CN116903425A - LLM-105/HNS jet blending crystal preparation device and preparation method - Google Patents
LLM-105/HNS jet blending crystal preparation device and preparation method Download PDFInfo
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- CN116903425A CN116903425A CN202310965833.0A CN202310965833A CN116903425A CN 116903425 A CN116903425 A CN 116903425A CN 202310965833 A CN202310965833 A CN 202310965833A CN 116903425 A CN116903425 A CN 116903425A
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- hns
- llm
- nozzle
- container bottle
- jet
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- 238000002156 mixing Methods 0.000 title claims abstract description 43
- 239000013078 crystal Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000005507 spraying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000006184 cosolvent Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 8
- 239000011259 mixed solution Substances 0.000 claims 2
- 239000007921 spray Substances 0.000 claims 1
- 239000002360 explosive Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 12
- 239000003814 drug Substances 0.000 description 8
- 230000005496 eutectics Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002288 cocrystallisation Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005474 detonation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a LLM-105/HNS jet blending crystal preparation device and a preparation method, which aim at solving the technical problem that the existing preparation method does not use engineering, and the technical scheme is as follows: the method comprises the steps of forming a cosolvent firstly by using the device, stirring, then opening the high-pressure gas tank, spraying the blending solution into the non-solvent bottle, standing, filtering and drying to obtain a sample.
Description
Technical Field
The invention belongs to the technical field of energetic material preparation, and particularly relates to a LLM-105/HNS jet blending crystal preparation device and a preparation method.
Background
Currently, there are two main directions in the study of energetic materials: firstly, a novel high-energy insensitive explosive is actively researched and developed, but the research period in the direction is long, the newly researched and developed explosive is difficult to produce in a large scale in a short time, and the stability of the explosive can be put into use only by long-term detection and authentication; secondly, the existing explosive is modified, namely, the physical and chemical properties of the explosive are improved through methods of cladding, thinning, recrystallization and the like, but the methods can not change the molecular composition and the crystal structure of the explosive, so that the modification effect is not ideal.
In recent years, a new means-eutectic technology for changing the physical and chemical properties of energetic materials from molecular level is developed, namely, different explosive components are subjected to hydrogen bond, pi-pi stacking effect, van der Waals force,
The non-covalent bond acting forces such as halogen bonds are combined to form supermolecules, and the non-covalent bond acting forces can not break covalent bonds in the molecules, so that the eutectic explosive can retain certain characteristics of the original single-component explosive, and meanwhile, the eutectic explosive has better performance than the single-component explosive due to stable acting forces among molecules in the crystal. The solvent volatilization method and the cooling crystallization method can realize eutectic, but the production period is long, and engineering is not utilized.
Disclosure of Invention
The invention aims to solve the problems and provide a LLM-105/HNS jet blending crystal preparation device and a preparation method.
In order to solve the technical problems, the invention adopts the following technical scheme:
the LLM-105/HNS jet blending crystal preparation device comprises a blending solution container bottle, a pipeline, a high-pressure gas tank, a non-solvent container bottle, a nozzle and a stirring rod, wherein the blending solution container bottle is connected with the nozzle through the pipeline, the high-pressure gas tank is also connected with the nozzle through the pipeline, the nozzle is arranged at the opening of the non-solvent container bottle, and the stirring rod is positioned in the non-solvent container bottle.
Further, the nozzle adopts a pneumatic atomizing nozzle.
The preparation method of the LLM-105/HNS jet blending crystal by using the LLM-105/HNS jet blending crystal preparation device comprises the following steps:
step 1): at room temperature, LLM-105 and HNS with the molar ratio of 0.5-5 are weighed and placed in a blending solution container bottle, and cosolvent is added for full dissolution;
step 2): stirring the non-solvent container bottle filled with the non-solvent by using a stirring rod;
step 3): opening a high-pressure gas tank, spraying high-pressure gas from a nozzle along a pipeline to enable vacuum to be formed at the joint of the pipeline on one side of the blending solution container bottle and the nozzle, generating pressure difference, spraying blending solution from the nozzle in an atomization mode along the pipeline to the nozzle, spraying the blending solution into a non-solvent, stopping stirring by a stirring rod after waiting for 5 minutes when the blending solution is not sprayed in the nozzle;
step 4): standing the suspension obtained in the non-solvent container bottle in the step 3), and filtering;
step 5): and (3) drying the product obtained in the step (4) in an oven to obtain a mixed crystal sample of LLM-105/HNS.
Further, the cosolvent in the step 1) adopts any one of dimethylformamide, dimethyl sulfoxide or N-methylpyrrolidone.
Further, the fully dissolving method in the step 1) comprises the steps of placing a blending solution container bottle in an ultrasonic oscillator for ultrasonic treatment at normal temperature for 30min or heating the blending solution to the room temperature-90 ℃.
Further, the non-solvent in the step 2) adopts water.
Further, the pneumatic spraying pressure in the step 3) is 0.2-1 MPa.
Further, the suspension in the step 4) is kept stand for 1-4 hours.
Further, the drying temperature in the step 5) is 40-70 ℃ and the drying time is 3-8 hours.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the preparation method of the particles by spraying, refining and co-crystallizing, the particles and the crystals are mixed in a eutectic way, and the refining and co-crystallizing preparation of LLM-105 and HNS are synchronously carried out, so that the method is simple and efficient, and is beneficial to large-scale production;
(2) The critical diameters of LLM-105 and HNS are smaller, and the two medicines have good high temperature resistance, and the two medicines are mixed in a eutectic way, so that the medicine can be used as an insensitive explosion-transmitting medicine or an impact tablet detonator medicine, and the multipurpose of the medicine is realized.
Drawings
FIG. 1 is a schematic diagram of the preparation structure of the present invention;
fig. 2 is a scanning electron microscope image of HNS;
FIG. 3 is a scanning electron microscope image of LLM-105;
FIG. 4 is a scanning electron microscope image of HNS/LLM-105 co-crystallization;
FIG. 5 is a graph of HNS/LLM-105 co-crystallization differential heat curves;
in the figure: 1. a co-solution container bottle; 2. a pipeline; 3. a high pressure gas tank; 4. a non-solvent container bottle; 5. a nozzle; 6. stirring rod.
Detailed Description
The invention is further described below with reference to the drawings and examples.
Example 1:
as shown in fig. 1-4, the LLM-105/HNS jet blending crystal preparation device comprises a blending solution container bottle 1, a pipeline 2, a high-pressure gas tank 3, a non-solvent container bottle 4, a pneumatic atomizing nozzle 5 and a stirring rod 6, wherein the blending solution container bottle 1 is connected with the nozzle 5 through the pipeline 2, the high-pressure gas tank 3 is also connected with the nozzle 5 through the pipeline 2, the nozzle 5 is arranged at the opening of the non-solvent container bottle 4, and the stirring rod 6 is positioned in the non-solvent container bottle 4.
A preparation method of LLM-105/HNS jet blending crystal comprises the following steps:
step 1): weighing LLM-105 and HNS with the molar ratio of 0.1g, placing the LLM-105 and the HNS in a blending solution container bottle 1, adding 30mL of Dimethylformamide (DMF) as a cosolvent, and placing the blending solution container bottle 1 in an ultrasonic vibration instrument for ultrasonic treatment at normal temperature for 30min; so that the water is fully dissolved;
step 2): the non-solvent container bottle 4 containing 120mL of water was stirred using the stirring bar 6;
step 3): opening a high-pressure gas tank 3, pneumatically spraying the high-pressure gas at the pressure of 0.2MPa, spraying the high-pressure gas from a nozzle 5 along a pipeline 2, simultaneously spraying the blending solution in a blending solution container bottle 1 from the nozzle 5 in an atomization mode under the action of the high-pressure gas through the pipeline 2, spraying the blending solution into water, stopping stirring by a stirring rod 6 after the blending solution is not sprayed in the nozzle 5 for 5 minutes; under the action of high-pressure gas, the two solute molecules collide with each other to form eutectic, after being sprayed out by the nozzle 5, initial small liquid drops are rapidly dispersed into water to start crystallization, and the small liquid drops dispersed into the water do not have the condition of aggregation of crystal grains and continuous growth, so that the purposes of eutectic and refinement are achieved;
step 4): standing the suspension obtained in the non-solvent container bottle 4 in the step 3) for 3 hours, and filtering;
step 5): and (3) placing the product obtained in the step (4) in an oven and drying at 60 ℃ for 6 hours to obtain the LLM-105/HNS blended crystal sample.
The cosolvent in the step 1) can also adopt dimethyl sulfoxide or N-methyl pyrrolidone.
The method for fully dissolving in the step 1) comprises the steps of placing a blending solution container bottle (1) in an ultrasonic vibration instrument for ultrasonic treatment at normal temperature for 30min or heating the blending solution to the room temperature of-90 ℃.
The pneumatic spraying pressure in the step 3) can be any value in the range of 0.2 to 1MPa.
The suspension in the step 4) can be kept still for any value in 1-4h.
The drying temperature in the step 5) can be any value in the range of 40-70 ℃, and the drying time can be any value in the range of 3-8 hours.
The prepared LLM-105/HNS cocrystal explosive can be detonated by using a voltage of 1.5kV, the energy is slightly improved compared with that of ultrafine HNS, the requirements of flying piece detonating are met, and the LLM-105/HNS cocrystal explosive can be used as a detonator medicament for a striking piece.
Example 2:
example 2 differs from example 1 in that:
the mass of LLM-105 and HNS in the step 1) is 0.2g and 0.5g respectively; the cosolvent is 16.5mL of Dimethylformamide (DMF), and the fully dissolving method is that the solution is heated to 90 ℃ by a blending solution container bottle 1;
the water in the non-solvent container bottle 5 in the step 2) is 900mL;
the pneumatic spraying pressure in the step 3) is 0.3MPa;
the suspension in the step 4) is kept stand for 4 hours;
in the step 5), the drying temperature is 70 ℃ and the drying time is 8 hours.
As shown in figure 5, the prepared mixed crystal sample is subjected to differential thermal analysis, the thermal stability of the mixed crystal sample is improved, the decomposition peak temperature is improved by more than 15 ℃ compared with that of single HNS (313 ℃), the heat resistance is better, the mixed crystal material is added with an adhesive and then used as a high-tank charge, detonation transfer can be realized in a groove with the thickness of 0.6mm multiplied by 0.6mm under the pressure of 280MPa, and the mixed crystal material can be used as a high-temperature-resistant booster medicine.
Claims (9)
1. LLM-105/HNS sprays blending crystal preparation facilities, its characterized in that includes blending solution container bottle (1), pipeline (2), high-pressure gas tank (3), non-solvent container bottle (4), nozzle (5) and stirring rod (6), blending solution container bottle (1) is connected with nozzle (5) through pipeline (2), high-pressure gas tank (3) are connected with nozzle (5) through pipeline (2) equally, nozzle (5) set up the opening part at non-solvent container bottle (4), stirring rod (6) are located non-solvent container bottle (4).
2. The LLM-105/HNS jet co-mingled crystal production apparatus according to claim 1, wherein the nozzles (5) are pneumatically atomized nozzles.
3. The method for preparing LLM-105/HNS jet blending crystal by using the LLM-105/HNS jet blending crystal preparing device as set forth in claim 1, comprising the steps of:
step 1): at room temperature, LLM-105 and HNS with the molar ratio of 0.5-5 are weighed and placed in a blending solution container bottle (1), and cosolvent is added for full dissolution;
step 2): stirring the non-solvent container bottle (4) filled with the non-solvent by using a stirring rod (6);
step 3): opening a high-pressure gas tank (3), spraying high-pressure gas from a nozzle (5) along a pipeline (2) to enable vacuum to be formed at the interface of the pipeline on one side of a blending solution container bottle (1) and the nozzle (5), generating pressure difference, enabling the blending solution to flow to the nozzle (5) along the pipeline (2), spraying the blending solution from the nozzle (5) in an atomization mode, spraying the blending solution into a non-solvent, stopping stirring by a stirring rod (6) after waiting for 5 minutes when the blending solution is not sprayed in the nozzle (5);
step 4): standing the suspension obtained in the non-solvent container bottle (4) in the step 3), and filtering;
step 5): and (3) drying the product obtained in the step (4) in an oven to obtain a mixed crystal sample of LLM-105/HNS.
4. The method for preparing LLM-105/HNS jet co-mixed crystals according to claim 3, wherein the co-solvent in the step 1) is any one of dimethylformamide, dimethyl sulfoxide or N-methylpyrrolidone.
5. The preparation method of LLM-105/HNS jet co-mixed crystals according to claim 3, wherein the fully dissolving method in the step 1) comprises the steps of placing the container bottle (1) of the co-mixed solution in an ultrasonic vibration apparatus at normal temperature for 30min or heating the co-mixed solution to room temperature-90 ℃.
6. The method for preparing LLM-105/HNS jet co-mixed crystals according to claim 3, wherein the non-solvent in the step 2) is water.
7. The method for preparing LLM-105/HNS jet co-mixed crystals according to claim 3, wherein the pneumatic spraying pressure in the step 3) is 0.2-1 MPa.
8. The method for preparing LLM-105/HNS jet co-mixed crystals as set forth in claim 3, wherein the standing time of the suspension in the step 4) is 1-4 hours.
9. The method for preparing LLM-105/HNS jet blending crystal according to claim 3, wherein the drying temperature in the step 5) is 40-70 ℃ and the drying time is 3-8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310965833.0A CN116903425A (en) | 2023-08-02 | 2023-08-02 | LLM-105/HNS jet blending crystal preparation device and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310965833.0A CN116903425A (en) | 2023-08-02 | 2023-08-02 | LLM-105/HNS jet blending crystal preparation device and preparation method |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120305150A1 (en) * | 2011-02-08 | 2012-12-06 | The Regents Of The University Of Michigan | Crystalline explosive material |
| CN103172476A (en) * | 2013-04-08 | 2013-06-26 | 中国工程物理研究院化工材料研究所 | Preparation method of submicron particle 1-oxo-diamino-3, 5-dinitropyrazine explosive |
| CN103408388A (en) * | 2013-08-26 | 2013-11-27 | 煤炭科学研究总院爆破技术研究所 | Powdery emulsion ammonium nitrate explosive |
| WO2015126375A1 (en) * | 2014-02-19 | 2015-08-27 | Halliburton Energy Services, Inc. | Co-crystal explosives for high temperature downhole operations |
| KR20170014949A (en) * | 2015-07-31 | 2017-02-08 | 국방과학연구소 | Method of producing hexanitrostilbene particles and apparatus thereof |
| CN208084164U (en) * | 2018-01-08 | 2018-11-13 | 南京航空航天大学 | The device of abrasive air jet stream finished surface texture based on non-newtonian fluid |
| CN113735665A (en) * | 2021-10-18 | 2021-12-03 | 中国工程物理研究院化工材料研究所 | LLM-105/SI eutectic explosive and preparation method thereof |
-
2023
- 2023-08-02 CN CN202310965833.0A patent/CN116903425A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120305150A1 (en) * | 2011-02-08 | 2012-12-06 | The Regents Of The University Of Michigan | Crystalline explosive material |
| CN103172476A (en) * | 2013-04-08 | 2013-06-26 | 中国工程物理研究院化工材料研究所 | Preparation method of submicron particle 1-oxo-diamino-3, 5-dinitropyrazine explosive |
| CN103408388A (en) * | 2013-08-26 | 2013-11-27 | 煤炭科学研究总院爆破技术研究所 | Powdery emulsion ammonium nitrate explosive |
| WO2015126375A1 (en) * | 2014-02-19 | 2015-08-27 | Halliburton Energy Services, Inc. | Co-crystal explosives for high temperature downhole operations |
| KR20170014949A (en) * | 2015-07-31 | 2017-02-08 | 국방과학연구소 | Method of producing hexanitrostilbene particles and apparatus thereof |
| CN208084164U (en) * | 2018-01-08 | 2018-11-13 | 南京航空航天大学 | The device of abrasive air jet stream finished surface texture based on non-newtonian fluid |
| CN113735665A (en) * | 2021-10-18 | 2021-12-03 | 中国工程物理研究院化工材料研究所 | LLM-105/SI eutectic explosive and preparation method thereof |
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