CN102992924B - Preparation method of benzotrifuroxan (BTF) and 2,4-dinitroanisole (DNAN) cocrystallized explosive - Google Patents
Preparation method of benzotrifuroxan (BTF) and 2,4-dinitroanisole (DNAN) cocrystallized explosive Download PDFInfo
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Abstract
The invention discloses a preparation method of a benzotrifuroxan (BTF) and 2,4-dinitroanisole (DNAN) cocrystallized explosive. The preparation method comprises the following steps of: (1) preparation of BTF-DNAN saturated solution, namely, adding sufficient quantity of BTF to a crystallization solvent at 20-50 DEG C, dissolving BTF and filtering the solution to obtain the BTF saturated solution; and adding DNAN to the BTF saturated solution to be dissolved and filtering the solution to obtain the BTF-DNAN mixed saturated solution; and (2) preparation of the BTF-DNAN cocrystallized explosive: putting the BTF-DNAN mixed saturated solution into a beaker, then standing in a constant temperature incubator, evaporating the solvent and drying the product, thus obtaining the BTF-DNAN cocrystallized explosive. The preparation method has the beneficial effects that the prepared BTF-DNAN cocrystallized explosive obviously reduces the sensitivity of BTF, obviously improves the energy of DNAN, has excellent detonation property, can serve as a novel insensitive detonating agent and has better application prospect in the insensitive ammunitions resistant to high overload and the like; 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 2,4-dinitroanisol (BTF-DNAN) eutectic explosive, the present invention insensitiveness detonate and insensitiveness ammunition in there is good application prospect.
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.Based on eutectic principle, the explosive molecules with high energy characteristic can be realized to mutual non covalent bond effect with the explosive molecules with low sense characteristic on molecular level, formation has unique texture, and the eutectic explosive simultaneously with high energy and low sense characteristic, to greatly expand the range of application of existing simple substance energetic material, and provide a kind of effective way for energetic material study on the modification.
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 the energy suitable with HMX and detonate performance preferably and be widely used in charging explosive in detonator.But because its sensitivity is higher, free-running property is poor, is difficult to powder charge, and its application is very restricted.The distinguishing features such as 2,4-dinitroanisol (DNAN) is the colourless yellow acicular crystals that arrives, and has sensitivity low, and fusing point is low, and cost is low be a kind of novel founding agent, but its energy are on the low side.In order to reduce the sensitivity of BTF and the energy of raising DNAN, height is felt to the BTF of high energy and the DNAN of low sense low energy formation eutectic, realize the effective adjusting of eutectic to explosive energy and security, and improve BTF security and free-running property and DNAN energy, expand its range of application.At present, about the preparation of BTF-DNAN 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 2,4-dinitroanisol (BTF-DNAN) eutectic explosive, for energetic material modification provides a kind of new way.
The preparation method of benzo three furoxans and 2,4-dinitroanisol eutectic explosive, is characterized in that comprising the following steps:
(1) preparation of benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) 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; 2,4-dinitroanisol is joined in benzo three furoxan saturated solutions and dissolved, filter, obtain the saturated solution that benzo three furoxans and 2,4-dinitroanisol mix;
(2) preparation of benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) eutectic explosive
By benzo three furoxans and 2, the saturated solution that 4-dinitroanisol mixes is placed in beaker, then be statically placed in constant incubator, evaporating solvent, passes through the formation of structure cell successively, grain growth, crystal formation, filter, dry, obtain benzo three furoxans and 2,4-dinitroanisol eutectic explosive.
Recrystallisation solvent described in step (1) can be a kind of or wherein several mixing in acetone, methylethylketone, ether, methyl alcohol, ethanol, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
Described in step (2), the temperature of constant incubator is 25-45 ℃.
BTF-DNAN eutectic explosive prepared by the present invention, significantly reduces the sensitivity of BTF, and obviously improves DNAN energy, has excellent detonation property, can be used as the novel insensitiveness medicament that detonates, and in the insensitiveness ammunitions such as anti high overload, has 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 2,4-dinitroanisol eutectic explosive.
Fig. 2 is the optical microscopy map of benzo three furoxans of the present invention and 2,4-dinitroanisol (BTF-DNAN) eutectic.
Fig. 3 is the DSC figure of benzo three furoxans of the present invention and 2,4-dinitroanisol (BTF-DNAN) 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 2,4-dinitroanisol eutectic explosive.The preparation process of benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) eutectic explosive is as follows:
(1) benzo three furoxans and 2, the preparation of 4-dinitroanisol (BTF-DNAN) saturated solution: enough benzo three furoxans (BTF) are joined in recrystallisation solvent, and temperature is 20 ℃-50 ℃, dissolves, filter, obtain benzo three furoxan saturated solutions; 2,4-dinitroanisol (DNAN) is joined in benzo three furoxan saturated solutions and dissolved, filter, obtain the saturated solution that benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) mix.According to embodiments of the invention, recrystallisation solvent can be a kind of or wherein several mixing in acetone, methylethylketone, ether, methyl alcohol, ethanol, Virahol, the trimethyl carbinol, tetrahydrofuran (THF), dioxane.
(2) preparation of benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) eutectic explosive: the saturated solution of benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) mixing is placed in to beaker, then be statically placed in constant incubator, the temperature of constant incubator is 25-45 ℃, and evaporating solvent passes through the formation of structure cell successively, grain growth, crystal formation, filter, dry, obtain benzo three furoxans and 2,4-dinitroanisol (BTF-DNAN) eutectic explosive.
Table 1 shows benzo three furoxans that preparation method of the present invention makes and the performance data of 2,4-dinitroanisol (BTF-DNAN) eutectic explosive and component explosive.Data from table 1 can find out that BTF-DNAN eutectic explosive has reduced the sensitivity of BTF, have improved sensitivity and the energy of DNAN, have excellent detonation property, can be used as the novel insensitiveness medicament that detonates, and in the insensitiveness ammunitions such as anti high overload, have good application prospect.
The performance data of table 1 benzo three furoxans and 2,4-dinitroanisol eutectic explosive and component explosive
Fig. 2 shows the optical microscopy map of benzo three furoxans of the present invention and 2,4-dinitroanisol (BTF-DNAN) eutectic explosive.As shown in Figure 2, BTF-DNAN eutectic explosive crystal is lurid chunk shape, crystal surface is smooth complete, crystallographic dimension is 400 μ m left and right, experimental result show its crystal shape and size all with raw material BTF and DNAN obvious difference, illustrate that eutectic provides a kind of new way for the control of explosive crystallization shape and size.
Fig. 3 shows the DSC figure of benzo three furoxans of the present invention and 2,4-dinitroanisol (BTF-DNAN) eutectic explosive and each component explosive.As shown in Figure 3, the maximum heat absorption melting hump temperature of BTF-DNAN eutectic explosive is 132 ℃, and it is apparently higher than raw material DNAN(95 ℃), lower than raw material BTF(197 ℃), and the exothermic maximum decomposition temperature of eutectic approaches raw material BTF, show to have significantly improved DNAN fusing point by eutectic technology.
Specific embodiment prepared by benzo three furoxans of the present invention and 2,4-dinitroanisol (BTF-DNAN) 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 adding enough BTF, temperature is 25 ℃, dissolves, and filters, and obtains the saturated solution of BTF.Then add enough DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 30 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 2
At room temperature, 100ml Virahol 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 DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 40 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 3
At room temperature, 80ml dioxane 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 DNAN,, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 45 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 4
At room temperature, 100ml ether 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 DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 45 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 5
At room temperature, 120ml ethanol 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 DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 40 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 6
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 DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 7
At room temperature, 60ml acetone and tetrahydrofuran (THF) (volume ratio 1:1) mixed solvent are 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 DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN eutectic explosive that obtains.
Embodiment 8
At room temperature, 80ml acetone and methylethylketone (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 DNAN, stir, dissolve, filter the mixing saturated solution that gained filtrate is BTF-DNAN.Filtrate is contained in beaker, is then still in the thermostat container of 35 ℃, allow solvent evaporation, crystallize out, the dry BTF-DNAN 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 2,4-dinitroanisol eutectic explosive, is characterized in that comprising the following steps:
(1) preparation of benzo three furoxans and 2,4-dinitroanisol 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; 2,4-dinitroanisol is joined in benzo three furoxan saturated solutions and dissolved, filter, obtain the saturated solution that benzo three furoxans and 2,4-dinitroanisol mix;
(2) preparation of benzo three furoxans and 2,4-dinitroanisol eutectic explosive
By benzo three furoxans and 2, the saturated solution that 4-dinitroanisol mixes is placed in beaker, then be statically placed in the constant incubator of 25-45 ℃, evaporating solvent, passes through the formation of structure cell successively, grain growth, crystal formation, filter, dry, obtain benzo three furoxans and 2,4-dinitroanisol eutectic explosive.
2. benzo three furoxans according to claim 1 and 2, the preparation method of 4-dinitroanisol eutectic explosive, is characterized in that recrystallisation solvent described in step (1) is a kind of or wherein several mixing in acetone, methylethylketone, 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 |
| CN108101861B (en) * | 2016-11-25 | 2022-01-04 | 南京理工大学 | Eutectic crystal |
| 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 |
| 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 |
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| CN101570459A (en) * | 2008-04-30 | 2009-11-04 | 南京理工大学 | Ethylenediamine perchlorate.triethylene diamine perchlorate eutectic initiating explosive and preparation method thereof |
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| CN101570459A (en) * | 2008-04-30 | 2009-11-04 | 南京理工大学 | Ethylenediamine perchlorate.triethylene diamine perchlorate eutectic initiating explosive and preparation method thereof |
Non-Patent Citations (7)
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| 7种BTF共晶的制备与表征;郭长艳等;《含能材料》;20120831;第20卷(第4期);第503-504页 * |
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