CN105418619B - A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane - Google Patents
A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane Download PDFInfo
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- CN105418619B CN105418619B CN201511000272.2A CN201511000272A CN105418619B CN 105418619 B CN105418619 B CN 105418619B CN 201511000272 A CN201511000272 A CN 201511000272A CN 105418619 B CN105418619 B CN 105418619B
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
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Abstract
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：Hexanitrohexaazaisowurtzitane solution is provided；Dilute solution is diluted crystallization to the Hexanitrohexaazaisowurtzitane solution successively according to the order of concentration from high to low, obtains speciality Hexanitrohexaazaisowurtzitane.Method provided by the invention is diluted crystallization according to the order of concentration from high to low by dilute solution to Hexanitrohexaazaisowurtzitane solution, single chmical compound explosive crystalline density is improved by diluting crystallization, reduce matter crystal internal defect, eliminate surface blemish, control crystal shape and granularity, so as to improve single chmical compound explosive quality, meet requirement.
Description
Technical field
The present invention relates to explosive field, more particularly to a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane.
Background technology
Hexanitrohexaazaisowurtzitane, be by Nielen of USN's weapons center et al. by for many years make great efforts in
Take the lead in synthesizing within 1987, be the Typical Representative of high-energy-density energetic material.The crystalline density of Hexanitrohexaazaisowurtzitane
HMX is superior to oxygen balance, there is excellent energy response, chemical stability is good, available for missile armament powder charge, solid fire
The high-energy-density energetic material such as arrow propellant and atom bomb priming field.
Hexanitrohexaazaisowurtzitane (CL-20) is polymorph, have four kinds of crystal formations for α, β, γ under normal temperature and pressure and
The crystalline density of ε, ε type Hexanitrohexaazaisowurtzitane reaches 2.04g/cm3~2.05g/cm3.The normal method in two steps of existing process
Synthesize Hexanitrohexaazaisowurtzitane：Six substitution hexaazaisopen wootz alkyls are synthesized by original amine first, then pass through six
Substitute the direct nitration reaction production Hexanitrohexaazaisowurtzitane of hexaazaisopen wootz alkyl, the obtained azepine of hexanitro six different 5
Hereby alkane is ε crystal formations, and crystal shape is mostly elongated bipyramid shape, and about 40 microns of median, granularity is small, it is difficult to meets cast mixing
Requirement of the explosive to Hexanitrohexaazaisowurtzitane granularity and crystal morphology.
The content of the invention
It is an object of the invention to provide a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, the present invention provides
The obtained speciality Hexanitrohexaazaisowurtzitane granularity of preparation method it is big, plane of crystal is round and smooth, without obvious water caltrop.
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：
Hexanitrohexaazaisowurtzitane solution is provided；
Dilute solution is entered to the Hexanitrohexaazaisowurtzitane solution successively according to the order of concentration from high to low
Row dilution crystallization, obtains speciality Hexanitrohexaazaisowurtzitane.
Preferably, the dilute solution be methyl acetate normal octane solution, methyl acetate normal octane solution, ethyl acetate just
N-heptane solution or the positive heptyl ester solution of ethyl acetate.
Preferably, the dilute solution includes the dilute solution of four gradient mass concentrations, specially the first dilute solution,
Second dilute solution, the 3rd dilute solution and the 4th dilute solution；It is first dilute solution, the second dilute solution, the 3rd dilute
The concentration for releasing solution and the 4th dilute solution differs 15%~20% successively.
Preferably, it is described dilution crystallization be specially：
The dilute solution stream is added in the Hexanitrohexaazaisowurtzitane solution and is diluted crystallization；
The flow acceleration of the dilute solution is 5~9Kg/h；
The dilution crystallization rate of the dilute solution of high concentration is less than the dilute solution of low quality concentration.
Preferably, the time of the dilution crystallization is 36~48h.
Preferably, the temperature of the dilution crystallization is 35 DEG C~50 DEG C.
Preferably, the polarity ester or polarity ketones solvent that the solvent in the Hexanitrohexaazaisowurtzitane solution is.
Preferably, the solvent is ethyl acetate, methyl acetate, acetone or methyl ethyl ketone.
Preferably, the mass ratio of solute and solvent is (2.0~3.0) in the Hexanitrohexaazaisowurtzitane solution:
1。
Preferably, also include after the dilution crystallization：The speciality Hexanitrohexaazaisowurtzitane is filtered, water
Sieve and the process dried.
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：There is provided
Hexanitrohexaazaisowurtzitane solution；By dilute solution according to concentration order from high to low successively to the nitrogen of hexanitro six
Miscellaneous different 5 hereby alkane solution be diluted crystallization, obtain speciality Hexanitrohexaazaisowurtzitane.Method provided by the invention passes through
Dilute solution is diluted crystallization according to the order of concentration from high to low to Hexanitrohexaazaisowurtzitane solution, by dilution
Crystallization improves single chmical compound explosive crystalline density, reduces matter crystal internal defect, eliminates surface blemish, controls crystal shape and granularity,
So as to improve single chmical compound explosive quality, meet requirement.The embodiment of the present application result shows that the resulting azepine of hexanitro six is different
5 hereby alkane plane of crystal it is round and smooth, without obvious corner angle, axial ratio is small, and no more than 1.5, circularities are high, not less than 0.85, granularity
Greatly, more than 200 microns, the physical property such as outward appearance, granularity, surface and internal flaw is different from conventional method and obtained median
Hexanitrohexaazaisowurtzitane, security performance is better than the obtained Hexanitrohexaazaisowurtzitane of conventional method, can be used for
Grain size distribution improves brisance, met not to increase degree of packing, improve charge process performance, reduction composite explosives sensitivity
Same application requirement.
Brief description of the drawings
Fig. 1 is the microstructure picture of CL-20 in the prior art；
Fig. 2 is the microstructure picture for the speciality CL-20 that the embodiment of the present invention 1 obtains.
Embodiment
The invention provides a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprise the following steps：
Hexanitrohexaazaisowurtzitane solution is provided；
Dilute solution is entered to the Hexanitrohexaazaisowurtzitane solution successively according to the order of concentration from high to low
Row dilution crystallization, obtains speciality Hexanitrohexaazaisowurtzitane.
Method provided by the invention, raw material CL-20 solution is recrystallized using dilute solution, obtained speciality CL-
20 product granularities are big, narrowly distributing, plane of crystal are round and smooth, without obvious corner angle, axial ratio≤1.5, circularities >=0.85, are suitable for
Grain size distribution, improve the performances such as powder charge performance, insensitiveness performance, degree of packing and the brisance of molten note and casting blasting charge.
The present invention is diluted crystallization using dilute solution to Hexanitrohexaazaisowurtzitane solution.The present invention is to described
The preparation method of Hexanitrohexaazaisowurtzitane solution does not have special limitation, using solution well known to those skilled in the art
The technical scheme of preparation.In the present invention, the solvent in the Hexanitrohexaazaisowurtzitane solution is preferably polarity
Esters solvent or polarity ketones solvent, more preferably ethyl acetate, methyl acetate, acetone or methyl ethyl ketone.In the present invention,
The mass ratio of solute and solvent is preferably (2.0~3.0) in the Hexanitrohexaazaisowurtzitane solution: 1, more preferably
(2.4~2.8)；1；In an embodiment of the present invention, the matter of solute and solvent in the Hexanitrohexaazaisowurtzitane solution
It can be specially 2.4: 1,2.5: 1,2.6: 1,2.7: 1 or 2.8: 1 to measure ratio.
After Hexanitrohexaazaisowurtzitane is preferably dissolved in solvent by the present invention, obtained lysate is filtered, removed
Wherein insoluble impurity is removed, obtains Hexanitrohexaazaisowurtzitane solution.
After obtaining Hexanitrohexaazaisowurtzitane solution, the present invention using dilute solution according to mass concentration from high to low
Order crystallization is diluted to the Hexanitrohexaazaisowurtzitane solution successively, obtain the azepine of speciality hexanitro six different 5
Hereby alkane.In the present invention, the dilute solution is preferably methyl acetate normal octane solution, methyl acetate normal octane solution, acetic acid
Ethyl ester n-heptane solution or the positive heptyl ester solution of ethyl acetate.
In the present invention, the dilute solution preferably comprises the dilute solution of four gradient mass concentrations, and specially
One dilute solution, the second dilute solution, the 3rd dilute solution and the 4th dilute solution；First dilute solution, the second dilution
The concentration of solution, the 3rd dilute solution and the 4th dilute solution preferably differs 15%~20% successively.In embodiments of the invention
In, in the dilute solution of aforementioned four gradient mass fraction, the concentration between the dilute solution of two neighboring gradient mass fraction
Difference is independently 15%, 16%, 17%, 18%, 19% or 20%.
Specifically, in the present invention, the mass concentration of first dilute solution is preferably 75%~60%, more preferably
70%~65%, most preferably 72%；The mass concentration of second dilute solution is preferably 40%~55%, more preferably
45%~52%, most preferably 50%；The mass concentration of 3rd dilute solution is preferably 25%~40%, more preferably
30%~35%, most preferably 33%；The mass concentration of 4th dilute solution is preferably 0%.
In the present invention, first dilute solution, the second dilute solution, the 3rd dilute solution and the 4th dilute solution
Mass ratio is preferably (0.3~0.8): (0.8~1.2): (0.5~1.0): 1, more preferably (0.4~0.7): (0.9~1.1):
(0.6~0.9): 1, most preferably 0.5: 1: 0.75: 1.In the present invention, the 4th dilute solution and the CL-20 solution
Mass ratio be preferably (1.0~2.0): 1, more preferably (1.2~1.8): 1, most preferably 1.4: 1.
In the present invention, the dilution crystallization is preferred is specially：
First dilute solution, second dilute solution, the 3rd dilute solution and the 4th dilute solution are successively
Stream is added to the CL-20 solution, and the speed that the stream adds is preferably 5~9Kg/h, and first dilute solution, the second dilution are molten
The flow acceleration of liquid, the 3rd dilute solution and the 4th dilute solution raises 0.5Kg/h~1Kg/h successively.
The relation that the present invention reduces successively according to dilute solution concentration, when being diluted crystallization, dilute solution stream is added to institute
The speed stated in CL-20 solution is raised successively, and crystallization is diluted according to rule from slow to fast.In the present invention, it is described dilute
Crystallization is released to carry out preferably under conditions of stirring.The dilute solution is injected into CL-20 by the present invention preferably in 36h~48h
In solution, crystallization, more preferably 39h~45h, most preferably 41h~43h are diluted.In the present invention, the dilution crystallization
Temperature be preferably 35 DEG C~50 DEG C, more preferably 40 DEG C~45 DEG C.
In the present invention, the preparation of the CL-20 solution and dilution crystallization process are carried out preferably in crystallization kettle.
After completing the crystallization, the material after crystallization is preferably carried out separation of solid and liquid, washing and drying by the present invention, obtains spy
Matter CL-20.The present invention does not have special limitation to the method for the separation of solid and liquid, the solid-liquid that who knows using those skilled in the art
The technical scheme of separation, can more specifically can be such as to filter by the way of filtering.The embodiment of the present invention is specifically adopted
The material after cooling is filtered with vacuum filter.The present invention does not have special limitation to the method for the washing, uses
The technical scheme of washing well known to those skilled in the art, it can such as use washing, number of the present invention to the washing
There is no special limitation.
In the present invention, the recyclable recycling of liquid phase part obtained after separation of solid and liquid, present invention balance consider mother liquor
Remain the concentration of the factors such as CL-20 contents, disposing mother liquor cost, utilization rate of equipment and installations, product yield, preferably control crystallization Mother liquor
In 40%~60%, more preferably 45%~55%, most preferably 50%.
The present invention does not have special limitation to the method for the drying, the skill for the drying who knows using those skilled in the art
Art scheme.In the present invention, the drying is preferably and drained.
After draining, granularity of the present invention preferably by obtained product according to target product requirement, taken out using screen cloth to described
Product after dry carries out water sieve, obtains target product wet product.In the present invention, the granularity of the target product can be specially 80 mesh
The mesh of the mesh of~40 mesh, 60 mesh~40 or 100 mesh~40, those skilled in the art can select the screen cloth of suitable mesh to carry out as needed
Water sieve；In an embodiment of the present invention, aperture may be selected is 0.425mm, 0.180mm, 0.100mm, 0.075mm or 0.045mm
Screen cloth.
After obtaining target product wet product, preferably the wet product is dried by the present invention, obtains speciality CL-20.The present invention
There is no special limitation to the method for the drying, using the technical scheme of drying well known to those skilled in the art.
In the present invention, the temperature of the drying is preferably 50 DEG C~55 DEG C.In the present invention, the moisture of the speciality CL-20 is excellent
Choosing is less than 0.10%.
In order to further illustrate the present invention, with reference to embodiment to Hexanitrohexaazaisowurtzitane provided by the invention
Preparation method be described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
By taking 400 liters of spheroidal crystal kettles as an example, speciality CL-20 is prepared, detailed process is as follows：
1st, at room temperature, 78kg ethyl acetate is added in dissolution kettle, under stirring condition, 30kg raw materials are added into dissolution kettle
CL-20, all lysate is filtered after dissolving, obtains CL-20 solution；
2nd, obtained CL-20 solution is added in spheroidal crystal kettle, at 35 DEG C~50 DEG C, by after first high concentration plus low dense
The order of degree, the ethyl acetate normal octane solution for flowing plus measuring respectively：72% ethyl acetate normal octane solution 39kg, 50% second
Acetoacetic ester normal octane 78kg, 33% ethyl acetate normal octane 58.5kg, finally plus normal octane 78kg, control flow acceleration are first slow
It is fast afterwards, added in 36~48 hours, control crystallization temperature is not less than 35 DEG C, and crystallization temperature is adjusted by chuck circulating water temperature；
3rd, blowing, the solvent in filtering layer is drained；
4th, crystallized stock is crossed into water sieve, collects 80~40 mesh (0.180mm~0.425mm) CL-20 and analyzed, it is desirable to
Thing content is not less than 80% between sieve；
5th, crystallized stock is placed in drying cupboard drying, under the conditions of 50 DEG C~55 DEG C, is dried to moisture less than 0.10%, obtains
To speciality CL-20.
Obtained speciality CL-20 is carried out microstructure detection by the present invention, as a result as shown in Fig. 2 Fig. 2 is implemented for the present invention
The microstructure picture for the speciality CL-20 that example 1 obtains, by compared with prior art CL-20 microstructure (Fig. 1),
Crystal shape is mostly elongated bipyramid shape in Fig. 1, and granularity is small, about 40 microns of median, and axial ratio is 2.1, circularities
For 0.74；In Fig. 2, plane of crystal is round and smooth, and without obvious corner angle, axial ratio is small, and no more than 1.5, circularities are high, more than 0.85,
Granularity is big, and median is more than 200 microns.
Analytical control indices, after meeting the requirement of speciality CL-20 contract standards, packaging, the indices such as embodiment of table 1
Shown in 1 obtained speciality CL-20 all technicals.
The all technical for the speciality NTO that the embodiment of the present invention 1 of table 1 obtains
Embodiment 2
Speciality CL-20 is prepared using the scheme of embodiment 1, unlike, the solvent that CL-20 is dissolved in the present embodiment is second
Sour methyl esters, dilute solution are methyl acetate normal octane.
Obtained speciality CL-20 is carried out microstructure detection by the present invention, is as a result shown, the speciality that the present invention is prepared
CL-20 planes of crystal are round and smooth, and without obvious corner angle, axial ratio is small, and circularities are high, and granularity is big.
Embodiment 3
Speciality CL-20 is prepared using the scheme of embodiment 1, unlike, in the present embodiment, dilute solution is acetic acid
Ethyl ester n-heptane solution；Crystallized stock crosses water sieve, collects 150~40 mesh (0.100mm~0.425mm) CL-20 and is analyzed,
It is required that thing content is not less than 85% between sieve.
Obtained speciality CL-20 is carried out microstructure detection by the present invention, is as a result shown, the speciality that the present invention is prepared
CL-20 planes of crystal are round and smooth, and without obvious corner angle, axial ratio is small, and circularities are high, and granularity is big.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of speciality Hexanitrohexaazaisowurtzitane, comprises the following steps：
Hexanitrohexaazaisowurtzitane solution is provided；
Order of the dilute solution according to concentration from high to low is dilute to Hexanitrohexaazaisowurtzitane solution progress successively
Crystallization is released, obtains speciality Hexanitrohexaazaisowurtzitane；
The dilute solution is methyl acetate normal octane solution, ethyl acetate normal octane solution or ethyl acetate n-heptane solution；
The dilute solution includes the dilute solution of four gradient mass concentrations, and specially the first dilute solution, the second dilution are molten
Liquid, the 3rd dilute solution and the 4th dilute solution；First dilute solution, the second dilute solution, the 3rd dilute solution and
The concentration of four dilute solutions differs 15%~20% successively.
2. the preparation method described in claim 1, it is characterised in that it is described dilution crystallization be specially：
The dilute solution stream is added in the Hexanitrohexaazaisowurtzitane solution and is diluted crystallization；
The flow acceleration of the dilute solution is 5~9Kg/h；
The dilution crystallization rate of the dilute solution of high concentration is less than the dilute solution of low quality concentration.
3. preparation method according to claim 1, it is characterised in that the time of the dilution crystallization is 36~48h.
4. preparation method according to claim 1, it is characterised in that the temperature of the dilution crystallization is 35 DEG C~50 DEG C.
5. preparation method according to claim 1, it is characterised in that in the Hexanitrohexaazaisowurtzitane solution
The polarity ester or polarity ketones solvent that solvent is.
6. preparation method according to claim 5, it is characterised in that the solvent is ethyl acetate, methyl acetate, acetone
Or methyl ethyl ketone.
7. according to the preparation method described in claim 1,5 or 6, it is characterised in that the Hexanitrohexaazaisowurtzitane is molten
The mass ratio of solute and solvent is (2.0~3.0) in liquid:1.
8. preparation method according to claim 1, it is characterised in that also include after the dilution crystallization：To the speciality
Hexanitrohexaazaisowurtzitane is filtered, the process of water sieve and drying.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106117229B (en) * | 2016-08-31 | 2018-01-02 | 山西北化关铝化工有限公司 | A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane |
| CN106553117A (en) * | 2016-10-17 | 2017-04-05 | 北京理工大学 | A kind of method that mechanical lapping prepares 20 crystal of spherical super fine ε CL |
| CN109485531A (en) * | 2018-12-13 | 2019-03-19 | 南京理工大学 | Superfine spherical CL-20 Composite Energetic Materials and preparation method thereof |
| CN111233589B (en) * | 2020-02-13 | 2021-10-22 | 山西北化关铝化工有限公司 | Preparation method of ultra-large particle hexanitrohexaazaisowurtzitane |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5874574A (en) * | 1996-12-17 | 1999-02-23 | Cordant Technologies Inc. | Process of crystallizing 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12,-hexaazatetracyclo 5.5.0.0.5,903,11!- dodecane |
| CN101624395A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Synthetic method of hexabenzylhexaazaisowurtzitane |
| CN101624394A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof |
| EP1327633B1 (en) * | 2002-01-09 | 2010-12-15 | Alliant Techsystems Inc. | Crystallization of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo(5.5.0.0.59O3,11)-dodecane |
| CN102596857A (en) * | 2009-09-29 | 2012-07-18 | Sme公司 | Hexanitrohexaazaisowurtzitane crystal suspensions, production of said suspensions and production of pyrotechnic objects |
| CN102898429A (en) * | 2012-09-18 | 2013-01-30 | 北京理工大学 | Recrystallization method for controlling crystal shape and narrow particle size distribution of epsilon-HNIW |
| CN103539800A (en) * | 2013-10-18 | 2014-01-29 | 中国工程物理研究院化工材料研究所 | Preparation method of large-particle hexanitrohexaazaisowurtzitane explosive |
-
2015
- 2015-12-29 CN CN201511000272.2A patent/CN105418619B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5874574A (en) * | 1996-12-17 | 1999-02-23 | Cordant Technologies Inc. | Process of crystallizing 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12,-hexaazatetracyclo 5.5.0.0.5,903,11!- dodecane |
| EP1327633B1 (en) * | 2002-01-09 | 2010-12-15 | Alliant Techsystems Inc. | Crystallization of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo(5.5.0.0.59O3,11)-dodecane |
| CN101624395A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Synthetic method of hexabenzylhexaazaisowurtzitane |
| CN101624394A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof |
| CN102596857A (en) * | 2009-09-29 | 2012-07-18 | Sme公司 | Hexanitrohexaazaisowurtzitane crystal suspensions, production of said suspensions and production of pyrotechnic objects |
| CN102898429A (en) * | 2012-09-18 | 2013-01-30 | 北京理工大学 | Recrystallization method for controlling crystal shape and narrow particle size distribution of epsilon-HNIW |
| CN103539800A (en) * | 2013-10-18 | 2014-01-29 | 中国工程物理研究院化工材料研究所 | Preparation method of large-particle hexanitrohexaazaisowurtzitane explosive |
Non-Patent Citations (3)
| Title |
|---|
| HNIW在乙酸乙酯-正庚烷溶剂体系中的结晶机制研究;李洪珍，等;《含能材料》;20121231;第20卷(第1期);30-34 * |
| ε-HNIW在不同溶剂中的晶型稳定性;刘进全，等;《含能材料》;20060430;第14卷(第2期);108-110 * |
| 特质CL-20 制备工艺研究;陈华华，等;《2014 年含能材料与钝感弹药技术学术研讨会论文集》;20141231;13-17 * |
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