CN110627590B - Method for controlling particle size of ammonium dinitramide by adopting emulsion template - Google Patents
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Abstract
The invention discloses a method for controlling the particle size of ammonium dinitramide by adopting an emulsion template, which can simultaneously solve the problems of moisture absorption and sphericization particle size control of ammonium dinitramide. The method adopts deionized water as a dinitroamide ammonium solvent, a functional filler as a template agent and a solvent which does not dissolve dinitroamide ammonium as a template agent dispersion medium, prepares a water-in-oil type emulsion system under the action of a high-speed homogenizer at normal temperature, and removes the solvent through vacuum drying, thereby obtaining dinitroamide ammonium composite powder coated by the template agent. The size of the ammonium dinitramide aqueous phase liquid drops is controlled by adjusting parameters such as oil/water volume ratio, ammonium dinitramide aqueous solution concentration, template dispersion solution concentration, template/ammonium dinitramide mass ratio and the like, and finally the particle size of the spherical ammonium dinitramide powder is regulated and controlled. The emulsion template method strategy provided by the invention can simultaneously adjust the particle size and the moisture absorption performance of ammonium dinitramide. The operation object of the emulsion template method is ammonium dinitramide aqueous solution, and the experimental operation is simple and safe.
Description
Technical Field
The invention relates to a method for controlling the particle size of ammonium dinitramide by adopting an emulsion template, belonging to the technical field of material form control.
Background
Ammonium dinitramide is used as an ionic high-energy oxidant, does not contain carbon and halogen in molecules, and can meet the requirements of high-energy charging, low characteristic signal and clean combustion of an engine when added into a propellant. Ammonium dinitramide as an environmentally friendly oxidizer is considered to be an ideal substitute for ammonium perchlorate, ammonium nitrate and other conventional propellant oxidizers. However, ammonium dinitramide synthesized products are mostly high-defect crystals such as needle type crystals and flaky crystals, and have the advantages of high sensitivity, strong hygroscopicity, easy agglomeration and caking, difficult flowing and scattering, low filling rate in the propellant and high drug slurry viscosity, thereby greatly influencing the technical performance, the energy performance and the storage life of the propellant. Therefore, post-treatment procedures such as micro-crystal morphology, particle size and distribution, macro-morphology control and the like are required to be carried out on the synthesized ammonium dinitramide so as to meet the requirements of the preparation process and comprehensive performance of the propellant.
At present, the micro and macro multi-scale structures of ammonium dinitramide are regulated and controlled by technologies such as natural crystallization control, melting cooling crystallization, surface coating and the like, and much attention is paid to the ammonium dinitramide. A solvent-non-solvent recrystallization method is adopted by a domestic research team (randow, He jin Xuan, Lu Yan, Wang Ying, Dinitre. crystallization control research of ammonium dinitramide, chemical propellant and high polymer material), the shape and the granularity of the ammonium dinitramide crystal are effectively controlled by controlling a feeding mode, introducing ultrasonic oscillation, adding a crystal growth control agent and the like, and the mechanical sensitivity of the ammonium dinitramide is reduced. In addition, spherical ammonium dinitramide particle particles are prepared by rapidly cooling and crystallizing ammonium dinitramide melts by a foreign research team (Ulrich Teipel, Tomas Heart, Horst H.Krause, Crystallization of phosphoric Ammonium Dinitramide (ADN) particles, the particle size and surface finish of ammonium dinitramide crystals are effectively controlled by introducing an emulsifier, adjusting the viscosity of a dispersion system and the stirring rate, and the hygroscopicity and mechanical sensitivity of the product are obviously improved. However, the preparation of ammonium dinitramide by the above method still has the following disadvantages: (1) the emulsion stabilizer is required to be added in the preparation process, which is not favorable for preparing high-quality ammonium dinitramide; (2) a large amount of solvent is needed in the preparation and post-treatment processes, and the residual solvent in the product can cause ammonium dinitramide recrystallization, so that the product appearance is influenced; (3) ammonium dinitramide is in a high-temperature molten state, and great potential safety hazard is brought to operation.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention provides a method for controlling the particle size of ammonium dinitramide by adopting an emulsion template. The adopted emulsion template agent is an oil/water interface stabilizer, the template agent dispersion medium is an oil phase, the ammonium dinitramide aqueous solution is a water phase, and the water-in-oil type emulsion is prepared by a high-speed homogenizer at room temperature. Spherical ammonium dinitramide powder with low moisture absorption and controllable particle size is obtained by adjusting the concentration of a template agent in a dispersion liquid, the concentration of an aqueous solution of ammonium dinitramide, the mass ratio of the template agent to the ammonium dinitramide, the volume ratio of a water phase to an oil phase, the rotating speed of a high-speed homogenizer and the homogenizing time. Compared with the reported preparation method of spherical ammonium dinitramide, the template used by the invention has the functions of an oil/water emulsion interface stabilizer and a moisture absorption prevention auxiliary agent, can coat the aqueous phase droplets of ammonium dinitramide with the template in the water-in-oil emulsion forming process, and has simple operation process; compared with the reported preparation method of spherical ammonium dinitramide, the method has the advantages that the operation object is the aqueous solution of ammonium dinitramide at room temperature, and the intrinsic safety of the operation process can be obviously improved.
The invention adopts the following technical scheme:
step one, surface modification of template agent
Adding 0.01-100 parts by mass of a template agent into 100-10000 parts by mass of a dispersion medium; dissolving 0.01-100 parts by mass of a hydrophobic modifier in 100-10000 parts by mass of a solvent; mixing the two parts, stirring for 1-24h at 20-300 ℃, condensing, refluxing and filtering a reaction system, ultrasonically dispersing a filtered product in 100-10000 parts by mass of a solvent for 1-100 min, and filtering to obtain a precipitation reaction product; repeating the above processes for 1-10 times, and vacuum drying the filtered product at 25-100 deg.C to obtain hydrophobic modified template agent;
step two, preparation of water-in-oil type emulsion
Ultrasonically dispersing a modified template agent in a dispersion medium; ammonium dinitramide was dissolved in deionized water with mechanical stirring. Mixing the two dispersions, and emulsifying by adopting a high-speed homogenizer to obtain an emulsion system taking a template agent dispersion medium as a continuous phase and a dinitramide ammonium aqueous solution as a dispersed phase;
step three, adjusting the size of dispersed phase droplets
Regulating the mass-volume ratio of the template agent to the dispersion medium to be 0.1-10 mg/mL-1The mass volume ratio of ammonium dinitramide to deionized water is 10-1000 mg.mL-1The volume ratio of the dispersion medium to the deionized water is 10:1-1:10, the rotating speed of a high-speed homogenizer is controlled to be 500 plus 10000rpm, and the emulsifying time is controlled to be 1-10min, so that ammonium dinitramide aqueous phase droplets with the diameter of 5-500 mu m are obtained;
step four, preparation of ammonium dinitramide powder
Standing the emulsion system at room temperature for 1-100h, recovering the solvent which is not emulsified, and then drying the product in vacuum for 1-48h until the weight of the product is constant to obtain template agent coated ammonium dinitramide spherical powder;
the hydrophobic modifier is at least one of laurylamine, octadecylamine, oleic acid and lactide;
the solvent of the hydrophobic modifier is at least one of methanol, N-dimethylformamide and dichloromethane;
the vacuum drying method is at least one of high-temperature vacuum drying and vacuum freeze drying;
the template agent is at least one of silicon dioxide, titanium dioxide, carbon nano tubes, nano cellulose, nano montmorillonite, hydroxyapatite, graphene oxide and graphene;
the dispersion medium is at least one of cyclohexane, heptane, dodecane, octadecane, dichloromethane, chloroform, toluene and liquid paraffin oil;
the ammonium dinitramide is at least one of needle, sheet and spherical.
The invention has the beneficial technical effects that:
the invention adopts functional filler as an oil/water emulsion template agent, and an emulsion template is constructed through filler surface modification and oil/water interface interaction, so that spherical ammonium dinitramide composite powder coated by the template agent is obtained. The emulsion template method does not need to add a surfactant, and the functional filler serving as the template agent has the functions of oil/water meter interface stabilization and barrier, and can simultaneously realize the sphericization of ammonium dinitramide powder and the barrier to water vapor. The size of the ammonium dinitramide aqueous phase liquid drops is controlled by adjusting parameters such as oil/water volume ratio, ammonium dinitramide aqueous solution concentration, template dispersion solution concentration, template/ammonium dinitramide mass ratio and the like, and finally the particle size of the spherical ammonium dinitramide powder is regulated and controlled. Meanwhile, the surface performance of the ammonium dinitramide can be adjusted by adjusting the physical and chemical properties of the template agent, so that the ammonium dinitramide is endowed with multifunctional characteristics. Compared with the existing ammonium dinitramide preparation method, the method can simultaneously adjust the particle size and the moisture absorption performance of ammonium dinitramide by adopting an emulsion template method strategy. In addition, the operation object of the emulsion template method is the ammonium dinitramide aqueous solution, and compared with a melt crystallization method, the safety of experimental operation is obviously improved. Based on the abundant variety and diversity of the template, the emulsion template method has important significance for developing ammonium dinitramide facing practical application.
Drawings
Fig. 1 is an optical microscope image of an emulsion in which a continuous phase of a graphene toluene dispersion prepared by an emulsion templating method in example 1 is coated with a dispersed phase of an aqueous solution of ammonium dinitramide.
Fig. 2 is an optical microscope image of the emulsion in which the dispersed phase of aqueous solution of ammonium dinitramide is coated with the continuous phase of graphene toluene dispersion prepared by emulsion templating method in example 1.
Fig. 3 is a Scanning Electron Microscope (SEM) picture of the graphene-coated ammonium dinitramide composite powder obtained in example 1 by the vacuum drying method.
Fig. 4 is a Scanning Electron Microscope (SEM) picture of the graphene-coated ammonium dinitramide composite powder obtained in example 1 by the vacuum drying method.
Detailed Description
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a method for controlling the particle size of ammonium dinitramide by using an emulsion template, which specifically comprises the following steps:
step one, surface modification of template agent graphene oxide
Adding 0.1g of graphene oxide into 100mL of deionized water; dissolving 1.0g of dodecylamine in 100mL of absolute ethyl alcohol by mass; mixing the two parts, stirring at 90 ℃ for 24 hours, condensing, refluxing and filtering a reaction system, ultrasonically dispersing a filtered product in 100mL of absolute ethyl alcohol for 30 minutes, and filtering to obtain a precipitated reaction product; repeating the process for 4 times, and drying the filtered product at 60 ℃ in vacuum to obtain alkylamine-modified graphene oxide;
step two, preparation of water-in-oil type emulsion
Ultrasonically dispersing 0.005g of alkylamine modified graphene oxide in 10mL of methylbenzene for 30min, wherein the ultrasonic power is 1000W, the frequency is 200Hz, and the temperature is 30 ℃; adding 0.5g ammonium dinitramide into 10mL deionized water, and stirring for 1h at 30 ℃; mixing the two dispersions, and emulsifying at 6000rpm for 3min by a high-speed homogenizer to obtain water-in-oil emulsion with toluene as continuous phase and aqueous solution of ammonium dinitramide as dispersed phase. The appearance of the emulsion is characterized by an optical microscope, and the result is shown in figure 1, the ammonium dinitramide aqueous solution forms spherical droplets in the emulsion, and the diameter of the dispersed phase droplet is about 60 um; the alkylamine modified graphene uniformly covers the surface of the dispersed phase liquid drop to form a coating layer.
Step three, adjusting the size of dispersed phase droplets of the emulsion
Adding 0.5g ammonium dinitramide into 5mL deionized water, and stirring for 1h at 30 ℃; and (3) adding the obtained solution into the graphene toluene dispersion liquid in the second step, and emulsifying for 3min at the rotating speed of 6000rpm through a high-speed homogenizer to obtain the water-in-oil emulsion taking toluene as a continuous phase and a dinitramide ammonium water solution as a dispersed phase. The appearance of the emulsion is characterized by an optical microscope, and the result is shown in figure 2, the ammonium dinitramide aqueous solution forms circular droplets in the emulsion, and the diameter of the droplets is about 20 um; the alkylamine modified graphene uniformly covers the surface of the dispersed phase liquid drop to form a coating layer.
Step four, preparation of ammonium dinitramide powder
And standing the emulsions obtained in the second step and the third step at 20 ℃ for 24h, recovering the non-emulsified toluene solvent, then placing the product in a vacuum drying oven, and drying at 60 ℃ under a 0.1kPa vacuum environment for 12h to obtain alkylamine modified graphene coated ammonium dinitramide solid-phase composite powder, wherein the particle diameters of the composite powder are respectively 15um and 5um, as shown in figures 3 and 4.
Example 2
This example shows a method of controlling the particle size of ammonium dinitramide using an emulsion template, with steps one, two and three being the same as in example 1, except for step four.
Step four, preparation of ammonium dinitramide powder
Standing the emulsion at 20 ℃ for 24h, removing the non-emulsified toluene solvent on the upper layer of the emulsion, then placing the product in a vacuum freeze dryer, and drying at-50 ℃ for 5h under a vacuum environment of 10Pa to obtain the alkylamine modified graphene coated ammonium dinitramide solid-phase composite powder.
Example 3
The embodiment provides a method for controlling the particle size of ammonium dinitramide by using an emulsion template, which specifically comprises the following steps:
step one, modifying the surface of template agent silicon dioxide
1.0g of silica was added to chloroform/oleic acid (molar ratio 1:2), stirred for 3 hours, and then methanol was added to the above mixed solution to obtain a silica nanoparticle precipitate. The resulting product was dispersed in chloroform, then methanol was added to precipitate, and the above operation was repeated 4 times to remove excess oleic acid. And drying the final precipitated product at 120 ℃ to obtain the oleic acid hydrophobically modified silicon dioxide.
Step two, preparation of water-in-oil type emulsion
Ultrasonically dispersing 0.005g of oleic acid modified silicon dioxide in 10mL of methylbenzene for 30min, wherein the ultrasonic power is 1000W, the frequency is 200Hz, and the temperature is 30 ℃; adding 0.5g ammonium dinitramide into 10mL deionized water, and stirring for 1h at 30 ℃; mixing the two dispersions, and emulsifying for 3min at 10000rpm by a high-speed homogenizer to obtain water-in-oil emulsion with toluene as continuous phase and aqueous solution of ammonium dinitramide as dispersed phase.
Step three, adjusting the size of dispersed phase droplets of the emulsion
0.5g ammonium dinitramide was added to 5mL deionized water and stirred at 30 ℃ for 1 h. And (3) adding the obtained solution into the oleic acid modified silicon dioxide dispersion liquid in the step two, and emulsifying the two dispersion liquids according to the experimental conditions in the step two to obtain the water-in-oil type emulsion taking chloroform as a continuous phase and a dinitramide ammonium water solution as a dispersed phase.
Step four, preparation of ammonium dinitramide powder
And standing the emulsions obtained in the second step and the third step at 20 ℃ for 24h, recovering the unemulsified toluene solvent on the upper layer of the emulsion, then placing the product in a vacuum drying oven, and drying at 60 ℃ under the vacuum environment of 0.1kPa for 12h to obtain two silicon dioxide coated ammonium dinitramide solid-phase composite powders with different particle sizes.
Example 4
The embodiment provides a method for controlling the particle size of ammonium dinitramide by using an emulsion template, which specifically comprises the following steps:
step one, hydroxyapatite surface modification
Hydroxyapatite is treated at a high temperature of 800 ℃ for 1h, and 2.0g of the product is dispersed in 30mL of dichloromethane; dispersing 2.0g of lactide in 30mL of dichloromethane, stirring and mixing the two dispersions, removing the solvent in a fume hood at room temperature, and drying the dried product at the high temperature of 200 ℃ for 24 hours to obtain surface graft modified hydroxyapatite;
step two, preparation of water-in-oil type emulsion
Adding 0.01g of modified hydroxyapatite into 10mL of dichloromethane, and ultrasonically dispersing for 20min at the temperature of 30 ℃; adding 1.0g ammonium dinitramide into 10mL deionized water, and stirring for 1h at 30 ℃; dispersing the two dispersions by a high-speed homogenizer for 5min to obtain a water-in-oil emulsion taking dichloromethane as a continuous phase and a dinitramide ammonium aqueous solution as a dispersed phase;
step three, adjusting the size of dispersed phase droplets of the emulsion
0.5g ammonium dinitramide was added to 5mL deionized water and stirred at 30 ℃ for 1 h. And (3) adding the obtained solution into the lactide modified hydroxyapatite dispersion liquid in the step two, and emulsifying the two dispersion liquids according to the experimental conditions in the step two to obtain the water-in-oil type emulsion taking dichloromethane as a continuous phase and a dinitramide ammonium water solution as a dispersed phase.
Step four, preparation of ammonium dinitramide powder
And standing the emulsion obtained in the step two at 20 ℃ for 24h, removing the solvent which is not emulsified, then placing the product in a vacuum drying oven, and drying the product at 60 ℃ in a 0.1kPa vacuum environment for 12h to obtain the hydroxylapatite coated ammonium dinitramide solid-phase composite powder with two different particle sizes.
Claims (3)
1. A method for controlling the particle size of ammonium dinitramide by adopting an emulsion template is characterized by comprising the following steps:
step one, surface modification of template agent
Adding 0.01-100 parts by mass of a template agent into 100-10000 parts by mass of a dispersion medium; dissolving 0.01-100 parts by mass of a hydrophobic modifier in 100-10000 parts by mass of a solvent; mixing the two parts, stirring for 1-24h at 20-300 ℃, condensing, refluxing and filtering a reaction system, ultrasonically dispersing a filtered product in 100-10000 parts by mass of a solvent for 1-100 min, and filtering to obtain a precipitation reaction product; ultrasonically dispersing the filtered product in 100-10000 parts by mass of a solvent for 1-100 minutes, repeating the process of filtering to obtain a precipitation reaction product for 1-10 times, and drying the filtered product in vacuum at 25-100 ℃ to obtain a hydrophobic modified template agent;
step two, preparation of water-in-oil type emulsion
Ultrasonically dispersing a hydrophobically modified template agent in a dispersion medium; dissolving ammonium dinitramide in deionized water by mechanical stirring, mixing the two parts, and emulsifying by a high-speed homogenizer to obtain an emulsion system with a template agent dispersion medium as a continuous phase and an ammonium dinitramide aqueous solution as a dispersed phase;
step three, adjusting the size of dispersed phase droplets
Adjusting the mass-to-volume ratio of the hydrophobically modified template to the dispersion medium in the second step to be 0.1-10 mg/mL-1The mass volume ratio of ammonium dinitramide to deionized water is 10-1000 mg.mL-1Controlling the volume ratio of the dispersion medium to the deionized water in the step two to be 10:1-1:10, controlling the rotating speed of a high-speed homogenizer to be 500-10000rpm, and emulsifying for 1-10min to obtain ammonium dinitramide aqueous phase droplets with the diameter of 5-500 mu m;
step four, preparation of ammonium dinitramide powder
Standing the emulsion system in the step two at room temperature for 1-100h, recovering the solvent which is not emulsified, and then drying the product in vacuum for 1-48h until the weight of the product is constant to obtain template agent coated ammonium dinitramide spherical powder;
in the first step, the hydrophobic modifier is one of dodecylamine, octadecylamine, oleic acid and lactide;
in the first step, the solvent of the hydrophobic modifier is one of methanol, N-dimethylformamide and dichloromethane;
in the first step, the template agent is one of silicon dioxide, titanium dioxide, carbon nano tubes, nano cellulose, nano montmorillonite, hydroxyapatite, graphene oxide and graphene;
in the second step, the dispersion medium is one of cyclohexane, heptane, dodecane, octadecane, dichloromethane, chloroform, toluene and liquid paraffin oil.
2. The method for controlling particle size of ammonium dinitramide according to claim 1 wherein in step two said ammonium dinitramide is in the form of one of needles, flakes and spheres.
3. The method for controlling particle size of ammonium dinitramide according to claim 1, wherein said vacuum drying method in step four is one of high temperature vacuum drying and vacuum freeze drying.
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