CN106866323A - Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and its fast preparation method - Google Patents
Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and its fast preparation method Download PDFInfo
- Publication number
- CN106866323A CN106866323A CN201710161578.9A CN201710161578A CN106866323A CN 106866323 A CN106866323 A CN 106866323A CN 201710161578 A CN201710161578 A CN 201710161578A CN 106866323 A CN106866323 A CN 106866323A
- Authority
- CN
- China
- Prior art keywords
- mtnp
- preparation
- cocrystallized
- cocrystallized explosives
- explosives
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002360 explosive Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 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 description 53
- YLTPBDJQPIRWTQ-UHFFFAOYSA-N 3,4,5-trinitro-1h-pyrazole Chemical class [O-][N+](=O)C1=NNC([N+]([O-])=O)=C1[N+]([O-])=O YLTPBDJQPIRWTQ-UHFFFAOYSA-N 0.000 title 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 title 1
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000002288 cocrystallisation Methods 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 230000005496 eutectics Effects 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 12
- 239000000243 solution Substances 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000005516 engineering process Methods 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
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000011549 crystallization solution Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 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 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003199 nucleic acid amplification method 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
- 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
Abstract
The invention discloses a kind of CL 20 and the fast preparation method of MTNP cocrystallized explosives, comprise the following steps：The preparation of step one, CL 20 and MTNP cocrystallization solution；CL 20 is added in alcohol solvent, high-temperature is risen to 20 DEG C 40 DEG C, MTNP is added after stirring and dissolving, obtain cocrystallization solution；The quick preparation of step 2, CL 20/MTNP cocrystallized explosives；The CL 20 and MTNP cocrystallization solution are continued to stir, and adjusts mixing speed to 50 200 revs/min, in whipping process, crystal is separated out rapidly, filtered, dried, obtain CL 20/MTNP cocrystallized explosives.The present invention also provides a kind of CL 20/MTNP cocrystallized explosives.Preparation method technological process of the invention is simple, easy to operate, and preparation condition is gentle, prepared by the expansion of suitable eutectic.
Description
Technical field
The present invention relates to energetic material technical field, and in particular to Hexanitrohexaazaisowurtzitane (CL-20) and 1- first
Base -3, the fast preparation method of 4,5- trinitro- pyrazoles (MTNP) cocrystallized explosives.
Background technology
Cocrystallized explosive has been increasingly becoming a kind of new strategy constructed new energetic material and regulate and control its performance, is ground by the world
One of the extensive concern of the person of studying carefully, and the focus as current international research and difficult point.At present, the preparation of cocrystallized explosive is mainly used
The mode of conventional solvent volatilization, the slow volatilization by solvent separates out crystal, and the cycle prepared by this method is long, and magnitude is small,
Efficiency is low, poor repeatability.In addition, as the increase of quantity of solvent is, it is necessary to expend the longer time, it is difficult to the technique for carrying out eutectic is put
Greatly.Therefore, using traditional preparation method can not furnish ample material for all round properties of eutectic is characterized, and seriously constrain altogether
Brilliant development and application.
One of the amplification technology of preparing of cocrystallized explosive, the challenge as energetic material area research how are broken through at present.This
The fast preparation method for using is invented, by the effect of stirring, eutectic can be made quickly to separate out.The preparation method process is simple,
Preparation efficiency is high, reproducible, and product crystalline quality is higher, the expansion large-scale production of suitable eutectic, can be the application of eutectic
Performance comprehensive assessment provides sufficient sample.At present, the quick preparation on CL-20/MTNP cocrystallized explosives there is no open source literature
Report.
The content of the invention
Instant invention overcomes the deficiencies in the prior art, there is provided the fast preparation method of a kind of CL-20 and MTNP cocrystallized explosives,
A kind of new method is provided for prepared by the expansion of cocrystallized explosive.
To solve above-mentioned technical problem, the present invention uses following technical scheme：
A kind of CL-20 and the fast preparation method of MTNP cocrystallized explosives, comprise the following steps：
The preparation of step one, CL-20 and MTNP cocrystallization solution
CL-20 is added in alcohol solvent, high-temperature is risen to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, be total to
Crystallization solution；
The quick preparation of step 2, CL-20/MTNP cocrystallized explosives
CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min,
In whipping process, crystal is separated out rapidly, filtered, dried, obtain CL-20/MTNP cocrystallized explosives.
It is another object of the present invention to provide a kind of CL-20/MTNP cocrystallized explosives, the CL-20/MTNP eutectics are fried
Medicine is prepared by above-mentioned fast preparation method.
Further scheme is：Described CL-20/MTNP cocrystallized explosives are in flake, and plane of crystal is completely smooth, put down
Equal particle diameter is 5 μm or so.
Compared with prior art, one of beneficial effect of the embodiment of the present invention is：Preparation method technological process of the invention
Simply, easy to operate, preparation condition is gentle, prepared by the expansion of suitable eutectic.
Brief description of the drawings
Fig. 1 is the quick preparation technology flow chart of one embodiment of the invention CL-20 and MTNP cocrystallized explosives.
Fig. 2 is the crystal morphology of CL-20/MTNP cocrystallized explosives in one embodiment of the invention.
Specific embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine by any way.
Any feature disclosed in this specification (including any accessory claim, summary and accompanying drawing), except non-specifically is chatted
State, can alternative features equivalent by other or with similar purpose replaced.I.e., unless specifically stated otherwise, each feature
It is an example in a series of equivalent or similar characteristics.
Below in conjunction with the accompanying drawings and embodiment is described in detail to specific embodiment of the invention.
As shown in figure 1, Fig. 1 shows the quick preparation technology flow chart of the present embodiment CL-20 and MTNP cocrystallized explosives.This
The preparation process of embodiment CL-20/MTNP cocrystallized explosives is as follows：
The preparation of step one, CL-20 and MTNP cocrystallization solution
CL-20 is added in absolute ethyl alcohol, high-temperature is risen to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, be total to
Crystallization solution；
The quick preparation of step 2, CL-20/MTNP cocrystallized explosives
CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min,
In whipping process, crystal is separated out rapidly, filtered, dried, obtain CL-20/MTNP cocrystallized explosives.
In general, the mol ratio of the CL-20 for adding and MTNP is 1：1.And do not have then for the consumption 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 explosives of the present invention is explained in detail below.
Embodiment 1
At room temperature, by 50ml absolute ethyl alcohols addition there-necked flask, 0.1095g CL-20 are added, is warming up to 20 DEG C, treated
0.0543g MTNP are added after CL-20 stirring and dissolvings, when CL-20 and MTNP are completely dissolved, cocrystallization solution is obtained.By cocrystallization
Solution continues stirring at 20 DEG C, then adjusts mixing speed to 50 revs/min, and during stirring, eutectic starts to separate out,
Solution turned cloudy, filtering is dried, and obtains micron order CL-20/MTNP cocrystallized explosives.
Embodiment 2
At room temperature, by 70ml absolute ethyl alcohols addition there-necked flask, 0.2175g CL-20 are added, is warming up to 35 DEG C, treated
0.1085g MTNP are added after CL-20 stirring and dissolvings, when CL-20 and MTNP are completely dissolved, cocrystallization solution is obtained.By cocrystallization
Solution continues stirring at 35 DEG C, then adjusts mixing speed to 150 revs/min, and during stirring, eutectic starts analysis
Go out, solution turned cloudy, filter, dry, obtain micron order CL-20/MTNP cocrystallized explosives.
Embodiment 3
At room temperature, by 100ml absolute ethyl alcohols addition there-necked flask, 0.438g CL-20 are added, is warming up to 40 DEG C, treated
0.217g MTNP are added after CL-20 stirring and dissolvings, when CL-20 and MTNP are completely dissolved, cocrystallization solution is obtained.By cocrystallization
Solution continues stirring at 40 DEG C, then adjusts mixing speed to 200 revs/min, and during stirring, eutectic starts analysis
Go out, solution turned cloudy, filter, dry, obtain micron order CL-20/MTNP cocrystallized explosives.
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 explosives that the fast preparation method of MTNP cocrystallized explosives is prepared from.Fig. 2 shows CL-20/ of the present invention
The crystal morphology of MTNP cocrystallized explosives.As shown in Figure 2, the present embodiment CL-20/MTNP cocrystallized explosives crystal in the form of sheets, particle diameter is big
Small about 5 μm, plane of crystal is smooth complete.
" one embodiment ", " another embodiment ", " embodiment " for being spoken of in this manual etc., refer to combining
Specific features, structure or the feature that the embodiment is described are included at least one embodiment of the application generality description.
It is not necessarily to refer to same embodiment that statement of the same race occur in multiple places in the description.Furthermore, it is understood that with reference to any
When individual embodiment describes specific features, structure or a feature, what is advocated is this to realize with reference to other embodiment
Feature, structure or feature also fall 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
Art personnel can be designed that a lot of other modification and implementation methods, and these modifications and implementation method will fall in the application
Within disclosed spirit and spirit.More specifically, in the range of disclosure claim, can be to theme group
The building block and/or layout for closing layout carry out various variations and modifications.Except 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 (3)
1. the fast preparation method of a kind of CL-20 and MTNP cocrystallized explosives, it is characterised in that comprise the following steps：
The preparation of step one, CL-20 and MTNP cocrystallization solution
CL-20 is added in alcohol solvent, high-temperature is risen to 20 DEG C -40 DEG C, MTNP is added after stirring and dissolving, obtain cocrystallization
Solution；
The quick preparation of step 2, CL-20/MTNP cocrystallized explosives
CL-20 the and MTNP cocrystallization solution is continued to stir, and adjusts mixing speed to 50-200 revs/min, in stirring
During, crystal is separated out rapidly, filter, dry, obtain CL-20/MTNP cocrystallized explosives.
2. a kind of CL-20/MTNP cocrystallized explosives, it is characterised in that the CL-20/MTNP cocrystallized explosives are by claim 1
What the quick Preparation Method was prepared.
3. CL-20/MTNP cocrystallized explosives according to claim 2, it is characterised in that：Described CL-20/MTNP cocrystallized explosives
In flake, plane of crystal is completely smooth, and average grain diameter is 5 μm.
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106866323A true CN106866323A (en) | 2017-06-20 |
| CN106866323B CN106866323B (en) | 2018-12-25 |
Family
ID=59172382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710161578.9A Expired - Fee Related CN106866323B (en) | 2017-03-17 | 2017-03-17 | Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive and its fast preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106866323B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133306A (en) * | 2021-11-19 | 2022-03-04 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,4-MDNP supramolecular explosive and preparation method thereof |
| CN114292150A (en) * | 2021-12-13 | 2022-04-08 | 西安近代化学研究所 | CL-20/DFTNAN eutectic explosive with low mechanical sensitivity and high detonation performance, and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103435427A (en) * | 2013-08-16 | 2013-12-11 | 中国工程物理研究院化工材料研究所 | Preparation method of hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive |
| CN103435426A (en) * | 2013-08-16 | 2013-12-11 | 中国工程物理研究院化工材料研究所 | Preparation method for benzotrifuroxan and m-dinitrobenzene eutectic explosive |
| CN104860786A (en) * | 2015-06-04 | 2015-08-26 | 西安近代化学研究所 | Preparation method of hexanitrohexaazaisowurtzitane and 2,5-dinitrotoluene eutectic explosive |
-
2017
- 2017-03-17 CN CN201710161578.9A patent/CN106866323B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103435427A (en) * | 2013-08-16 | 2013-12-11 | 中国工程物理研究院化工材料研究所 | Preparation method of hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive |
| CN103435426A (en) * | 2013-08-16 | 2013-12-11 | 中国工程物理研究院化工材料研究所 | Preparation method for benzotrifuroxan and m-dinitrobenzene eutectic explosive |
| CN104860786A (en) * | 2015-06-04 | 2015-08-26 | 西安近代化学研究所 | Preparation method of hexanitrohexaazaisowurtzitane and 2,5-dinitrotoluene eutectic explosive |
Non-Patent Citations (1)
| Title |
|---|
| 吴欣欣: "CL-20***系列共结晶体系的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133306A (en) * | 2021-11-19 | 2022-03-04 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,4-MDNP supramolecular explosive and preparation method thereof |
| CN114292150A (en) * | 2021-12-13 | 2022-04-08 | 西安近代化学研究所 | CL-20/DFTNAN eutectic explosive with low mechanical sensitivity and high detonation performance, and preparation method and application 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106866323B (en) | 2018-12-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2017143809A (en) | METHOD FOR OBTAINING VERMICULITE PVC THERMAL STABILIZER | |
| WO2016029841A1 (en) | Nickel cobalt oxide mesoporous microsphere and preparation method therefor | |
| CN106866323A (en) | Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and its fast preparation method | |
| CN103107301A (en) | Novel lithium ion battery diaphragm with inorganic coating and preparation method thereof | |
| CN107739611A (en) | A kind of quick and easy preparation room temperature CsPbX3The method of perovskite quantum dot | |
| JP2018532686A (en) | Method for producing graphene quantum dots having different oxygen contents, graphene quantum dots, and fluorescent material | |
| CN104310321A (en) | Preparation method of porous g-C3N4 semi-conducting material | |
| CN105428612B (en) | A kind of nanometer MoO2‑MoSe2@SFC lithium ion battery negative materials and preparation method thereof | |
| CN108893185B (en) | Method for preparing microalgae grease by magnetic hydrophobic eutectic solvent assisted flash extraction | |
| CN109659552A (en) | A kind of lithium ion battery anode slurry and preparation method thereof | |
| CN105752961A (en) | Nitrogen-phosphorus-doped carbon material with communicated hierarchical ducts and synthesizing method of nitrogen-phosphorus-doped carbon material | |
| CN100390220C (en) | A hydrogel preparation method | |
| CN103435427A (en) | Preparation method of hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive | |
| CN103865104A (en) | Preparation method of core-shell nano-particles | |
| CN107572595A (en) | A kind of preparation method of hollow loose structure iron oxide cathode material | |
| CN106430125A (en) | Preparation method of porous g-C3N4 rod | |
| CN106699550A (en) | Preparation method of nano Cu-CuBTC type metal organic framework material | |
| CN102992925B (en) | Method for preparing BTF-HNIW (benzotrifuroxan- hexanitrohexaazaisowurtzitane) eutectic explosive | |
| CN110127757A (en) | A kind of brookite type titanium dioxide and its preparation method and application | |
| CN107723320B (en) | Method for directly preparing crystal monascus orange pigment | |
| CN103980075A (en) | Preparation method for explosive having micro-nano multistage structure | |
| CN109735305A (en) | A method of composite phase-change material is prepared based on waste ceramic tile polishing material | |
| CN106145127A (en) | A kind of preparation method of hollow microsphere silicon dioxide | |
| CN109305867B (en) | Hexogen explosive crystal and preparation method thereof | |
| CN105777788A (en) | Europium-based metal-organic framework hexagonal sheet and preparing method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20181225 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |