CN102992923B - Preparation method of benzotrifuroxan (BTF) and trinitrotoluene (TNT) cocrystallized explosive - Google Patents
Preparation method of benzotrifuroxan (BTF) and trinitrotoluene (TNT) cocrystallized explosive Download PDFInfo
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Abstract
The invention discloses a preparation method of a benzotrifuroxan (BTF) and trinitrotoluene (TNT) cocrystallized explosive. The preparation method comprises the following steps of: (1) preparation of BTF-TNT saturated solution, namely, adding sufficient quantity of BTF to a crystallization solvent, raising the temperature to 20-50 DEG C, dissolving BTF and filtering the solution to obtain the BTF saturated solution; and adding sufficient quantity of TNT to the BTF saturated solution to be dissolved and filtering the solution to obtain the BTF-TNT mixed saturated solution; and (2) preparation of the BTF-TNT cocrystallized explosive: putting the BTF-TNT mixed saturated solution into a beaker, then standing in a constant temperature incubator, evaporating the solvent and drying the product, thus obtaining the BTF-TNT cocrystallized explosive. The preparation method has the beneficial effects that the prepared BTF-TNT cocrystallized explosive has good safety and detonation property and excellent free-flowing property, can serve as the component of explosives, gunpowder and propellants and has better application prospect in high-energy insensitive ammunitions; and the preparation method has the advantages of simple process flow, convenience in operation, mild reaction conditions, good safety and high product quality.
Description
Technical field
The invention belongs to energetic material field, be specifically related to the preparation method of benzo three furoxans and tritonal (BTF-TNT) eutectic explosive, the present invention has good application prospect in high explosive and insensitiveness ammunition.
Background technology
The density of the performance of energetic material (detonation energy, heat-resistant quality, sensitivity) and material, fusing point etc. are closely related.Because its energy of synthetic so far explosive and sensitivity are contradictories, its sensitivity of explosive that energy is higher also may be higher.Serious contradiction between existing energetic material energy and security, has restricted it and has further developed and apply.The at present modification to existing single chmical compound explosive, adopts the methods such as recrystallization, superpolymer be coated and compound conventionally, and these traditional method of modifying all do not change that explosive is inner to be formed and crystalline structure, so modified effect is undesirable, in the urgent need to researching and developing a kind of effective modification approach.Eutectic, as a kind of new modification technology, it is a kind of solid-state engineering that is mainly used in medicine, optics and semiconductor material research, its ultimate principle is that two or more different types of molecule is acted on by intermolecular non covalent bond (hydrogen bond, ionic linkage, Van der Waals force and pi-pi bond etc.), microcosmic is combined in same lattice, forms the polycomponent molecular crystal with ad hoc structure and performance.By eutectic technology, can effectively overcome that former explosive density is low or sensitivity is high or the defect such as heat-resistant quality is poor, and give the performance that eutectic explosive is new, for explosive modification provides a new more effective way.Eutectic technology becomes a kind of energetic material (explosive, propelling agent and gunpowder) performance and synthetic very competitive means of new explosive improved gradually.
Benzo three [1,2,5]-nitrous oxide is luxuriant-(Isosorbide-5-Nitrae, 7) trioxide, claim again benzo three furoxans (BTF), be a kind of rich nitrogen without hydrogen explosive, there is higher density and energy, it detonates excellent property and is widely used in charging explosive in detonator.But its sensitivity is higher, and free-running property is poor, is difficult to powder charge, its application is very restricted.The distinguishing features such as it is low that tritonal (TNT) has sensitivity, and fusing point is low, and cost is low are widely used as founding agent in castexplosive formula.In order to reduce the sensitivity of BTF, the TNT of itself and low sense is formed to eutectic, realize eutectic and efficiently fall sense, improve its security, expand its range of application.At present, about the preparation of BTF-TNT eutectic explosive, without open source literature, report.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of benzo three furoxans and tritonal (BTF-TNT) eutectic explosive, for energetic material study on the modification provides novel method.
The preparation method of benzo three furoxans and tritonal eutectic explosive, comprises the following steps:
(1) preparation of benzo three furoxans and tritonal saturated solution
Enough benzo three furoxans are joined in recrystallisation solvent, and temperature is 20 ℃-50 ℃, dissolves, and filters, and obtains benzo three furoxan saturated solutions; Enough tritonal is joined in benzo three furoxan saturated solutions and dissolved, filter, obtain the saturated solution that benzo three furoxans mix with tritonal;
(2) preparation of benzo three furoxans and tritonal eutectic explosive
The saturated solution that benzo three furoxans are mixed with tritonal is placed in beaker, is then statically placed in constant incubator evaporating solvent, pass through successively the formation of structure cell, grain growth, crystal formation, filter, dry, obtain benzo three furoxans and tritonal eutectic explosive.
Recrystallisation solvent described in step (1) is a kind of or wherein several mixing in acetone, methylethylketone, benzene, ether, methyl alcohol, ethanol, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
The temperature of constant incubator described in step (2) is for being 25-45 ℃.
Benzo three furoxans prepared by the present invention and tritonal (BTF-TNT) eutectic have good security and detonation property, have good free-running property simultaneously, can be used as the composition of explosive, gunpowder and propelling agent, in high-energy insensitive ammunition, there is good application prospect.Preparation method's technical process of the present invention is simple, easy to operate, and reaction conditions is gentle, and security is good, and product quality is high.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive.
Fig. 2 is the optical microscopy map of benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive.
Fig. 3 is the DSC figure of benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive and each component explosive.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.
Fig. 1 shows preparation technology's schema of benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive.The preparation process of benzo three furoxans and tritonal (BTF-TNT) eutectic explosive is as follows:
(1) preparation of benzo three furoxans and tritonal (BTF-TNT) saturated solution
Enough benzo three furoxans (BTF) are joined in recrystallisation solvent, increase the temperature to 20 ℃-50 ℃, dissolve, filter, obtain benzo three furoxan saturated solutions; Enough tritonal (TNT) is joined in benzo three furoxan saturated solutions and dissolved, filter, obtain benzo three furoxans and tritonal (BTF-TNT) saturated solution;
(2) preparation of benzo three furoxans and tritonal (BTF-TNT) eutectic explosive
Benzo three furoxans and tritonal (BTF-TNT) saturated solution are placed in to beaker, then be statically placed in constant incubator, evaporating solvent, pass through successively the formation of structure cell, grain growth, crystal formation, filter, dry, obtain benzo three furoxans and tritonal (BTF-TNT) eutectic explosive.
Table 1 shows the performance data of benzo three furoxans and tritonal (BTF-TNT) eutectic explosive and each component explosive.From table 1, data can find out that BTF-TNT eutectic explosive has better security compared with BTF, compared with TNT, there is higher sensitivity and energy, therefore BTF-TNT eutectic explosive has good security and detonation property, have good free-running property simultaneously, can be used as the composition of explosive, gunpowder and propelling agent, in high-energy insensitive ammunition, there is good application prospect.
The performance data of table 1 benzo three furoxans and tritonal eutectic explosive and component explosive
Fig. 2 shows the optical microscopy map of benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive.As shown in Figure 2, BTF-TNT eutectic explosive crystal is yellow prism-shaped, perfect crystalline, smooth surface, size is 500 about μ m, and its pattern and size are obviously different from raw material BTF and TNT, and result shows that eutectic can effectively control crystallization shape and the size of explosive crystal.
Fig. 3 shows the DSC figure of benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive and each component explosive.As shown in Figure 3, the maximum endotherm peak temperature of BTF-TNT eutectic explosive is 130 ℃, apparently higher than the maximum endotherm peak temperature of raw material TNT, shows that the fusing point of eutectic is higher than TNT, adopts eutectic technology can effectively regulate the fusing point of explosive.
Specific embodiment prepared by benzo three furoxans of the present invention and tritonal (BTF-TNT) eutectic explosive is described in detail in detail below.
Embodiment 1
At room temperature, 50ml acetone is added in there-necked flask, then under agitation add enough BTF, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 30 ℃, allow solvent evaporation, crystallize out, the dry BTF-TNT eutectic explosive that obtains.
Embodiment 2
At room temperature, 100ml ethanol is added in there-necked flask, then under agitation add enough BTF, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 30 ℃, allow solvent evaporation, crystallize out, the dry BTF-TNT eutectic explosive that obtains.
Embodiment 3
At room temperature, 80ml tetrahydrofuran (THF) is added in there-necked flask, then under agitation add enough BTF, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out, the dry BTF-TNT eutectic explosive that obtains.
Embodiment 4
At room temperature, 90ml methyl alcohol is added in there-necked flask, then under agitation add enough BTF, temperature is elevated to 35 ℃, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 30 ℃, allow solvent evaporation, crystallize out.The dry BTF-TNT eutectic explosive that obtains.
Embodiment 5
At room temperature, the 110ml trimethyl carbinol is added in there-necked flask, then under agitation add enough BTF, temperature is elevated to 40 ℃, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out.The dry BTF-TNT eutectic explosive that obtains.
Embodiment 6
At room temperature, 100ml Virahol is added in there-necked flask, then under agitation add enough BTF, temperature is elevated to 35 ℃, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out.The dry BTF-TNT eutectic explosive that obtains.
Embodiment 7
At room temperature, 100ml methylethylketone and benzene (volume ratio 1:1) mixed solvent are added in there-necked flask, then under agitation add enough BTF, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 40 ℃, allow solvent evaporation, crystallize out, the dry BTF-TNT eutectic explosive that obtains.
Embodiment 8
At room temperature, 80ml ethyl acetate and isopropyl acetate (volume ratio 1:1) mixed solvent are added in there-necked flask, then under agitation add enough BTF, temperature is elevated to 30 ℃, dissolve, filter, obtain the saturated solution of BTF.Then add enough TNT, stir, dissolve, filter, gained filtrate is BTF-TNT saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out.The dry BTF-TNT eutectic explosive that obtains.
Although with reference to explanatory embodiment of the present invention, invention has been described here, above-described embodiment is only preferably embodiment of the present invention, embodiments of the present invention are not restricted to the described embodiments, 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.
Claims (2)
1. the preparation method of benzo three furoxans and tritonal eutectic explosive, is characterized in that comprising the following steps:
(1) preparation of benzo three furoxans and tritonal saturated solution
Enough benzo three furoxans are joined in recrystallisation solvent, and temperature is 20 ℃-50 ℃, dissolves, and filters, and obtains benzo three furoxan saturated solutions; Enough tritonal is joined in benzo three furoxan saturated solutions and dissolved, filter, obtain the saturated solution that benzo three furoxans mix with tritonal;
(2) preparation of benzo three furoxans and tritonal eutectic explosive
The saturated solution that benzo three furoxans are mixed with tritonal is placed in beaker, is then statically placed in constant incubator evaporating solvent, pass through successively the formation of structure cell, grain growth, crystal formation, filter, dry, obtain benzo three furoxans and tritonal eutectic explosive;
The temperature of described constant incubator is for being 25-45 ℃.
2. the preparation method of benzo three furoxans according to claim 1 and tritonal eutectic explosive, is characterized in that the described recrystallisation solvent of step (1) is one or more mixing in acetone, methylethylketone, benzene, ether, methyl alcohol, ethanol, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
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| 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 |
| CN104817416A (en) * | 2015-03-30 | 2015-08-05 | 中国工程物理研究院化工材料研究所 | Preparation method of ammonium picrate and crown ether eutectic explosive |
| CN104788268B (en) * | 2015-04-09 | 2017-06-06 | 中国工程物理研究院化工材料研究所 | The preparation method of ammonium perchlorate and crown ether eutectic oxidant |
| CN106397350A (en) * | 2016-08-31 | 2017-02-15 | 山西北化关铝化工有限公司 | Preparation method of characteristic benzotrifuroxan |
| CN108101861B (en) * | 2016-11-25 | 2022-01-04 | 南京理工大学 | Eutectic crystal |
| CN106748592B (en) * | 2016-12-07 | 2019-07-19 | 中国工程物理研究院化工材料研究所 | Diamide ammonium and crown ether eutectic oxidant and preparation method thereof |
| CN106518577B (en) * | 2016-12-07 | 2018-08-14 | 中国工程物理研究院化工材料研究所 | TNT/TNCB cocrystallized explosives and preparation method thereof |
| CN106905088B (en) * | 2017-03-17 | 2018-08-14 | 中国工程物理研究院化工材料研究所 | Three furoxan of benzo and nitro-chlorobenzene cocrystallized explosive and preparation method thereof |
| CN107098864B (en) * | 2017-05-12 | 2024-01-30 | 南京理工大学 | Eutectic compound of sodium pentazole and 4-amino-1, 2, 4-triazole and preparation method thereof |
| CN111056885B (en) * | 2019-11-12 | 2021-10-29 | 北京理工大学 | DAF and DNP eutectic explosive and preparation method thereof |
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