CN114591126A - Thermocuring intelligent gunpowder and preparation method thereof - Google Patents
Thermocuring intelligent gunpowder and preparation method thereof Download PDFInfo
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- CN114591126A CN114591126A CN202210264596.0A CN202210264596A CN114591126A CN 114591126 A CN114591126 A CN 114591126A CN 202210264596 A CN202210264596 A CN 202210264596A CN 114591126 A CN114591126 A CN 114591126A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/12—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide the material being two or more oxygen-yielding compounds
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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
- C06B21/0033—Shaping the mixture
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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
- C06B21/0033—Shaping the mixture
- C06B21/0058—Shaping the mixture by casting a curable composition, e.g. of the plastisol type
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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
- C06B21/0033—Shaping the mixture
- C06B21/0075—Shaping the mixture by extrusion
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/001—Fillers, gelling and thickening agents (e.g. fibres), absorbents for nitroglycerine
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/08—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with a nitrated organic compound
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a thermosetting intelligent gunpowder and a preparation method thereof. The disclosed gunpowder includes a base gunpowder, a crystalline polymer and a stimulus responsive additive; the basic gunpowder comprises an adhesive, a solid explosive, metal powder, a plasticizer and a thermal initiator. The preparation method comprises the steps of melting and mixing the binder and the crystalline polymer at a certain temperature to obtain a mixture; adding solid explosive, metal powder and stimulus response additive into the obtained mixture, uniformly mixing, adding thermal initiator, and continuously uniformly mixing to obtain the intelligent programmable gunpowder. The invention can endow gunpowder with the stimulation response capability, has the environment sensing and feedback capability and endows the gunpowder with the characteristic of intelligent deformation.
Description
Technical Field
The invention relates to thermocuring intelligent gunpowder, in particular to an energetic material which is suitable for 3D printing and extrusion molding processes and can deform automatically under the stimulation of temperature, humidity, an electric field, a magnetic field and the like.
Background
Gunpowder is used as an energy source for weapon launching, and the self chemistry is converted into heat energy through combustion, and meanwhile, a large amount of gas products are generated. The gunpowder can be controllably combusted in a barrel weapon or a rocket engine, a large amount of high-temperature and high-pressure gas generated is expanded to do work, and finally the chemical energy of the gunpowder is converted into the kinetic energy of the weapon. The existing gunpowder manufacturing technology adopted at home and abroad mainly comprises the processes of pouring, pressing and stretching, a novel 3D printing technology and the like, and the prepared gunpowder with a specific structure can release energy in a combustion mode according to a set mode.
NC/DIANP/HATO propellant preparation and performance research [ J ] weapon equipment engineering bulletin, 2021,42(2): 199-; effect of aluminum powder content on GAP insensitive propellant Performance [ J ] energetic materials 2021,29 (10): 928-; influence of bonding agent on mechanical property of HTPE propellant [ J ]. chemical propellant and high polymer material, 2018,16(2):39-42, an HTPE-based propellant formula is reported in 2018, and a propellant grain is prepared by vacuum casting molding. Mechanical ball milling method for preparing Al/C composite particles and its effect on HTPB propellant performance [ J ]. Proc. of Beijing university of Physics. 2021,41 (12): 1322-1330, an HTPB propellant formulation containing highly active AL/C composite particles was reported. Proceedings of the Combustion Institute,2019,37(3): 3135-.
The prepared gunpowder is a three-dimensional material with a set shape no matter a conventional pressing and stretching process, a pouring process or a 3D printing process, the prepared energetic material can be combusted or exploded only according to a set mode after excitation, and the gunpowder does not have the characteristics of environmental perception and response and is difficult to adapt to a complex and constantly changing combat environment.
Disclosure of Invention
Aiming at the defects or shortcomings of the prior art, the invention provides a thermosetting intelligent gunpowder.
Therefore, the hot-set-phone intelligent gunpowder provided by the invention comprises base gunpowder, crystalline polymer and stimulus response additive;
the base gunpowder comprises a binder, a solid explosive and a plasticizer, or comprises the binder, the solid explosive, the plasticizer, metal powder and a thermal initiator;
the crystalline polymer is selected from one or a mixture of polyethylene glycol, poly cis-1, 4-isoprene, poly trans-1, 4-isoprene, poly cis-1, 4-butadiene, poly trans-1, 4-isoprene, poly trans-1, 4-chloroprene, polyethylene oxide, polytetrahydrofuran, poly hexamethyloxy ether, poly octamethylene oxy ether, poly sebacic acid diester, poly caprolactone and polycaprolactone;
the stimulus response additive is selected from one or more of graphite, graphene, carbon nano tubes, carbon fibers, ferroferric oxide and ferric oxide.
Alternatively, the mass percentage of the crystalline polymer in the intelligent programmable gunpowder is 1.5-5%, the mass percentage of the stimulus response additive is 0.2-1%, and the balance is other components, wherein the mass percentage is calculated by 100%.
Optionally, the relative molecular mass of the crystalline polymer is 5000-100000. More specifically, the crystalline polymer has a relative molecular mass of 30000 to 70000.
The intelligent programmable gunpowder comprises, by 100%, 0-0.2% of thermal initiator, 40-75% of solid explosive, 0-30% of metal powder, 2-10% of plasticizer and the balance of other components.
Optionally, the solid explosive is an energy-containing solid oxidant, and the particle size of the energy-containing solid oxidant is 0.2-150 μm. Further, 0.2 to 40 μm can be selected.
Alternatively, the metal powder has a particle size of 0.1 to 200 μm. Further 1-50 um can be selected.
Alternatively, the binder comprises a thermosetting binder and a curing agent;
the thermosetting binder is selected from one or more of hydroxyl-terminated butadiene binder, hydroxyl-terminated copolyether binder, glycidyl azide polyether, 3-bis-azidomethyloxetane polyether, 3-azidomethyl-3-methyloxetane polyether, poly-3-nitrate methyl-3-methyloxetane and polyglycidyl ether nitrate;
the curing agent is selected from one or a mixture of more of biuret polyisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate and naphthalene diisocyanate.
The intelligent programmable gunpowder comprises, by 100%, 10-25% of a thermosetting binder, 1-3% of a curing agent and the balance of other components.
The invention also provides a preparation method of the thermosetting intelligent gunpowder. The provided method comprises the following steps:
melting and mixing the binder, the plasticizer and the crystalline polymer at a certain temperature to obtain a mixture, wherein the certain temperature is 0-20 ℃ higher than the melting point temperature of the crystalline polymer;
adding solid explosive, metal powder and stimulus response additive into the obtained mixture, uniformly mixing, adding thermal initiator, and continuously uniformly mixing to obtain the intelligent programmable gunpowder.
The preparation method further comprises the following steps: and forming and curing the intelligent programmable gunpowder, wherein the forming adopts casting forming, pressure-stretch forming or 3D printing forming.
And optionally, the curing temperature is 50-75 ℃, and the time is 2-4 days.
The invention can endow the gunpowder with stimulus response capability, has the characteristics of environment perception and feedback capability and endows the gunpowder with intelligent deformation.
The specific impulse of the gunpowder is more than or equal to 250s (1s is 9.8 N.s/kg), the tensile elongation is more than or equal to 20%, the recovery rate is more than or equal to 80%, and the gunpowder can be controllably deformed under specific (temperature, humidity, electric field, magnetic field and the like) excitation or stimulation.
Detailed Description
Unless otherwise defined, the terms, methods, or processes herein are understood or implemented using existing methods or processes as would be recognized by one of ordinary skill in the relevant art.
According to the invention, the low-melting-point crystalline polymer and the stimulus response additive are added into the gunpowder, so that on one hand, the crystalline polymer is crystallized and melted under different conditions, and the material is stretched and shrunk to deform, so that the gunpowder grain has a self-deformation function; meanwhile, the intelligent gunpowder can reach the deformation condition under the excitation or stimulation of external controllable specific (temperature, humidity, electric field, magnetic field and the like) along with time, so that the intelligent gunpowder can finish intelligent deformation. The crystalline polymer is selected from one or a mixture of more of polyethylene glycol, poly cis-1, 4-isoprene, poly trans-1, 4-isoprene, poly cis-1, 4-butadiene, poly trans-1, 4-isoprene, poly trans-1, 4-chloroprene, polyethylene oxide, polytetrahydrofuran, poly hexamethyloxy ether, poly octamethylene oxy ether, poly sebacic acid diester, poly caprolactone and polycaprolactone; the stimulus response additive is selected from one or more of graphite, graphene, carbon nano tubes, carbon fibers, ferroferric oxide and ferric oxide.
The basic gunpowder disclosed by the invention is a gunpowder formula well known in the field and mainly comprises a binder, a solid explosive and a plasticizer, or the binder, the solid explosive, the plasticizer, metal powder and a thermal initiator. The specific components and proportions of the basic powder can be selected and optimized by those skilled in the art according to the prior art and the purpose of the invention. Example (c):
the solid explosive may be selected from one or more mixtures of 1,3, 5-trinitro-1, 3, 5-triazacyclohexane (RDX) and 1,3,5, 7-tetranitro-1, 3,5, 7-tetraazacyclooctane (HMX), hexanitrohexaazaisopentane (CL-20), 1,3, 3-Trinitroazetidine (TNAZ), 1-diamino-2, 2-dinitroethylene (FOX-7), Nitroguanidine (NQ), triaminotrinitrobenzene (TATB), triaminoguanidine nitrate (TAGN), potassium perchlorate (AP), ammonium perchlorate (AN) and Nitrocotton (NC).
The metal powder can be one or a mixture of aluminum powder, magnesium powder and zinc powder.
The thermal initiator may be selected from one or more mixtures of triphenyl bismuth (TPB), maleic acid, maleic anhydride, dibutyltin dilaurate (T12), and dioctyl sebacate (DOS).
The plasticizer is selected from one or more of Nitroglycerin (NG), azidonitramine (DA), terrestrial root (DEGDN), pseudoroot (TEGDN), trimethylolethane trinitrate (TMETN), nitrooxyethyl-nitramine (NENA) and triacetin.
The binder may be selected from binders conventional in the art. One preferred adhesive includes a heat-curable adhesive and a curing agent; the thermosetting binder is selected from one or more of hydroxyl-terminated butadiene (HTPB) binder, hydroxyl-terminated copolyether (HTPE) binder, Glycidyl Azide Polyether (GAP), 3-bis-azidomethyloxetane Polyether (PBAMO), 3-azidomethyl-3-methyloxetane Polyether (PAMMO), poly-3-nitrate methyl-3-methyloxetane (PNIMMO) and polyglycidyl ether nitrate (PGN); the curing agent is selected from one or more of biuret polyisocyanate (N100), Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), isophorone diisocyanate (MDI), Hexamethylene Diisocyanate (HDI) and Naphthalene Diisocyanate (NDI).
The specific components and proportions of the base powder, the crystalline polymer and the stimulus-responsive additive, and the relevant preparation process parameters can be selected and optimized by those skilled in the art according to the above disclosure and the purpose of the present invention. The present invention is further illustrated by the following examples, but is not limited thereto. The component materials used in the following examples are all commercially available products.
Example 1:
the formulation of this example is as follows: 6% of hydroxyl-terminated copolyether (HTPE) and 12.5% of Glycidyl Azide Polyether (GAP); 2% of Toluene Diisocyanate (TDI); 0.1% of dibutyltin dilaurate (T12); 4% of polycaprolactone (molecular weight of 80000-90000, melting point of 71 ℃); RDX crystals 30% (particle size 0.2-40 μm); 15% of potassium perchlorate (AP); 20% of aluminum powder (granularity is 1-50 mu m) and 10% of nitroglycerin; 0.4 percent of graphene.
The preparation method comprises the following steps:
(1) preparing a binder: adding HTPE, GAP, TDI, NG and PCL into a stirrer, setting the temperature above the melting point of the crystalline polymer (75-80 ℃), rotating at 200 r/s and lasting for 1-2 h.
(2) Gunpowder formula preparation: adding RDX, AP, aluminum powder and graphene into the prepared binder, keeping the rotating speed and the temperature unchanged, stirring for 1h, adding T12, and continuing stirring for 0.5 h. And obtaining the intelligent gunpowder formula.
(3) Preparing the materials into a sample with a required shape by using an extrusion type 3D printer (preferably, the needle diameter is 0.2 mm-4 mm, and the diameter of the needle is 1.0mm in the embodiment), and putting the sample into an oven for curing, wherein the curing process comprises the following steps: 60 ℃ for 3 days.
Comparative example 1:
this comparative example differs from example 1 in that no polycaprolactone and graphene were added to the formulation.
Example 2:
unlike example 1, the formulation of this example is as follows: 5% of hydroxyl-terminated butadiene (HTPB), 18% of Glycidyl Azide Polyether (GAP); 3% of diphenylmethane diisocyanate (MDI); 0.2% of triphenyl bismuth (TPB); 4% of polycaprolactone (molecular weight of 50000-60000, melting point of 64 ℃) 5%; 62 percent of octogen (RDX) crystals (the particle size is 40-70 mu m); 6.4% of Nitroglycerin (NG); 0.4 percent of carbon nano tube.
The preparation process is different from the embodiment 1 in that the mixing temperature is set to be 70-75 ℃.
Comparative example 2:
this comparative example differs from example 2 in that no polycaprolactone and carbon nanotubes were added to the formulation.
Example 3:
unlike example 1, the formulation of this example is as follows: 5% of hydroxyl-terminated copolyether (HTPE) and 10% of Glycidyl Azide Polyether (GAP); 1% of Toluene Diisocyanate (TDI); 0.1% of dibutyltin dilaurate (T12); 4% of polycaprolactone (with molecular weight of 5000-10000 and melting point of 37 ℃) 5%; 45% of CL-20 crystals (particle size 80-110 μm); 10% of potassium perchlorate (AP); 15% of aluminum powder (the particle size is 150-; 8.5% of Nitroglycerin (NG); ferroferric oxide 0.4 percent.
The preparation process is different from the embodiment 1 in that the mixing temperature is set to be 45-50 ℃.
Comparative example 3:
the comparative example is different from example 3 in that polycaprolactone and ferroferric oxide are not added in the formula.
Example 4:
the formulation of this example is as follows:
6% of hydroxyl-terminated copolyether (HTPE) and 12% of Glycidyl Azide Polyether (GAP); 1% of Toluene Diisocyanate (TDI); 0.1% of dioctyl sebacate (DOS); 5% of polyethylene glycol (with the molecular weight of 6000-12000 and the melting point of 64 ℃); CL-20 crystals 67% (particle size 120-; 8.5% of Nitroglycerin (NG); 0.4 percent of ferric oxide.
Comparative example 4:
this comparative example differs from example 4 in that no polyethylene glycol and no iron oxide were added to the formulation.
The energetic materials prepared in the above examples and comparative examples were tested for pyrotechnic power, tensile strength, elongation, and length recovery after exposure to a stimulus (heat, electricity, magnetic field) according to GJB772A-97 "gunpowder test methods". The results are shown in table 1, where: the control was a conventional GAP base powder with a composition of 25% GAP, 17% AP, 35% RDX, 18% aluminum powder.
Compared with the traditional energetic material product, the product of the invention has higher tensile elongation and has recovery capability under heat, electricity and magnetic fields.
TABLE 1 comparison of energy and deformability of the articles
Claims (11)
1. The heat-curing intelligent gunpowder is characterized by comprising base gunpowder, crystalline polymer and stimulus response additive;
the base gunpowder comprises a binder, a solid explosive and a plasticizer, or comprises the binder, the solid explosive, the plasticizer, metal powder and a thermal initiator;
the crystalline polymer is selected from one or a mixture of polyethylene glycol, poly cis-1, 4-isoprene, poly trans-1, 4-isoprene, poly cis-1, 4-butadiene, poly trans-1, 4-isoprene, poly trans-1, 4-chloroprene, polyethylene oxide, polytetrahydrofuran, poly hexamethyloxy ether, poly octamethylene oxy ether, poly sebacic acid diester, poly caprolactone and polycaprolactone;
the stimulus response additive is selected from one or more of graphite, graphene, carbon nano tubes, carbon fibers, ferroferric oxide and ferric oxide.
2. The thermally curable intelligent gunpowder according to claim 1, wherein the mass percentage of the crystalline polymer in the intelligent programmable gunpowder is 1.5-5%, the mass percentage of the stimulus-responsive additive is 0.2-1%, and the balance is other components, based on 100%.
3. The thermally curable intelligent powder according to claim 1, wherein the crystalline polymer has a relative molecular mass of 5000 to 100000.
4. The thermally-cured intelligent gunpowder as claimed in claim 2, wherein the thermal initiator in the intelligent programmable gunpowder accounts for 0-0.2% by mass, the solid explosive accounts for 40-75% by mass, the metal powder accounts for 0-30% by mass, the plasticizer accounts for 2-10% by mass, and the balance is other components, based on 100%.
5. The thermally-cured intelligent gunpowder according to claim 1, wherein the solid explosive is an energetic solid oxidizer, and the grain size of the energetic solid oxidizer is 0.2-150 μm.
6. The thermally curable intelligent powder according to claim 1, wherein the metal powder has a particle size of 0.1 to 200 μm.
7. The thermally curable smart powder of claim 1, wherein said binder comprises a thermosetting binder and a curing agent;
the thermosetting binder is selected from one or more of hydroxyl-terminated butadiene binder, hydroxyl-terminated copolyether binder, glycidyl azide polyether, 3-bis-azidomethyloxetane polyether, 3-azidomethyl-3-methyloxetane polyether, poly-3-nitrate methyl-3-methyloxetane and polyglycidyl ether nitrate;
the curing agent is selected from one or more of biuret polyisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate and naphthalene diisocyanate.
8. The thermally curable intelligent gunpowder according to claim 7, wherein the intelligent programmable gunpowder comprises 10-25% by mass of thermosetting binder, 1-3% by mass of curing agent and the balance of other components, based on 100%.
9. The method for preparing the thermally-curable intelligent powder according to claim 1, wherein the method comprises:
melting and mixing the binder, the plasticizer and the crystalline polymer at a certain temperature to obtain a mixture, wherein the certain temperature is 0-20 ℃ higher than the melting point temperature of the crystalline polymer;
adding solid explosive, metal powder and stimulus response additive into the obtained mixture, uniformly mixing, adding thermal initiator, and continuously uniformly mixing to obtain the intelligent programmable gunpowder.
10. The method for preparing the thermally-curable intelligent powder according to claim 9, further comprising: and forming and curing the intelligent programmable gunpowder, wherein the forming adopts casting forming, pressure-stretch forming or 3D printing forming.
11. The method for preparing the thermosetting intelligent powder according to claim 9, wherein the curing temperature is 50 to 75 ℃ and the time is 2 to 4 days.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956921A (en) * | 2022-06-30 | 2022-08-30 | 哈尔滨工业大学 | Magnetically deformable solid rocket mixed gel propellant and preparation method thereof |
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| USH1341H (en) * | 1990-12-14 | 1994-08-02 | High energy propellant formulation | |
| CN102149756A (en) * | 2008-07-18 | 2011-08-10 | 陶氏环球技术有限责任公司 | Polyolefin compositions suitable for elastic articles |
| US8986473B1 (en) * | 2008-09-03 | 2015-03-24 | The United States Of America As Represented By The Secretary Of The Navy | High burning rate tactical solid rocket propellant, and related method |
| US20210276931A1 (en) * | 2018-11-27 | 2021-09-09 | Lynntech, Inc. | Energetic Feedstock for Additive Manufacturing |
| CN113774514A (en) * | 2021-09-14 | 2021-12-10 | 武汉纺织大学 | Shape memory composite fiber with hydrothermal stimulus responsiveness |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| USH1341H (en) * | 1990-12-14 | 1994-08-02 | High energy propellant formulation | |
| CN102149756A (en) * | 2008-07-18 | 2011-08-10 | 陶氏环球技术有限责任公司 | Polyolefin compositions suitable for elastic articles |
| US8986473B1 (en) * | 2008-09-03 | 2015-03-24 | The United States Of America As Represented By The Secretary Of The Navy | High burning rate tactical solid rocket propellant, and related method |
| US20210276931A1 (en) * | 2018-11-27 | 2021-09-09 | Lynntech, Inc. | Energetic Feedstock for Additive Manufacturing |
| CN113774514A (en) * | 2021-09-14 | 2021-12-10 | 武汉纺织大学 | Shape memory composite fiber with hydrothermal stimulus responsiveness |
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| CN114956921A (en) * | 2022-06-30 | 2022-08-30 | 哈尔滨工业大学 | Magnetically deformable solid rocket mixed gel propellant and preparation method thereof |
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