CN103435426B - The preparation method of benzo three furoxan and m-dinitrobenzene eutectic explosive - Google Patents
The preparation method of benzo three furoxan and m-dinitrobenzene eutectic explosive Download PDFInfo
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- CN103435426B CN103435426B CN201310360809.0A CN201310360809A CN103435426B CN 103435426 B CN103435426 B CN 103435426B CN 201310360809 A CN201310360809 A CN 201310360809A CN 103435426 B CN103435426 B CN 103435426B
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Abstract
The invention discloses the preparation method of a kind of benzo three furoxan and m-dinitrobenzene eutectic explosive, first benzo three furoxan and Meta-dinitrobenzene saturated solution is prepared by recrystallisation solvent, then by this saturated solution constant incubator evaporating solvent, crystallization forms benzo three furoxan and m-dinitrobenzene eutectic explosive.The invention has the beneficial effects as follows: benzo three furoxan and m-dinitrobenzene eutectic explosive have excellent security and good detonation property, have excellent free-running property simultaneously, can be used as novel booster explosive composition, in the low responsive ammunition of high energy, there is good application prospect, and preparation method, technical process simple and stable, easy to operate, reaction conditions is gentle, security is good, and product quality is high.
Description
Technical field
The invention belongs to energetic material field, be specifically related to the preparation method of benzo three furoxan and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive, the present invention has good application prospect in high energy muting sensitive sense booster explosive.
Background technology
The performance (detonation energy, security etc.) of energetic material is closely related with the component, molecular structure etc. of material.Owing to there is serious contradiction between existing energetic material energy and security, its sensitivity of explosive that namely energy is higher also may be higher, constrains it and further develop and apply.Therefore, the contradiction between energetic material energy in the urgent need to address and security.On the one hand, synthesize the low responsive energetic material of new high energy, not only process is complicated, and the cycle is long, also will consider its application performance, and therefore new energetic material almost can not drop into practical application.On the other hand, to the modification of existing single chmical compound explosive, usually adopt the methods such as the coated and compound of recrystallization, superpolymer, these traditional method of modifying all do not change explosive inside composition and crystalline structure, therefore modified effect is undesirable, in the urgent need to researching and developing a kind of effectively modification approach.Eutectic, as a kind of new modification technology, be mainly used in the solid-state engineering of one of medicine, optics and semiconductor material research, its ultimate principle is acted on by non-covalent intermolecular key (hydrogen bond, ionic linkage, Van der Waals force and pi-pi bond etc.) by two or more different types of molecule, microcosmic is combined in same lattice, forms the polycomponent molecular crystal with ad hoc structure and performance.Effectively can overcome that former explosive density is low or sensitivity is high by eutectic technology or the defect such as heat-resistant quality is poor, and give cocrystallized explosive new performance, for explosive modification provides a new more effective way.Eutectic technology becomes one gradually and improves energetic material (explosive, propelling agent and gunpowder) performance and the very competitive means of the new explosive of synthesis.
Benzo three [1,2,5]-nitrous oxide luxuriant-(1,4,7) trioxide, also known as benzo three furoxan (BTF), be a kind of rich nitrogen without hydrogen explosive, there is higher density and energy, its excellent property and be widely used in the priming system powder charges such as detonator of detonating.But its sensitivity is higher, it is made to be extremely restricted in Desensitive ammunition application aspect.Meta-dinitrobenzene (m-DNB) has significant low sensitivity, low melting point, and the features such as low cost widely use as founding agent in castexplosive formula.In order to reduce BTF sensitivity, by introducing eutectic technology, itself and the DNB of low sensitivity being formed eutectic, realizes eutectic and efficiently fall sense, improve its security, raising DNB detonation energy, expands their ranges of application simultaneously.At present, the preparation about BTF-DNB cocrystallized explosive is reported without open source literature.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, the embodiment of the preparation method of a kind of benzo three furoxan and m-dinitrobenzene eutectic explosive is provided, to expect that realizing explosive by eutectic efficiently falls sense, improves the problems such as safety performance, for 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:
A preparation method for benzo three furoxan and m-dinitrobenzene eutectic explosive, comprises the following steps:
(1) preparation of benzo three furoxan and Meta-dinitrobenzene saturated solution
Join in recrystallisation solvent by enough benzo three furoxans, temperature is 20 DEG C-50 DEG C, dissolves, and filters, obtains benzo three furoxan saturated solution; Enough Meta-dinitrobenzenes are joined in benzo three furoxan saturated solution and dissolve, filter, obtain the saturated solution that benzo three furoxan mixes with Meta-dinitrobenzene;
(2) preparation of benzo three furoxan and m-dinitrobenzene eutectic explosive
The saturated solution that benzo three furoxan mixes with Meta-dinitrobenzene is placed in beaker, is then statically placed in constant incubator, evaporating solvent, successively through the formation of nucleus, grain growth, crystal formation, filter, dry, obtain benzo three furoxan and m-dinitrobenzene eutectic explosive.
Further technical scheme is: the recrystallisation solvent described in 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: described in step (2), the temperature of constant incubator is 25 DEG C-45 DEG C.
Compared with prior art, one of beneficial effect of the present invention is: benzo three furoxan prepared by the present invention and m-dinitrobenzene eutectic explosive have excellent security and good detonation property, have excellent free-running property simultaneously, can be used as novel booster explosive composition, in the low responsive ammunition of high energy, there is good application prospect.Preparation method's technical process simple and stable of the present invention, easy to operate, 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 furoxan of the present invention and m-dinitrobenzene eutectic explosive.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be not intended to limit the present invention.
Fig. 1 shows preparation technology's schema of benzo three furoxan of the present invention and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive.The preparation process of benzo three furoxan and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive is as follows:
(1) preparation of benzo three furoxan and Meta-dinitrobenzene (BTF-DNB) saturated solution
Enough benzo three furoxans (BTF) are joined in recrystallisation solvent, increases the temperature to 20 DEG C-50 DEG C, dissolve, filter, obtain benzo three furoxan saturated solution; Enough Meta-dinitrobenzenes (DNB) are joined in benzo three furoxan saturated solution and dissolve, filter, obtain benzo three furoxan 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 furoxan and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive
Benzo three furoxan and Meta-dinitrobenzene (BTF-DNB) saturated solution are placed in beaker, then be statically placed in constant incubator, evaporating solvent, successively through the formation of nucleus, grain growth, crystal formation, filter, drying, obtains benzo three furoxan and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive; The temperature of constant incubator is 25 DEG C-45 DEG C.
Table 1 shows the performance data of benzo three furoxan and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive and each component explosive.Data as can be seen from table 1: the impact sensitivity of eutectic improves 140% relative to BTF, energy comparatively DNB adds 26%, BTF-DNB cocrystallized explosive has better security, higher energy, therefore BTF-DNB cocrystallized 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 good application prospect.
The performance data of table 1 benzo three furoxan and m-dinitrobenzene eutectic explosive and component explosive
Specific embodiment prepared by benzo three furoxan of the present invention and Meta-dinitrobenzene (BTF-DNB) cocrystallized explosive is described in detail in detail below.
Embodiment 1
At room temperature, add in there-necked flask by 100ml ethanol, then under agitation add enough BTF, control temperature is 25 DEG C, dissolves, and filters, obtains the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate be contained in beaker, be then still in the thermostat container of 30 DEG C, allow solvent evaporate, crystallize out, drying obtains BTF-DNB cocrystallized 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 DEG C, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 25 DEG C, allow solvent evaporate, crystallize out.Drying obtains BTF-DNB cocrystallized explosive.
Embodiment 3
At room temperature, add in there-necked flask by 50ml acetone, then under agitation add enough BTF, control temperature is 20 DEG C, dissolves, and filters, obtains the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate be contained in beaker, be then still in the thermostat container of 30 DEG C, allow solvent evaporate, crystallize out, drying obtains BTF-DNB cocrystallized explosive.
Embodiment 4
At room temperature, 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 BTF-DNB saturated solution.Filtrate be contained in beaker, be then still in the thermostat container of 35 DEG C, allow solvent evaporate, crystallize out, drying obtains BTF-DNB cocrystallized explosive.
Embodiment 5
At room temperature, 85ml Virahol is added in there-necked flask, then under agitation add enough BTF, temperature is elevated to 35 DEG C, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 35 DEG C, allow solvent evaporate, crystallize out.Drying obtains BTF-DNB cocrystallized 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 DEG C, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 45 DEG C, allow solvent evaporate, crystallize out.Drying obtains BTF-DNB cocrystallized 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 adds enough BTF, temperature is elevated to 50 DEG C, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate be contained in beaker, be then still in the thermostat container of 40 DEG C, allow solvent evaporate, crystallize out, drying obtains BTF-DNB cocrystallized 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 adds enough BTF, temperature is elevated to 40 DEG C, dissolve, filter, obtain the saturated solution of BTF.Then add enough DNB, stir, dissolve, filter, gained filtrate is BTF-DNB saturated solution.Filtrate is contained in beaker, is then still in the thermostat container of 35 DEG C, allow solvent evaporate, crystallize out.Drying obtains BTF-DNB cocrystallized explosive.
Although with reference to multiple 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 amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of, accompanying drawing open in the application and claim, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (3)
1. a preparation method for benzo three furoxan and m-dinitrobenzene eutectic explosive, is characterized in that: comprise the following steps:
(1) preparation of benzo three furoxan and Meta-dinitrobenzene saturated solution
Join in recrystallisation solvent by enough benzo three furoxans, temperature is 20 DEG C-50 DEG C, dissolves, and filters, obtains benzo three furoxan saturated solution; Enough Meta-dinitrobenzenes are joined in benzo three furoxan saturated solution and dissolve, filter, obtain the saturated solution that benzo three furoxan mixes with Meta-dinitrobenzene;
(2) preparation of benzo three furoxan and m-dinitrobenzene eutectic explosive
The saturated solution that benzo three furoxan mixes with Meta-dinitrobenzene is placed in beaker, is then statically placed in constant incubator, evaporating solvent, successively through the formation of nucleus, grain growth, crystal formation, filter, dry, obtain benzo three furoxan and m-dinitrobenzene eutectic explosive.
2. the preparation method of benzo three furoxan according to claim 1 and m-dinitrobenzene eutectic explosive, is characterized in that: the recrystallisation solvent described in 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 furoxan according to claim 1 and m-dinitrobenzene eutectic explosive, is characterized in that: described in step (2), the temperature of constant incubator is 25 DEG C-45 DEG C.
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| CN108101861B (en) * | 2016-11-25 | 2022-01-04 | 南京理工大学 | Eutectic crystal |
| CN106866323B (en) * | 2017-03-17 | 2018-12-25 | 中国工程物理研究院化工材料研究所 | Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive and its fast preparation method |
| CN106866322B (en) * | 2017-03-17 | 2018-12-25 | 中国工程物理研究院化工材料研究所 | Hexanitrohexaazaisowurtzitane and 1- methyl -3,4,5- trinitro- pyrazoles cocrystallized explosive 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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