CN109956844A - A kind of preparation method of fluoropolymer/metal composite energetic material - Google Patents
A kind of preparation method of fluoropolymer/metal composite energetic material Download PDFInfo
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- CN109956844A CN109956844A CN201910255402.9A CN201910255402A CN109956844A CN 109956844 A CN109956844 A CN 109956844A CN 201910255402 A CN201910255402 A CN 201910255402A CN 109956844 A CN109956844 A CN 109956844A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0008—Compounding the ingredient
- C06B21/0016—Compounding the ingredient the ingredient being nitrocellulose or oranitro cellulose based propellant; Working up; gelatinising; stabilising
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
- C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate
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Abstract
The invention discloses a kind of fluoropolymer/metal composite energetic material preparation methods, and ammonium perchlorate is entrained in fluoropolymer metal system containing energy by the method that solution crystallizes, forms novel Composite Energetic Materials.Utilize the pressure output and combustion reaction performance of the gaseous product enhancing system that ammonium perchlorate decomposition generates, oxidation reaction occurs for the reaction product carbon of ammonium perchlorate decomposition generates simultaneously gas and fluoropolymer metal system, increase the release of energy and pressure, to dramatically increase the energy and reactivity of fluoropolymer metal system containing energy.The present invention effectively increase fluoropolymer metal containing can system energy and pressure output, combustion rate from smoulder switch to detonation, explosion.It is expected to be applied in fields such as solid propellant, metallic explosive and gas generators by the novel system containing energy that doping is formed.
Description
Technical field
The present invention relates to energetic material technical field more particularly to a kind of preparations of fluoropolymer/metal composite energetic material
Method.
Background technique
Energetic material, which refers to, can independently carry out fast chemical reaction and export the compound or mixture of energy, be weapon system
System injure and power source.Wherein fluoropolymer/metal containing can system existed due to the energy density of superelevation and excellent reactivity worth
Solid propellant, explosive and reactive fragmentation etc. are widely used.Such as polytetrafluoroethylene (PTFE) (PTFE)/A1 compound system
Energy 21KJ/cm3, polytetrafluoroethylene (PTFE) (PTFE)/Mg energy density is 9.6KJ/g.
It studies for many years and application finds that, since the reaction of this kind of material is intermolecular reaction, energyreleaserate is passed
The physical processes control such as heat and mass transfer.And the minimum mass transfer distance of existing fluoropolymer metal system containing energy is in hundred nanoscales；
Simultaneous reactions product is mostly metal fluoride and carbon, and pressure output is lower, generally in tens of megapascal ranks.Slow heat and mass
Make the reaction rate of material lower with low pressure output, combustion rate is the range in 1Km/s, it is difficult to occur effective
Explosion or detonation reaction, actual exothermic heat of reaction value is also much smaller than theoretical combustion heat.The fluoropolymer metal that powder mixes is contained
Energy system is prepared into structural material, can improve influence of the heat and mass to reactivity worth.Typically fluoropolymer metal is contained
Energy material is prepared into Multilayer-film nanometer structure, due to high mass transfer and reaction interface, can dramatically increase reaction calorific value.The present invention
Applicant prepares the PTFE/ metal energetic material of core-shell structure, Ke Yiti in earlier innovation in-situ chemical vapor deposition method
The stabilization and reactivity (ZL201210058533.6) of high material.Present invention applicant devises superlattices knot in early period
The fluoropolymer metal energetic material system of structure, effectively reduces the firing temperature of material, increases reactivity
(ZL201410224837.4).Although these methods can have some improvement in terms of exothermic heat of reaction value and reactivity,
But still can not effective solution pressure output it is low, energy release it is incomplete the problems such as.
An important factor for pressure is mass transfer in influence material reaction process, however the reaction of fluoropolymer metal energetic material produces
Object is solid, and the boiling point if reaction product is A1F3 is 1272 DEG C, so pressure output is difficult to obtain effective solution.Other one
The reaction of the system containing energy of a aspect fluoropolymer metal generates a large amount of carbon, and carbon is most important fuel for energetic material, but
Due to a lack of oxidant in fluoropolymer metal system, so release heat and pressure can not be reacted.
Summary of the invention
The purpose of the present invention is to provide a kind of fluoropolymer/metal composite energetic material preparation methods, pass through solution knot
Crystalline substance, containing that can adulterate oxidant ammonium perchlorate (AP) in system, can significantly improve the reaction calorific value and pressure of system in fluoropolymer metal
Output may make the reaction of fluoropolymer metal system to switch to rank of exploding by burning.The NEW TYPE OF COMPOSITE energetic material of preparation due to
High reaction calorific value, pressure output and combustion explosion characteristic, has in metallic explosive, solid propellant and gas generator
Potential application prospect.Preparation method of the present invention is easy to operate simultaneously, is easy to mass production.
The present invention through the following technical solutions to achieve the above objectives:
It is water-soluble to be dispersed in AP by a kind of preparation method of fluoropolymer/metal composite energetic material for polytetrafluoroethylene (PTFE) (PTFE)
In liquid, water is set to volatilize in 60-80 DEG C of heating, AP is crystallized in the solution and is precipitated on the surface PTFE, and drying obtains AP after removing water and mixes
Miscellaneous PTFE particle；And/or
Poly- two vinylidene (PVDF) is dissolved in dimethylformamide (DMF), AP aqueous solution is added drop-wise to poly- two inclined fluorine
In the DMF solution of ethylene (PVDF), stirred crystallization obtains the fluoropolymer particle of AP doping after filtering drying water removal；
The fluoropolymer of AP doping and high activity metal are added in binder solution, are stirred, drying solvent flashing obtains
The fluoropolymer metal energetic material adulterated to AP.
Further scheme is: the fluoropolymer is polytetrafluoroethylene (PTFE) (PTFE) or poly- two vinylidene (PVDF)
It is one or two kinds of.
Further scheme is: the high activity metal is the one or more of aluminium, magnesium or boron.
Further scheme is: the mass ratio of the fluoropolymer and high activity metal is 4: 1~1: 1.
Further scheme is: mass fraction of the AP in fluoropolymer metal system containing energy is 1~25%.
Further scheme is: the mass fraction of the AP aqueous solution is 1~25%.
Further scheme is: the binder is 1: 1 copolymer binder of vinylidene-chlorotrifluoroethylene
(F2311), 1: 3 copolymer of 1: 4 copolymer of vinylidene-chlorotrifluoroethylene (F2314) or vinylidene-chlorotrifluoroethylene
(F2313)。
Another aspect of the present invention passes through a kind of fluoropolymer being prepared by above-mentioned method/metal composite energetic material.
The present invention is low for the reaction calorific value and pressure output of fluoropolymer metal energetic material system, combustion rate
Slowly, the disadvantage that reaction not exclusively waits adulterates oxidant AP by solution crystallization in fluoropolymer metal system, utilizes oxidant AP
The gaseous product enhancing pressure output and reaction mass transfer rate of decomposition, improve combustion reaction performance, while utilizing AP decomposition product
Output pressure and energy are reacted with the carbon product of fluoropolymer metal, so that fluoropolymer metal is containing can the combustion heat value of system and anti-
It answers performance to be obviously improved, i.e., reacts to form oxycarbide by carbon, increase the energy and pressure output of system.
The beneficial effects of the present invention are:
(1) pressure output is improved by adulterating oxidant AP in fluoropolymer metal system containing energy, enhances and reacted
Journey mass transfer rate and reactivity.
(2) AP decomposition product is reacted with the reaction product carbon of fluoropolymer metal system further enhances energy and pressure,
Promote conversion of the reaction of fluoropolymer metal system containing energy from smoulder to combustion explosion.
(3) preparation process operating procedure is simple, is easy to mass preparation, is expected to by the novel system containing energy that doping is formed
It is applied in fields such as solid propellant, metallic explosive and gas generators.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, the described embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without making creative work it is obtained it is all its
Its embodiment belongs to the range that the present invention is protected.
Embodiment 1
Polytetrafluoroethylene (PTFE) (PTFE) powder of 5g is added in the AP aqueous solution that 50mL mass fraction is 1%, stirring point
It dissipating, so that water is volatilized being heated to 60-80 DEG C, AP is precipitated in water-soluble middle crystallization, it is entrained in the surface PTFE, after 60 DEG C of drying water removals
The PTFE particle adulterated to AP.The aluminium powder of the AP of the above-mentioned preparation PTFE adulterated and 1.5g is sequentially added to the binder of F2311
It in solution, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal energetic material of AP doping.
Embodiment 2
Polytetrafluoroethylene (PTFE) (PTFE) powder of 5g is added in the AP aqueous solution that 100mL mass fraction is 5%, stirring point
It dissipates, so that water is volatilized being heated to 70 DEG C, AP is precipitated in water-soluble middle crystallization, is entrained in the surface PTFE, obtains after 60 DEG C of drying water removals
The PTFE particle of AP doping.The aluminium powder of the AP of the above-mentioned preparation PTFE adulterated and 3g is sequentially added to the binder solution of F2311
In, it is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal energetic material of AP doping.
Embodiment 3
Polytetrafluoroethylene (PTFE) (PTFE) powder of 5g is added in the AP aqueous solution that 100mL mass fraction is 5%, stirring point
It dissipates, so that water is volatilized being heated to 80 DEG C, AP is precipitated in water-soluble middle crystallization, is entrained in the surface PTFE, obtains after 60 DEG C of drying water removals
The PTFE particle of AP doping.The boron powder of the AP of the above-mentioned preparation PTFE adulterated and 3g is sequentially added to the binder solution of F2311
In, it is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal energetic material of AP doping.
Embodiment 4
Polytetrafluoroethylene (PTFE) (PTFE) powder of 5g is added in the AP aqueous solution that 100mL mass fraction is 3%, stirring point
It dissipates, so that water is volatilized being heated to 75 DEG C, AP is precipitated in water-soluble middle crystallization, is entrained in the surface PTFE, obtains after 60 DEG C of drying water removals
The PTFE particle of AP doping.The boron powder of the AP of the above-mentioned preparation PTFE adulterated and 4g is sequentially added to the binder solution of F2311
In, it is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal energetic material of AP doping.
Embodiment 5
Polytetrafluoroethylene (PTFE) (PTFE) powder of 5g is added in the AP aqueous solution that 100mL mass fraction is 1%, stirring point
It dissipates, so that water is volatilized being heated to 65 DEG C, AP is precipitated in water-soluble middle crystallization, is entrained in the surface PTFE, obtains after 60 DEG C of drying water removals
The PTFE particle of AP doping.The aluminium powder of the AP of the above-mentioned preparation PTFE adulterated and 5g is sequentially added to the binder solution of F2314
In, it is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal energetic material of AP doping.
Embodiment 6
Polytetrafluoroethylene (PTFE) (PTFE) powder of 5g is added in the AP aqueous solution that 100mL mass fraction is 5%, stirring point
It dissipates, so that water is volatilized being heated to 68 DEG C, AP is precipitated in water-soluble middle crystallization, is entrained in the surface PTFE, obtains after 60 DEG C of drying water removals
The PTFE particle of AP doping.The boron powder of the AP of the above-mentioned preparation PTFE adulterated and 4g is sequentially added to the binder solution of F2313
In, it is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal energetic material of AP doping.
Embodiment 7
The AP aqueous solution 10mL that mass fraction is 25% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the aluminium powder of the PVDF total 5g and 4g of AP doping
It sequentially adds in the binder solution of F2313, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal of AP doping
Energetic material.
Embodiment 8
The AP aqueous solution 10mL that mass fraction is 20% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the aluminium powder of the PVDF total 5g and 2g of AP doping
It sequentially adds in the binder solution of F2311, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal of AP doping
Energetic material.
Embodiment 9
The AP aqueous solution 10mL that mass fraction is 25% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the magnesium powder of the PVDF total 5g and 3g of AP doping
It sequentially adds in the binder solution of F2314, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal of AP doping
Energetic material.
Embodiment 10
The AP aqueous solution 10mL that mass fraction is 10% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the boron powder of the PVDF total 5g and 3g of AP doping
It sequentially adds in the binder solution of F2314, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal of AP doping
Energetic material.
Embodiment 11
The AP aqueous solution 10mL that mass fraction is 10% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the aluminium powder of the PVDF total 5g and 4g of AP doping
It sequentially adds in the binder solution of F2313, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal of AP doping
Energetic material.
Embodiment 12
The AP aqueous solution 10mL that mass fraction is 10% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the boron powder of the PVDF total 5g and 3g of AP doping
It sequentially adds in the binder solution of F2311, is stirred, solvent volatilization, 60 DEG C of drying obtain the fluoropolymer metal of AP doping
Energetic material.
Embodiment 13
The AP aqueous solution 10mL that mass fraction is 10% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the aluminium of the PVDF total 5g and 1.5g of AP doping
It sequentially adds in the binder solution of F2313, is stirred with the boron powder of 1.5g, solvent volatilization, 60 DEG C of drying obtain AP doping
Fluoropolymer metal energetic material.
Embodiment 14
The AP aqueous solution 10mL that mass fraction is 10% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By the magnesium of the PVDF total 5g and 1.3g of AP doping
It sequentially adds in the binder solution of F2311, is stirred with the boron powder of 1.5g, solvent volatilization, 60 DEG C of drying obtain AP doping
Fluoropolymer metal energetic material.
Embodiment 15
The AP aqueous solution 10mL that mass fraction is 10% is slowly dropped to the DMF solution of poly- two vinylidene (PVDF)
In, stirred crystallization 30min obtains the PVDF of AP doping after filtering drying water removal.By AP doping PVDF total 5g and 2g aluminium and
The boron powder of 1g sequentially adds in the binder solution of F2314, is stirred, and solvent volatilization, 60 DEG C of drying obtain the fluorine of AP doping
Polymers metal energetic material.
In above-mentioned each embodiment, additive amount those skilled in the art of binder solution can be according to experiment condition voluntarily
It determines, the application is not limited thereof.
The experimental data of the application section Example is as shown in table 1, and wherein comparative example is existing PTFE/A1 material containing energy
Material；
The experimental data of 1 the application section Example of table
| Sample | Reaction calorific value | Pressure output | Combustion characteristics |
| PTFE/Al | 2020J/g | 3.2MPa | Burning |
| Implement 1 | 3670J/g | 5.7MPa | Burning |
| Implement 2 | 8670J/g | 9.9MPa | Detonation |
| Implement 7 | 5850J/g | 8.2MPa | Detonation |
| Implement 8 | 4530J/g | 6.3MPa | Burning |
| Implement 9 | 3948J/g | 4.3MPa | Burning |
| Implement 10 | 2680J/g | 2.3MPa | Burning |
The pressure output and combustion reaction performance for the gaseous product enhancing system that the application is generated using ammonium perchlorate decomposition,
Simultaneously ammonium perchlorate decomposition generate gas and fluoropolymer metal system reaction product carbon occur oxidation reaction, increase energy and
The release of pressure, to dramatically increase the energy and reactivity of fluoropolymer metal system containing energy.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
It is further to note that specific technical features described in the above specific embodiments, in reconcilable situation
Under, it can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention is to various possible combinations
No further explanation will be given for mode.In addition, various embodiments of the present invention can be combined randomly, as long as its
Without prejudice to thought of the invention, it should also be regarded as the disclosure of the present invention.
Claims (8)
1. a kind of fluoropolymer/metal composite energetic material preparation method, which is characterized in that polytetrafluoroethylene (PTFE) is dispersed in AP water
In solution, water is set to volatilize in 60-80 DEG C of heating, AP, which is crystallized in the solution and is precipitated, obtains AP behind the surface PTFE, drying water removal
The PTFE particle of doping；And/or
Poly- two vinylidene is dissolved in dimethylformamide, AP aqueous solution is added drop-wise in the DMF solution of poly- two vinylidene,
Stirred crystallization obtains the fluoropolymer particle of AP doping after filtering drying water removal；
The fluoropolymer of AP doping and high activity metal are added in binder solution, are stirred, drying solvent flashing obtains AP
The fluoropolymer metal energetic material of doping.
2. a kind of preparation method of fluoropolymer/metal composite energetic material according to claim 1, which is characterized in that institute
The fluoropolymer stated is the one or two kinds of of polytetrafluoroethylene (PTFE) or poly- two vinylidene.
3. a kind of preparation method of fluoropolymer/metal composite energetic material according to claim 1, which is characterized in that institute
The high activity metal stated is the one or more of aluminium, magnesium or boron.
4. a kind of preparation method of fluoropolymer/metal composite energetic material according to claim 1, which is characterized in that institute
The mass ratio of the fluoropolymer and high activity metal stated is 4: 1~1: 1.
5. a kind of preparation method of fluoropolymer/metal composite energetic material according to claim 1, which is characterized in that institute
Mass fraction of the AP stated in fluoropolymer metal system containing energy is 1~25%.
6. a kind of preparation method of fluoropolymer/metal composite energetic material according to claim 1, which is characterized in that institute
The mass fraction for the AP aqueous solution stated is 1~25%.
7. a kind of preparation method of fluoropolymer/metal composite energetic material according to claim 1, which is characterized in that institute
The binder stated be 1: 1 copolymer binder of vinylidene-chlorotrifluoroethylene, 1: 4 copolymer of vinylidene-chlorotrifluoroethylene,
Or 1: 3 copolymer of vinylidene-chlorotrifluoroethylene.
8. the fluoropolymer that method according to claim 1-7 is prepared/metal composite energetic material.
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| CN110343020A (en) * | 2019-08-12 | 2019-10-18 | 中国工程物理研究院化工材料研究所 | A kind of preparation method of Nanometallization explosive |
| CN110452075A (en) * | 2019-07-24 | 2019-11-15 | 西北工业大学 | The preparation method of polymer matrix Composite Energetic Materials coating modification nano-metal particle |
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