CN109438149A - A kind of thermosetting property composite solidpropellant and preparation method thereof - Google Patents
A kind of thermosetting property composite solidpropellant and preparation method thereof Download PDFInfo
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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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- 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
- C06B33/04—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
- 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
- C06B33/06—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
- 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
- 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 present invention relates to a kind of thermosetting property composite solidpropellants and preparation method thereof, belong to composite solidpropellant preparation technical field.The uniform slurry of solid propellant without curing agent is made by vertical mixer hybrid mode or the continuous hybrid mode of twin-screw, then slurry is transported to screw extrusion molding apparatus using screw feeder, and squeeze out through spray head；The regulation of curing reaction rate is realized by temperature at control spray head and spray outlet environment temperature, realizes layer-by-layer bonding forming；Molding solid propellant is finally placed in constant temperature in oil bath baking oven and stores 120h~168h, is solidified after the completion.This method can realize thermosetting property composite solidpropellant increasing material manufacturing, and complicated Types of Medicine solid engines can be achieved in future, layering variable thrust solid engines are manufactured with propellant charge.
Description
Technical field
The present invention relates to a kind of thermosetting property composite solidpropellants and preparation method thereof, belong to composite solidpropellant preparation
Technical field.
Background technique
Composite solidpropellant is a kind of by the grouping of the groups such as oxidant, metal incendiary composition, polymer binder, energetic material
At containing can plyability polymer-function material.Conventional composite solid propellant is mixed using vertical or flat mixer,
Realize that motor grain produces using vacuum pouring system.Composite solidpropellant powder column manufacturing process be related to raw material premix,
The multiple working procedures such as mixing, core model disposition, casting, solidification, demoulding, shaping generally realize the control of propellant Types of Medicine using special core model
System, it is difficult to realize some complex-shaped and layering variable thrust solid propellant grain manufacture.Meanwhile composite solidpropellant
Due to carrying burn required oxidant and metal fuel, it is heated in production, manufacture, use process, light, impacts, rubs
The burning even safety accident of explosion easily occur for the stimulation of the external conditions such as wiping, electrostatic sensitivity.Conventional propellant powder column manufacturing process
It cannot achieve the completely isolated of operator and solid propellant, belong to job that requires special skills, process dangerous is higher, operator's training
It is big to support difficulty.
Summary of the invention
Technology of the invention solves the problems, such as: overcome the deficiencies in the prior art, proposes that a kind of thermosetting property complex solid promotes
Agent and preparation method thereof.
The technical solution of the invention is as follows:
A kind of thermosetting property composite solidpropellant, the composition of the solid propellant include oxidant, metal fuel, bonding
Agent, curing agent, crosslinking agent, curing catalysts and auxiliary agent；
It is 100% calculating, the mass percentage of each component with the gross mass of the solid propellant are as follows:
Oxidant: 60%~66%；
Metal fuel: 16%~20%；
Adhesive: 12%~18%；
Curing agent: 0.5%~2%；
Crosslinking agent: 0.3%~2%
Curing catalysts: 0.05%~0.15%
Auxiliary agent: 1%~2%
The oxidant is the mixture of one or both of ammonium perchlorate (AP), ammonium nitrate (AN)；
The metal fuel is one or more of aluminium powder, Al-Mg alloy powder, aluminum-boron alloy powder, fluorine aluminium alloy
Mixture；
The adhesive is end hydroxy butadiene (HTPB), ethylene oxide/tetrahydrofuran copolyether (PET), poly- second
One of glycol (PEG), KZ (sebacic acid dioctyl ester), nitroglycerine (NG), triethylene glycol dinitrate (TEGDN) or
Two or more mixtures；
The curing agent is the mixture of one or more of HDI, TDI, IPDI, DDI；
The crosslinking agent is the mixture of one or both of triethanolamine (TEA), trimethylolpropane (TMP)；
The curing catalysts are three-(3- nitrobenzophenone) bismuths, three-(4- nitrobenzophenone) bismuths, three-(ethoxyl phenenyls)
The mixture of one or more of bismuth；
The auxiliary agent is that anti-aging agent N- methyl paranitroaniline 0.5%~1% (is with the gross mass of the solid propellant
100% calculate), combustion catalyst iron oxide 0.2%~0.5% (with the gross mass of the solid propellant be 100% calculate), in
Property polymer bonds mixture BAG-78C 0.3%~0.5% (being 100% to calculate with the gross mass of the solid propellant).
A kind of preparation method of thermosetting property composite solidpropellant, comprising the following steps:
Step 1, oxidant, metal fuel, adhesive, curing agent, crosslinking agent, curing catalysts and auxiliary agent are prepared into
One slurry；
Step 2, uniform slurry step 1 being prepared is transported to the spiral shell for having heating function by screw feeder
In rod-type extrusion molding apparatus, molding machine temperature is to pass through molding dress after propellant slurry is preheated between 35 DEG C~45 DEG C
The spray head set squeezes out；
Step 3, the propellant slurry that spray head squeezes out successively piles up molding in three-dimensional movement platform, in squeezing for molding machine
Hot-air mouth for controlling export environment temperature is set at spray head out, and hot blast temperature range is 45 DEG C~65 DEG C, in forming process
The propellant slurry temperature of middle extrusion is promoted rapidly, the curing reaction of the adhesive and curing agent speed under the control of curing catalysts
Rate is accelerated, and realizes the layer-by-layer bonding forming of propellant charge；
Step 4, the propellant charge of bonding forming in step 3 is stood to 120h~168h under the conditions of 30 DEG C~50 DEG C,
Molding is fully cured in realization, obtains the propellant charge of uniform compact.
In the step 1, temperature when preparing uniform slurry is 30 DEG C~40 DEG C, uses vertical mixer hybrid mode
Or the uniform slurry of the continuous hybrid mode of twin-screw；
In the step 2, the extrusion pressure at the spray head of the molding machine is 0.1MPa~5.0MPa, and spray head goes out
Mouth diameter is 1.0mm~5.0mm；
In the step 3, when piling up molding, every layer with a thickness of 0.05mm~1.0mm.
Compared with prior art, the beneficial effects of the present invention are:
(1) this method can realize the increasing material manufacturing of thermosetting property composite solidpropellant, be suitable for some complex-shaped and divide
The manufacture of layer variable thrust solid propellant grain.
(2) this method promotes the degree of automation using composite solidpropellant powder column manufacturing process is simplified, and reduces technique danger
It is dangerous.
(3) this method realizes extrusion propellant in such a way that blowing hot-air at extrusion molding apparatus preheating, spray head reheats
The homogeneity of slurry temperature controls, and then realizes effective control of formulation cured reaction rate, each to be layered different depth solidification path
Degree is consistent.
(4) the present invention relates to a kind of thermosetting property composite solidpropellants to increase material preparation method, belongs to composite solidpropellant
Preparation technical field.The present invention passes through vertical mixer hybrid mode first or the continuous hybrid mode of twin-screw is made without solidification
The uniform slurry of the solid propellant of agent；Slurry is transported to screw extrusion molding apparatus using screw feeder again, and is passed through
Spray head squeezes out；The regulation of curing reaction rate is realized by temperature at control spray head and spray outlet environment temperature, is realized successively viscous
It is connected into type；Molding solid propellant is finally placed in constant temperature in oil bath baking oven and stores 120h~168h, is solidified after the completion.The party
Method can realize thermosetting property composite solidpropellant increasing material manufacturing, and complicated Types of Medicine solid engines can be achieved in future, layering can be changed and push away
Power solid engines are manufactured with propellant charge.
It tests solid propellant density, mechanical property prepared by this method is obtained, test result shows to increase material system
Standby compound solidity propellant theoretical specific impulse, theoretical characteristic velocity, density, mechanical property, the propellant with traditional handicraft preparation
Quite.
Theoretical specific impulse, theoretical characteristic velocity: minimum freely according to Q/Gt60-95 composite solidpropellant performance calculation
It can method and program calculating acquisition.
Density: according to the density measurement method of QJ917A-97 composite solidpropellant and lining, heat-insulating material；
Mechanical property: being tested according to GJB 770B-2005 gunpowder test method, and test temperature is 20 DEG C.
Specific embodiment
The present invention is described in detail With reference to embodiment, but protection scope is not limited to that, any
Within the technical scope of the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, should all cover
Within protection scope of the present invention.
Unspecified part of the present invention belongs to common sense well known to those skilled in the art.
Specific embodiment is as follows:
Step 1, under the conditions of 30 DEG C~40 DEG C, by vertical mixer hybrid mode or the continuous hybrid mode of twin-screw,
Realize that oxidant, metal fuel, adhesive, curing agent, crosslinking agent, curing catalysts, the solid propellant raw material of auxiliary agent are equal
Even mixing, is made uniform slurry, and the recipe ingredient and content of embodiment 1-6 is as shown in table 1；
1 embodiment 1-5 series propellant formulation of table composition and content (%)
Step 2, propellant mixture slurry is transported to the screw for having heating function to squeeze out by screw feeder
Molding machine, extrusion molding apparatus are made of screw rod, sleeve, printing head, heating element, constant temperature controller.Molding machine temperature
Degree is set as between 35 DEG C~45 DEG C, is squeezed out after propellant slurry is preheated by spray head；
Propellant slurry is squeezed out from the printing head of screw extrusion molding apparatus after step 3, preheating, and in three-dimensional motion
Molding is successively piled up on platform, the motion path of spray head is controlled by three-dimensional motion controller, is arranged at printing head for controlling
The hot-air mouth of export environment temperature processed, hot blast temperature range are 45 DEG C~65 DEG C.The propellant slurry squeezed out in forming process
By heating twice, temperature is promoted rapidly, is caused the effect of thermal sensitivity curing catalysts and is promoted the solidification of adhesive and curing agent anti-
It answers rate to accelerate, realizes the layer-by-layer bonding forming of propellant charge.Used printing head diameter is 1.0mm~5.0mm, is printed
For the thickness set in journey as 0.05mm~1.0mm, the extrusion pressure of spray outlet is 0.1MPa~5.0MPa.
Step 4, under the conditions of 40 DEG C~50 DEG C, molding propellant charge is stood into 120h~168h, realization is fully cured
Molding, obtains the propellant charge of uniform compact.The technological parameter of embodiment 1-5 is as shown in table 2, and the prepared performance of propellant is such as
Shown in table 3.
The technological parameter of 2 embodiment 1-5 increasing material manufacturing of table
The 3 embodiment 1-5 performance of propellant of table
| Project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Specific impulse (Ns/kg) | 2582.3 | 2579.1 | 2548.6 | 2554.6 | 2552.2 |
| Characteristic velocity (m/s) | 1581.0 | 1582.2 | 1562.1 | 1564.5 | 1561.2 |
| Propellant density (g/cm3) | 1.78 | 1.74 | 1.70 | 1.79 | 1.62 |
| Intensity (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 (10)
1. a kind of thermosetting property composite solidpropellant, it is characterised in that: the composition of the solid propellant includes oxidant, metal combustion
Material, adhesive, curing agent, crosslinking agent, curing catalysts and auxiliary agent；
It is 100% calculating, the mass percentage of each component with the gross mass of the solid propellant are as follows:
Oxidant: 60%~66%；
Metal fuel: 16%~20%；
Adhesive: 12%~18%；
Curing agent: 0.5%~2%；
Crosslinking agent: 0.3%~2%
Curing catalysts: 0.05%~0.15%
Auxiliary agent: 1%~2%.
2. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the oxidant is height
The mixture of one or both of ammonium chlorate (AP), ammonium nitrate (AN).
3. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the metal fuel is
The mixture of one or more of aluminium powder, Al-Mg alloy powder, aluminum-boron alloy powder, fluorine aluminium alloy.
4. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the adhesive is end
Hydroxyl polybutadiene (HTPB), ethylene oxide/tetrahydrofuran copolyether (PET), polyethylene glycol (PEG), (sebacic acid two is pungent by KZ
Ester), nitroglycerine (NG), one or more of triethylene glycol dinitrate (TEGDN) mixture.
5. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the curing agent is
The mixture of one or more of HDI, TDI, IPDI, DDI.
6. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the crosslinking agent is three
The mixture of one or both of ethanol amine (TEA), trimethylolpropane (TMP).
7. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the curing catalysts
For the mixed of one or more of three-(3- nitrobenzophenone) bismuths, three-(4- nitrobenzophenone) bismuths, three-(ethoxyl phenenyl) bismuths
Close object.
8. a kind of thermosetting property composite solidpropellant according to claim 1, it is characterised in that: the auxiliary agent includes anti-
Old agent N- methyl paranitroaniline, combustion catalyst iron oxide and neutral polymer binder BAG-78C；
It is 100% calculating with the gross mass of the solid propellant, the mass percentage of anti-aging agent N- methyl paranitroaniline is
0.5%~1%, the mass percentage of combustion catalyst iron oxide is 0.2%~0.5%, neutral polymer binder BAG-
The mass percentage of 78C is 0.3%~0.5%.
9. a kind of preparation method of thermosetting property composite solidpropellant, it is characterised in that the following steps are included:
Step 1, oxidant, metal fuel, adhesive, curing agent, crosslinking agent, curing catalysts and auxiliary agent are prepared into uniform slurry
Material；
Step 2, uniform slurry step 1 being prepared is transported to screw extrusion molding apparatus by screw feeder
In, propellant slurry is squeezed out by the spray head of molding machine；
Step 3, the propellant slurry that spray head in step 2 squeezes out successively is piled up into three-dimensional movement platform molding, is built into
Type column；
Step 4, the block shaping column that step 3 obtains is solidified, obtains propellant charge.
10. a kind of preparation method of thermosetting property composite solidpropellant according to claim 9, it is characterised in that: described
Step 1 in, temperature when preparing uniform slurry is 30 DEG C~40 DEG C, continuous using vertical mixer hybrid mode or twin-screw
The uniform slurry of hybrid mode；
In the step 2, the temperature of screw extrusion molding apparatus is between 35 DEG C~45 DEG C；
Extrusion pressure at the spray head of screw extrusion molding apparatus is 0.1MPa~5.0MPa, and spray outlet diameter is 1.0mm
~5.0mm；
In the step 3, the hot-air mouth that control export environment temperature is provided at the spray head of Composite Propellant Slurry, hot wind temperature are squeezed out
Spending range is 45 DEG C~65 DEG C；
When piling up molding, every layer with a thickness of 0.05mm~1.0mm；
In the step 4, solidification temperature is 30 DEG C~50 DEG C, and curing time is 120h~168h.
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| 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 |
| CN111892966A (en) * | 2020-07-24 | 2020-11-06 | 北京理工大学 | High-energy metal fuel for boron-containing propellant |
| CN111925263A (en) * | 2020-06-10 | 2020-11-13 | 湖北航天化学技术研究所 | High-combustion-speed azide micro-smoke propellant and preparation process thereof |
| 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 |
| CN115784813A (en) * | 2022-11-25 | 2023-03-14 | 西安交通大学 | Mixing method and mixing system of 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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| 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 |
| CN111925263A (en) * | 2020-06-10 | 2020-11-13 | 湖北航天化学技术研究所 | High-combustion-speed azide micro-smoke propellant and preparation process 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 |
| CN111892966A (en) * | 2020-07-24 | 2020-11-06 | 北京理工大学 | High-energy metal fuel for boron-containing propellant |
| 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 |
| CN115784813A (en) * | 2022-11-25 | 2023-03-14 | 西安交通大学 | Mixing method and mixing system of composite 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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