CN114539009A - Preparation method of high-stability high-compatibility modified aluminum-lithium alloy powder - Google Patents
Preparation method of high-stability high-compatibility modified aluminum-lithium alloy powder Download PDFInfo
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Abstract
The invention provides a preparation method of high-stability high-compatibility modified aluminum-lithium alloy powder, which is characterized in that the aluminum-lithium alloy powder is ultrasonically dispersed in an organic solvent to obtain an aluminum-lithium alloy powder dispersion liquid; adding alkyl methoxysilane and micromolecular methoxysilane into the aluminum lithium alloy powder dispersion liquid, stirring and reacting for 30-180 min at normal temperature, and enabling the alkyl methoxysilane and the micromolecular methoxysilane to perform a coupling reaction on the surface of the aluminum lithium alloy powder to form a compact copolymer coating layer; and then carrying out suction filtration, washing and vacuum drying to obtain the modified aluminum-lithium alloy powder. According to the invention, the compact coupling coating layer is formed by the alkyl methoxysilane and the micromolecular methoxysilane, so that the stability of the aluminum-lithium alloy powder is improved, the combustion performance of the aluminum-lithium alloy powder is not reduced after the aluminum-lithium alloy powder is stored in a high-temperature and high-humidity environment, the compatibility of the aluminum-lithium alloy powder in the composite solid propellant is improved, a technical guarantee is provided for the practical application of the aluminum-lithium alloy powder in energetic materials such as the composite solid propellant, and the aluminum-lithium alloy powder has the advantages of simple process, easiness in large-scale preparation, low cost and the like.
Description
Technical Field
The invention relates to a method for modifying aluminum-lithium alloy powder, in particular to a method for preparing high-stability high-compatibility modified aluminum-lithium alloy powder, and belongs to the technical field of energetic materials.
Background
The high-activity metal powder plays an important role in the fields of explosives and powders, solid propellants and the like. Among them, the aluminum lithium alloy powder has excellent thermal reactivity as compared with aluminum powder. The aluminum lithium alloy powder is used as the high-energy additive of the solid propellant, so that the corrosion of high-temperature gas to an engine spray pipe can be effectively reduced, the loss of two-phase flow can be reduced, the specific impulse of the propellant is improved, and the aluminum lithium alloy powder is an ideal fuel in the solid propellant. However, the research and application of the aluminum lithium alloy powder are still in the exploration stage.
Because of the activity of the lithium electrode, the lithium electrode is easy to generate Li by chemical reaction with water and air2O or LiOH, Li2O and LiOH can react with aluminum and aluminum oxide to damage the surface structure of the aluminum-lithium alloy powder, so that the stability and compatibility of the aluminum-lithium alloy powder are poor, and the aluminum-lithium alloy powder cannot be practically applied to a solid propellant at present. Therefore, the aluminum lithium alloy powder needs to be stabilized to improve the safety of the aluminum lithium alloy powder in the preparation, storage and transportation processes of the propellant.
Researches show that the core-shell structure is constructed by coating the surface of the high-activity metal powder, so that the air can be blocked to keep the activity of the aluminum powder, and the surface of the aluminum powder can be modified. The Chinese invention patent CN110550990A discloses a preparation method of polymerized tannic acid coated aluminum powder/silicon powder, which can effectively protect the activity of aluminum powder or silicon powder, can provide additional combustion heat, and promotes the rapid combustion reaction of the aluminum powder or the silicon powder, thereby improving the combustion performance of the solid propellant. The Chinese invention patent CN11500091A discloses a preparation method of a polyphenol compound/nitrogen-containing polymer coated micro-nano aluminum powder, which not only improves the stability of the aluminum powder in a hot liquid, but also increases the active sites and the oxidation efficiency of the oxidation reaction of the aluminum powder, improves the burning rate of the aluminum powder and can improve the detonation performance of explosives.
However, the above-mentioned coating method of aluminum powder is not suitable for coating aluminum lithium alloy powder. The aluminum lithium alloy powder is coated by adopting the method, so that the aluminum lithium alloy powder is violently reacted and decomposed. This is because the activity of the aluminum lithium alloy powder is much higher than that of the aluminum powder. In addition, the assembly and the forming of the composite solid propellant are usually completed under the conditions of high temperature and high humidity. Although the invention improves the reactivity of the metal powder in the composite solid propellant and the explosive, the aluminum lithium alloy powder still has the problems of poor stability and compatibility in the solid propellant, and cannot resist the oxidation corrosion of the modified aluminum lithium alloy powder under high-temperature and high-humidity environments in the process of assembling and forming the aluminum-containing explosive, so that the requirements of the actual assembling and forming processes of the composite solid propellant cannot be met.
Disclosure of Invention
The invention aims to provide a preparation method of high-stability high-compatibility modified aluminum-lithium alloy powder aiming at the defects of oxidation corrosion and poor compatibility of the aluminum-lithium alloy powder in high-temperature and high-humidity environments, so as to obtain the modified aluminum-lithium alloy powder which can stably exist in the high-temperature and high-humidity environments, improve the activity and the compatibility of the aluminum-lithium alloy powder, and play a vital role in assembly molding and practical application of composite solid propellants and the like.
Preparation of modified aluminum-lithium alloy powder
The invention relates to a preparation method of high-stability high-compatibility modified aluminum-lithium alloy powder, which is characterized in that the aluminum-lithium alloy powder is ultrasonically dispersed in an organic solvent to obtain an aluminum-lithium alloy powder dispersion liquid; adding alkyl methoxysilane and micromolecular methoxysilane into the aluminum lithium alloy powder dispersion liquid, stirring and reacting for 30-180 min at normal temperature, and enabling the alkyl methoxysilane and the micromolecular methoxysilane to perform a coupling reaction on the surface of the aluminum lithium alloy powder to form a compact copolymer coating layer; and then carrying out suction filtration, washing and vacuum drying to obtain the modified aluminum-lithium alloy powder.
The lithium in the aluminum lithium alloy powder containsThe amount is 3-10%; the organic solvent is one of toluene, xylene, dimethyl sulfoxide, N-dimethylformamide, methanol and ethanol; the mass concentration of the aluminum-lithium alloy dispersion liquid is 0.1-2 g mL-1。
The alkyl methoxy silane is at least one of octadecyl trimethoxy silane, hexadecyl trimethoxy silane, mercaptopropyl trimethoxy silane, aminopropyl trimethoxy silane, 3-glycidoxy-propyl trimethoxy silane, 3-isocyanatopropyl trimethoxy silane, 1H,2H, 2H-heptadecafluorodecyl trimethoxy silane, 1H,2H, 2H-tridecafluorooctyl methyl dimethoxy silane and trifluoropropyl methyl dimethoxy silane, and the mass ratio of the aluminum lithium alloy powder to the alkyl methoxy silane is 1: 0.001-1: 0.2.
The micromolecular methoxysilane is at least one of methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, tetramethoxysilane, ethyltrimethoxysilane, diethyldimethoxysilane and triethylmethoxysilane, and the mass ratio of the alkylmethoxysilane to the micromolecular methoxysilane is 1: 5-1: 0.2.
The content of the obtained copolymer coating layer is less than or equal to 3 percent of the mass of the aluminum-lithium alloy powder.
Secondly, testing the stability of the modified aluminum lithium alloy powder in a high-temperature and high-humidity environment
The modified aluminum-lithium alloy powder prepared by the invention has excellent oxidation resistance, can be stably stored for more than 5 years in 50-90% of humid air at 40-70 ℃, has no gas release, and has the combustion performance reduced by less than or equal to 2%.
In order to prove that the modified aluminum lithium alloy powder prepared by the invention has excellent stability in high-temperature and high-humidity environments, the modified aluminum lithium alloy powder prepared by the invention and unmodified aluminum lithium alloy powder are compared and studied.
FIG. 1 is a graph showing the stability comparison of the Al-Li alloy powder (lithium content 5%) modified by trifluoropropylmethyldimethoxysilane and triethylmethoxysilane according to the present invention (left) with the unmodified Al-Li alloy powder (right) under the same conditions. The result shows that the modified aluminum-lithium alloy powder (lithium content is 5%) of the invention has no gas release after standing for 60 days in the environment with the temperature of 40 ℃ and the humidity of 50%, and the combustion performance is reduced by less than 1%. The unmodified aluminum lithium alloy powder stands for 24 hours in an environment with the temperature of 40 ℃ and the humidity of 50 percent, and obvious hardening and decomposition phenomena occur. Therefore, the modified aluminum lithium alloy powder can effectively improve the stability of the aluminum lithium alloy powder in high-temperature and high-humidity environments.
Compatibility of modified aluminum-lithium alloy powder
In order to confirm that the modified aluminum lithium alloy powder prepared by the invention has excellent compatibility, the powder charge test of the composite solid propellant is carried out. Through comparison, a large number of air holes appear in the charging process of the unmodified aluminum-lithium alloy powder, and the propellant is not formed. In the charging process of the modified aluminum lithium alloy powder, no air hole is generated, the propellant is well formed, and the strength is higher. Therefore, the modified aluminum-lithium alloy powder prepared by the invention obviously improves the compatibility of the aluminum-lithium alloy powder and has good compatibility with each component in the composite solid propellant.
FIG. 2 is a comparison of the compatibility in propellants of trifluoropropylmethyldimethoxysilane and triethylmethoxysilane modified aluminum lithium alloy powders (lithium content 5%) (left) of the present invention with unmodified aluminum lithium alloy powders (lithium content 5%) (right) under the same conditions. The result shows that the modified aluminum lithium alloy powder (lithium content is 5%) has no any air hole in the charging process, the propellant is well formed, and the strength is higher. And the unmodified aluminum lithium alloy powder has a large amount of pores. Therefore, the modified aluminum-lithium alloy powder can effectively improve the compatibility of the aluminum-lithium alloy powder in the propellant.
In summary, compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the alkyl methoxysilane and the micromolecular methoxysilane are added into the aluminum lithium alloy powder dispersion liquid, and the coupling reaction of the alkyl methoxysilane and the micromolecular methoxysilane on the surface of the aluminum lithium alloy powder is completed by stirring and reacting at normal temperature, so that a compact copolymer coating layer is formed, the activity of the aluminum lithium alloy powder is improved, the combustion stability of the aluminum lithium alloy powder is ensured in high-temperature and high-humidity environments, the compatibility of the aluminum lithium alloy powder in the composite solid propellant is also improved, and a technical support is provided for the practical application of the aluminum lithium alloy powder in an energetic material;
2. the copolymer coating layer formed by adopting the alkyl methoxylsilane and the micromolecular methoxylsilane has higher long-term stability, can improve the surface electrical property of the aluminum-lithium alloy powder particles, is favorable for preventing the agglomeration among the particles and improves the dispersion suspension property;
3. compared with preparation methods such as laser, electric arc, vapor deposition and the like, the method has the advantages of low equipment requirement, simplicity, easiness in operation, environment-friendly process, low cost, easiness in large-scale production and the like, and provides an aluminum-lithium alloy powder modification technical approach which is easy to industrialize for assembly forming and practical application of composite solid propellants and the like.
Drawings
FIG. 1 is a graph showing the stability comparison between the trifluoropropylmethyldimethoxysilane and triethylmethoxysilane modified aluminum lithium alloy powder (lithium content: 5%) (left) according to the present invention and unmodified aluminum lithium alloy powder (right) under the same conditions.
FIG. 2 is a comparison of the compatibility of Trifluoropropylmethyldimethoxysilane and Triethylmethoxysilane modified aluminum lithium alloy powder (lithium content 5%) (left) with unmodified aluminum lithium alloy powder (right) in the propellant under the same conditions.
Detailed Description
The preparation method and properties of the modified aluminum-lithium alloy powder with high stability and high compatibility of the invention are further described by the following specific examples.
Example 1
Under normal temperature and pressure, adding 42g of aluminum lithium alloy powder (with the lithium content of 3%) into 100 mL of toluene, and performing ultrasonic dispersion for 0.5 min to obtain an aluminum lithium alloy powder dispersion liquid; sequentially adding 0.3g of mercaptopropyl trimethoxysilane and 0.12g of methyl trimethoxysilane into the aluminum lithium alloy powder dispersion liquid, stirring and reacting for 90 min at normal temperature, and forming a compact copolymer coating layer on the surface of the aluminum lithium alloy powder; and then carrying out suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder marked as AlLi-1. Calculated by mass, the content of the coating layer is 1 percent of the mass of the aluminum lithium alloy powder.
Stability of the modified aluminum lithium alloy powder: the modified aluminum-lithium alloy powder is put in 60 percent humid air at 50 ℃ for 30 days, no gas is released, and the combustion performance is reduced by less than 1 percent; the microstructure of the modified aluminum-lithium alloy powder is not changed (similar to that in FIG. 1).
Compatibility of the modified aluminum lithium alloy powder: the alloy powder has no any air hole in the charging process, the propellant is well formed, the strength is higher, and the alloy powder has good compatibility in the composite solid propellant (similar to figure 2).
Example 2
Adding 67 g of aluminum lithium alloy powder (with the lithium content of 3%) into 100 mL of dimethylbenzene at normal temperature and normal pressure, and performing ultrasonic dispersion for 0.5 min to obtain an aluminum lithium alloy powder dispersion liquid; adding 3-isocyanate propyl trimethoxy silane and 0.17 g dimethyl dimethoxy silane into the aluminum lithium alloy powder dispersion liquid in sequence, stirring and reacting for 120 min at normal temperature, and forming a compact copolymer coating layer on the surface of the aluminum lithium alloy powder; and then carrying out suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder, wherein the powder is marked as AlLi-2. Calculated by mass, the content of the coating layer is 1 percent of the mass of the aluminum lithium alloy powder.
Stability of the modified aluminum lithium alloy powder: the modified aluminum-lithium alloy powder is put in humid air with the temperature of 55 ℃ and the humidity of 65 percent for 30 days, no gas is released, and the combustion performance is reduced by less than 1 percent; the microstructure of the modified aluminum-lithium alloy powder is not changed (similar to that in FIG. 1).
Compatibility of the modified aluminum lithium alloy powder: the alloy powder has no any air hole in the charging process, the propellant is well formed, the strength is higher, and the alloy powder has good compatibility in the composite solid propellant (similar to figure 2).
Example 3
Adding 33 g of aluminum lithium alloy powder (lithium content is 5%) into 100 mL of dimethyl sulfoxide at normal temperature and normal pressure, and performing ultrasonic dispersion for 0.5 min to obtain an aluminum lithium alloy powder dispersion liquid; then 0.5g of 1H,1H,2H, 2H-heptadecafluorodecyl trimethoxy silane and 0.16 g of tetramethoxy silane are sequentially added into the aluminum lithium alloy powder dispersion liquid, and the mixture is stirred and reacts for 30 min at normal temperature, so that a compact copolymer coating layer is formed on the surface of the aluminum lithium alloy powder; and then carrying out suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder, wherein the powder is marked as AlLi-3. Calculated by mass, the content of the coating layer is 1.5 percent of the mass of the aluminum lithium alloy powder.
Stability of the modified aluminum lithium alloy powder: the modified aluminum-lithium alloy powder is put in 55 percent humid air at 60 ℃ for 90 days, no gas is released, and the combustion performance is reduced by less than 1 percent; the microstructure of the modified aluminum-lithium alloy powder is not changed (similar to that in FIG. 1).
Compatibility of the modified aluminum lithium alloy powder: the alloy powder has no any air hole in the charging process, the propellant is well formed, the strength is higher, and the alloy powder has good compatibility in the composite solid propellant (similar to figure 2).
Example 4
Adding 100 g of aluminum lithium alloy powder (with the lithium content of 5%) into 100 mL of ethanol at normal temperature and normal pressure, and performing ultrasonic dispersion for 0.5 min to obtain an aluminum lithium alloy powder dispersion liquid; sequentially adding 1 g of trifluoropropylmethyldimethoxysilane and 1 g of triethylmethoxysilane into the aluminum lithium alloy powder dispersion liquid, stirring and reacting for 60 min at normal temperature, and forming a compact copolymer coating layer on the surface of the aluminum lithium alloy powder; and then carrying out suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder, wherein the powder is marked as AlLi-4. Calculated by mass, the content of the coating layer is 2 percent of the mass of the aluminum lithium alloy powder.
Stability of the modified aluminum lithium alloy powder: the modified aluminum-lithium alloy powder is put in humid air with the temperature of 55 ℃ and the humidity of 65 percent for 60 days, no gas is released, and the combustion performance is reduced by less than 1 percent; the microstructure of the modified aluminum-lithium alloy powder is not changed (as shown in figure 1).
Compatibility of the modified aluminum lithium alloy powder: the alloy powder has no any air hole in the charging process, the propellant is well formed, the strength is higher, and the alloy powder has good compatibility in the composite solid propellant (shown in figure 2).
Example 5
200 g of aluminum-lithium alloy powder (lithium content: 10%) was added to 100 mL of the alloy powder at normal temperature and pressureN,NUltrasonic dispersion is carried out for 0.5 min in dimethylformamide to obtain aluminum lithium alloy powder dispersion liquid; 2g of 1H,1H,2H, 2H-tridecafluorooctylmethyldimethyl etherAdding oxysilane and 4 g of tetraethoxysilane into the aluminum lithium alloy powder dispersion liquid, stirring and reacting for 90 min at normal temperature, and forming a compact copolymer coating layer on the surface of the aluminum lithium alloy powder; and then carrying out suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder, wherein the powder is marked as AlLi-5. Calculated by mass, the content of the coating layer is 3 percent of the mass of the aluminum lithium alloy powder.
Stability of the modified aluminum lithium alloy powder: the modified aluminum-lithium alloy powder is placed in 60 ℃ humid air for 60 days, no gas is released, and the combustion performance is reduced by less than 1%; the microstructure of the modified aluminum-lithium alloy powder is not changed (similar to that in FIG. 1).
Compatibility of the modified aluminum lithium alloy powder: the alloy powder has no any air hole in the charging process, the propellant is well formed, the strength is higher, and the alloy powder has good compatibility in the composite solid propellant (similar to figure 2).
Claims (9)
1. A preparation method of modified aluminum lithium alloy powder with high stability and compatibility comprises the steps of ultrasonically dispersing the aluminum lithium alloy powder in an organic solvent to obtain an aluminum lithium alloy powder dispersion liquid; adding alkyl methoxysilane and micromolecular methoxysilane into the aluminum lithium alloy powder dispersion liquid, stirring and reacting for 30-180 min at normal temperature, and enabling the alkyl methoxysilane and the micromolecular methoxysilane to perform a coupling reaction on the surface of the aluminum lithium alloy powder to form a compact copolymer coating layer; and then carrying out suction filtration, washing and vacuum drying to obtain the modified aluminum-lithium alloy powder.
2. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the lithium content in the aluminum lithium alloy powder is 3-10%.
3. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the organic solvent is one of toluene, xylene, dimethyl sulfoxide, N-dimethylformamide, methanol and ethanol.
4. The modified aluminum with high stability and high compatibility as claimed in claim 1The preparation method of the lithium alloy powder is characterized by comprising the following steps: the mass concentration of the aluminum lithium alloy powder dispersion liquid is 0.1-2 g mL-1。
5. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the alkyl methoxy silane is at least one of octadecyl trimethoxy silane, hexadecyl trimethoxy silane, mercaptopropyl trimethoxy silane, aminopropyl trimethoxy silane, 3-glycidoxy-propyl trimethoxy silane, 3-isocyanate propyl trimethoxy silane, 1H,2H, 2H-heptadecafluorodecyl trimethoxy silane, 1H,2H, 2H-tridecafluorooctyl methyl dimethoxy silane and trifluoropropyl methyl dimethoxy silane.
6. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the mass ratio of the aluminum lithium alloy powder to the alkyl methoxy silane is 1: 0.001-1: 0.2.
7. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the micromolecular methoxysilane is at least one of methyltrimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, tetramethoxysilane, ethyltrimethoxysilane, diethyldimethoxysilane and triethylmethoxysilane.
8. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the mass ratio of the alkyl methoxysilane to the micromolecular methoxysilane is 1: 0.2-1: 5.
9. The method for preparing the high-stability high-compatibility modified aluminum-lithium alloy powder according to claim 1, wherein the method comprises the following steps: the content of the copolymer coating layer is less than or equal to 3% of the mass of the aluminum lithium alloy powder.
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