CN112266313B - alpha-AlH3-PVDF double-shell structure compound, preparation method and application - Google Patents
alpha-AlH3-PVDF double-shell structure compound, preparation method and application Download PDFInfo
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- CN112266313B CN112266313B CN202011073319.9A CN202011073319A CN112266313B CN 112266313 B CN112266313 B CN 112266313B CN 202011073319 A CN202011073319 A CN 202011073319A CN 112266313 B CN112266313 B CN 112266313B
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- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
- C06B45/32—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound
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- C—CHEMISTRY; METALLURGY
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- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0008—Compounding the ingredient
Abstract
The invention discloses an alpha-AlH3The PVDF double-shell structure compound comprises an inner core, a first shell wrapping the inner core and a second shell wrapping the first shell from inside to outside; the kernel is alpha-AlH3A core, the first shell layer is Al2O3The second shell layer is a polymer layer; the polymer layer is a material layer formed by polyvinylidene fluoride (PVDF). With alpha-AlH3/Al2O3With alpha-AlH3/Al2O3PVDF (polyvinylidene fluoride) as comparison, and double-shell structure compound alpha-AlH synthesized by the method3/Al2O3The thermal stability of PVDF is significantly improved.
Description
Technical Field
The invention relates to a polymer alpha-AlH3Double-shell structure compound, preparation method and application, and alpha-AlH can be remarkably improved by using double-shell structure3Thermal stability of (3).
Background
Hydrogen is introduced in the combustion process of the solid propellant, so that the average relative molecular mass of the fuel gas can be effectively reduced; meanwhile, the high combustion heat value of the hydrogen is beneficial to improving the temperature of the combustion chamber and the specific impulse. Aluminum trihydride is a light metal hydride with a relatively high hydrogen content, up to 10.08%, has a hydrogen storage density of 148g/L, twice that of liquid hydrogen (70.8g/L), has a higher heat of combustion value than aluminum powder, and is an ideal solid propellant fuel. At present, AlH3A total of 7 different crystal forms include: alpha, alpha', beta, gammaDelta, epsilon and zeta, wherein the thermodynamic properties of the alpha crystal form are relatively stable, and the alpha crystal form is the only crystal form with application value in the formulation of the solid propellant. However, currently α -AlH is to be substituted3The solid propellant is applied to the solid propellant, and the decomposition phenomenon existing in the range of room temperature and the process temperature of the solid propellant needs to be solved.
Disclosure of Invention
The invention aims to provide a polymer alpha-AlH3Double-shell structure compound, preparation method and application thereof for improving AlH3Thermal stability of (2).
In order to realize the technical task, the technical scheme adopted by the invention is as follows:
alpha-AlH3-a PVDF double shell structure composite comprising, from inside to outside, an inner core, a first shell surrounding the inner core, a second shell surrounding the first shell;
the kernel is alpha-AlH3A core with a first shell layer of Al2O3The second shell layer is a polymer layer; the polymer layer is a material layer formed by PVDF.
Further, the diameter of the inner core is 200 nm-40 um; the thickness of the first shell layer is 5-30 nm; the thickness of the second shell layer is 1-15 nm.
The invention also discloses the alpha-AlH3-a method for preparing a PVDF double-shell structure composite, the method for preparing the composite comprising:
cleaning of alpha-AlH using acidic solutions3Obtaining alpha-AlH3/Al2O3Core/shell structure material, prepared by reacting alpha-AlH3/Al2O3And (3) placing the core/shell structure material and PVDF in a solvent system of water and DMF, and stirring and dispersing to obtain the composite material.
Further, the acidic solution is a dilute hydrochloric acid solution. The concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min. The alpha-AlH3/Al2O3The mass ratio of the core/shell structure material to the PVDF is (20-60) to (1-3). The stirring time is 0.5-4 h. The solvent system is a mixture of water and Dimethylformamide (DMF).
Preferred alpha-AlH in accordance with the invention3-a process for the preparation of a PVDF double shell structure composite, the process preferably comprising the steps of:
(1) obtaining alpha-AlH by acid washing3/Al2O3：α-AlH3Adding the mixture into a dilute acid solution for cleaning, filtering, and cleaning for 3 times by using a volatile organic solvent, wherein the cleaning time is 6-7 min. Finally, the alpha-AlH is obtained as off-white powder after freeze drying3/Al2O3。
(2)α-AlH3Preparation of PVDF double-shell structure composite: dissolving 5-30 mg of PVDF in dimethylformamide; mixing 100-600 mg of alpha-AlH3/Al2O3Adding the mixture into deionized water, performing ultrasonic treatment, stirring and dispersing for 3-30 min; the PVDF-containing DMF solution was slowly added to the alpha-AlH3/Al2O3The suspension is rapidly stirred at the same time; filtering, washing with ethanol for 3 times, and freeze drying to obtain gray powder of alpha-AlH3-a PVDF double shell structure composite.
alpha-AlH of the invention3PVDF double-shell structure composite, or alpha-AlH obtained according to the preparation method disclosed in the invention3The PVDF double-shell structure composite can be used for preparing solid propellant fuel.
Compared with the prior art, the invention has the following advantages and positive technical effects:
alpha-AlH of the invention3/Al2O3The PVDF double-shell structure compound realizes the further promotion of alpha-AlH on the basis of the acid pickling treatment method3Purpose of thermal stability, alpha-AlH obtained by synthesis3/Al2O3The PVDF double-shell structure compound can be used as a solid propellant fuel, the preparation process of the double-shell structure is carried out at normal temperature, and the preparation method is safe and reliable and is suitable for large-scale production.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure without limiting the disclosure. In the drawings:
FIG. 1 is a schematic view of the alpha-AlH of the present invention3/Al2O3SEM pictures of core/shell structures;
FIG. 2 is a schematic view of the alpha-AlH of the present invention3/Al2O3XRD pattern of core/shell structure;
FIG. 3 shows α -AlH prepared in example 13/Al2O3SEM image of PVDF double-shell structure compound;
FIG. 4 shows α -AlH prepared in example 13/Al2O3Thermal stability curve at 60 ℃ for a PVDF double-shell structure composite.
FIG. 5 shows α -AlH prepared in example 13/Al2O3X-ray photoelectron spectrum of the PVDF double-shell structure composite.
FIG. 6 shows α -AlH prepared in example 13/Al2O3Total reflection infrared (ATR-FTIR) spectra of PVDF double-shell structure composites.
The following detailed description of specific embodiments of the present disclosure is provided in connection with the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present disclosure, are given by way of illustration and explanation only, not limitation.
Detailed Description
The invention designs and synthesizes alpha-AlH3/Al2O3PVDF double-shell composite, i.e. Polymer-AlH3A double shell structured composite. PVDF has good hydrophobicity and chemical stability, and can inhibit the diffusion process of H element, thereby improving alpha-AlH3Compatibility and thermal stability of the composition to alpha-AlH3Has the stabilizing effect. By adding Al to2O3The surface of the PVDF coating can effectively improve alpha-AlH3Is helpful for promoting alpha-AlH3Research on the practical application of the solid propellant.
The double-shell structure compound comprises an inner core, a first shell wrapping the inner core and a second shell wrapping the first shell from inside to outside; the inner core is alpha-AlH3A core with a first shell layer of Al2O3The second shell layer is a polymer layer; the polymer layer is a layer of PVDF material. The diameter of the inner core is 200 nm-40 um; the thickness of the first shell layer is 5-30 nm; the thickness of the second shell layer is 1-15 nm.
In order to further improve the alpha-AlH based on acid pickling passivation3The invention provides an alpha-AlH3/Al2O3A preparation method of a PVDF double-shell structure compound. The general technical concept of the preparation method is as follows: cleaning of alpha-AlH using acidic solutions3Obtaining alpha-AlH3/Al2O3Core/shell structure material, prepared by reacting alpha-AlH3/Al2O3And (3) placing the core/shell structure material and PVDF in a solvent system of water and DMF, and stirring and dispersing to obtain the composite material.
Further, the acidic solution is a dilute hydrochloric acid solution. The concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min. The alpha-AlH3/Al2O3The mass ratio of the core/shell structure material to the PVDF is (20-60) to (1-3). The stirring time is 0.5-4 h. The solvent-non-solvent system is a mixture of water and DMF.
In order to achieve the aim, the invention provides alpha-AlH3/Al2O3The preferable technical steps of the preparation method of the PVDF double-shell structure compound are as follows:
(1) obtaining alpha-AlH by acid washing3/Al2O3：
Firstly, preparing a dilute acid solution; secondly, taking a certain amount of synthesized alpha-AlH3Adding the mixture into a dilute acid solution, stirring for 6-7 min, filtering, washing for 3 times by using a volatile organic solvent, and finally freezing and drying to obtain off-white powder.
(2)α-AlH3/Al2O3Preparation of PVDF double-shell structure compound
Firstly, dissolving 5-30 mgPVDF in DMF; then, 100-600 mg of alpha-AlH is added3/Al2O3Adding the mixture into deionized water, performing ultrasonic treatment, stirring and dispersing for 3-30 min; the PVDF-containing DMF solution was slowly added to the alpha-AlH3/Al2O3In the suspension, the suspension is stirred,simultaneously stirring rapidly; filtering, washing with ethanol for 3 times, and freeze drying to obtain gray powder sample polymer-AlH3A double shell structured composite.
Through experimental analysis and research, the concentration of dilute hydrochloric acid solution and the cleaning time are calculated for Al2O3The layer thickness has a direct influence, and the specific experimental data are as follows:
α-AlH3/Al2O3obtaining a shell structure:
washing of alpha-AlH by dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3The specific data for studying the relationship between the dilute hydrochloric acid concentration, the cleaning time and the first shell thickness for the core/shell structure material are shown in table 1:
TABLE 1
| Dilute hydrochloric acid concentration (V%) | Cleaning time (min) | Al2O3Layer thickness (nm) |
| 5 | 6 | 5 |
| 10 | 6 | 12 |
| 12 | 7 | 16 |
α-AlH3/Al2O3The SEM and XRD patterns of the core/shell structure are shown in fig. 1 and 2, respectively.
Example 1:
(1) obtaining alpha-AlH by acid washing3/Al2O3
Firstly, preparing a dilute hydrochloric acid solution with the volume fraction of 10%; secondly, taking a certain amount of synthesized alpha-AlH3Adding into dilute hydrochloric acid solution, stirring for 5min, filtering, washing with ethanol for 3 times, and freeze drying to obtain off-white powder.
(2)α-AlH3/Al2O3Preparation of PVDF double-shell structure compound
First, 30mg of PVDF was added to 20ml of DMF solvent and dissolved with stirring. Then 600mg of alpha-AlH is taken3/Al2O3Adding into 100ml deionized water, ultrasonic treating and stirring for dispersing for 10 min. The PVDF-containing DMF solution was slowly added to the alpha-AlH over 20min3/Al2O3To the suspension, it was then stirred rapidly for 2h, filtered and washed 3 times with ethanol. Finally, freeze-drying to obtain a gray powder sample of Polymer-AlH3A double shell structured composite.
α-AlH3/Al2O3Structural and thermal stability characterization of the PVDF double-shell structure compound:
synthetic alpha-AlH3/Al2O3The SEM image of the PVDF double-shell structure compound is shown in FIG. 3, the overall appearance of the compound is still particles, but the surface of the compound obviously has a coating layer and alpha-AlH3/Al2O3Have significant differences in surface topography.
Thermal stability characterization experiments were performed under vacuum at 60 ℃, as shown in fig. 4: as can be seen from this, the alpha-AlH3/Al2O3As a control, the thermal stability, alpha-AlH, was measured as the percentage decomposition at the same constant temperature time3/Al2O3The thermal stability of the PVDF double-shell structure compound is obviously higher than that of alpha-AlH3/Al2O3。
Referring to FIG. 5, is an alpha-AlH of the present invention3/Al2O3X-ray photoelectron spectrum of the PVDF double-shell structure composite. The F1s peak in the figure indicates the presence of a PVDF layer on the surface of the composite.
Referring to FIG. 6, is an alpha-AlH of the present invention3/Al2O3Total reflection infrared (ATR-FTIR) spectra of PVDF double-shell structure composites. As can be seen, the relative alpha-AlH3/Al2O3，α-AlH3/Al2O3The PVDF complex is 1173cm-1Has one more absorption peak, which is derived from-CF in PVDF2Symmetric stretching vibration of the group.
Example 2:
(1) obtaining alpha-AlH by acid washing3/Al2O3
Firstly, preparing a dilute hydrochloric acid solution with the volume fraction of 5%; secondly, taking a certain amount of synthesized alpha-AlH3Adding into dilute hydrochloric acid solution for 6min, filtering, washing with ethanol for 3 times, and freeze drying to obtain off-white powder sample.
(2)α-AlH3/Al2O3Preparation of PVDF double-shell structure compound
First, 10mg of PVDF was added to 20ml of DMF solvent and dissolved with stirring. Then 300mg of alpha-AlH is taken3/Al2O3Adding into 100ml deionized water, ultrasonic treating and stirring for dispersing for 10 min. The PVDF-containing DMF solution was slowly added to the alpha-AlH over 15min3/Al2O3To the suspension, it was then stirred rapidly for 1h, filtered and washed 3 times with ethanol. Finally, freeze-drying to obtain a gray powder sample of Polymer-AlH3A double shell structured composite.
Example 3:
(1) obtaining alpha-AlH by acid washing3/Al2O3
Firstly, preparing a dilute hydrochloric acid solution with the volume fraction of 8%; secondly, taking a certain amount of synthesized alpha-AlH3Adding into dilute hydrochloric acid solution for 6min, filtering, washing with ethanol for 3 times, and freeze drying to obtain off-white powder sample.
(2)α-AlH3/Al2O3Preparation of PVDF double-shell structure compound
First, 5mg of PVDF was added to 20ml of DMF solvent and dissolved with stirring. Then 100mg of alpha-AlH is taken3/Al2O3Adding into 100ml deionized water, ultrasonic treating and stirring for dispersing for 3 min. The PVDF-containing DMF solution was slowly added to the alpha-AlH over 5min3/Al2O3To the suspension, it was then stirred rapidly for 0.5h, filtered and washed 3 times with ethanol. Finally, freeze-drying to obtain a gray powder sample of Polymer-AlH3A double shell structured composite.
Example 4:
(1) obtaining alpha-AlH by acid washing3/Al2O3
Firstly, preparing a dilute hydrochloric acid solution with a volume fraction of 12%; secondly, taking a certain amount of synthesized alpha-AlH3Adding into dilute hydrochloric acid solution for 6min, filtering, washing with ethanol for 3 times, and freeze drying to obtain off-white powder sample.
(2)α-AlH3/Al2O3Preparation of PVDF double-shell structure compound
First, 20mg of PVDF was added to 20ml of DMF solvent and dissolved with stirring. Taking 400mg of alpha-AlH3/Al2O3Adding into 100ml deionized water, ultrasonic treating and stirring for 5 min. The PVDF-containing DMF solution was slowly added to the alpha-AlH over 10min3/Al2O3To the suspension, it was then stirred rapidly for 1.5h, filtered and washed 3 times with ethanol. Finally, freeze-drying to obtain a gray powder sample of Polymer-AlH3A double shell structured composite.
The scheme realizes the enhancement of alpha-AlH3For the purpose of thermal stability, to help advance the alpha-AlH3The application of the solid propellant in the preparation of the composite propellant is researched.
The preferred embodiments of the present disclosure are described in detail with reference to the accompanying drawings, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all belong to the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (3)
1. alpha-AlH3-a PVDF double shell structure composite, characterized in that the double shell structure composite, from inside to outside, comprises an inner core, a first shell surrounding the inner core, a second shell surrounding the first shell; the kernel is alpha-AlH3A core with a first shell layer of Al2O3The second shell layer is a polymer layer; the polymer layer is a material layer formed by PVDF, and the diameter of the inner core is 200 nm-40 um; the thickness of the first shell layer is 5-30 nm; the thickness of the second shell layer is 1-15 nm;
α-AlH3-the preparation method of the PVDF double-shell structure compound comprises the following steps: cleaning of alpha-AlH using acidic solutions3Obtaining alpha-AlH3/Al2O3Core/shell structure material, prepared by reacting alpha-AlH3/Al2O3Placing the core/shell structure material and PVDF in a solvent system, stirring and dispersing to obtain the composite material;
the acid solution is a dilute hydrochloric acid solution, the concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min; alpha-AlH3/Al2O3The mass ratio of the core/shell structure material to the PVDF is (20-60) to (1-3); the stirring time is 0.5-4 h, and the solvent system is a mixture of deionized water and dimethylformamide.
2. alpha-AlH3-PVDF double-shell structure composite preparation method, characterized in that, the alpha-AlH3-PVDF double-shell structure composite is alpha-AlH of claim 13PVDF double-shell structure composite, method for its productionThe method comprises the following steps:
(1) obtaining alpha-AlH by acid washing3/Al2O3：α-AlH3Adding the mixture into a dilute acid solution for cleaning for 6-7 min, filtering, cleaning for 3 times by using a volatile organic solvent, and finally freeze-drying to obtain off-white powder alpha-AlH 3/Al2O 3;
(2) preparing an alpha-AlH 3-PVDF double-shell structure compound: dissolving 5-30 mg of PVDF in dimethylformamide; adding 100-600 mg of alpha-AlH 3/Al2O3 into deionized water, performing ultrasonic treatment, stirring and dispersing for 3-30 min; the PVDF-containing DMF solution was slowly added to the alpha-AlH3/Al2O3The suspension is rapidly stirred at the same time; filtering, washing with ethanol for 3 times, and freeze drying to obtain gray powder of alpha-AlH3-a PVDF double shell structure composite.
3. alpha-AlH according to claim 13-use of a PVDF double shell structure composite for the preparation of a solid propellant fuel.
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