CN102924192A - Method for preparing micro-nano TATB (triamino trinitrobenzene) explosive granules - Google Patents
Method for preparing micro-nano TATB (triamino trinitrobenzene) explosive granules Download PDFInfo
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- CN102924192A CN102924192A CN2012103613501A CN201210361350A CN102924192A CN 102924192 A CN102924192 A CN 102924192A CN 2012103613501 A CN2012103613501 A CN 2012103613501A CN 201210361350 A CN201210361350 A CN 201210361350A CN 102924192 A CN102924192 A CN 102924192A
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Abstract
The invention discloses a method for preparing micro-nano TATB (triamino trinitrobenzene) explosive granules. The method comprises the following steps of: (1) preparation of explosive solution, wherein the TATB explosive is dissolved to prepare the explosive solution without impurities; (2) preparation of non-solvent medium, wherein water and dispersant are uniformly mixed to prepare the non-solvent medium, and the non-solvent medium is cooled by putting in a refrigerator or adding ice cakes and other mode; (3) mixed crystallization, wherein the TATB explosive solution prepared in the step (1) and the non-solvent medium prepared in the step are mixed to crystallize to form micro-nano explosive granules, and the non-solvent medium in the mixing process is kept at a temperature of lower than 10 DEG C; and (4) post-treatment, wherein the micro-nano explosive granule liquid prepared in the step (3) are subjected to solid-liquid separation, washing purification and drying to obtain the micro-nano TATB explosive product. The method has the characteristics of simple process flow and convenience in operation, and is applicable to industrial large-scale production. By adopting the method, micro-nano TATB powder with average granular diameter of 170nm and d50 of 100nm can be obtained by controlling process parameters.
Description
Technical field
The invention belongs to material science, particularly relate to the preparation method of the following micro-nano TATB blasting explosive granules of a kind of particle diameter 1 μ m.
Background technology
TATB(1,3,5-triamino-2,4,6-trinitrobenzene) owing to height insensitiveness, the moderate model who becomes insensitive high energy explosive (IHE) of energy, enjoy the concern in energetic material field.But TATB is insensitiveness too, detonate, the high explosive trains application facet is restricted.After the TATB refinement, its explosion transfer performance that detonates will significantly improve, therefore ultra-fine TATB particularly the following micro/nano level TATB of 1 μ m except the excellent properties that keeps plain particles size TATB height insensitiveness, its critical diameter is less, to film flying, the short pulse sensitivity of detonating, and detonation wave propagates faster more stablely, is expected to impact sheet detonator start medicine and booster explosive for non-sensitive type, and is significant to improving the weapons system security reliability.
The preparation technology of micro-nano TATB and technology also are subject to domestic and international expert and scholar's attention, the particularly U.S. and have carried out more research work since the eighties in 20th century in this field, and the scholar of the domestic work that conducts a research in this field is few.Take a broad view of the refinement of TATB, adoptable method mainly contains: mechanical milling method, ball milled, comminution by gas stream, crystallization process, emulsion method etc.Mechanical milling method and ball milled are very easily brought more mechanical impurity into, and more serious fine particle reunion phenomenon can occur when refineing to a certain degree; Comminution by gas stream needs complicated airing system and purification process system, and pulverizing material loss amount in early stage is larger; Emulsion method need to use more emulsifying agent class material, not only the not easy to clean removal of cost height and later stage; That crystallization process has is easy and simple to handle, be easy to amplify, can obtain fine particle and high-specific surface area and become the good method of the micro-nano explosive of preparation.Different according to the concrete ways of realizing micro-nano, crystallization process can adopt various ways, the most investigator has all adopted solvent/non-solvent method or neutralisation, these two kinds of methods have all been utilized the crystallography principle, generally all at several microns, the particle that neutralisation obtains is thicker for the ultra-fine TATB granular size that obtains.Be difficult to be refined to the problem of micro/nano level for TATB, the preparation method of micro-nano TATB has been studied in this discovery, adopts this method can obtain even particle size, narrow diameter distribution, the volume average particle size TATB explosive below 200nm.
Summary of the invention
One of purpose of the embodiment of the invention is to provide a kind of micro-nano TATB explosive preparation method.
The present invention is achieved in that
A kind of preparation method of micro-nano TATB blasting explosive granules comprises the steps:
(1) preparation of explosive solution.With the dissolving of TATB explosive, make pure explosive solution;
(2) preparation of non-solvent medium.With water and dispersion agent mixing, make the non-solvent medium, and by putting into refrigerator-freezer or adding ice cube the non-solvent medium is cooled off;
(3) mixed crystallization.Non-solvent medium mixed crystallization with TATB explosive solution and the step (2) of step (1) preparation are prepared forms micro-nano blasting explosive granules, and the non-solvent medium temperature remains on below 10 ℃ in the mixing process;
(4) aftertreatment.The micro-nano blasting explosive granules feed liquid that step (3) obtains is carried out solid-liquid separation, washing purifying, drying, obtain micro/nano level TATB explosive product.
The solvent of the employed dissolving of step (1) TATB explosive is the vitriol oil, is generally the vitriol oil of 98.3% mass concentration, and not excessive sulfuric acid concentration also can reach requirement of the present invention greater than 70% the time.
The resulting TATB explosive of step (1) concentration of polymer solution is between 2%～30%.
The described dispersion agent of step (2) is a kind of in alkylbenzene sulfonate, OP-10, this dish series.OP-10 is a kind of industrial chemicals, and composition is alkylphenol polyoxyethylene.
It is 0 ℃～10 ℃ that the described non-solvent medium of step (2) is cooled to temperature.
It is explosive solution to be added drop-wise in the non-solvent or under pressure be ejected in the non-solvent under normal pressure that the described explosive solution of step (3) mixes with the non-solvent medium, or the non-solvent medium is added drop-wise in the explosive solution or under pressure under normal pressure is ejected in the explosive solution.
When the described explosive solution of step (3) mixes with the non-solvent medium, the explosive solution of per 1 part of volume, the non-solvent medium of corresponding at least 5 parts of volumes.
The non-solvent medium is in the height disturbance state by stirring during the described mixed crystallization of step (3).
The described solid-liquid separation of step (4) can adopt a kind of in filtering of centrifugation, membrane sepn or filter plate.
The described drying of step (4) can adopt a kind of in lyophilize, room temperature vacuum-drying or the spraying drying.
The inventive method has technical process characteristics simple, easy and simple to handle, and is applicable to industrialized mass production.Adopt the inventive method, by the control process parameter, can obtain that volume average particle size can reach about 170nm, d
50Reach the micro-nano TATB powder about 100nm.
The hybrid mode of explosive solution and non-solvent medium among the above-mentioned preparation method, non-solvent medium temperature are larger for the TATB particle size influences, adopt mode, non-solvent medium that explosive solution is joined in the non-solvent medium to remain on the easier little micro-nano TATB product of grain diameter that makes of lower temperature.
Description of drawings
The typical volume size distribution of the micro-nano TATB of Fig. 1;
The micro-nano TATB stereoscan photograph that Fig. 2 normal pressure dripping method obtains;
The micro-nano TATB stereoscan photograph that Fig. 3 pressure injection method obtains.
Embodiment
In crystallizer, add 4000g deionized water and 1.0gOP-10 mixing, for subsequent use after being chilled in advance 2 ℃; Under the room temperature, in molten medicine still, add 100g TATB and the 2000g vitriol oil, stir, make explosive entirely molten, remove stirring, explosive solution is transferred to the liquid still; With agitator the non-solvent medium in the crystallizer is turned round strongly, again the explosive solution in the liquid still is added drop-wise in the non-solvent under normal pressure, add ice cube while dripping, the non-solvent medium temperature is remained on about 2 ℃; The refinement feed liquid that obtains at last-45 ℃ of lower lyophilizes, obtains the micro-nano TATB explosive of 92g, volume average particle size 171nm, d through repeatedly washing, centrifugation under the 10000r/min
50=107nm.
In crystallizer, add 4000g deionized water and 1.0gOP-10 mixing, for subsequent use after being chilled in advance 2 ℃; Under the room temperature, in molten medicine still, add 100g TATB and the 1000g vitriol oil, stir, make explosive entirely molten, remove stirring, explosive solution is transferred to the liquid still; With agitator the non-solvent medium in the crystallizer is turned round strongly, again the explosive solution in the liquid still is added drop-wise in the non-solvent under normal pressure, add ice cube while dripping, the non-solvent medium temperature is remained on about 2 ℃; The refinement feed liquid that obtains at last-45 ℃ of lower lyophilizes, obtains the micro-nano TATB explosive of 91g, volume average particle size 922nm, d through repeatedly washing, centrifugation under the 10000r/min
50=2591nm.
In crystallizer, add 4000g deionized water and 1.0gOP-10 mixing, for subsequent use after being chilled in advance 10 ℃; Under the room temperature, in molten medicine still, add 100g TATB and the 2000g vitriol oil, stir, make explosive entirely molten, remove stirring, explosive solution is transferred to the liquid still; With agitator the non-solvent medium in the crystallizer is turned round strongly, again the explosive solution in the liquid still is added drop-wise in the non-solvent under normal pressure, add ice cube while dripping, the non-solvent medium temperature is remained on about 10 ℃; The refinement feed liquid that obtains at last-40 ℃ of lower lyophilizes, obtains the micro-nano TATB explosive of 90g, volume average particle size 1769nm, d through repeatedly washing, centrifugation under the 10000r/min
50=1531nm.
In crystallizer, add 4000g deionized water and 1.0g Sodium dodecylbenzene sulfonate, mixing, for subsequent use after being chilled in advance 4 ℃; Under the room temperature, in molten medicine still, add 100g TATB and the 2000g vitriol oil, stir, make explosive entirely molten, remove stirring, explosive solution is transferred to the liquid still; With agitator the non-solvent medium in the crystallizer is turned round strongly, again the explosive solution in the liquid still is added drop-wise in the non-solvent under normal pressure, add ice cube while dripping, the non-solvent medium temperature is remained on about 4 ℃; The refinement feed liquid that obtains is separated through repeatedly washing, nanometer film, at last-40 ℃ of lower lyophilizes, obtains the micro-nano TATB explosive of 92g, volume average particle size 655nm, d
50=183nm.
In crystallizer, add 4000g deionized water and 1.0gOP-10 mixing, for subsequent use after being chilled in advance 4 ℃; Under the room temperature, in molten medicine still, add 100g TATB and the 2000g vitriol oil, stir, make explosive entirely molten, remove stirring, explosive solution is transferred to the liquid still; With agitator the non-solvent medium in the crystallizer is turned round strongly, again the explosive solution in the liquid still is added drop-wise in the non-solvent under normal pressure, add ice cube while dripping, the non-solvent medium temperature is remained on about 4 ℃; The refinement feed liquid that obtains is carried out vacuum-drying at last through repeatedly washing, centrifugation under the 10000r/min under 10 ℃, obtain the micro-nano TATB explosive of 91g, volume average particle size 340nm, d
50=150nm.
In crystallizer, add 4000g deionized water and 1.0gOP-10 mixing, for subsequent use after being chilled in advance 3 ℃; Under the room temperature, in molten medicine still, add 100g TATB and the 2000g vitriol oil, stir, make explosive entirely molten, remove stirring, explosive solution is transferred to the liquid still; With agitator the non-solvent medium in the crystallizer is turned round strongly, again the explosive solution in the liquid still is mapped in the non-solvent by micropore jet under 0.3MPa pressure, add ice cube while spraying, the non-solvent medium temperature is remained on about 3 ℃; The refinement feed liquid that obtains is carried out lyophilize at last through repeatedly washing, centrifugation under the 10000r/min under-40 ℃, obtain the micro-nano TATB explosive of 91g, volume average particle size 604nm, d
50=219nm.
Can find out that from accompanying drawing 1 the typical volume size distribution of micro-nano TATB has two peak values, substantially about 0.2 μ m and 1.8 μ m.And can find out that from accompanying drawing 2,3 although dual mode can obtain the less micro-nano TATB blasting explosive granules of particle diameter, the micro-nano TATB grain diameter that adopts gunite to obtain is less than the particle that dripping method obtains, particle diameter is more even.
Claims (9)
1. the preparation method of a micro-nano TATB blasting explosive granules is characterized in that comprising the steps:
(1) preparation of explosive solution; With the dissolving of TATB explosive, make pure explosive solution;
(2) preparation of non-solvent medium; With water and dispersion agent mixing, make the non-solvent medium, and by putting into refrigerator-freezer or adding ice cube the non-solvent medium is cooled off;
(3) mixed crystallization; Non-solvent medium mixed crystallization with TATB explosive solution and the step (2) of step (1) preparation are prepared forms micro-nano blasting explosive granules, and the non-solvent medium temperature remains on below 10 ℃ in the mixing process;
(4) aftertreatment; The micro-nano blasting explosive granules feed liquid that step (3) obtains is carried out solid-liquid separation, washing purifying, drying, obtain micro/nano level TATB explosive product.
2. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1 is characterized in that the solvent of the employed dissolving of step (1) TATB explosive is the vitriol oil.
3. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1 and 2 is characterized in that the resulting TATB explosive of step (1) concentration of polymer solution is between 2%～30%.
4. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1 is characterized in that the described dispersion agent of step (2) is a kind of in alkylbenzene sulfonate, OP-10, this dish series.
5. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1 is characterized in that it is 0 ℃～10 ℃ that the described non-solvent medium of step (2) is cooled to temperature.
6. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1, it is characterized in that it is explosive solution to be added drop-wise in the non-solvent medium or under pressure be ejected in the non-solvent medium that the described explosive solution of step (3) mixes with the non-solvent medium under normal pressure, or the non-solvent medium is added drop-wise in the explosive solution or under pressure under normal pressure is ejected in the explosive solution.
7. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1, when it is characterized in that the described explosive solution of step (3) mixes with the non-solvent medium, the explosive solution of per 1 part of volume, the non-solvent medium of corresponding at least 5 parts of volumes.
8. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1 is characterized in that the described solid-liquid separation of step (4) can adopt a kind of in filtering of centrifugation, membrane sepn or filter plate.
9. the preparation method of described micro-nano TATB blasting explosive granules according to claim 1 is characterized in that the described drying of step (4) can adopt a kind of in lyophilize, room temperature vacuum-drying or the spraying drying.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708984A (en) * | 2013-12-26 | 2014-04-09 | 中国工程物理研究院化工材料研究所 | Method for performing heat treatment on sensitized explosive |
| CN103980075A (en) * | 2014-04-30 | 2014-08-13 | 中国工程物理研究院化工材料研究所 | Preparation method for explosive having micro-nano multistage structure |
| CN104649850A (en) * | 2015-02-09 | 2015-05-27 | 中国工程物理研究院化工材料研究所 | High polymer bonded explosive enhancing mechanical properties with nanoparticles and preparation method of high polymer bonded explosive |
| CN106397076A (en) * | 2016-08-30 | 2017-02-15 | 中国工程物理研究院化工材料研究所 | Explosive with both high activity and process stability and preparation method thereof |
| CN107698412A (en) * | 2017-09-05 | 2018-02-16 | 中北大学 | Explosive eutectic preparation based on pneumatic nebulization antisolvent crystallisation |
| CN109776444A (en) * | 2019-03-11 | 2019-05-21 | 中国工程物理研究院化工材料研究所 | Method based on natural subsidence process preparation high dispersive DAAF nano-powder |
| CN112047791A (en) * | 2020-08-18 | 2020-12-08 | 南京理工大学 | Explosive continuous preparation system and method based on active micro mixer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6310253B1 (en) * | 1985-05-22 | 2001-10-30 | The United States Of America As Represented By The Department Of Energy | Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene of submicron particle size |
| US20020129880A1 (en) * | 2001-03-15 | 2002-09-19 | Lee Kien-Yin | Synthesis of fine-grained TATB |
| US20100317894A1 (en) * | 2009-06-15 | 2010-12-16 | Alliant Techsystems Inc. | Methods of producing 1,3,5-triamino-2,4,6-trinitrobenzene |
-
2012
- 2012-09-25 CN CN2012103613501A patent/CN102924192A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6310253B1 (en) * | 1985-05-22 | 2001-10-30 | The United States Of America As Represented By The Department Of Energy | Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene of submicron particle size |
| US20020129880A1 (en) * | 2001-03-15 | 2002-09-19 | Lee Kien-Yin | Synthesis of fine-grained TATB |
| US20100317894A1 (en) * | 2009-06-15 | 2010-12-16 | Alliant Techsystems Inc. | Methods of producing 1,3,5-triamino-2,4,6-trinitrobenzene |
Non-Patent Citations (5)
| Title |
|---|
| GUANGCHENG YANG,ETAL: "Preparation and Characterization of Nano-TATB Explosive", 《PROPELLANTS,EXPLOSIVES,PYROTECHNICS》 * |
| VEERA M.BODDU,ETAL: "2,4,6-Triamino-1,3,5-trinitrobenzene (TATB) and TATB-based formulations—A", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
| YANG LI, ETAL: "Preparation of Ultrafine TATB and the Technology for Crystal Morphology Control", 《CHINESE JOURAL OF CHEMISTRY》 * |
| 曾贵玉等: "亚微米TATB除酸方法比较", 《兵工学报》 * |
| 曾贵玉等: "冲击结晶技术制备亚微米TATB粒子的研究", 《火炸药学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708984A (en) * | 2013-12-26 | 2014-04-09 | 中国工程物理研究院化工材料研究所 | Method for performing heat treatment on sensitized explosive |
| CN103708984B (en) * | 2013-12-26 | 2015-11-11 | 中国工程物理研究院化工材料研究所 | A kind of method of thermal treatment sensitizing explosive |
| CN103980075A (en) * | 2014-04-30 | 2014-08-13 | 中国工程物理研究院化工材料研究所 | Preparation method for explosive having micro-nano multistage structure |
| CN103980075B (en) * | 2014-04-30 | 2016-06-08 | 中国工程物理研究院化工材料研究所 | The preparation method with micro-nano multi-level structure explosive |
| CN104649850A (en) * | 2015-02-09 | 2015-05-27 | 中国工程物理研究院化工材料研究所 | High polymer bonded explosive enhancing mechanical properties with nanoparticles and preparation method of high polymer bonded explosive |
| CN106397076A (en) * | 2016-08-30 | 2017-02-15 | 中国工程物理研究院化工材料研究所 | Explosive with both high activity and process stability and preparation method thereof |
| CN107698412A (en) * | 2017-09-05 | 2018-02-16 | 中北大学 | Explosive eutectic preparation based on pneumatic nebulization antisolvent crystallisation |
| CN109776444A (en) * | 2019-03-11 | 2019-05-21 | 中国工程物理研究院化工材料研究所 | Method based on natural subsidence process preparation high dispersive DAAF nano-powder |
| CN112047791A (en) * | 2020-08-18 | 2020-12-08 | 南京理工大学 | Explosive continuous preparation system and method based on active micro mixer |
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Application publication date: 20130213 |