained to be 2-20 min.
4. The method for preparing the HMX explosive with the snowflake flake-shaped structure according to claim 1, wherein the method comprises the following steps: in the second step, the prepared HMX explosive with the snowflake-shaped structure has the particle size of 80-200 mu m, the thickness of the flake layer of 1-3 mu m and the purity of the product of more than 99 percent.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936534A (en) * | 2014-05-09 | 2014-07-23 | 北京理工大学 | Idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and preparation method thereof |
| CN106518883A (en) * | 2016-10-12 | 2017-03-22 | 中国工程物理研究院化工材料研究所 | Nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and massive preparation method thereof |
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| US20100024933A1 (en) * | 2003-02-28 | 2010-02-04 | Stec Iii Daniel | Methods for making and using high explosive fills for very small volume applications |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936534A (en) * | 2014-05-09 | 2014-07-23 | 北京理工大学 | Idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and preparation method thereof |
| CN106518883A (en) * | 2016-10-12 | 2017-03-22 | 中国工程物理研究院化工材料研究所 | Nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and massive preparation method thereof |
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