CN106866323B - Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive and its fast preparation method - Google Patents
Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive and its fast preparation method Download PDFInfo
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- CN106866323B CN106866323B CN201710161578.9A CN201710161578A CN106866323B CN 106866323 B CN106866323 B CN 106866323B CN 201710161578 A CN201710161578 A CN 201710161578A CN 106866323 B CN106866323 B CN 106866323B
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- Prior art keywords
- mtnp
- preparation
- cocrystallized explosive
- cocrystallized
- explosive
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- NDYLCHGXSQOGMS-UHFFFAOYSA-N CL-20 Chemical compound [O-][N+](=O)N1C2N([N+]([O-])=O)C3N([N+](=O)[O-])C2N([N+]([O-])=O)C2N([N+]([O-])=O)C3N([N+]([O-])=O)C21 NDYLCHGXSQOGMS-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000002360 explosive Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- YBMMWNXKXKUSEB-UHFFFAOYSA-N 1-methyl-3,4,5-trinitropyrazole Chemical class CN1N=C([N+]([O-])=O)C([N+]([O-])=O)=C1[N+]([O-])=O YBMMWNXKXKUSEB-UHFFFAOYSA-N 0.000 title description 2
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000002288 cocrystallisation Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000005496 eutectics Effects 0.000 abstract description 12
- 239000000243 solution Substances 0.000 description 15
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011549 crystallization solution Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses the fast preparation methods of a kind of CL-20 and MTNP cocrystallized explosive, comprising the following steps: Step 1: the preparation of CL-20 and MTNP cocrystallization solution；CL-20 is added in alcohol solvent, temperature is increased to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, obtains cocrystallization solution；Step 2: the quick preparation of CL-20/MTNP cocrystallized explosive；CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min, in whipping process, is precipitated crystal rapidly, is filtered, it is dry, obtain CL-20/MTNP cocrystallized explosive.The present invention also provides a kind of CL-20/MTNP cocrystallized explosives.Preparation method process flow of the invention is simple, and easy to operate, preparation condition is mild, is suitable for the expansion preparation of eutectic.
Description
Technical field
The present invention relates to energetic material technical fields, and in particular to Hexanitrohexaazaisowurtzitane (CL-20) and 1- first
Base -3,4, the fast preparation method of 5- trinitro- pyrazoles (MTNP) cocrystallized explosive.
Background technique
Cocrystallized explosive has been increasingly becoming a kind of new strategy constructed novel energetic material and regulate and control its performance, is ground by the world
The extensive concern for the person of studying carefully, and one of hot spot and the difficult point for becoming current international research.Currently, the preparation of cocrystallized explosive mainly uses
Crystal is precipitated by the slow volatilization of solvent in the mode of conventional solvent volatilization, and the period of this method preparation is long, and magnitude is small,
Low efficiency, poor repeatability.In addition, needing to expend the longer time with the increase of quantity of solvent, the technique for being difficult to carry out eutectic is put
Greatly.Therefore, it uses traditional preparation method that cannot characterize for all round properties of eutectic to furnish ample material, seriously constrain altogether
Brilliant development and application.
The amplification technology of preparing for how breaking through cocrystallized explosive at present, becomes one of the challenge of energetic material area research.This
The fast preparation method that invention uses can be such that eutectic is quickly precipitated by the effect of stirring.The preparation method simple process,
Preparation efficiency is high, and reproducible, product crystalline quality is higher, is suitable for the expansion large-scale production of eutectic, can be the application of eutectic
Performance, which fully assesses, provides sufficient sample.Currently, the quick preparation about CL-20/MTNP cocrystallized explosive there is no open source literature
Report.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, provide the fast preparation method of a kind of CL-20 and MTNP cocrystallized explosive,
A kind of new method is provided for the expansion preparation of cocrystallized explosive.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of fast preparation method of CL-20 and MTNP cocrystallized explosive, comprising the following steps:
Step 1: the preparation of CL-20 and MTNP cocrystallization solution
CL-20 is added in alcohol solvent, temperature is increased to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, obtains
Cocrystallization solution；
Step 2: the quick preparation of CL-20/MTNP cocrystallized explosive
CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min,
It in whipping process, precipitates crystal rapidly, filters, it is dry, obtain CL-20/MTNP cocrystallized explosive.
It is another object of the present invention to provide a kind of CL-20/MTNP cocrystallized explosive, the CL-20/MTNP eutectic
Explosive is prepared by above-mentioned fast preparation method.
Further scheme is: the CL-20/MTNP cocrystallized explosive is flaky, and plane of crystal is completely smooth, puts down
Equal partial size is 5 μm or so.
Compared with prior art, the beneficial effect of the embodiment of the present invention first is that: preparation method process flow of the invention
Simply, easy to operate, preparation condition is mild, is suitable for the expansion preparation of eutectic.
Detailed description of the invention
Fig. 1 is the quick preparation technology flow chart of one embodiment of the invention CL-20 and MTNP cocrystallized explosive.
Fig. 2 is the crystal morphology of CL-20/MTNP cocrystallized explosive in one embodiment of the invention.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification (including any accessory claim, abstract and attached drawing), except non-specifically chatting
It states, can be replaced by other alternative features that are equivalent or have similar purpose.That is, unless specifically stated, each feature is only
It is an example in a series of equivalent or similar characteristics.
Specific embodiments of the present invention will be described in detail with reference to the accompanying drawings and embodiments.
As shown in Figure 1, Fig. 1 shows the quick preparation technology flow chart of the present embodiment CL-20 Yu MTNP cocrystallized explosive.This
The preparation process of embodiment CL-20/MTNP cocrystallized explosive is as follows:
Step 1: the preparation of CL-20 and MTNP cocrystallization solution
CL-20 is added in dehydrated alcohol, temperature is increased to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, is total to
Crystallization solution；
Step 2: the quick preparation of CL-20/MTNP cocrystallized explosive
CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min,
It in whipping process, precipitates crystal rapidly, filters, it is dry, obtain CL-20/MTNP cocrystallized explosive.
In general, the molar ratio of the CL-20 and MTNP that are added are 1:1.And do not have then for the dosage of etoh solvent
Body requirement, as long as CL-20 and MTNP can be dissolved in ethanol solution.
Specifically, the specific embodiment of the fast preparation method of CL-20/MTNP cocrystallized explosive of the present invention is explained in detail below.
Embodiment 1
At room temperature, 50ml dehydrated alcohol is added in three-necked flask, 0.1095g CL-20 is added, is warming up to 20 DEG C, to
0.0543g MTNP is added after CL-20 stirring and dissolving, when CL-20 and MTNP are completely dissolved, obtains cocrystallization solution.By cocrystallization
Solution continues to stir at 20 DEG C, then adjusts mixing speed to 50 revs/min, during stirring, eutectic starts to analyse
Out, solution becomes cloudy, and filters, dry, obtains micron order CL-20/MTNP cocrystallized explosive.
Embodiment 2
At room temperature, 70ml dehydrated alcohol is added in three-necked flask, 0.2175g CL-20 is added, is warming up to 35 DEG C, to
0.1085g MTNP is added after CL-20 stirring and dissolving, when CL-20 and MTNP are completely dissolved, obtains cocrystallization solution.By cocrystallization
Solution continues to stir at 35 DEG C, then adjusts mixing speed to 150 revs/min, during stirring, eutectic starts to analyse
Out, solution becomes cloudy, and filters, dry, obtains micron order CL-20/MTNP cocrystallized explosive.
Embodiment 3
At room temperature, 100ml dehydrated alcohol is added in three-necked flask, 0.438g CL-20 is added, is warming up to 40 DEG C, to
0.217g MTNP is added after CL-20 stirring and dissolving, when CL-20 and MTNP are completely dissolved, obtains cocrystallization solution.By cocrystallization
Solution continues to stir at 40 DEG C, then adjusts mixing speed to 200 revs/min, during stirring, eutectic starts to analyse
Out, solution becomes cloudy, and filters, dry, obtains micron order CL-20/MTNP cocrystallized explosive.
As shown in Fig. 2, according to another embodiment of the invention, present embodiment discloses above-described embodiment CL-20 with
The CL-20/MTNP cocrystallized explosive that the fast preparation method of MTNP cocrystallized explosive is prepared.Fig. 2 shows CL-20/ of the present invention
The crystal morphology of MTNP cocrystallized explosive.As shown in Figure 2, crystal, partial size are big in the form of sheets for the present embodiment CL-20/MTNP cocrystallized explosive
About 5 μm small, plane of crystal is smooth complete.
" one embodiment " for being spoken of in the present specification, " another embodiment ", " embodiment " etc., refer to combining
Specific features, structure or the feature of embodiment description are included at least one embodiment generally described herein.
It is not centainly to refer to the same embodiment that statement of the same race, which occur, in multiple places in the description.Furthermore, it is understood that in conjunction with any
When a embodiment describes a specific features, structure or feature, to be advocated be realized in conjunction with other embodiments it is this
Feature, structure or feature are also fallen within the scope of the present invention.
Although reference be made herein to invention has been described for the multiple explanatory embodiments invented, however, it is to be understood that this
Field technical staff can be designed that a lot of other modification and implementations, these modifications and implementations will fall in the application
Within disclosed scope and spirit.More specifically, it is disclosed in the scope of the claims in the application, it can be to theme group
The building block and/or layout for closing layout carry out a variety of variations and modifications.In addition to the modification carried out to building block and/or layout
Outer with improving, to those skilled in the art, other purposes also will be apparent.
Claims (1)
1. the fast preparation method of a kind of CL-20 and MTNP cocrystallized explosive, it is characterised in that the following steps are included:
Step 1: the preparation of CL-20 and MTNP cocrystallization solution
CL-20 is added in alcohol solvent, temperature is increased to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, obtains cocrystallization
Solution；
Step 2: the quick preparation of CL-20/MTNP cocrystallized explosive
CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min, is being stirred
In the process, it precipitates crystal rapidly, filters, dry, obtaining flaky, the complete smooth, average grain diameter of plane of crystal is 5 μm
CL-20/MTNP cocrystallized explosive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710161578.9A CN106866323B (en) | 2017-03-17 | 2017-03-17 | Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive and its fast preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710161578.9A CN106866323B (en) | 2017-03-17 | 2017-03-17 | Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive and its fast preparation method |
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| Publication Number | Publication Date |
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| CN106866323A CN106866323A (en) | 2017-06-20 |
| CN106866323B true CN106866323B (en) | 2018-12-25 |
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| CN114133306B (en) * | 2021-11-19 | 2023-05-02 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,4-MDNP supermolecular explosive and preparation method thereof |
| CN114292150B (en) * | 2021-12-13 | 2022-10-25 | 西安近代化学研究所 | CL-20/DFTNAN eutectic explosive with low mechanical sensitivity and high detonation performance, preparation method and application |
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| US6783615B1 (en) * | 2002-01-29 | 2004-08-31 | The United States Of America As Represented By The Secretary Of The Army | Insensitive explosives for high speed loading applications |
| CN103435426B (en) * | 2013-08-16 | 2015-09-09 | 中国工程物理研究院化工材料研究所 | The preparation method of benzo three furoxan and m-dinitrobenzene eutectic explosive |
| CN103435427B (en) * | 2013-08-16 | 2015-09-09 | 中国工程物理研究院化工材料研究所 | The preparation method of Hexanitrohexaazaisowurtzitane and para benzoquinone cocrystallized explosive |
| CN104860786B (en) * | 2015-06-04 | 2017-08-08 | 西安近代化学研究所 | A kind of preparation method of Hexanitrohexaazaisowurtzitane and 2,5 dinitrotoluene (DNT) cocrystallized explosives |
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