CN109128147B - Surface coating method of spherical aluminum powder - Google Patents
Surface coating method of spherical aluminum powder Download PDFInfo
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- CN109128147B CN109128147B CN201810769282.XA CN201810769282A CN109128147B CN 109128147 B CN109128147 B CN 109128147B CN 201810769282 A CN201810769282 A CN 201810769282A CN 109128147 B CN109128147 B CN 109128147B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
Abstract
The invention discloses a surface coating method of spherical aluminum powder, belonging to the technical field of surface modification, comprising the following steps: firstly, dissolving an energy-containing high polymer material containing nitrocotton into ethyl acetate at room temperature to form an energy-containing high polymer sol, then dispersing spherical aluminum powder into the ethyl acetate, then uniformly mixing the materials in the two steps, then adding an aqueous solution containing an emulsifier, then adding an aqueous solution containing a dispersing agent into the system, coating the spherical aluminum powder with the energy-containing high polymer material and dispersing the spherical aluminum powder into spherical liquid drops, then adding a salt solution for dehydration and leaching, and finally, separating and drying to obtain the aluminum powder particles with the surface coated with the energy-containing high polymer material. The method is simple and convenient to operate, safe and nontoxic, and low in energy consumption. The aluminum powder particles coated on the surface of the energy-containing high polymer material containing nitrocotton can keep good free-running property and water resistance. The invention is suitable for batch surface coating treatment of spherical aluminum powder.
Description
Technical Field
The invention belongs to the technical field of surface modification, and particularly relates to a surface coating method of spherical aluminum powder.
Background
The aluminum powder is used as an additive of the high-energy solid propellant, can effectively improve the energy of the propellant during combustion and the driving force to the rocket, but the micro-nano aluminum powder is easy to agglomerate in the storage process and is not beneficial to improving the energy of the propellant. The coating on the surface of the aluminum powder can effectively prevent the aluminum powder from being oxidized and improve the dispersibility and the combustion performance of the aluminum powder in the propellant.
At present, researchers at home and abroad have conducted a great deal of research on aluminum powder surface coating materials, such as silicon dioxide coating, oleic acid coating, metal coating, polystyrene coating, and the like. Chinese patent CN106984804 discloses a method for preparing nano aluminum powder microcapsules, which initiates styrene in-situ dispersion polymerization reaction in alcohol ether mixed solution, although the treatment method has simple preparation process, large consumption of methanol and ether in the treatment process, considerable economy, pollution to the operation environment and unsuitability for implementation under industrialized conditions, and the introduction of polystyrene to the surface of aluminum powder is not beneficial to the improvement of energy of a propellant system. Chinese patent CN108176851 discloses an aluminum powder coating protection method, wherein paraffin is used for preparing a protection layer solution, aluminum powder is added, the solution is stirred in vacuum to expel the solvent, and the solution is sieved and dried.
The surface coating modification research of the nano aluminum powder in China has some problems, the surface of the aluminum powder contains a certain amount of oxide shell layers by adopting in-situ coating and passivation coating methods, the content of active aluminum is reduced, most coating layers are inert substances, the energy level and the combustion performance of a propellant are influenced, and the application of the aluminum powder in the fields of the propellant and the explosive is limited. In addition, no report that energetic material polymer is successfully applied to aluminum powder surface coating modification is found.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a surface coating method of spherical aluminum powder.
The technical solution for realizing the purpose of the invention is as follows: a surface coating method of spherical aluminum powder comprises the following steps:
step 2, dispersing spherical aluminum powder into ethyl acetate under the stirring condition;
step 3, uniformly mixing the energy-containing polymer sol obtained in the step 1 with the material obtained in the step 2;
step 4, gradually adding an aqueous solution containing an emulsifier into the material obtained in the step 3 under the stirring condition for primary dispersion to obtain a polymer emulsion in which spherical aluminum powder is dispersed;
step 5, adding a water solution containing a dispersing agent into the high polymer emulsion obtained in the step 4 under the stirring condition for secondary dispersion, so that the energy-containing high polymer material is coated on the surface of the spherical aluminum powder;
step 6, adding a salt solution into the material system obtained in the step 5 under the stirring condition for dehydration and leaching, so that the solvent and water in the energetic polymer material coated on the surface of the spherical aluminum powder are gradually removed;
step 7, performing solid-liquid separation on the material obtained in the step 6 by adopting a filtering or centrifuging mode to obtain coated solid particles;
and 8, drying the solid particles obtained by solid-liquid separation in the step 7 by adopting a conventional mode, wherein the dried solid particles are spherical aluminum powder coated with the energetic polymer material on the surface.
Compared with the prior art, the invention has the following remarkable advantages: 1) according to the invention, the surface coating of spherical aluminum powder is realized by using the energetic polymer material containing nitrocotton, so that the oxidation and inactivation of aluminum are prevented, and the energy level and the combustion performance of the propellant are improved; 2) the spherical aluminum powder coated with the energetic polymer material on the surface has good free-running property, compact coating layer and excellent water resistance; 3) the invention adopts ethyl acetate and water as process media for surface treatment, and closed cycle is carried out, and the operation process is safe and environment-friendly; 4) the method can be completed at room temperature, and has simple process flow and strong operability.
The present invention is described in further detail below with reference to the attached drawing figures.
Drawings
FIG. 1 is a flow chart of the surface coating method of spherical aluminum powder of the present invention.
FIG. 2 is a diagram of the appearance of spherical aluminum powder before coating.
FIG. 3 is a distribution diagram of the particle size before coating with spherical aluminum powder.
FIG. 4 is a diagram of the appearance of the spherical aluminum powder coated in example 1 of the present invention.
FIG. 5 is a distribution diagram of the particle size of the spherical aluminum powder coated in example 1 of the present invention.
FIG. 6 is a diagram of the appearance of the spherical aluminum powder coated in example 2 of the present invention.
FIG. 7 is a distribution diagram of the particle size of the spherical aluminum powder coated in example 2 of the present invention.
FIG. 8 is a graph of the appearance of the spherical aluminum powder coated in example 3 of the present invention.
FIG. 9 is a distribution diagram of the particle size of the spherical aluminum powder coated in example 3 of the present invention.
Detailed Description
With reference to fig. 1, the surface coating method of spherical aluminum powder of the present invention includes the following steps:
And 2, dispersing the spherical aluminum powder into ethyl acetate under the stirring condition, wherein the mass ratio of the ethyl acetate to the spherical aluminum powder is not less than 6. Wherein the spherical aluminum powder is micron-sized spherical aluminum powder, and the particle size range of the micron-sized spherical aluminum powder is 1-100 microns. The mass ratio of the energy-containing high polymer material containing nitrocotton in the step 1 to the spherical aluminum powder in the step 2 is 1: 100-1: 10.
And 3, uniformly mixing the energy-containing polymer sol obtained in the step 1 with the material obtained in the step 2.
And 4, gradually adding an aqueous solution containing an emulsifier into the material obtained in the step 3 under the stirring condition for primary dispersion to obtain a polymer emulsion in which spherical aluminum powder is dispersed. Wherein the emulsifier is a surfactant, the mass concentration of the water solution containing the emulsifier is 0.05-1%, and the dosage of the water solution containing the emulsifier is 0.2-0.8 times of the total mass of the ethyl acetate used in the step 1 and the step 2.
And 5, adding an aqueous solution containing a dispersing agent into the high polymer emulsion obtained in the step 4 under the stirring condition for secondary dispersion, so that the energy-containing high polymer material is coated on the surface of the spherical aluminum powder. Wherein the dispersant is one of Arabic gum, gelatin, methylcellulose, polyethylene glycol and polyvinyl alcohol, the mass concentration of the aqueous solution containing the dispersant is 0.05-2%, and the dosage of the aqueous solution containing the dispersant is 2-5 times of the total mass of the ethyl acetate used in the step 1 and the step 2.
And 6, adding a salt solution into the material system obtained in the step 5 under the stirring condition for dehydration and leaching, so that the solvent and the water in the energetic polymer material coated on the surface of the spherical aluminum powder are gradually removed. Wherein the salt solution is one of a sodium sulfate solution, a potassium nitrate solution and a sodium chloride solution, the mass concentration of the salt solution is 0.2-4%, and the dosage of the salt solution is 8-12 times of the total mass of the ethyl acetate used in the step 1 and the step 2.
And 7, carrying out solid-liquid separation on the material obtained in the step 6 by adopting a filtering or centrifuging mode to obtain coated solid particles.
And 8, drying the solid particles obtained by solid-liquid separation in the step 7 by adopting a conventional mode, wherein the drying temperature is lower than 70 ℃, and the dried solid particles are spherical aluminum powder coated with the energetic polymer material on the surface.
The present invention will be described in further detail with reference to examples.
Example 1
At room temperature, an energetic polymer material with 100% of nitrocotton content is adopted as a coating material of spherical aluminum powder, and firstly, the energetic polymer material and an ethyl acetate solvent are adopted to prepare an energetic polymer sol with the mass concentration of 5%. Weighing 36g of ethyl acetate, pouring the ethyl acetate into a reaction device, starting stirring, regulating the rotation speed to 550rpm, weighing 6g of spherical aluminum powder (the particle size range is 1-100 mu m, and the average particle size is 26.57 mu m), pouring the spherical aluminum powder into the reaction device, dispersing for 10min, adding 1.2g of the energy-containing polymer sol according to the condition that the energy-containing polymer material accounts for 1 percent of the mass of the aluminum powder, and mixing and stirring for 20 min. Adding 29.7g (0.8 times of the weight of the ethyl acetate) of OP-10 emulsifier aqueous solution with the mass concentration of 0.3 percent into the material containing the energy polymer sol dispersed with the aluminum powder step by step, and emulsifying for 30min to obtain the polymer emulsion dispersed with the spherical aluminum powder. 185.8g (5 times of the weight of the ethyl acetate) of a gelatin solution with a mass concentration of 0.25% was added to the system to perform secondary dispersion for 30 min. Next, 446.1g (12 times the mass of the ethyl acetate used) of a potassium nitrate solution having a mass concentration of 4% was added to the above-mentioned material system, followed by dehydration and leaching for 60 minutes. And performing solid-liquid separation in a suction filtration mode, drying the separated solid particles in an oven at 50 ℃ to constant weight, obtaining the solid particles after drying, namely the spherical aluminum powder coated with the energetic polymer material on the surface, uniformly collecting the separated filtrate, distilling and recovering the solvent in the filtrate, and recycling the solvent. Fig. 2 is an appearance profile of the spherical aluminum powder before coating, fig. 3 is a particle size distribution diagram of the spherical aluminum powder before coating, fig. 4 is an appearance profile of the spherical aluminum powder after coating treatment in the present embodiment, and fig. 5 is a particle size distribution diagram of the spherical aluminum powder after coating treatment in the present embodiment.
Comparing the free-running property and the water resistance of the spherical aluminum powder before and after coating, respectively weighing 2g of the spherical aluminum powder before and after coating by using a precision electronic balance with the precision of 0.0001g, respectively placing the spherical aluminum powder before and after coating into a 50ml volumetric flask, adding 30ml of water, standing for a week in a constant-temperature water bath at 70 ℃, separating and drying solid particles, observing the appearance change of the solid particles and researching the mass change of the solid particles. The result shows that the spherical aluminum powder before coating is seriously agglomerated after being soaked in water by the method, and the mass change rate is plus 43.1 percent, which indicates that the water resistance is poor; in the embodiment, the appearance of the coated sample is almost unchanged after the sample is soaked in water by the method, the mass change rate is-0.03%, hydrolysis reaction is not generated, and the water resistance is good. The average particle size was 26.63. mu.m.
Example 2
A process similar to that of example 1 was used, with only part of the material ratios and types being changed, and without changing the order of addition and the treatment time. At room temperature, double-base absorbent containing 70% nitrocotton is used as an energetic polymer material to carry out aluminum powder surface coating, and energetic polymer sol with the mass concentration of 5% is prepared. Weighing 36g of ethyl acetate, pouring the ethyl acetate into a reaction device, starting stirring, regulating the rotation speed to 550rpm, weighing 6g of spherical aluminum powder (the particle size range is 1-100 mu m, and the average particle size is 26.57 mu m), pouring the spherical aluminum powder into the reaction device, dispersing for 10min, adding 6g of the energy-containing polymer sol according to the condition that the energy-containing polymer material accounts for 5% of the mass of the aluminum powder, and mixing and stirring for 20 min. 29.7g (0.8 time of the mass of the ethyl acetate used) of an aqueous solution of a Span-85 emulsifier with the mass concentration of 0.3 percent is gradually added into the material containing the energetic polymer sol in which the aluminum powder is dispersed, and the mixture is emulsified for 30min to obtain the polymer emulsion in which the spherical aluminum powder is dispersed. 185.7g (5 times of the weight of the ethyl acetate) of gum arabic solution with a mass concentration of 0.25% was added to the system, and the mixture was dispersed for 30 min. 445.6g (12 times the mass of the ethyl acetate used) of a 4% sodium sulfate solution was added to the above-mentioned material system, followed by dehydration and leaching for 60 minutes. Solid-liquid separation is carried out in the same way as in example 1, the solid particles are dried to constant weight, and the filtrate is collected and treated uniformly. Fig. 6 is an appearance and morphology diagram of the spherical aluminum powder after being coated in the embodiment, and fig. 7 is a particle size distribution diagram of the spherical aluminum powder after being coated in the embodiment. The sample coated in this example was subjected to the water immersion treatment in the same manner as in example 1, and the appearance was hardly changed, the mass change rate was-0.01%, hydrolysis reaction did not occur, and the water resistance was good. The average particle size was 35.79. mu.m.
Example 3
A process similar to that of example 1 was used, with only part of the material ratios and types being changed, and without changing the order of addition and the treatment time. At room temperature, double-base absorbent with 40% mass concentration of nitrocotton is used as an energy-containing high polymer material to coat aluminum powder, and energy-containing high polymer sol with 5% mass concentration is prepared. Weighing 36g of ethyl acetate, pouring the ethyl acetate into a reaction device, starting stirring, regulating the rotation speed to 550rpm, weighing 6g of spherical aluminum powder (the particle size range is 1-100 mu m, and the average particle size is 26.57 mu m), pouring the spherical aluminum powder into the reaction device, dispersing for 10min, adding 12g of the energy-containing polymer sol according to the condition that the energy-containing polymer material accounts for 10% of the mass of the aluminum powder, and mixing and stirring for 20 min. And gradually adding 29.2g (0.8 time of the mass of the ethyl acetate) of Tween-80 emulsifier aqueous solution with the mass concentration of 0.3% into the material containing the energetic polymer sol in which the aluminum powder is dispersed, and emulsifying for 30min to obtain the polymer emulsion in which the spherical aluminum powder is dispersed. 182.7g (5 times the mass of the ethyl acetate used) of a methylcellulose solution having a mass concentration of 0.25% was added to the system, followed by secondary dispersion for 30 minutes. Then, 438.5g (12 times the mass of the ethyl acetate used) of a 4% sodium chloride solution was added to the above-mentioned material system, followed by dehydration and leaching for 60 minutes. Solid-liquid separation is carried out in the same way as in example 1, the solid particles are dried to constant weight, and the filtrate is collected and treated uniformly. Fig. 8 is an appearance profile of the spherical aluminum powder after being coated in the embodiment, and fig. 9 is a particle size distribution diagram of the spherical aluminum powder after being coated in the embodiment. The sample coated in this example was subjected to the water immersion treatment in the same manner as in example 1, and the appearance was hardly changed, the mass change rate was-0.02%, hydrolysis reaction did not occur, and the water resistance was good. The average particle size was 48.52. mu.m.
Examples 4 to 19
6g of spherical aluminum powder having a particle size ranging from 1 μm to 100 μm and an average particle size of 26.57 μm was coated by the same process as in example 1, and the same immersion treatment as in example 1 was carried out on the samples of each example by changing only the material ratio without changing the charging order and the treatment time, and the results are shown in the following table.
The above examples are merely illustrative for clarity and are not intended to limit the embodiments. It will be apparent to those skilled in the art that other variations and modifications can be made on the basis of the foregoing description, and it is intended to cover all such modifications and variations as fall within the true spirit and scope of the invention.
The method of the invention has simple operation, safety, no toxicity and low energy consumption. The aluminum powder particles coated on the surface of the energy-containing high polymer material containing nitrocotton can keep good free-running property and water resistance. The invention is suitable for batch surface coating treatment of spherical aluminum powder.
Claims (9)
1. The surface coating method of the spherical aluminum powder is characterized by comprising the following steps:
step 1, dissolving an energy-containing high polymer material containing nitrocotton into ethyl acetate under the stirring condition to form energy-containing high polymer sol;
step 2, dispersing spherical aluminum powder into ethyl acetate under the stirring condition;
step 3, uniformly mixing the energy-containing polymer sol obtained in the step 1 with the material obtained in the step 2;
step 4, gradually adding an aqueous solution containing an emulsifier into the material obtained in the step 3 under the stirring condition for primary dispersion to obtain a polymer emulsion in which spherical aluminum powder is dispersed;
step 5, adding a water solution containing a dispersing agent into the high polymer emulsion obtained in the step 4 under the stirring condition for secondary dispersion, so that the energy-containing high polymer material is coated on the surface of the spherical aluminum powder;
step 6, adding a salt solution into the material system obtained in the step 5 under the stirring condition for dehydration and leaching, so that the solvent and water in the energetic polymer material coated on the surface of the spherical aluminum powder are gradually removed;
step 7, performing solid-liquid separation on the material obtained in the step 6 by adopting a filtering or centrifuging mode to obtain coated solid particles;
and 8, drying the solid particles obtained by solid-liquid separation in the step 7 by adopting a conventional mode, wherein the dried solid particles are spherical aluminum powder coated with the energetic polymer material on the surface.
2. The surface coating method of spherical aluminum powder according to claim 1, wherein in step 1, the nitrogen content of the nitrocotton in the energetic polymer material containing nitrocotton is greater than or equal to 11.5%, the mass ratio of the nitrocotton in the energetic polymer material is not less than 40%, and the mass concentration of the energetic polymer material in the energetic polymer sol is 2-10%.
3. The method for coating the surface of spherical aluminum powder as claimed in claim 1, wherein the mass ratio of ethyl acetate to spherical aluminum powder in step 2 is not less than 6.
4. The method for coating the surface of spherical aluminum powder as claimed in claim 1, wherein the spherical aluminum powder in step 2 is micron-sized spherical aluminum powder with a particle size ranging from 1 μm to 100 μm.
5. The method for coating the surface of spherical aluminum powder according to claim 1, wherein the mass ratio of the energetic polymer material containing nitrocotton in the step 1 to the spherical aluminum powder in the step 2 is 1:100 to 1: 10.
6. The method for coating the surface of spherical aluminum powder according to claim 1, wherein the emulsifier in step 4 is a surfactant, the mass concentration of the emulsifier-containing aqueous solution is 0.05-1%, and the amount of the emulsifier-containing aqueous solution is 0.2-0.8 times of the total mass of the ethyl acetate used in step 1 and step 2.
7. The method for coating the surface of spherical aluminum powder according to claim 1, wherein the dispersant in step 5 is one of acacia, gelatin, methylcellulose, polyethylene glycol and polyvinyl alcohol, the mass concentration of the aqueous solution containing the dispersant is 0.05-2%, and the amount of the aqueous solution containing the dispersant is 2-5 times of the total mass of the ethyl acetate used in step 1 and step 2.
8. The method for coating the surface of spherical aluminum powder according to claim 1, wherein the salt solution in step 6 is one of a sodium sulfate solution, a potassium nitrate solution and a sodium chloride solution, the mass concentration of the salt solution is 0.2-4%, and the amount of the salt solution is 8-12 times the total mass of the ethyl acetate used in step 1 and step 2.
9. The method for coating the surface of spherical aluminum powder as claimed in claim 1, wherein the drying temperature of the drying treatment in step 8 is lower than 70 ℃.
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| CN115259977B (en) * | 2021-04-30 | 2023-09-05 | 南京理工大学 | Preparation method of loose-structure nitrocotton base powder for environment-friendly fireworks |
| CN113458389B (en) * | 2021-06-30 | 2023-06-20 | 中国科学院空间应用工程与技术中心 | Composite powder of polystyrene coated aluminum alloy, alloy slurry, preparation method and stereolithography printing method |
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