CN109438149B - Thermosetting composite solid propellant and preparation method thereof - Google Patents
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
- C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
- C06B45/105—The resin being a polymer bearing energetic groups or containing a soluble organic explosive
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- 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
- C06B33/04—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 an inorganic nitrogen-oxygen salt
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- C—CHEMISTRY; METALLURGY
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- 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
- C06B33/06—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 an inorganic oxygen-halogen salt
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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
- C06B33/08—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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- C—CHEMISTRY; METALLURGY
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- 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
- C06B33/14—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 at least one being an inorganic nitrogen-oxygen salt
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
- C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
- C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
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Abstract
The invention relates to a thermosetting composite solid propellant and a preparation method thereof, belonging to the technical field of preparation of composite solid propellants. Preparing uniform solid propellant slurry without a curing agent by a vertical mixer mixing mode or a double-screw continuous mixing mode, conveying the slurry to a screw extrusion molding device by a screw feeder, and extruding the slurry through a nozzle; the solidification reaction rate is regulated and controlled by controlling the temperature at the spray head and the ambient temperature at the outlet of the spray head, and layer-by-layer bonding molding is realized; finally, the formed solid propellant is placed in an oil bath oven for constant temperature storage for 120-168 h, and after-curing is completed. The method can realize the additive manufacturing of the thermosetting composite solid propellant, and can realize the manufacturing of the propellant grain for the complex-type solid engine and the layered variable-thrust solid engine in the future.
Description
Technical Field
The invention relates to a thermosetting composite solid propellant and a preparation method thereof, belonging to the technical field of preparation of composite solid propellants.
Background
The composite solid propellant is an energetic composite high-molecular functional material consisting of an oxidant, a metal combustion agent, a high-molecular adhesive, an energetic material and the like. The traditional composite solid propellant is mixed by a vertical or horizontal mixer, and the production of the engine grain is realized by a vacuum pouring system. The manufacturing process of the composite solid propellant grain relates to a plurality of procedures such as raw material premixing, mixing, core mould disposal, pouring, curing, demoulding, shaping and the like, generally uses a special core mould to realize propellant grain control, and is difficult to realize the manufacturing of some solid propellant grains with complicated shapes and layered variable thrust. Meanwhile, the composite solid propellant carries the oxidant and the metal fuel required by combustion, and is stimulated by external conditions such as heat, light, impact, friction, electrostatic sensitivity and the like in the production, manufacture and use processes, so that safety accidents of combustion and even explosion are easy to occur. The traditional propellant grain manufacturing process can not realize the complete isolation of operators and solid propellants, belongs to special operation, and has high process danger and high culture difficulty of operators.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a thermosetting composite solid propellant and a preparation method thereof.
The technical solution of the invention is as follows:
the thermosetting composite solid propellant consists of oxidant, metal fuel, adhesive, curing agent, cross-linking agent, curing catalyst and assistant;
calculated by taking the total mass of the solid propellant as 100 percent, the solid propellant comprises the following components in percentage by mass:
oxidizing agent: 60% -66%;
metal fuel: 16% -20%;
adhesive: 12 to 18 percent;
curing agent: 0.5 to 2 percent;
a crosslinking agent: 0.3 to 2 percent
Curing catalyst: 0.05 to 0.15 percent
Auxiliary agent: 1 to 2 percent
The oxidant is one or a mixture of Ammonium Perchlorate (AP) and Ammonium Nitrate (AN);
the metal fuel is one or a mixture of more than two of aluminum powder, aluminum-magnesium alloy powder, aluminum-boron alloy powder and fluorine-aluminum alloy;
the adhesive is one or a mixture of more than two of hydroxyl-terminated polybutadiene (HTPB), ethylene oxide/tetrahydrofuran copolyether (PET), polyethylene glycol (PEG), KZ (dioctyl sebacate), Nitroglycerin (NG) and triethylene glycol dinitrate (TEGDN);
the curing agent is one or a mixture of more than two of HDI, TDI, IPDI and DDI;
the cross-linking agent is one or a mixture of two of Triethanolamine (TEA) and Trimethylolpropane (TMP);
the curing catalyst is one or a mixture of more than two of tri- (3-nitrophenyl) bismuth, tri- (4-nitrophenyl) bismuth and tri- (ethoxyphenyl) bismuth;
the auxiliary agent is 0.5-1% of anti-aging agent N-methyl paranitroaniline (calculated by taking the total mass of the solid propellant as 100%), 0.2-0.5% of combustion catalyst ferric oxide (calculated by taking the total mass of the solid propellant as 100%), and 0.3-0.5% of neutral polymer bonding agent BAG-78C (calculated by taking the total mass of the solid propellant as 100%).
A preparation method of a thermosetting composite solid propellant comprises the following steps:
step 1, preparing an oxidant, a metal fuel, an adhesive, a curing agent, a cross-linking agent, a curing catalyst and an auxiliary agent into uniform slurry;
step 2, conveying the uniform slurry prepared in the step 1 to a screw type extrusion molding device with a heating function through a screw type feeder, wherein the temperature of the molding device is 35-45 ℃, and preheating the propellant slurry and then extruding the preheated propellant slurry through a nozzle of the molding device;
step 3, the propellant slurry extruded by the nozzle is piled up and formed layer by layer on a three-dimensional motion platform, a hot air port for controlling the ambient temperature of an outlet is arranged at the extrusion nozzle of the forming device, the temperature range of the hot air is 45-65 ℃, the temperature of the extruded propellant slurry is rapidly increased in the forming process, the curing reaction rate of the adhesive and the curing agent is accelerated under the control of the curing catalyst, and the propellant grain is bonded and formed layer by layer;
and 4, standing the propellant grains formed by bonding in the step 3 for 120-168 hours at the temperature of 30-50 ℃ to realize complete curing and forming and obtain uniform and compact propellant grains.
In the step 1, the temperature for preparing the uniform slurry is 30-40 ℃, and the uniform slurry is prepared by a vertical mixer mixing mode or a double-screw continuous mixing mode;
in the step 2, the extrusion pressure at the nozzle of the forming device is 0.1MPa to 5.0MPa, and the diameter of the nozzle outlet is 1.0mm to 5.0 mm;
in the step 3, the thickness of each layer is 0.05 mm-1.0 mm during stacking and molding.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method can realize additive manufacturing of the thermosetting composite solid propellant, and is suitable for manufacturing the layered variable thrust solid propellant grains with complex shapes.
(2) The method simplifies the manufacturing process of the composite solid propellant grain, improves the automation degree and reduces the process danger.
(3) The method realizes the uniformity control of the temperature of the extruded propellant slurry by preheating the extrusion molding device and blowing hot air at the spray head for reheating, thereby realizing the effective control of the curing reaction rate of the formula and ensuring that the curing degrees of different layers are consistent.
(4) The invention relates to a method for preparing a thermosetting composite solid propellant additive, and belongs to the technical field of preparation of composite solid propellants. Firstly, preparing solid propellant uniform slurry without a curing agent in a vertical mixer mixing mode or a double-screw continuous mixing mode; then the slurry is conveyed to a screw extrusion molding device by a screw feeder and is extruded by a nozzle; the solidification reaction rate is regulated and controlled by controlling the temperature at the spray head and the ambient temperature at the outlet of the spray head, and layer-by-layer bonding molding is realized; finally, the formed solid propellant is placed in an oil bath oven for constant temperature storage for 120-168 h, and after-curing is completed. The method can realize the additive manufacturing of the thermosetting composite solid propellant, and can realize the manufacturing of the propellant grain for the complex-type solid engine and the layered variable-thrust solid engine in the future.
The density and the mechanical property of the solid propellant prepared by the method are tested, and the test result shows that the theoretical specific impulse, the theoretical characteristic speed, the density and the mechanical property of the composite solid propellant prepared by the additive are equivalent to those of the propellant prepared by the traditional process.
Theoretical specific impulse and theoretical characteristic speed: the minimum free energy is calculated according to the thermal performance of the Q/Gt60-95 composite solid propellant and a program.
Density: the density measurement method of the QJ917A-97 composite solid propellant, the lining and the heat-insulating material is adopted;
mechanical properties: the test is carried out according to the GJB 770B-2005 gunpowder test method, and the test temperature is 20 ℃.
Detailed Description
The present invention is described in detail with reference to the following embodiments, but the scope of the invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention should be covered by the scope of the present invention.
The invention is not described in detail and is within the knowledge of a person skilled in the art.
The specific embodiment is as follows:
step 1, uniformly mixing raw materials of solid propellants of an oxidant, metal fuel, an adhesive, a curing agent, a crosslinking agent, a curing catalyst and an auxiliary agent by a vertical mixer mixing mode or a double-screw continuous mixing mode at the temperature of 30-40 ℃ to prepare uniform slurry, wherein the formula components and the content of the examples 1-6 are shown in table 1;
table 1 examples 1-5 series propellant formulation compositions and contents (%)
And 2, conveying the mixed propellant slurry to a screw type extrusion molding device with a heating function through a screw type feeder, wherein the extrusion molding device consists of a screw, a sleeve, a printing nozzle, a heating part and a constant temperature controller. The temperature of the forming device is set to be 35-45 ℃, and the propellant slurry is preheated and then extruded out through a spray head;
and 3, extruding the preheated propellant slurry from a printing spray head of the screw rod type extrusion molding device, and stacking and molding layer by layer on a three-dimensional motion platform, wherein the motion path of the spray head is controlled by a three-dimensional motion controller, a hot air port for controlling the ambient temperature of an outlet is arranged at the printing spray head, and the temperature range of the hot air is 45-65 ℃. The propellant slurry extruded in the forming process is heated twice, the temperature is rapidly raised, the action of a thermosensitive curing catalyst is initiated to accelerate the curing reaction rate of the adhesive and the curing agent, and the layer-by-layer bonding forming of the propellant grains is realized. The diameter of the adopted printing nozzle is 1.0 mm-5.0 mm, the set layer thickness in the printing process is 0.05 mm-1.0 mm, and the extrusion pressure of the nozzle outlet is 0.1 MPa-5.0 MPa.
And 4, standing the formed propellant grains for 120-168 hours at the temperature of 40-50 ℃ to realize complete curing and forming and obtain uniform and compact propellant grains. The process parameters for examples 1-5 are shown in Table 2, and the properties of the propellants produced are shown in Table 3.
Table 2 process parameters for additive manufacturing of examples 1-5
Table 3 examples 1-5 propellant properties
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Nibble (N.s/kg) | 2582.3 | 2579.1 | 2548.6 | 2554.6 | 2552.2 |
| Characteristic speed (m/s) | 1581.0 | 1582.2 | 1562.1 | 1564.5 | 1561.2 |
| Density of propellant (g/cm)3) | 1.78 | 1.74 | 1.70 | 1.79 | 1.62 |
| Strength (MPa) | 0.50 | 0.94 | 0.93 | 0.74 | 0.79 |
| Elongation at Break (%) | 60.3 | 51.1 | 52.7 | 54.0 | 38.5 |
Claims (1)
1. A preparation method of a thermosetting composite solid propellant is characterized by comprising the following steps: the solid propellant comprises an oxidant, a metal fuel, an adhesive, a curing agent, a cross-linking agent, a curing catalyst and an auxiliary agent;
calculated by taking the total mass of the solid propellant as 100 percent, the solid propellant comprises the following components in percentage by mass:
oxidizing agent: 60% -66%;
metal fuel: 16% -20%;
adhesive: 12% -18%;
curing agent: 0.5 to 2 percent;
a crosslinking agent: 0.3 to 2 percent
Curing catalyst: 0.05% -0.15%
Auxiliary agent: 1% -2%;
the oxidant is one or a mixture of ammonium perchlorate and ammonium nitrate;
the metal fuel is one or a mixture of more than two of aluminum powder, aluminum-magnesium alloy powder, aluminum-boron alloy powder and fluorine-aluminum alloy;
the adhesive is one or a mixture of more than two of hydroxyl-terminated polybutadiene, ethylene oxide/tetrahydrofuran copolyether, polyethylene glycol, dioctyl sebacate, nitroglycerin and triethylene glycol dinitrate;
the curing agent is one or a mixture of more than two of HDI, TDI, IPDI and DDI;
the cross-linking agent is one or a mixture of triethanolamine and trimethylolpropane;
the curing catalyst is one or a mixture of more than two of tri- (3-nitrophenyl) bismuth, tri- (4-nitrophenyl) bismuth and tri- (ethoxyphenyl) bismuth;
the auxiliary agent comprises an anti-aging agent N-methyl paranitroaniline, a combustion catalyst iron oxide and a neutral polymer bonding agent BAG-78C;
calculated by taking the total mass of the solid propellant as 100%, the mass percentage content of the anti-aging agent N-methyl paranitroaniline is 0.5% -1%, the mass percentage content of the combustion catalyst ferric oxide is 0.2% -0.5%, and the mass percentage content of the neutral polymer bonding agent BAG-78C is 0.3% -0.5%;
the preparation method of the thermosetting composite solid propellant comprises the following steps:
step 1, preparing an oxidant, a metal fuel, an adhesive, a curing agent, a cross-linking agent, a curing catalyst and an auxiliary agent into uniform slurry;
step 2, conveying the uniform slurry prepared in the step 1 to a screw type extrusion molding device through a screw type feeder, and extruding the propellant slurry through a spray head of the molding device;
step 3, piling and forming the propellant slurry extruded by the sprayer in the step 2 on a three-dimensional moving platform layer by layer to obtain a piled and formed column;
step 4, solidifying the built forming column obtained in the step 3 to obtain a propellant grain;
in the step 1, the temperature for preparing the uniform slurry is 30-40 ℃, and the uniform slurry is prepared by using a vertical mixer mixing mode or a double-screw continuous mixing mode;
in the step 2, the temperature of the screw type extrusion molding device is 35-45 ℃;
the extrusion pressure at the nozzle of the screw type extrusion molding device is 0.1-5.0 MPa, and the diameter of the nozzle outlet is 1.0-5.0 mm;
in the step 3, a hot air port for controlling the ambient temperature of an outlet is arranged at a spray head for extruding propellant slurry, and the temperature range of hot air is 45-65 ℃;
when stacking and forming are carried out, the thickness of each layer is 0.05 mm-1.0 mm;
in the step 4, the curing temperature is 30-50 ℃, and the curing time is 120-168 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110358598A (en) * | 2019-06-05 | 2019-10-22 | 东南大学 | A kind of solid fuel powder column slurry and preparation method thereof, Method of printing |
| CN111233593A (en) * | 2020-03-13 | 2020-06-05 | 北京星际荣耀空间科技有限公司 | Vertical additive manufacturing method of solid propellant |
| CN111333474A (en) * | 2020-03-13 | 2020-06-26 | 北京星际荣耀空间科技有限公司 | Solid propellant and horizontal additive manufacturing method thereof |
| CN111925263B (en) * | 2020-06-10 | 2022-01-04 | 湖北航天化学技术研究所 | High-combustion-speed azide micro-smoke propellant and preparation process thereof |
| CN111892966B (en) * | 2020-07-24 | 2021-10-08 | 北京理工大学 | High-energy metal fuel for boron-containing propellant |
| CN115073245A (en) * | 2021-03-10 | 2022-09-20 | 南京理工大学 | Rapid 3D printing and forming method for photo-thermal composite curing of butylated hydroxytoluene solid propellant |
| CN115784813B (en) * | 2022-11-25 | 2024-04-16 | 西安交通大学 | Mixing method and mixing system for composite solid propellant |
| CN116789507A (en) * | 2023-06-21 | 2023-09-22 | 湖北航天化学技术研究所 | High-solid-content solid propellant and preparation method thereof |
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