CN103435426A - Preparation method for benzotrifuroxan and m-dinitrobenzene eutectic explosive - Google Patents
Preparation method for benzotrifuroxan and m-dinitrobenzene eutectic explosive Download PDFInfo
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- CN103435426A CN103435426A CN2013103608090A CN201310360809A CN103435426A CN 103435426 A CN103435426 A CN 103435426A CN 2013103608090 A CN2013103608090 A CN 2013103608090A CN 201310360809 A CN201310360809 A CN 201310360809A CN 103435426 A CN103435426 A CN 103435426A
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Abstract
The invention discloses a preparation method for a benzotrifuroxan and m-dinitrobenzene eutectic explosive. The preparation method comprises the following steps: firstly, preparing a benzotrifuroxan and m-dinitrobenzene saturated solution through a crystallization solvent; secondly, evaporating the solvent of the saturated solution by a constant temperature incubator and crystallizing to form the benzotrifuroxan and m-dinitrobenzene eutectic explosive. The benzotrifuroxan and m-dinitrobenzene eutectic explosive has the benefits of excellent safety, good detonation performance and good free-running property, can serve as a component of a novel booster explosive, has a good application prospect in high-energy low-sensitive ammunitions, and is simple and stable in preparation method and process flow, convenient to operate, moderate in reaction conditions, good in safety and high in quality.
Description
Technical field
The invention belongs to the energetic material field, be specifically related to the preparation method of benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) eutectic explosive, the present invention has application prospect preferably in high energy muting sensitive sense booster explosive.
Background technology
The component of the performance of energetic material (detonation energy, security etc.) and material, molecular structure etc. are closely related.Owing between existing energetic material energy and security, having serious contradiction, its sensitivity of explosive that energy is higher also may be higher, restricted it and further developed and apply.Therefore, the contradiction between energetic material energy in the urgent need to address and security.On the one hand, the low responsive energetic material of synthetic new high energy, process complexity not only, the cycle is long, also will consider its application performance, and therefore newly energetic material almost can not drop into practical application.On the other hand, to the modification of existing single chmical compound explosive, the method such as usually adopt recrystallization, superpolymer to coat and compound, these traditional method of modifying all do not change that explosive is inner to be formed and crystalline structure, therefore 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, be mainly used in a kind of solid-state engineering of 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.Can effectively overcome that former explosive density is low or sensitivity is high or the defect such as heat-resistant quality is poor by the eutectic technology, and give the performance that the eutectic explosive is new, for explosive modification provides a new more effective way.The 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 the hydrogen explosive, there is higher density and energy, it detonates excellent property and is widely used in the priming system powder charges such as detonator.But its sensitivity is higher, it is being extremely restricted aspect insensitiveness ammunition applications.Meta-dinitrobenzene (m-DNB) has significant low sensitivity, low melting point, and the characteristics such as low cost are widely used as the founding agent in the castexplosive formula.In order to reduce the BTF sensitivity, by introducing the eutectic technology, the DNB formation eutectic by it with low sensitivity, realize that sense efficiently falls in eutectic, improves its security, improves the DNB detonation energy simultaneously, expands their ranges of application.At present, about the preparation of BTF-DNB eutectic explosive, without open source literature, report.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, the preparation method's of a kind of benzo three furoxans and Meta-dinitrobenzene eutectic explosive embodiment is provided, realize that by eutectic the problems such as sense, raising safety performance efficiently fall in explosive with expectation, for the energetic material study on the modification provides novel method.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
The preparation method of a kind of benzo three furoxans and Meta-dinitrobenzene eutectic explosive comprises the following steps:
(1) preparation of benzo three furoxans and Meta-dinitrobenzene 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 Meta-dinitrobenzenes are joined in benzo three furoxan saturated solutions and dissolve, filter, obtain the saturated solution that benzo three furoxans mix with Meta-dinitrobenzene;
(2) preparation of benzo three furoxans and Meta-dinitrobenzene eutectic explosive
The saturated solution that benzo three furoxans are mixed with Meta-dinitrobenzene 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 benzo three furoxans and Meta-dinitrobenzene eutectic explosive.
Further technical scheme is: the described recrystallisation solvent of step (1) is one or more mixing in ethanol, methyl alcohol, acetone, methylethylketone, benzene, ether, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
Further technical scheme is: the temperature of constant incubator described in step (2) is 25 ℃-45 ℃.
Compared with prior art, one of beneficial effect of the present invention is: benzo three furoxans and Meta-dinitrobenzene eutectic explosive prepared by the present invention have excellent security and good detonation property, have good free-running property simultaneously, can be used as novel booster explosive composition, in the low responsive ammunition of high energy, there is application prospect preferably.Preparation method's technical process simple and stable of the present invention, easy to operate, the reaction conditions gentleness, security is good, and product quality is high.
The accompanying drawing explanation
Preparation technology's schema that Fig. 1 is benzo three furoxans of the present invention and Meta-dinitrobenzene 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 benzo three furoxans of the present invention and Meta-dinitrobenzene (BTF-DNB) eutectic explosive.The preparation process of benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) eutectic explosive is as follows:
(1) preparation of benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) 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 Meta-dinitrobenzenes (DNB) are joined in benzo three furoxan saturated solutions and dissolve, filter, obtain benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) saturated solution; Recrystallisation solvent is one or more mixing in ethanol, methyl alcohol, acetone, methylethylketone, benzene, ether, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
(2) preparation of benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) eutectic explosive
Benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) 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 benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) eutectic explosive; The temperature of constant incubator is 25 ℃-45 ℃.
Table 1 shows the performance data of benzo three furoxans and Meta-dinitrobenzene (BTF-DNB) eutectic explosive and each component explosive.From table 1, data can be found out: the impact sensitivity of eutectic has improved 140% with respect to BTF, energy has increased by 26% than DNB, BTF-DNB eutectic explosive has better security, higher energy, therefore BTF-DNB eutectic explosive has excellent security and good detonation property, can be used as novel low sense booster explosive composition, in the low responsive ammunition of high energy, there is application prospect preferably.
The performance data of table 1 benzo three furoxans and Meta-dinitrobenzene eutectic explosive and component explosive
Specific embodiment prepared by benzo three furoxans of the present invention and Meta-dinitrobenzene (BTF-DNB) eutectic explosive below is described in detail in detail.
Embodiment 1
At room temperature, 100ml ethanol is added in there-necked flask, then under agitation add enough BTF, controlling temperature is 25 ℃, dissolves, and filters, and obtains the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 30 ℃, allow the solvent evaporation, crystallize out, drying obtains BTF-DNB eutectic explosive.
Embodiment 2
At room temperature, 90ml methyl alcohol is 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 DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 25 ℃, allow the solvent evaporation, crystallize out.Drying obtains BTF-DNB eutectic explosive.
Embodiment 3
At room temperature, 50ml acetone is added in there-necked flask, then under agitation add enough BTF, controlling temperature is 20 ℃, dissolves, and filters, and obtains the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 30 ℃, allow the solvent evaporation, crystallize out, drying obtains BTF-DNB eutectic explosive.
Embodiment 4
At room temperature, the 70ml 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 DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 35 ℃, allow the solvent evaporation, crystallize out, drying obtains BTF-DNB eutectic explosive.
Embodiment 5
At room temperature, the 85ml 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 DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 35 ℃, allow the solvent evaporation, crystallize out.Drying obtains BTF-DNB eutectic explosive.
Embodiment 6
At room temperature, the 100ml trimethyl carbinol is added in there-necked flask, then under agitation add enough BTF, temperature is elevated to 45 ℃, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 45 ℃, allow the solvent evaporation, crystallize out.Drying obtains BTF-DNB 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 BTF, temperature is elevated to 50 ℃, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 40 ℃, allow the solvent evaporation, crystallize out, drying obtains BTF-DNB eutectic explosive.
Embodiment 8
At room temperature, 80ml Virahol and methyl alcohol (volume ratio 1:1) mixed solvent are 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 DNB, stir, dissolve, filter, gained filtrate is the BTF-DNB saturated solution.Filtrate is contained in beaker, then is still in the thermostat container of 35 ℃, allow the solvent evaporation, crystallize out.Drying obtains BTF-DNB 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 benzo three furoxans and Meta-dinitrobenzene eutectic explosive is characterized in that: comprise the following steps:
(1) preparation of benzo three furoxans and Meta-dinitrobenzene 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 Meta-dinitrobenzenes are joined in benzo three furoxan saturated solutions and dissolve, filter, obtain the saturated solution that benzo three furoxans mix with Meta-dinitrobenzene;
(2) preparation of benzo three furoxans and Meta-dinitrobenzene eutectic explosive
The saturated solution that benzo three furoxans are mixed with Meta-dinitrobenzene 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 benzo three furoxans and Meta-dinitrobenzene eutectic explosive.
2. the preparation method of benzo three furoxans according to claim 1 and Meta-dinitrobenzene eutectic explosive, it is characterized in that: the described recrystallisation solvent of step (1) is one or more mixing in ethanol, methyl alcohol, acetone, methylethylketone, benzene, ether, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
3. the preparation method of benzo three furoxans according to claim 1 and Meta-dinitrobenzene eutectic explosive, it is characterized in that: the temperature of constant incubator described in step (2) is 25 ℃-45 ℃.
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Cited By (4)
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| 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 |
| CN108101861A (en) * | 2016-11-25 | 2018-06-01 | 南京理工大学 | A kind of eutectic |
| CN111056885A (en) * | 2019-11-12 | 2020-04-24 | 北京理工大学 | DAF and DNP eutectic explosive and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN111056885A (en) * | 2019-11-12 | 2020-04-24 | 北京理工大学 | DAF and DNP eutectic explosive and preparation method thereof |
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