CN105985206A - Method for coating and sensitivity reduction of HMX by using TATB - Google Patents
Method for coating and sensitivity reduction of HMX by using TATB Download PDFInfo
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- CN105985206A CN105985206A CN201510054386.9A CN201510054386A CN105985206A CN 105985206 A CN105985206 A CN 105985206A CN 201510054386 A CN201510054386 A CN 201510054386A CN 105985206 A CN105985206 A CN 105985206A
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- tatb
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Abstract
The invention discloses a method for coating and sensitivity reduction of HMX (cyclotetramethylene tetranitramine) by using TATB (triamino trinitrobenzene). The method comprises the following steps: adding a binder, a solvent and HMX into a beaker, performing heating and stirring until the materials are dissolved uniformly, and then performing vacuum filtration and drying to prepare HMX with surface activity and cohesiveness; dissolving TATB in concentrated sulfuric acid, and performing stirring until the TATB is dissolved to obtain a mixed solution of TATB and concentrated sulfuric acid; adding the prepared HMX with surface activity and cohesiveness and an ice-water mixture into a four-neck flask, and slowly dropwise adding the mixed solution of TATB and concentrated sulfuric acid into the four-neck flask by virtue of a constant pressure dropping funnel while performing rapid stirring to obtain a suspension; and performing vacuum filtration on the obtained suspension, washing filter cakes with a detergent until the pH value of the obtained filtrate is close to neutral, and performing drying to obtain mixed explosives in which TATB coats HMX. According to the method disclosed by the invention, the concentrated sulfuric acid is used as a solvent to refine the TATB so as to directly form a coating layer on the surface of the HMX, the binder is used during coating to effectively prevent cracking-off of the TATB, the reaction condition is mild, and the reaction operation is simple.
Description
One technical field
The present invention relates to the cladding fall sensing method of a kind of explosive, particularly directly exist for solvent refinement TATB with concentrated sulphuric acid
The new method of HMX Surface Creation clad fall sense.
Two background technologies
Along with the development of military science technology, survival ability and security performance to modern weapons propose increasingly
High requirement.Catastrophic failure that the aircraft carriers such as U.S.'s " enterprise number " are occurred and the most for over ten years ammunition process,
Storage, transport and use during unexpected major accident make people have a profound understanding of, it is necessary to develop low rapid wear ammunition, send out
Exhibition desensitized explosive, the emphasis of explosive research from attempting to increase substantially on the premise of energy transfers to ensure security performance
Appropriateness carries on high-octane direction.
HMX (HMX, HMX) is the high explosive that current composite performance is best, and it has highly dense
Degree, high-energy, thermostability high.The sixties to the seventies, HMX itself as a monomer high explosive,
Worldwide being widely studied, the eighties starts industrial applications.But exist sensitivity difference defect, easily because of high temperature,
Shocks etc. stimulate and unexpected induced detonation occur.And TATB (photoacoustic spectroscopy) is that a kind of energy is higher, sensitivity is relatively low,
The safety explosive that powder column size appropriateness just can be detonated, its mechanical sensitivity and heat sensitivity are the lowest, heat-resist.Both domestic and external
Research experiment shows, the sensitivity of coated explosive and the energy made with TATB cladding HMX are the most ideal.
It is mainly direct physical mixing method, ultrasonic in situ cladding process both at home and abroad by the method for TATB cladding fall sense HMX
And prepare cocrystallized explosive method.Preparing coated explosive by direct physical mixing method, coated particle is submicron TATB, bag
Degree of covering is the highest, and sensitivity reduces inconspicuous.
For improving TATB, the cladding of HMX is dropped sense effect, Sun Jie et al. at energetic material, 2006,13 (5): 330-332
In report and utilize sonochemistry synthetic method, at HMX particle surface in-situ preparation TATB, be prepared for HMX/TATB multiple
Compound.But this technique exists, and equipment cost is high, operate the shortcoming such as complexity and dangerous height.
Jin P.Shen et al. reports employing DMSO conduct in Cryst.Growth Des.2011,11,1759-1765
Solvent, water, as non-solvent, is prepared for cocrystallized explosive.But TATB dissolubility in DMSO is less in this technique,
Relatively costly, and crystallization process is difficult to control to.
Three summary of the invention
It is an object of the invention to provide a kind of low cost, reaction condition is gentle, easily operated, coating product degree is good
The method of TATB cladding fall sense HMX.
The technical solution realizing the object of the invention is: a kind of TATB cladding fall sense HMX method, including with
Lower step:
The first step, by adding binding agent, solvent and HMX in beaker, heats and stirs to being uniformly dissolved, then vacuum
Sucking filtration, dry preparing have surface activity and close-burning HMX；
Second step, is dissolved in TATB in concentrated sulphuric acid and stirs to dissolving, obtaining the mixed solution of TATB concentrated sulphuric acid；
3rd step, adds four mouthfuls by have surface activity and close-burning HMX and the mixture of ice and water prepared by the first step
In flask, the mixed solution of TATB concentrated sulphuric acid in second step is slowly dropped into this four-hole boiling flask by constant pressure funnel,
Dropping limit, limit is quickly stirred and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with detergent washing filter cake to filtrate pH value close to neutral,
Be dried TATB cladding HMX composite explosives.
Binding agent described in the first step is one or several in Estane-5703, fluorubber, beta-schardinger dextrin-, polyvinyl alcohol
Mixture, dissolve binding agent solvent be one or several the mixture in dichloroethanes, acetone, ethyl acetate,
Binding agent is 1-4% with the ratio (g/ml) of solvent, and binding agent is 0-5% with the mass ratio of HMX.
TATB described in second step is 1:1-1:5 with the ratio (g/ml) of concentrated sulphuric acid.
Described in 3rd step, the mass ratio of TATB Yu HMX is 1:5-1:20.
In 4th step, product detergent is sodium hydroxide or sodium bicarbonate alkaline solution, and baking temperature is 20～60 DEG C.
Compared with the prior art, its remarkable advantage is the present invention: the covered effect of (1) HMX is good, solves tradition bag
The best problem of cladding of coating method；(2) use binding agent during cladding, effectively prevent coming off of TATB；(3)
Reaction condition is gentle, operation is simple, eliminates the use of ultrasound wave；(4) TATB dissolubility in concentrated sulfuric acid is high
Solve the problem that solvent utilization rate is low.
Four accompanying drawing explanations
Fig. 1 is the process chart of the method for present invention TATB cladding fall sense HMX.
Fig. 2 is the HMX Electronic Speculum figure after cladding.
Fig. 3 is HMX corner angle enlarged drawing after cladding.
Fig. 4 is HMX surface enlarged drawing after cladding.
Fig. 5 is the infrared spectrum comparison diagram before and after cladding.
Five detailed description of the invention
Below in conjunction with the accompanying drawings and the present invention is described in further detail by detailed description of the invention.
In conjunction with Fig. 1, the present invention method of TATB cladding fall sense HMX, comprise the following steps:
The first step, by adding binding agent, solvent and HMX in beaker, heats and stirs to being uniformly dissolved, then vacuum
Sucking filtration, dry preparing have surface activity and close-burning HMX；
Second step, is dissolved in TATB in concentrated sulphuric acid and stirs to dissolving, obtaining the mixed solution of TATB concentrated sulphuric acid；
3rd step, adds four mouthfuls by have surface activity and close-burning HMX and the mixture of ice and water prepared by the first step
In flask, the mixed solution of TATB concentrated sulphuric acid in second step is slowly dropped into this four-hole boiling flask by constant pressure funnel,
Dropping limit, limit is quickly stirred and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with detergent washing filter cake to filtrate pH value close to neutral,
Be dried TATB cladding HMX composite explosives.
Binding agent described in the first step is one or several in Estane-5703, fluorubber, beta-schardinger dextrin-, polyvinyl alcohol
Mixture, dissolve binding agent solvent be one or several the mixture in dichloroethanes, acetone, ethyl acetate,
Binding agent is 1%-4% with the ratio (g/ml) of solvent, and binding agent is 0-5% with the mass ratio of HMX.
TATB described in second step is 1:1-1:5 with the ratio (g/ml) of concentrated sulphuric acid.
Described in 3rd step, the mass ratio of TATB Yu HMX is 1:5-1:20.
In 4th step, product detergent is sodium hydroxide or sodium bicarbonate alkaline solution, and baking temperature is 20～60 DEG C.
The following examples can make those skilled in the art that the present invention is more fully understood, but limits never in any form
The present invention.
Embodiment 1
The first step, will add 0.09g Estane-5703,6ml dichloroethanes and 3g HMX, 60 DEG C of bars of constant temperature in beaker
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under part, then vacuum filtration, dry preparing have surface work
Property and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 1ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium carbonate washing filter cake to filtrate pH value close to neutral,
At 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 284.58 DEG C.Impact sensitivity is 0%, and friction sensitivity is 0%.
Record scanning electron microscope (SEM) photograph such as accompanying drawing 2, accompanying drawing 3, accompanying drawing 4, infrared spectrogram such as accompanying drawing 5.
Embodiment 2
The first step, will add 0.09g Estane-5703 and beta-schardinger dextrin-, 9ml dichloroethanes and 3g HMX in beaker,
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under the conditions of constant temperature 60 DEG C, then vacuum filtration, dry system
Must have surface activity and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 1ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium hydroxide washing filter cake to filtrate pH value close in
Property, at 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 284.02 DEG C.Impact sensitivity is 0%, and friction sensitivity is 4%.
Embodiment 3
The first step, will add 0.15g Estane-5703,3.75ml dichloroethanes and the mixed solution of ethyl acetate in beaker
With 3g HMX, with 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under the conditions of constant temperature 60 DEG C, then vacuum is taken out
Filter, dry preparing have surface activity and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 1ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium carbonate washing filter cake to filtrate pH value close to neutral,
At 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 284.37 DEG C.Impact sensitivity is 0%, and friction sensitivity is 0%.
Embodiment 4
The first step, will add 0.09g Estane-5703 and beta-schardinger dextrin-, 6ml dichloroethanes and 3g HMX in beaker,
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under the conditions of constant temperature 60 DEG C, then vacuum filtration, dry system
Must have surface activity and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 0.53ml concentrated sulphuric acid and stirs to dissolving, obtaining TATB concentrated sulphuric acid
Mixed solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium carbonate washing filter cake to filtrate pH value close to neutral,
At 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 284.21 DEG C.Impact sensitivity is 0%, and friction sensitivity is 0%.
Embodiment 5
The first step, by beaker adds 0.09g Estane-5703,6ml dichloroethanes and the mixed solution of acetone and
3g HMX, with 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under the conditions of constant temperature 60 DEG C, then vacuum filtration,
It is dried to prepare and there is surface activity and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 2.65ml concentrated sulphuric acid and stirs to dissolving, obtaining TATB concentrated sulphuric acid
Mixed solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium hydroxide washing filter cake to filtrate pH value close in
Property, at 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 283.99 DEG C.Impact sensitivity is 4%, and friction sensitivity is 0%.
Embodiment 6
The first step, will add 0.09g fluorubber, the mixed solution of 6ml acetoneand ethyl acetate and 3g HMX in beaker,
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under the conditions of constant temperature 60 DEG C, then vacuum filtration, dry system
Must have surface activity and close-burning HMX；
Second step, is dissolved in 0.6g TATB in 1.2ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium carbonate washing filter cake to filtrate pH value close to neutral,
At 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 284.15 DEG C.Impact sensitivity is 4%, and friction sensitivity is 8%.
Embodiment 7
The first step, will add 0.09g Estane-5703,6ml dichloroethanes and 3g HMX, 60 DEG C of bars of constant temperature in beaker
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under part, then vacuum filtration, dry preparing have surface work
Property and close-burning HMX；
Second step, is dissolved in 0.15g TATB in 0.3ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium hydroxide washing filter cake to filtrate pH value close in
Property, at 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 283.87 DEG C.Impact sensitivity is 4%, and friction sensitivity is 8%.
Embodiment 8
The first step, will add 0.09g Estane-5703,6ml dichloroethanes and 3g HMX, 60 DEG C of bars of constant temperature in beaker
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under part, then vacuum filtration, dry preparing have surface work
Property and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 1ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium hydroxide washing filter cake to filtrate pH value close in
Property, at 20 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 283.94 DEG C.Impact sensitivity is 4%, and friction sensitivity is 0%.
Embodiment 9
The first step, will add 0.09g Estane-5703,6ml dichloroethanes and 3g HMX, 60 DEG C of bars of constant temperature in beaker
With 200r/min rotating speed magnetic agitation 30min to being uniformly dissolved under part, then vacuum filtration, dry preparing have surface work
Property and close-burning HMX；
Second step, is dissolved in 0.53g TATB in 1ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
3rd step, will have surface activity and close-burning HMX3g and 200ml mixture of ice and water prepared by the first step
Add in four-hole boiling flask, by the mixed solution of TATB concentrated sulphuric acid in second step by constant pressure funnel be slowly dropped into this four
Mouth flask, dropping limit, limit is quickly stirred 1h and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with sodium hydroxide washing filter cake to filtrate pH value close in
Property, at 40 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 284.54 DEG C.Impact sensitivity is 8%, and friction sensitivity is 12%.
Embodiment 10
The first step, is dissolved in 0.53g TATB in 1ml concentrated sulphuric acid and stirs to dissolving, obtaining the mixed of TATB concentrated sulphuric acid
Close solution；
Second step, adds HMX3g and 200ml mixture of ice and water in four-hole boiling flask, by dense for TATB in first step sulfur
The mixed solution of acid is slowly dropped into this four-hole boiling flask by constant pressure funnel, and dropping limit, limit is quickly stirred 1h and suspended
Liquid；
3rd step, the suspension of vacuum filtration the 3rd step gained, with sodium carbonate washing filter cake to filtrate pH value close to neutral,
At 60 DEG C be dried TATB cladding HMX composite explosives.
Dsc analysis exothermic decomposition temperature is 283.49 DEG C.Impact sensitivity is 16%, and friction sensitivity is 12%.
Claims (5)
1. the method with TATB cladding fall sense HMX, it is characterised in that comprise the following steps:
The first step, by adding binding agent, solvent and HMX in beaker, heats and stirs to being uniformly dissolved, then vacuum
Sucking filtration, dry preparing have surface activity and close-burning HMX；
Second step, is dissolved in TATB in concentrated sulphuric acid and stirs to dissolving, obtaining the mixed solution of TATB concentrated sulphuric acid；
3rd step, adds four mouthfuls by have surface activity and close-burning HMX and the mixture of ice and water prepared by the first step
In flask, the mixed solution of TATB concentrated sulphuric acid in second step is slowly dropped into this four-hole boiling flask by constant pressure funnel,
Dropping limit, limit is quickly stirred and is obtained suspension；
4th step, the suspension of vacuum filtration the 3rd step gained, with detergent washing filter cake to filtrate pH value close to neutral,
Be dried TATB cladding HMX composite explosives.
The method of TATB the most according to claim 1 cladding fall sense HMX, it is characterised in that first step institute
Stating binding agent is one or several the mixture in Estane-5703, fluorubber, beta-schardinger dextrin-, polyvinyl alcohol, molten
The solvent solving binding agent is one or several the mixture in dichloroethanes, acetone, ethyl acetate, and binding agent is with molten
The ratio (g/ml) of agent is 1-4%, and binding agent is 0-5% with the mass ratio of HMX.
The method of TATB the most according to claim 1 cladding fall sense HMX, it is characterised in that second step institute
The ratio (g/ml) stating TATB and concentrated sulphuric acid is 1:1-1:5.
The method of TATB the most according to claim 1 cladding fall sense HMX, it is characterised in that in the 3rd step
The mass ratio of described TATB Yu HMX is 1:5-1:20.
The method of TATB the most according to claim 1 cladding fall sense HMX, it is characterised in that in the 4th step
Product detergent is sodium hydroxide or sodium bicarbonate alkaline solution, and baking temperature is 20～60 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107986921A (en) * | 2017-11-28 | 2018-05-04 | 中国工程物理研究院化工材料研究所 | A kind of method for coating of TATB planes of crystal |
| CN109836300A (en) * | 2017-11-28 | 2019-06-04 | 南京理工大学 | A kind of high thermostability PBX explosive and preparation method thereof |
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| CN103086812A (en) * | 2013-02-04 | 2013-05-08 | 中国工程物理研究院化工材料研究所 | Preparation method of bicomponent energetic material core-shell structure |
| CN103351269A (en) * | 2013-06-06 | 2013-10-16 | 西安近代化学研究所 | Heatproof mixing explosive and preparation method thereof |
| 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 |
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| CN103086812A (en) * | 2013-02-04 | 2013-05-08 | 中国工程物理研究院化工材料研究所 | Preparation method of bicomponent energetic material core-shell structure |
| CN103351269A (en) * | 2013-06-06 | 2013-10-16 | 西安近代化学研究所 | Heatproof mixing explosive and preparation method thereof |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107986921A (en) * | 2017-11-28 | 2018-05-04 | 中国工程物理研究院化工材料研究所 | A kind of method for coating of TATB planes of crystal |
| CN109836300A (en) * | 2017-11-28 | 2019-06-04 | 南京理工大学 | A kind of high thermostability PBX explosive and preparation method thereof |
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Application publication date: 20161005 |