CN114589302B - Preparation method of high-stability modified aluminum-lithium alloy powder of heat-resistant liquid - Google Patents
Preparation method of high-stability modified aluminum-lithium alloy powder of heat-resistant liquid Download PDFInfo
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- CN114589302B CN114589302B CN202210191486.6A CN202210191486A CN114589302B CN 114589302 B CN114589302 B CN 114589302B CN 202210191486 A CN202210191486 A CN 202210191486A CN 114589302 B CN114589302 B CN 114589302B
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of high-stability modified aluminum-lithium alloy powder of heat-resistant liquid, which comprises the steps of dispersing aminosilane in an organic solvent to obtain aminosilane dispersion liquid; adding aluminum lithium alloy powder into the dispersion liquid, and stirring and reacting for 10 to 20 min at normal temperature to hydrolyze and graft aminosilane on the surface of the aluminum lithium alloy powder; and then adding the double-claw silane, stirring and reacting for 30-120 min at normal temperature, condensing the double-claw silane with aminosilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating, and performing suction filtration, washing and vacuum drying to obtain the modified aluminum lithium alloy powder. According to the invention, a compact trace polysiloxane coating layer is formed through the autocatalytic hydrolysis reaction of aminosilane and bipedal silane, so that the heat-resistant liquid performance of the aluminum-lithium alloy powder is improved, and the aluminum-lithium alloy powder can stably exist in a mixed solution of hot water at 70 ℃ and hot water/ethyl acetate; but also meets the application requirements of the aluminum-lithium alloy powder in the composite solid propellant, and improves the specific impulse value of the composite solid propellant.
Description
Technical Field
The invention relates to a method for modifying aluminum-lithium alloy powder, in particular to a method for preparing heat-resistant liquid high-stability 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. Therefore, the aluminum-lithium alloy powder is used as the high-energy additive of the solid propellant, which not only can effectively reduce the erosion of high-temperature fuel gas to the engine nozzle, but also can reduce the loss of two-phase flow, and simultaneously improves the specific impulse of the propellant, thereby being an ideal fuel in the solid propellant. However, the research and application of the aluminum lithium alloy powder are still in the exploration stage at present.
Because the lithium electrode is active, the lithium electrode is easy to generate Li by chemical reaction with water and air 2 O or LiOH, li 2 O 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 high-activity aluminum powder/silicon powder coated with polymeric tannic acid, which effectively protects the activity of the aluminum powder or the silicon powder, can provide additional combustion heat and promote the rapid combustion reaction of the aluminum powder or the silicon powder, thereby improving the combustion performance of a solid propellant.
However, the assembly and formation of the composite solid propellant are usually completed under high temperature liquid phase environment conditions. Although the invention improves the reactivity of the metal powder in the composite solid propellant and the explosive, the aluminum lithium alloy powder has the problem of poor stability in the solid propellant, cannot resist the oxidative corrosion of the modified aluminum lithium alloy powder in the high-temperature liquid-phase environment in the assembling and forming process of the aluminum-containing explosive, obviously cannot meet the actual assembling and forming process requirements of the composite solid propellant, and further cannot meet the specific impact requirement of the composite solid propellant.
Disclosure of Invention
The invention aims to solve the bottleneck problems that the stability of the aluminum lithium alloy powder in a high-temperature liquid phase is poor and the aluminum lithium alloy powder cannot be applied to systems such as a solid propellant and the like, and provides a preparation method of a high-stability modified aluminum lithium alloy powder of a heat-resistant liquid, so that the modified aluminum lithium alloy powder which can stably exist in a high-temperature liquid phase environment can be obtained under a low cladding amount, the specific impulse value of the aluminum lithium alloy powder applied to the solid propellant is improved, and the preparation method plays a vital role in assembly molding and practical application of a composite solid propellant and the like.
1. Preparation of modified aluminum-lithium alloy powder
A preparation method of high-stability modified aluminum-lithium alloy powder of heat-resistant liquid is characterized in that aminosilane is dispersed in an organic solvent to obtain aminosilane dispersion liquid; adding aluminum lithium alloy powder into the dispersion liquid, stirring and reacting for 10 to 20 min at normal temperature, and hydrolyzing and grafting amino silane on the surface of the aluminum lithium alloy powder; and then adding the double-paw silane, stirring and reacting for 30 to 120 min at normal temperature, condensing the double-paw silane with aminosilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating layer, and performing suction filtration, washing and vacuum drying to obtain the modified aluminum lithium alloy powder.
The content of lithium in the aluminum-lithium alloy powder is 5 to 15 percent, and the organic solvent is one of N, N-dimethylformamide, N-methyl-2-pyrrolidone, dimethyl sulfoxide, ethyl acetate, ethanol and methanol.
The aminosilane is at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, phenylaminomethyltriethoxysilane, phenylaminomethyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane, 3-urea propyl triethoxysilane, aminopropylmethyldimethoxysilane and aminopropylmethyldiethoxysilane, and the mass ratio of the aluminum lithium alloy powder to the aminosilane is 1.
The double-paw silane is at least one of bis (trimethoxy silicon) ethane, bis (triethoxy silicon) ethane and bis (triethoxy silicon) propane, and the mass ratio of the double-paw silane to the aminosilane is (1).
The content of the polysiloxane coating layer is less than or equal to 2 percent of the mass of the aluminum lithium alloy powder.
2. Stability test of modified aluminum lithium alloy powder in high-temperature liquid phase environment
The content of the coating layer of the modified aluminum-lithium alloy powder prepared by the method is less than or equal to 2 wt%, the coating layer can stably exist in a mixed solution of hot water at 70 ℃ and hot water/ethyl acetate for 2 hours, no obvious reaction is caused, and hydrogen is not released.
In order to prove that the modified aluminum lithium alloy powder prepared by the invention has excellent stability in a high-temperature liquid phase environment, the modified aluminum lithium alloy powder prepared by the invention and unmodified aluminum lithium alloy powder are compared and studied.
FIG. 1 is a scanning electron micrograph of aminopropyltrimethoxysilane and bis (trimethoxysilyl) ethane modified aluminum lithium alloy powder (lithium content 10%) (left) compared with unmodified aluminum lithium alloy powder (right) under the same conditions. Compared with unmodified aluminum lithium alloy powder, the surface of the modified aluminum lithium alloy powder prepared by the invention forms a compact polysiloxane coating layer, which is beneficial to improving the stability of the aluminum lithium alloy powder in a high-temperature liquid phase environment.
FIG. 2 is a graph showing the stability of the N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and bis (triethoxysilyl) ethane modified aluminum lithium alloy powder (lithium content 15%) (left) in comparison with the unmodified aluminum lithium alloy powder (right) under the same conditions. The result shows that the modified aluminum-lithium alloy powder prepared by the invention does not have obvious reaction and does not release hydrogen when standing in hot water at the temperature of 70 ℃ for 2 hours. And the unmodified aluminum lithium alloy powder stands still in water at the temperature of 25 ℃ for 5min, so that severe hydrolysis reaction occurs, and a large amount of gas is generated. Therefore, the modified aluminum-lithium alloy powder can effectively improve the stability of the aluminum-lithium alloy powder in a high-temperature liquid phase environment.
3. Specific impact of modified aluminum-lithium alloy powder in composite solid propellant
In order to prove that the modified aluminum-lithium alloy powder prepared by the invention can improve the specific impulse when being applied to the composite solid propellant, the charge test of the composite solid propellant is carried out on the modified aluminum-lithium alloy powder. 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, the strength is high, the specific impact value is 249s, and the specific impact is improved by 2 to 3s compared with that of a solid propellant based on aluminum powder. Therefore, the modified aluminum-lithium alloy powder prepared by the invention can be applied to the formula of the composite solid propellant, and the specific impulse value of the composite solid propellant can be improved.
In summary, compared with the prior art, the invention has the following beneficial effects:
1. the invention utilizes aminosilane and double-paw silane to carry out autocatalytic hydrolytic condensation on the surface of the aluminum-lithium alloy powder to form a compact polysiloxane coating layer, and the modified aluminum-lithium alloy powder is obtained after suction filtration, washing and vacuum drying. The heat-resistant liquid performance of the aluminum lithium alloy powder is improved, so that the aluminum lithium alloy powder can stably exist in hot water at 70 ℃ and a hot water/ethyl acetate mixed solution; but also meets the application requirements of the aluminum-lithium alloy powder in the composite solid propellant, and improves the specific impulse value of the composite solid propellant.
2. The polysiloxane coating layer formed by the invention has better long-term stability, can improve the surface electrical property of the aluminum-lithium alloy powder particles, is favorable for preventing the particles from agglomerating, 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, simple method, easy operation, environment-friendly process, low cost and easy large-scale production, provides a novel technical approach for surface modification of the aluminum-lithium alloy powder, which is easy to industrialize, and lays a foundation for practical application of the aluminum-lithium alloy powder in the aspects of composite solid propellant and the like.
Drawings
FIG. 1 is a scanning electron micrograph of 10% modified Al-Li alloy powder (left) modified with aminopropyltrimethoxysilane and bis (trimethoxysilyl) ethane and unmodified Al-Li alloy powder (right) under the same conditions.
FIG. 2 is a graph showing the stability comparison between the modified 15% Al-Li alloy powder of the present invention (left) modified with N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and bis (triethoxysilyl) ethane and the unmodified Al-Li alloy powder (right) under the same conditions.
Detailed Description
The preparation method and properties of the heat-resistant liquid high-stability modified aluminum lithium alloy powder of the invention are further explained by the following specific examples.
Example 1
Adding 0.1 g of aminopropyltrimethoxysilane into 100 ml of N-dimethylformamide at normal temperature and normal pressure, and stirring for 0.5 min to obtain a silane dispersion liquid; then 5 g of 10% aluminum lithium alloy powder is added into the solution, and the solution is stirred for 10 min to hydrolyze and graft aminopropyl trimethoxy silane on the surface of the aluminum lithium alloy; and then adding 0.05 g of bis (trimethoxysilyl) ethane, stirring for 30 min at room temperature, condensing with aminopropyltrimethoxysilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating layer, and performing suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder, wherein the label of the modified aluminum lithium alloy powder is AlLi-1. Calculated by mass, the content of the polysiloxane coating layer is 1.2 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 placed in hot water at 70 ℃ for 2 hours, no gas is released, and the micro morphology is not changed.
Example 2
Adding 0.2 g of aminopropyltriethoxysilane into 100 mL of methanol at normal temperature and normal pressure, and stirring for 0.5 min to obtain a silane dispersion liquid; then 10 g of 10% aluminum lithium alloy powder is added into the solution, and the solution is stirred for 12 min to ensure that aminopropyltriethoxysilane is hydrolyzed and grafted on the surface of the aluminum lithium alloy; then adding 0.2 g of bis (triethoxysilyl) ethane, stirring for 50 min at room temperature, and condensing with aminopropyltriethoxysilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating layer; 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 polysiloxane coating layer is 0.8 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 a mixed solution of hot water and ethyl acetate at 70 ℃ for 2 hours, no gas is released, and the micro morphology is not changed.
Example 3
Adding 0.4 g of phenylaminomethyl triethoxysilane into 100 mL of methanol at normal temperature and pressure, and stirring for 0.5 min to obtain a silane dispersion; adding 15 g of 15% aluminum lithium alloy powder into the solution, and stirring for 15 min to hydrolyze and graft N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane on the surface of the aluminum lithium alloy; then adding 0.6 g of bis (triethoxysilyl) ethane, stirring for 60 min at room temperature, and condensing with phenylaminomethyl triethoxysilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polymer coating layer; 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 polysiloxane 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 placed in a mixed solution of hot water and ethyl acetate at 70 ℃ for 2 hours, no gas is released, and the micro morphology is not changed.
Example 4
At normal temperature and normal pressure, 0.67 g of aminopropylmethyldimethoxysilane is added into 100 mL of ethyl acetate, and the mixture is stirred for 0.5 min to obtain a silane dispersion liquid; then 10 g of 15 percent aluminum lithium alloy powder is added into the solution, and the solution is stirred for 18 min to ensure that aminopropyl methyl dimethoxy silane is hydrolyzed and grafted on the surface of the aluminum lithium alloy; then adding 1.0 g of bis (trimethoxysilyl) ethane, stirring for 90 min at room temperature, and condensing with aminopropylmethyldimethoxysilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating layer; 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 polysiloxane coating layer is 1.3 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 hot water at 70 ℃ for 2 hours, no gas is released, and the microscopic morphology is not changed.
Example 5
Under normal temperature and pressure, 1.13 g of aminopropylmethyldiethoxysilane is added into 100 mL of xylene, and stirred for 0.5 min to obtain a silane dispersion liquid; adding 15 g of 5% aluminum lithium alloy powder into the solution, and stirring for 20 min to hydrolyze and graft aminopropyl methyl diethoxy silane on the surface of the aluminum lithium alloy; then 2.25 g of bis (triethoxysilyl) ethane is added and stirred for 120 min at room temperature, and the mixture is condensed with aminopropyl methyl diethoxysilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating layer; 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 polysiloxane coating layer is 1.8 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 hot water at 70 ℃ for 2 hours, no gas is released, and the microscopic morphology is not changed.
Claims (3)
1. A preparation method of high-stability modified aluminum-lithium alloy powder of heat-resistant liquid comprises the steps of dispersing aminosilane in an organic solvent to obtain aminosilane dispersion liquid; adding aluminum lithium alloy powder into the dispersion liquid, and stirring and reacting for 10 to 20 min at normal temperature to hydrolyze and graft aminosilane on the surface of the aluminum lithium alloy powder; then adding the double-claw silane, stirring and reacting for 30-120 min at normal temperature, condensing the double-claw silane with aminosilane hydrolyzed on the surface of the aluminum lithium alloy to form a compact polysiloxane coating layer, and performing suction filtration, washing and vacuum drying to obtain modified aluminum lithium alloy powder;
the organic solvent is one of N, N-dimethylformamide, N-methyl-2-pyrrolidone, dimethyl sulfoxide, ethyl acetate, ethanol and methanol;
the aminosilane is at least one of aminopropyltrimethoxysilane, aminopropyltriethoxysilane, anilinomethyltriethoxysilane, anilinomethyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane, 3-urea propyl triethoxysilane, aminopropylmethyldimethoxysilane and aminopropylmethyldiethoxysilane, and the mass ratio of the aluminum lithium alloy powder to the aminosilane is 1;
the double-paw silane is at least one of bis (trimethoxy silicon) ethane, bis (triethoxy silicon) ethane and bis (triethoxy silicon) propane, and the mass ratio of the double-paw silane to the aminosilane is (1).
2. The method for preparing the high-stability modified aluminum-lithium alloy powder of the heat-resistant liquid according to claim 1, wherein the method comprises the following steps: the lithium content in the aluminum lithium alloy powder is 5 to 15 percent.
3. The method for preparing the high-stability modified aluminum-lithium alloy powder of the heat-resistant liquid according to claim 1, wherein the method comprises the following steps: the content of the polysiloxane coating layer is less than or equal to 2 percent of the mass of the aluminum lithium alloy powder.
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