CN104817416A - Preparation method of ammonium picrate and crown ether eutectic explosive - Google Patents
Preparation method of ammonium picrate and crown ether eutectic explosive Download PDFInfo
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- CN104817416A CN104817416A CN201510145772.9A CN201510145772A CN104817416A CN 104817416 A CN104817416 A CN 104817416A CN 201510145772 A CN201510145772 A CN 201510145772A CN 104817416 A CN104817416 A CN 104817416A
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Abstract
The invention discloses a preparation method of an ammonium picrate and crown ether eutectic explosive. The method comprises the following steps: preparing a saturated ammonium picrate solution at 20-50DEG C, and adding a proper amount of crown ether into the saturated ammonium picrate solution to prepare an ammonium picrate and crown ether mixed saturated solution; and filtering, evaporating to remove a solvent, and drying to obtain the ammonium picrate and crown ether eutectic explosive. The preparation method has the advantages of simple process flow, convenient operation, mild reaction conditions, good safety and high product quality. The ammonium picrate/crown ether eutectic explosive has the advantages of low hygroscopicity, good safety and excellent fluidity, can be used in main charges, blasting powders and propellants as a composition component, and has a good application prospect in insensitive ammunitions.
Description
Technical field
Embodiments of the present invention relate to energetic material field, and more specifically, embodiments of the present invention relate to the preparation method of a kind of ammonium picrate and crown ether cocrystallized explosive, and the present invention has good application prospect in desensitized explosive.
Background technology
Eutectic mainly refers to two or more differing molecular, by noncovalent intermolecular interactions power, microcosmic combines and forms the new crystal of orderly homogenization, it effectively can overcome former compound defect, give new compound excellent properties, therefore, eutectic technology has become a kind of New Policy constructing novel cpd and regulating compound performance.In energetic material field, how effectively to realize the energy of simple substance energetic material and the matched well of security, one of focus becoming current research.Adopt conventional crystal method of modifying as recrystallization, the methods such as the coated and compound of superpolymer, fail to change inside composition and the crystalline structure of explosive, therefore modified effect is undesirable, in the urgent need to researching and developing a kind of effectively modification approach.At present, eutectic technology becomes energetic material gradually and constructs the new way with modification.By the explosive molecules of different performance by eutectic technology, form cocrystallized explosive, the defect of former explosive can be overcome and give the new multiple excellent properties of eutectic structure explosive.
Crown ether, also known as large cyclic ethers, is the macrocylc compound that a class contains multiple Sauerstoffatom, has larger ring cavity, and containing comparatively strong hydrogen bonding acceptor groups, can with positive ion, especially complexing of metal ion.2，4，6-trinitrophenol ammonium, again ammonium picrate (D explosive), preparation technology is simple, and not containing heavy metal ion, explosion product toxicity is little, can separately and crown ether mixed packing high explosive anti-tank cartridge, and can mix with saltpetre and substitute black powder, for propellant charge.But its sensitivity is higher, water absorbability is strong, and free-running property is poor, is difficult to powder charge, makes it apply and is very restricted.Crown ether and ammonium picrate eutectic is not also used efficiently to reduce the hygroscopic report of ammonium picrate at present.
Summary of the invention
In order to overcome, ammonium picrate water absorbability is strong, free-running property is poor, be difficult to the defect of powder charge in the present invention, provides the preparation method of a kind of ammonium picrate and crown ether cocrystallized explosive.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
A preparation method for ammonium picrate and crown ether cocrystallized explosive, is characterized in that it comprises other step:
(1) preparation of ammonium picrate and crown ether saturated solution
Appropriate ammonium picrate is joined in recrystallisation solvent, then 20 ~ 50 DEG C are warming up to, filter after dissolving, obtain ammonium picrate saturated solution, again appropriate crown ether is joined in ammonium picrate saturated solution, keep temperature to be 20 ~ 50 DEG C, filter after dissolving, obtain the saturated solution of ammonium picrate and crown ether mixing;
(2) preparation of ammonium picrate and crown ether cocrystallized explosive
The saturated solution of the ammonium picrate prepare step (1) and crown ether mixing filters, filtrate is placed in beaker, then evaporating solvent in constant incubator is statically placed in, successively through formation, the grain growth of structure cell, final formation crystal, then carries out filtering, drying obtains ammonium picrate and crown ether cocrystallized explosive.
Further technical scheme is: in the preparation method of described ammonium picrate and crown ether cocrystallized explosive, crown ether is the ring compound be made up of 6 Sauerstoffatoms and 12 carbon atoms, and namely 18-is preced with (ether)-6.Crown ether contains comparatively strong hydrogen bonding acceptor groups, and has larger ring cavity, and easy and ammonium root positively charged ion forms non covalent bond.In order to reduce the water absorbability of ammonium picrate, itself and crown ether being formed eutectic, realizes eutectic efficiently reduction water absorbability, improving its security, expanding its range of application.
Further technical scheme is: in the preparation method of described ammonium picrate and crown ether cocrystallized explosive, solvent is one or more the mixture in methyl alcohol, ethanol, Virahol, the trimethyl carbinol, acetone.
Further technical scheme is: the temperature in the preparation method of described ammonium picrate and crown ether cocrystallized explosive during evaporating solvent in constant incubator is 25 ~ 45 DEG C.
Compared with prior art, one of beneficial effect of the present invention is: 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.Ammonium picrate/crown ether eutectic has lower water absorbability and good security, has excellent free-running property simultaneously, can be used as the composition of main charge, gunpowder and propelling agent, in low sense ammunition, have good application prospect.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow process of ammonium picrate of the present invention and crown ether cocrystallized explosive.
Fig. 2 is the crystalline structure of ammonium picrate of the present invention and crown ether cocrystallized explosive.
Fig. 3 is the XRD spectra of ammonium picrate of the present invention and crown ether cocrystallized 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.
The present invention prepares the technical process of ammonium picrate and crown ether cocrystallized explosive as shown in Figure 1.
Embodiment 1
At room temperature, 40ml acetone is added in there-necked flask, then under agitation add enough ammonium picrates, dissolve, filter, obtain the saturated solution of ammonium picrate; Then add enough 18-and be preced with (ether)-6, stir, dissolve, filter, filtrate is contained in beaker; Then be still in the thermostat container of 30 DEG C, allow solvent evaporate, crystallize out, drying obtains ammonium picrate and crown ether cocrystallized explosive.
Embodiment 2
At 30 DEG C, 50ml methyl alcohol is added in there-necked flask, then under agitation add enough ammonium picrates, dissolve, filter, obtain the saturated solution of ammonium picrate; Then add enough 18-and be preced with (ether)-6, stir, dissolve, filter, filtrate is contained in beaker; Then be still in the thermostat container of 35 DEG C, allow solvent evaporate, crystallize out, drying obtains ammonium picrate and crown ether cocrystallized explosive.
Embodiment 3
At 35 DEG C, 60ml ethanol is added in there-necked flask, then under agitation add enough ammonium picrates, dissolve, filter, obtain the saturated solution of ammonium picrate.Then add enough 18-and be preced with (ether)-6, stir, dissolve, filter, filtrate is contained in beaker.Then be still in the thermostat container of 35 DEG C, allow solvent evaporate, crystallize out, drying obtains ammonium picrate and crown ether cocrystallized explosive.
Embodiment 4
At room temperature, 50ml Virahol is added in there-necked flask, then under agitation add enough ammonium picrates, temperature is elevated to 35 DEG C, dissolve, filter, obtain the saturated solution of ammonium picrate.Then add enough 18-and be preced with (ether)-6, stir, dissolve, filter, filtrate is contained in beaker.Then be still in the thermostat container of 25 DEG C, allow solvent evaporate, crystallize out.Drying obtains ammonium picrate and crown ether cocrystallized explosive.
Embodiment 5
At room temperature, the 100ml trimethyl carbinol and methyl alcohol (volume ratio 1:1) are added in there-necked flask, then under agitation adds enough ammonium picrates, temperature is elevated to 40 DEG C, dissolve, filter, obtain the saturated solution of ammonium picrate.Then add enough crown ether 18-and be preced with (ether)-6, stir, dissolve, filter, filtrate is contained in beaker.Then be still in the thermostat container of 45 DEG C, allow solvent evaporate, crystallize out.Drying obtains ammonium picrate and crown ether cocrystallized explosive.
The ammonium picrate of the various embodiments described above gained and crown ether cocrystallized explosive and its component property comparative result are as table 1.
Table 1 ammonium picrate compares with its component property with crown ether cocrystallized explosive
As can be seen from Table 1, crown ether and ammonium picrate cocrystallized explosive crystalline density are about 1.3 ~ 1.4gcm
-3, and non-hygroscopic, improve the free-running property of dunnite, make it be easy to powder charge, range of application is widened.Fig. 2 is the crystalline structure of ammonium picrate of the present invention and crown ether cocrystallized explosive, and Fig. 3 is the XRD spectra of ammonium picrate of the present invention and crown ether 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 (4)
1. a preparation method for ammonium picrate and crown ether cocrystallized explosive, is characterized in that it comprises other step:
(1) preparation of ammonium picrate and crown ether saturated solution
Appropriate ammonium picrate is joined in recrystallisation solvent, then 20 ~ 50 DEG C are warming up to, filter after dissolving, obtain ammonium picrate saturated solution, again appropriate crown ether is joined in ammonium picrate saturated solution, keep temperature to be 20 ~ 50 DEG C, filter after dissolving, obtain the saturated solution of ammonium picrate and crown ether mixing;
(2) preparation of ammonium picrate and crown ether cocrystallized explosive
The saturated solution of the ammonium picrate prepare step (1) and crown ether mixing filters, filtrate is placed in beaker, then evaporating solvent in constant incubator is statically placed in, successively through formation, the grain growth of structure cell, final formation crystal, then carries out filtering, drying obtains ammonium picrate and crown ether cocrystallized explosive.
2. the preparation method of ammonium picrate according to claim 1 and crown ether cocrystallized explosive, is characterized in that described crown ether is ring compound 18-hat (ether)-6 be made up of 6 Sauerstoffatoms and 12 carbon atoms.
3. the preparation method of ammonium picrate according to claim 1 and crown ether cocrystallized explosive, is characterized in that described solvent is one or more the mixture in methyl alcohol, ethanol, Virahol, the trimethyl carbinol, acetone.
4. the preparation method of ammonium picrate according to claim 1 and crown ether cocrystallized explosive, temperature when it is characterized in that described evaporating solvent in constant incubator is 25 ~ 45 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748592A (en) * | 2016-12-07 | 2017-05-31 | 中国工程物理研究院化工材料研究所 | ADN and crown ether eutectic oxidant and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992923A (en) * | 2012-11-01 | 2013-03-27 | 中国工程物理研究院化工材料研究所 | Preparation method of benzotrifuroxan (BTF) and trinitrotoluene (TNT) cocrystallized explosive |
| CN102992925A (en) * | 2012-11-01 | 2013-03-27 | 中国工程物理研究院化工材料研究所 | Method for preparing BTF-HNIW (benzotrifuroxan- hexanitrohexaazaisowurtzitane) eutectic explosive |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992923A (en) * | 2012-11-01 | 2013-03-27 | 中国工程物理研究院化工材料研究所 | Preparation method of benzotrifuroxan (BTF) and trinitrotoluene (TNT) cocrystallized explosive |
| CN102992925A (en) * | 2012-11-01 | 2013-03-27 | 中国工程物理研究院化工材料研究所 | Method for preparing BTF-HNIW (benzotrifuroxan- hexanitrohexaazaisowurtzitane) eutectic explosive |
Non-Patent Citations (2)
| Title |
|---|
| TU LEE等: ""Stabilization and spheroidization of ammonium nitrate: Co-crystallization with crown ethers and spherical crystallization by solvent screen"", 《CHEMICAL ENGINEERING JOURNAL》 * |
| 郭长艳等: ""共晶炸药研究进展"", 《材料导报A：综述篇》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748592A (en) * | 2016-12-07 | 2017-05-31 | 中国工程物理研究院化工材料研究所 | ADN and crown ether eutectic oxidant and preparation method thereof |
| 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 |
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