CN103435427A - Preparation method of hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive - Google Patents
Preparation method of hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive Download PDFInfo
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- CN103435427A CN103435427A CN2013103590716A CN201310359071A CN103435427A CN 103435427 A CN103435427 A CN 103435427A CN 2013103590716 A CN2013103590716 A CN 2013103590716A CN 201310359071 A CN201310359071 A CN 201310359071A CN 103435427 A CN103435427 A CN 103435427A
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Abstract
The invention discloses a preparation method of a hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive. Firstly a saturated solution of hexanitrohexaazaisowurtzitane and a saturated solution of p-benzoquinone are prepared using a crystallization solvent, and then the solvent is allowed to evaporate through a constant-temperature incubator, followed by crystallization to prepare a hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive. The invention has the benefits as follows: the crystal density of the hexanitrohexaazaisowurtzitane/p-benzoquinone cocrystal explosive is up to 1.737 g/cm3, the melting point of the cocrystal explosive is 132 DEG C and is greatly increased by 17 DEG C as compared with relatively-pure component PBQ, and the cocrystal decomposition temperature is lower than that of both CL-20 and BQ and 207 DEG C lower than that of PBQ. Therefore, by virtue of cocrystallization, the thermal decomposition behavior of the explosive can be obviously controlled, the high efficiency and desensitivity of cocrystallization of the explosive are achieved, the safety of the explosive is improved, and the explosive has a good application prospect in high-energy low-sensitivity ammunition.
Description
Technical field
The invention belongs to the energetic material field, be specifically related to the preparation method of Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive, the present invention has application prospect preferably in the low responsive main charge of high energy.
Background technology
Hexanitrohexaazaisowurtzitane (CL-20), be a kind of cage shape high explosive, has higher density and energy, in the high energy powder charge with to improve weapons and ammunitions significant aspect efficiently injuring.But its sensitivity is higher, it is being extremely restricted aspect low sense ammunition applications.How effectively to reduce its sensitivity, become focus and the emphasis of correlative study person's research.Adopt the common sensing method that falls, as ordinary methods such as solution weight crystallization, macromolecular material coatings, often it is fallen to the sense DeGrain.Recently, the eutectic technology becomes a kind of emerging explosive modification method, and it can effectively regulate performance between explosive, and gives the performance that the eutectic explosive is new, for explosive modification provides a new more effective way.Eutectic preparation at present is mainly to obtain by a large amount of solvents and Subjective and Objective molecule experiment screening, and effectively the acquisition of synthon is more difficult.In order to reduce the CL-20 sensitivity, obtain effective synthon, by adopting the eutectic technology, itself and PBQ are formed to eutectic, realize that sense efficiently falls in eutectic, improve its security, expand their range of application.At present, about the preparation of CL-20-PBQ eutectic explosive, without open source literature, report.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, provides the preparation method's of a kind of Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive embodiment, to expect soluble problem.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
The preparation method of a kind of Hexanitrohexaazaisowurtzitane and para benzoquinone eutectic explosive comprises the following steps:
(1) preparation of Hexanitrohexaazaisowurtzitane and para benzoquinone saturated solution
Enough Hexanitrohexaazaisowurtzitanes are joined in recrystallisation solvent, and temperature is 30 ℃-50 ℃, dissolves, and filters, and obtains the Hexanitrohexaazaisowurtzitane saturated solution; Enough para benzoquinone are joined in the Hexanitrohexaazaisowurtzitane saturated solution and dissolve, filter, obtain the saturated solution that Hexanitrohexaazaisowurtzitane mixes with para benzoquinone;
(2) preparation of Hexanitrohexaazaisowurtzitane and para benzoquinone eutectic explosive
The saturated solution that Hexanitrohexaazaisowurtzitane is mixed with para benzoquinone is placed in beaker, then is statically placed in constant incubator evaporating solvent, pass through successively the formation of nucleus, grain growth, crystal formation, filter, drying, obtain Hexanitrohexaazaisowurtzitane and para benzoquinone eutectic explosive.
Further technical scheme is: the described recrystallisation solvent of step (1) is one or more mixing in ethanol, methyl alcohol, methylethylketone, acetone, ethyl acetate, benzene, ether, Virahol, the trimethyl carbinol, tetrahydrofuran (THF).
Further technical scheme is: the temperature of constant incubator described in step (2) is for being 30 ℃-45 ℃.
Compared with prior art, one of beneficial effect of the present invention is: Hexanitrohexaazaisowurtzitane and its crystalline density of para benzoquinone eutectic explosive are up to 1.737g/cm
3, the fusing point of eutectic explosive is 132 ℃, than pure component PBQ, significantly improves 17 ℃, and the decomposition temperature of eutectic is hanged down 207 ℃ all lower than CL-20 and PBQ than PBQ is obvious, and therefore, by eutectic, the thermal decomposition behavior of explosive has obtained significant regulation and control; Sense efficiently falls in the eutectic of having realized explosive, has improved the security of explosive, and this explosive has application prospect preferably in the low responsive ammunition of high energy, and the synthon that the eutectic explosive " is handed in hand " shape can effectively instruct other eutectic design, uses manpower and material resources sparingly.
The accompanying drawing explanation
Preparation technology's schema that Fig. 1 is Hexanitrohexaazaisowurtzitane of the present invention and para benzoquinone (CL-20-PBQ) eutectic explosive.
The molecular structure that Fig. 2 is Hexanitrohexaazaisowurtzitane of the present invention and para benzoquinone (CL-20-PBQ) eutectic explosive.
The synthon structure iron that Fig. 3 is Hexanitrohexaazaisowurtzitane of the present invention and para benzoquinone (CL-20-PBQ) eutectic explosive.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Fig. 1 shows preparation technology's schema of Hexanitrohexaazaisowurtzitane of the present invention and para benzoquinone (CL-20-PBQ) eutectic explosive.The preparation process of Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive is as follows:
(1) preparation of Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) saturated solution
Enough Hexanitrohexaazaisowurtzitanes (CL-20) are joined in recrystallisation solvent, increase the temperature to 30 ℃-50 ℃, dissolve, filter, obtain the Hexanitrohexaazaisowurtzitane saturated solution; Enough para benzoquinone (PBQ) are joined in the Hexanitrohexaazaisowurtzitane saturated solution and dissolve, filter, obtain Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) saturated solution; Recrystallisation solvent is any one or a few the mixture in ethanol, methyl alcohol, methylethylketone, acetone, ethyl acetate, benzene, ether, Virahol, the trimethyl carbinol, tetrahydrofuran (THF).
(2) preparation of Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive
Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) saturated solution are placed in to beaker, then be statically placed in constant incubator, evaporating solvent, pass through successively the formation of nucleus, grain growth, crystal formation, filter, drying, obtain Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive.In constant incubator, the temperature of evaporating solvent crystallization is 30 ℃-45 ℃.
Fig. 2 shows the molecular structure that Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive are confirmed by clicking diffraction analysis.Known from the monocrystalline interpretation of result: this eutectic, CL-20 molecule and PBQ molecule are with the 1:1(mol ratio) pass through N-O ... H hydrogen bond and the interphase interaction of π effect equimolecular form.The eutectic molecular formula is C
12h
10o
14n
12, belong to rhombic system, the Pna21 spacer, its crystalline density is up to 1.737g/cm
3, than component PBQ(1.318g/cm
3) significantly improved 31.8%.
Fig. 3 shows Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive molecules interaction rule, by analysis, find, CL-20 molecule in this eutectic and PBQ molecule, by " handing in hand " type synthon, infinitely extend to form in structure cell.
Table 1 has meaned the Thermal Parameter that Hexanitrohexaazaisowurtzitane and para benzoquinone (CL-20-PBQ) eutectic explosive record by differential thermal analysis (DSC).As seen from the table: 132 ℃ of the fusing points of eutectic, significantly improve 17 ℃ than pure component PBQ, be conducive to increase the thermostability of explosive; And the decomposition temperature of eutectic is hanged down 207 ℃ all lower than CL-20 and PBQ than PBQ is obvious, can make explosive to thermo-responsive, be applied in special pyrotechnics.After the explosive eutectic, fusing point raising and decomposition temperature reduce the thermal decomposition behavior that shows can significantly regulate and control by eutectic explosive.
The Thermal Parameter of table 1 eutectic and component
| Sample | Fusing point (℃) | Decomposition temperature (℃) |
| CL-20 | Nothing | 244 |
| PBQ | 115 | 442 |
| The CL-20-PBQ eutectic | 132 | 235 |
Specific embodiment prepared by Hexanitrohexaazaisowurtzitane of the present invention and para benzoquinone (CL-20-PBQ) eutectic explosive below is described in detail in detail.
Embodiment 1
At room temperature, 60ml ethanol is added in there-necked flask, then under agitation add enough CL-20, temperature is elevated to 30 ℃, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 30 ℃, allow the solvent evaporation, crystallize out, drying obtains CL-20-PBQ eutectic explosive.
Embodiment 2
At room temperature, 50ml methyl alcohol is added in there-necked flask, then under agitation add enough CL-20, temperature is elevated to 35 ℃, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 30 ℃, allow the solvent evaporation, crystallize out.Drying obtains CL-20-PBQ eutectic explosive.
Embodiment 3
At room temperature, the 50ml ethyl acetate is added in there-necked flask, then under agitation add enough CL-20, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 30 ℃, allow the solvent evaporation, crystallize out, drying obtains CL-20-PBQ eutectic explosive.
Embodiment 4
At room temperature, the 100ml tetrahydrofuran (THF) is added in there-necked flask, then under agitation add enough CL-20, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 35 ℃, allow the solvent evaporation, crystallize out, drying obtains CL-20-PBQ eutectic explosive.
Embodiment 5
At room temperature, the 80ml Virahol is added in there-necked flask, then under agitation add enough CL-20, temperature is elevated to 35 ℃, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 30 ℃, allow the solvent evaporation, crystallize out.Drying obtains CL-20-PBQ eutectic explosive.
Embodiment 6
At room temperature, the 80ml trimethyl carbinol is added in there-necked flask, then under agitation add enough CL-20, temperature is elevated to 40 ℃, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 40 ℃, allow the solvent evaporation, crystallize out.Drying obtains CL-20-PBQ eutectic explosive.
Embodiment 7
At room temperature, 60ml methylethylketone and acetone (volume ratio 1:1) mixed solvent are added in there-necked flask, then under agitation add enough CL-20, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, temperature is elevated to 50 ℃, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 45 ℃, allow the solvent evaporation, crystallize out, drying obtains CL-20-PBQ eutectic explosive.
Embodiment 8
At room temperature, 60ml Virahol and methyl alcohol (volume ratio 1:1) mixed solvent are added in there-necked flask, then under agitation add enough CL-20, temperature is elevated to 45 ℃, dissolve, filter, obtain the saturated solution of CL-20.Then add enough PBQ, stir, dissolve, filter, gained filtrate is the CL-20-PBQ saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 35 ℃, allow the solvent evaporation, crystallize out.Drying obtains CL-20-PBQ eutectic explosive.
Although with reference to a plurality of explanatory embodiment of the present invention, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.More particularly, in the scope of, accompanying drawing open in the application and claim, can carry out multiple modification and improvement to building block and/or the layout of subject combination layout.Except modification that building block and/or layout are carried out with improving, to those skilled in the art, other purposes will be also obvious.
Claims (3)
1. the preparation method of a Hexanitrohexaazaisowurtzitane and para benzoquinone eutectic explosive is characterized in that:
Comprise the following steps:
(1) preparation of Hexanitrohexaazaisowurtzitane and para benzoquinone saturated solution
Enough Hexanitrohexaazaisowurtzitanes are joined in recrystallisation solvent, and temperature is 30 ℃-50 ℃, dissolves, and filters, and obtains the Hexanitrohexaazaisowurtzitane saturated solution; Enough para benzoquinone are joined in the Hexanitrohexaazaisowurtzitane saturated solution and dissolve, filter, obtain the saturated solution that Hexanitrohexaazaisowurtzitane mixes with para benzoquinone;
(2) preparation of Hexanitrohexaazaisowurtzitane and para benzoquinone eutectic explosive
The saturated solution that Hexanitrohexaazaisowurtzitane is mixed with para benzoquinone is placed in beaker, then is statically placed in constant incubator evaporating solvent, pass through successively the formation of nucleus, grain growth, crystal formation, filter, drying, obtain Hexanitrohexaazaisowurtzitane and para benzoquinone eutectic explosive.
2. the preparation method of Hexanitrohexaazaisowurtzitane according to claim 1 and para benzoquinone eutectic explosive, it is characterized in that: the described recrystallisation solvent of step (1) is one or more mixing in ethanol, methyl alcohol, methylethylketone, acetone, ethyl acetate, benzene, ether, Virahol, the trimethyl carbinol, tetrahydrofuran (THF).
3. the preparation method of Hexanitrohexaazaisowurtzitane according to claim 1 and para benzoquinone eutectic explosive, it is characterized in that: the temperature of constant incubator described in step (2) is 30 ℃-45 ℃.
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| CN106810409A (en) * | 2017-01-24 | 2017-06-09 | 中国工程物理研究院化工材料研究所 | Embedded Subjective and Objective explosive crystal based on gas displacement technology and preparation method thereof |
| CN106831278A (en) * | 2017-01-24 | 2017-06-13 | 中国工程物理研究院化工材料研究所 | A kind of Subjective and Objective explosive with crystalline density high and preparation method thereof |
| CN106866322A (en) * | 2017-03-17 | 2017-06-20 | 中国工程物理研究院化工材料研究所 | Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and preparation method thereof |
| CN106866323A (en) * | 2017-03-17 | 2017-06-20 | 中国工程物理研究院化工材料研究所 | Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and its fast preparation method |
| WO2022188233A1 (en) * | 2021-03-12 | 2022-09-15 | 汕头大学 | Use of tmpd-txbq cocrystal material in laser ignition |
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| 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 |
| 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 |
| CN106810409A (en) * | 2017-01-24 | 2017-06-09 | 中国工程物理研究院化工材料研究所 | Embedded Subjective and Objective explosive crystal based on gas displacement technology and preparation method thereof |
| CN106831278A (en) * | 2017-01-24 | 2017-06-13 | 中国工程物理研究院化工材料研究所 | A kind of Subjective and Objective explosive with crystalline density high and preparation method thereof |
| CN106831278B (en) * | 2017-01-24 | 2018-09-25 | 中国工程物理研究院化工材料研究所 | A kind of Subjective and Objective explosive and preparation method thereof with high crystalline density |
| CN106810409B (en) * | 2017-01-24 | 2018-09-25 | 中国工程物理研究院化工材料研究所 | Embedded Subjective and Objective explosive crystal based on gas displacement technology and preparation method thereof |
| CN106866322A (en) * | 2017-03-17 | 2017-06-20 | 中国工程物理研究院化工材料研究所 | Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and preparation method thereof |
| CN106866323A (en) * | 2017-03-17 | 2017-06-20 | 中国工程物理研究院化工材料研究所 | Hexanitrohexaazaisowurtzitane and the trinitro- pyrazoles cocrystallized explosive of 1 methyl 3,4,5 and its fast preparation method |
| WO2022188233A1 (en) * | 2021-03-12 | 2022-09-15 | 汕头大学 | Use of tmpd-txbq cocrystal material in laser ignition |
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