CN110963866B - Temperature-sensitive time-varying solid propellant - Google Patents
Temperature-sensitive time-varying solid propellant Download PDFInfo
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- CN110963866B CN110963866B CN201911355347.7A CN201911355347A CN110963866B CN 110963866 B CN110963866 B CN 110963866B CN 201911355347 A CN201911355347 A CN 201911355347A CN 110963866 B CN110963866 B CN 110963866B
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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
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
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- 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
- C06B23/002—Sensitisers or density reducing agents, foam stabilisers, crystal habit modifiers
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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
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Abstract
The invention relates to a temperature-sensitive time-varying solid propellant, which comprises the following components in percentage by mass: temperature-sensitive additive: 0.5 to 2.5 percent; curing agent: 0.2% -1.0%; curing catalyst: 0.01-0.04%; oxidizing agent: 65 to 70 percent; metal fuel: 16% -20%; adhesive: 5% -10%; plasticizer: 2% -5%; other components: 0.25 to 2.5 percent. The temperature-sensitive time-varying solid propellant is based on a formula of a medium-energy butylated hydroxytoluene solid propellant, realizes viscosity control of an HTPB/plasticizer/temperature-sensitive additive continuous phase within the temperature range of 20-40 ℃ through adjustment of the type and content of a temperature-sensitive additive, enables the temperature-sensitive time-varying solid propellant to have the characteristics of adjustable drug slurry viscosity within the temperature range of 20-40 ℃ of 560 Pa.s-1656 Pa.s and room temperature shaping below 40 ℃, and is suitable for additive manufacturing process research of the solid propellant.
Description
Technical Field
The invention belongs to the field of composite solid propellants, and particularly relates to a temperature-sensitive time-varying solid propellant.
Background
The composite solid propellant is used as a main power source of the missile weapon, and the comprehensive performance of the composite solid propellant is important for improving the operational efficiency of the missile weapon. Under the direct drive of a digital model, the additive manufacturing technology is oriented to the direct forming of the microstructure, so that the precise control and the great improvement of the performance of the solid propellant can be realized, the limitation of manufacturing on design is expected to be broken, the on-demand design and the on-demand manufacturing of the solid propellant are realized, the energy release efficiency of the solid propellant is greatly improved, and the forming of a multi-burning-rate complex topological structure is realized. With the continuous maturity of energetic material additive manufacturing technology and equipment, the development of a composite solid propellant formula suitable for an additive manufacturing process and the improvement of the comprehensive performance become research hotspots.
At present, the formulas of the double-base/modified double-base propellant, the thermoplastic composite solid propellant and the light-cured composite solid propellant pass additive manufacturing verification tests in sequence. For example, Sunyong realizes the extrusion molding of double-base gunpowder at 70 ℃ (Nanjing university of science and technology, [ D ], 2017), but a certain amount of ethyl acetate solvent is added in the manufacturing process, because the solvent volatilizes, a molded sample shrinks greatly, the difficulty in controlling molding precision is not facilitated, and meanwhile, the problem of abnormal combustion or structural strength caused by a large number of holes generated by volatilization of the internal solvent needs to be considered. Chinese patent CN 106346774A, CN 106863801B reports an additive manufacturing method of thermoplastic solid propellant, which also needs to be implemented by adding solvents such as methanol and ethanol. Chinese patent CN 109627133a reports a thermoplastic composite solid propellant and a preparation method thereof, although the adverse effect of solvent addition is successfully eliminated, in order to ensure controllable extrusion of propellant slurry in the additive manufacturing process, the processing temperature is slightly higher than the melting temperature of 95 ℃, and the control of process safety under high temperature process conditions is adverse. Meanwhile, the thermoplastic propellant has no high-molecular cross-linked network inside, the basic mechanical property of the thermoplastic propellant is lower than that of a thermosetting propellant formula, and the application range has certain limitation. Chocolate type propellant [ chemical propellant and high polymer material, 15 th volume in 2017, 5 th volume, 71-74] for additive manufacturing research reported by Wangwei et al has good processing performance, but the solid content is only 80%, and the energy performance is low. McClain M S and the like design two high-solid-content and high-viscosity composite propellant formula systems of HTPB containing 85% of potassium perchlorate (AP) and photocuring resin [ M.S. McClain, Proceedings of the Combustion Institute 000(2018) 1-8 ], in order to realize the sensitivity of the solid propellant to an ultraviolet light source, the method also relates to the problems of substitution or modification of a butylated hydroxytoluene adhesive, screening of a photosensitive curing agent/photosensitive curing catalyst system and the like, has large difference in the aspect of a forming reaction mechanism, and the regulation ways of important performances of the obtained photosensitive solid propellant, such as mechanics, Combustion and the like, still need to be optimized and are temporarily difficult to be directly applied. The existing composite solid propellant formula for additive manufacturing research has the conditions of solvent addition assistance, propellant curing system change, high manufacturing process temperature, no macromolecular cross-linked network and the like, and is unfavorable for realization and batch production of a solid propellant additive manufacturing process.
The butylated hydroxytoluene propellant is a composite solid propellant which is most commonly applied to the current weaponry, belongs to a thermosetting propellant, and is generally mixed by a vertical mixer under the process condition of 50-60 ℃, vacuum poured and solidified at constant temperature of 50 ℃ to realize engine filling. The butylated hydroxyl propellant slurry is not only a high solids suspension, but also a thermoset material. As a thermosetting material, the rheological behavior is complex and can be roughly divided into three stages: viscous state, gel state and solid state, the time of the process being dependent on the curing system. Because of the difference in curing reaction rates between different curing systems, the three states of the curing system change with the system. In the initial stage, because the curing and crosslinking degree of the medicinal slurry is not high in the initial stage, the continuous phase molecular motion of the medicinal slurry is intensified along with the increase of the temperature, and the intermolecular action is weakened, so that the mobility of the medicinal slurry is enhanced, the phenomenon that the viscosity of the medicinal slurry is reduced along with the increase of the temperature is shown, and the temperature is dominant; after a certain period of time, the molecular weight of the continuous phase increases along with the progress of the curing reaction to form a cross-linked network, the mobility of the slurry is hindered by the increase of the viscosity, the viscosity of the slurry gradually increases until the slurry becomes solid, and the curing time is dominant at the moment. Within the temperature range of 40 ℃ to 20 ℃, the curing reaction rate of the composite solid propellant is reduced along with the reduction of the temperature, and the key factor influencing the rheological property of the mixed slurry is the rheological property of the continuous phase molecules of the slurry. The continuous phase of the butylated hydroxytoluene propellant mainly comprises HTPB and plasticizer molecules, is liquid at normal temperature, has limited viscosity reduction range within the temperature range of 20-40 ℃, can still stand and level macroscopically at room temperature below 40 ℃, cannot realize room temperature setting, and does not meet the requirements of additive manufacturing processes.
The temperature-sensitive additive represented by ethylene-vinyl acetate copolymer and/or saturated triglyceride is mutually soluble with a butylated hydroxyanisole system, the viscosity of a molten mass is sharply increased along with the reduction of the temperature, and an inflection point exists in a viscosity curve at the melting temperature. In the temperature range of 20-40 ℃, the viscosity of the HTPB/plasticizer/temperature-sensitive additive continuous phase increases more than that of the HTPB/plasticizer continuous phase along with the reduction of the temperature. The variation range of the continuous phase viscosity can be regulated and controlled by regulating the type and the content of the temperature-sensitive additive, so that the viscosity of the drug slurry in the temperature range of 20-40 ℃ of the temperature-sensitive time-varying solid propellant can be regulated, and the drug slurry has the characteristic of room-temperature shaping on the premise of not influencing the service life of the drug slurry.
Disclosure of Invention
The invention aims to make up for the defects of the prior art, provides a temperature-sensitive time-varying solid propellant, and is suitable for the material increase manufacturing process research of the solid propellant.
The design idea adopted by the invention is as follows: based on a formula of the medium-energy butylated hydroxytoluene solid propellant, viscosity control of the HTPB/plasticizer/temperature-sensitive additive continuous phase within the temperature range of 20-40 ℃ is realized through a technical approach of regulating the type and content of the temperature-sensitive additive, and the temperature-sensitive time-varying solid propellant has the characteristics of adjustable viscosity of 560 Pa.s-1656 Pa.s of drug slurry within the temperature range of 20-40 ℃ and room-temperature shaping below 40 ℃ on the premise of not influencing the service life of the drug slurry.
The technical scheme adopted by the invention is as follows: a temperature-sensitive time-varying solid propellant comprises the following components in percentage by mass:
temperature-sensitive additive: 0.5 to 2.5 percent;
curing agent: 0.2% -1.0%;
curing catalyst: 0.01-0.04%;
oxidizing agent: 65 to 70 percent;
metal fuel: 16% -20%;
adhesive: 5% -10%;
plasticizer: 2% -5%;
other components: 0.25% -2.5%;
wherein the temperature-sensitive additive comprises one or the combination of ethylene-vinyl acetate copolymer (the content of vinyl acetate is between 15 and 45 percent) and saturated triglyceride; the adhesive is hydroxyl-terminated polybutadiene (HTPB), and the hydroxyl value is 0.47 mmol/g-0.70 mmol/g; the plasticizer is one or a combination of diisooctyl sebacate, dioctyl adipate, dioctyl phthalate and naphthenic oil KN 4006.
Further, the curing agent is one or a combination of toluene diisocyanate TDI, hexamethylene diisocyanate HDI, polyfunctional isocyanate N-100 and isophorone diisocyanate IPDI.
Further, the curing catalyst is one or a combination of triphenyl bismuth, tri (4-ethoxyphenyl) bismuth, tri (3-ethoxyphenyl) bismuth, tri (4-nitrophenyl) bismuth and tri (3-nitrophenyl) bismuth.
Further, the oxidant is one or a combination of ammonium perchlorate, octogen, hexogen and hexanitrohexaazaisowurtzitane.
Further, the metal fuel is micron aluminum powder, nano aluminum powder or a combination thereof.
Further, the other components comprise a mechanical property regulator, a combustion property regulator, an anti-aging agent and the like.
Further, the mechanical property regulator is one or the combination of tri-1- (2-methyl aziridine) phosphine oxide, boron trifluoride triethanolamine complex, triethanolamine and enamine bonding agent.
Furthermore, the combustion performance regulator is one or the combination of iron oxide, octyl ferrocene, 3-amino 1,2, 4-triazole complex copper perchlorate, copper chromite, ammonium oxalate, sodium oxalate and diethyl oxalate; the anti-aging agent is one or the combination of N, N-dimethylaniline, N-cyclohexyl-N' -phenyl p-phenylenediamine, methylene diphenylamine and N-cyclohexyl p-ethoxyaniline.
Furthermore, the temperature-sensitive time-varying solid propellant has adjustable drug slurry viscosity of 560 Pa.s-1656 Pa.s within the temperature range of 20-40 ℃, and the setting temperature is room temperature below 40 ℃.
Compared with the prior art, the invention has the following advantages:
1) the temperature-sensitive additive has wide raw material sources and is easy to realize batch production.
2) The temperature-sensitive time-varying solid propellant formula additive manufacturing process is low in temperature and high in safety coefficient, and the process does not involve the conditions of solvent addition, adhesive modification, curing condition change and the like.
3) The formula of the temperature-sensitive time-varying solid propellant is based on the formula of the traditional medium-energy butylated hydroxytoluene solid propellant, and the basic performances of the formula such as mechanics, combustion, energy and the like are similar to those of the medium-energy butylated hydroxytoluene solid propellant, so that the formula is easy to popularize and apply in weapon equipment.
The energy level (theoretical specific impulse and theoretical characteristic speed), density, safety performance, viscosity and service life of the obtained propellant are tested, and the test result shows that the prepared temperature-sensitive time-varying solid propellant has the energy level equivalent to that of a middle-energy thermosetting propellant, the service life is longer than 5h, the medicine slurry viscosity in the temperature range of 20-40 ℃ is 560 Pa.s-1656 Pa.s and is adjustable, and the propellant is shaped at the room temperature below 40 ℃.
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.
In the performance test:
energy level: 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;
viscosity and pot life: the test is carried out according to the QJ1813.2-2005 composite solid propellant slurry viscosity and service life measuring method.
Example 1
1) Temperature-sensitive time-varying solid propellant formula 1
2) Formulation properties of propellant
Example 2
1) Temperature-sensitive time-varying solid propellant formula 2
2) Formulation properties of propellant
| Test items | Formulation Properties |
| Theoretical specific impulse (N.s/kg) | 2584.04 |
| Density (g/cm)3) | 1.76 |
| Viscosity (Pa. s) of the slurry at 40 deg.C | 560.0 |
| Viscosity (Pa. s) of the slurry at 30 DEG C | 704.3 |
| Viscosity (Pa. s) of the slurry at 20 deg.C | 917.2 |
| Setting temperature (. degree. C.) | Room temperature below 20 deg.C |
| Service life (h) at 50 DEG C | Greater than 5h |
Example 3
1) Temperature-sensitive time-varying solid propellant formula 3
2) Formulation properties of propellant
| Test items | Formulation Properties |
| Theoretical specific impulse (N.s/kg) | 2602.46 |
| Density (g/cm)3) | 1.75 |
| Viscosity (Pa. s) of the slurry at 40 deg.C | 634.5 |
| Viscosity (Pa. s) of the slurry at 30 DEG C | 817.9 |
| Viscosity (Pa. s) of the slurry at 20 deg.C | 1115.6 |
| Setting temperature (. degree. C.) | Room temperature below 30 deg.C |
| Service life (h) at 50 DEG C | Greater than 5h |
Example 4
1) Temperature-sensitive time-varying solid propellant formula 4
2) Formulation properties of propellant
| Test items | Formulation Properties |
| Theoretical specific impulse (N.s/kg) | 2568.63 |
| Density (g/cm)3) | 1.76 |
| Viscosity (Pa. s) of the slurry at 40 deg.C | 852.4 |
| Viscosity (Pa. s) of the slurry at 30 DEG C | 1303.4 |
| Viscosity (Pa. s) of the slurry at 20 deg.C | 1656.0 |
| Setting temperature (. degree. C.) | Room temperature below 40 deg.C |
| Service life (h) at 50 DEG C | Greater than 5h |
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. The temperature-sensitive time-varying solid propellant is characterized by comprising the following components in percentage by mass:
temperature-sensitive additive: 0.5 to 2.5 percent;
curing agent: 0.2% -1.0%;
curing catalyst: 0.01-0.04%;
oxidizing agent: 65 to 70 percent;
metal fuel: 16% -20%;
adhesive: 5% -10%;
plasticizer: 2% -5%;
other components: 0.25% -2.5%;
the temperature-sensitive additive comprises an ethylene-vinyl acetate copolymer and/or saturated triglyceride, wherein the content of vinyl acetate in the ethylene-vinyl acetate copolymer is in the range of 15-45% by mass percentage;
the adhesive is hydroxyl-terminated polybutadiene, and the hydroxyl value is 0.47 mmol/g-0.70 mmol/g;
the plasticizer is one or a combination of more of diisooctyl sebacate, dioctyl adipate, dioctyl phthalate and naphthenic oil KN 4006.
2. The temperature-sensitive time-varying solid propellant of claim 1, wherein: the curing agent is one or a combination of more of toluene diisocyanate TDI, hexamethylene diisocyanate HDI, polyfunctional isocyanate N-100 and isophorone diisocyanate IPDI.
3. The temperature-sensitive time-varying solid propellant of claim 1, wherein: the curing catalyst is one or the combination of more of triphenyl bismuth, tri (4-ethoxyphenyl) bismuth, tri (3-ethoxyphenyl) bismuth, tri (4-nitrophenyl) bismuth and tri (3-nitrophenyl) bismuth.
4. The temperature-sensitive time-varying solid propellant of claim 1, wherein: the oxidant is one or the combination of ammonium perchlorate, octogen, hexogen and hexanitrohexaazaisowurtzitane.
5. The temperature-sensitive time-varying solid propellant of claim 1, wherein: the metal fuel is micron aluminum powder and/or nano aluminum powder.
6. The temperature-sensitive time-varying solid propellant of claim 1, wherein: the other components comprise a mechanical property regulator, a combustion property regulator and an anti-aging agent.
7. The temperature-sensitive time-varying solid propellant according to claim 6, wherein: the mechanical property regulator is one or the combination of tri-1- (2-methyl aziridine) phosphine oxide, boron trifluoride triethanolamine complex, triethanolamine and enamine bonding agent.
8. The temperature-sensitive time-varying solid propellant of claim 7, wherein: the combustion performance regulator is one or the combination of ferric oxide, octyl ferrocene, 3-amino 1,2, 4-triazole complex copper perchlorate, copper chromite, ammonium oxalate, sodium oxalate and diethyl oxalate; the anti-aging agent is one or a combination of N, N-dimethylaniline, N-cyclohexyl-N' -phenyl p-phenylenediamine, methylene diphenylamine and N-cyclohexyl-p-ethoxyaniline.
9. The temperature-sensitive time-varying solid propellant of claim 1, wherein: the temperature-sensitive time-varying solid propellant has adjustable drug slurry viscosity 560 Pa.s-1656 Pa.s within the temperature range of 20-40 ℃, and the setting temperature is room temperature below 40 ℃.
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| CN109627133B (en) * | 2018-12-05 | 2021-07-09 | 湖北航天化学技术研究所 | Thermoplastic composite solid propellant and preparation method thereof |
| CN112500253B (en) * | 2020-12-02 | 2022-04-12 | 湖北航天化学技术研究所 | Temperature-sensitive time-varying high-energy solid propellant |
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| US6174391B1 (en) * | 1999-08-30 | 2001-01-16 | The United States Of America As Represented By The Secretary Of The Army | Magnesium-fueled pyrotechnic compositions and processes based on elvax-cyclohexane coating technology |
| CN105130720B (en) * | 2014-05-30 | 2017-11-14 | 湖北航天化学技术研究所 | A kind of high energy low burning rate temperature-sensitivity coefficient propellant |
| CN105777459B (en) * | 2014-12-26 | 2018-06-19 | 湖北航天化学技术研究所 | Low residue gas generator propellant of a kind of low pressure index and preparation method thereof |
| CN106588522B (en) * | 2016-11-29 | 2018-05-29 | 湖北航天化学技术研究所 | Low melting point thermoplastic propellant and preparation method thereof |
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| CN109305869B (en) * | 2018-10-31 | 2021-04-30 | 湖北航天化学技术研究所 | Carborane propellant and preparation method thereof |
| CN109384636B (en) * | 2018-12-26 | 2020-09-22 | 湖北航天化学技术研究所 | Hydrocarbon fuel-rich propellant and preparation method thereof |
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