CN111892468A - alpha-AlH3/Al2O3/C60Double-shell structure compound, synthesis method and application - Google Patents
alpha-AlH3/Al2O3/C60Double-shell structure compound, synthesis method and application Download PDFInfo
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Abstract
The invention discloses an alpha-AlH3/Al2O3/C60Double-shell structure compound, synthetic method and application, alpha-AlH3/Al2O3/C60The composite with the double-shell structure comprises an inner core, a first shell layer wrapping the inner core and a second shell layer wrapping the first shell layer from inside to outside; the kernel is alpha-AlH3A core, the first shell layer is Al2O3Layer, the second shell layer is modified C60A layer; modification C60Layer is C60A material layer formed by carrying carboxyl. With alpha-AlH3By contrast, the alpha-AlH synthesized by the method3/Al2O3/C60The thermal stability of the compound with a double-shell structure is obviously improved, and C in the compound structure60The content is less than 1%. alpha-AlH of the invention3/Al2O3/C60The 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/Al2O3/C60The 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.
Description
Technical Field
The invention belongs to the field of solid fuels, and particularly relates to alpha-AlH3/Al2O3/C60Double-shell structure compound, synthesis 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: α, α', β, γ, ζ, whereinThe alpha crystal form has relatively stable thermodynamic properties and is the only crystal form with application value in the formula 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.
C60Can be used as an additive of a solid propellant, and can release additional tension energy and binding energy when the carbon cage structure is broken. Based on the method, the invention designs and synthesizes alpha-AlH3/Al2O3/C60Double shell structure of composite in which C is present60The content is less than 1 percent, but the alpha-AlH can be obviously improved3Thermal stability, contributing to propulsion of alpha-AlH3Research on the practical application of the solid propellant.
Disclosure of Invention
In order to further improve the alpha-AlH based on acid pickling passivation3The invention provides an alpha-AlH3/Al2O3/C60A double-shell structure compound, a synthetic method and application.
To achieve the above object, the present invention is realized by:
alpha-AlH3/Al2O3/C60The composite with the double-shell structure comprises an inner core, a first shell layer wrapping the inner core and a second shell layer wrapping the first shell layer from inside to outside;
the kernel is alpha-AlH3A core, the first shell layer is Al2O3Layer, the second shell layer is modified C60A layer;
modification C60Layer is C60A material layer formed by carrying carboxyl.
Optionally, 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.
Optionally, alpha-AlH3/Al2O3/C60Preparation method of double-shell structure compoundThe method comprises the following steps:
cleaning alpha-AlH with dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3Core/shell materials of construction, alpha-AlH3/Al2O3Core/shell structure material and modified C60Stirring and dispersing in a toluene/tetrahydrofuran mixed solvent to obtain the alpha-AlH3/Al2O3/C60A double shell structured composite.
Optionally, the concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min.
Optionally, alpha-AlH3/Al2O3Core/shell structure material and modified C60The mass ratio of (A) to (B) is 5: 1; the volume ratio of toluene to tetrahydrofuran in the toluene/tetrahydrofuran mixed solvent is 2; the stirring and dispersing time is 4-12 h.
Optionally, said modification C60The preparation method comprises the following steps:
collecting 170mg of 4-carboxybenzaldehyde and 150mg of C60And 90mg sarcosine in turn in 50ml chlorobenzene; refluxing the chlorobenzene solution at 135 ℃ for 16h under nitrogen atmosphere; the solvent component in the product was removed by rotary evaporation to obtain a dark brown powder, which was then dispersed in a toluene/tetrahydrofuran mixed solvent (v/v ═ 2), and separated by silica gel column chromatography to obtain brown modified C60And (3) sampling.
alpha-AlH3/Al2O3/C60The method for synthesizing the double-shell structure compound comprises the following steps:
cleaning alpha-AlH with dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3Core/shell materials of construction, alpha-AlH3/Al2O3Core/shell structure material and modified C60Stirring and dispersing in a toluene/tetrahydrofuran mixed solvent to obtain the alpha-AlH3/Al2O3/C60A double shell structured composite.
Optionally, the concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min;
α-AlH3/Al2O3core/shell structure material and modified C60The mass ratio of (A) to (B) is 5: 1; the volume ratio of toluene to tetrahydrofuran in the toluene/tetrahydrofuran mixed solvent is 2; the stirring and dispersing time is 4-12 h.
Optionally, said modification C60The preparation method comprises the following steps:
collecting 170mg of 4-carboxybenzaldehyde and 150mg of C60And 90mg sarcosine in turn in 50ml chlorobenzene; refluxing the chlorobenzene solution at 135 ℃ for 16h under nitrogen atmosphere; the solvent component in the product was removed by rotary evaporation to obtain a dark brown powder, which was then dispersed in a toluene/tetrahydrofuran mixed solvent (v/v ═ 2), and separated by silica gel column chromatography to obtain brown modified C60And (3) sampling.
The alpha-AlH of the invention3/Al2O3/C60Use of a double shell structure composite for the preparation of a solid propellant fuel.
The invention has the advantages and positive effects that:
alpha-AlH of the invention3/Al2O3/C60The 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/Al2O3/C60The 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 shows modification C obtained in example 160(ii) an infrared spectrum;
FIG. 2 shows α -AlH prepared in example 13/Al2O3/C60TEM image of double-shell structure compound with Al in the middle of two dotted lines2O3Layer of C in the red circle60A molecule;
FIG. 3. alpha. -AlH of example 13/Al2O3/C60Thermal stability curve of the double shell structure composite at 60 ℃;
FIG. 4 is example 1. alpha. -AlH3/Al2O3/C60Thermal stability curves (different hydrochloric acid concentrations versus washing time) of the double shell structure composites at 60 ℃;
FIG. 5 is a view of alpha-AlH3/Al2O3With alpha-AlH3/Al2O3/C60XRD pattern of the double-shell structure compound.
Detailed Description
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.
alpha-AlH of the invention3/Al2O3/C60Double shell structure compound: the inner core is alpha-AlH3The first shell layer on the surface is Al2O3Layer, the second shell layer is modified C60Layer, modification C60Molecular attachment to Al2O3Layer surface, the thickness of the layer can be quantified by TEM characterization (see fig. 1); to C60The purpose of the modification is to make C60A large number of carboxyl groups are carried on the molecule, so that the Al is more easily attached to the Al2O3The surface of the layer. The compound comprises an inner core, a first shell layer wrapping the inner core and a second shell layer wrapping the first shell layer; the inner core is alpha-AlH3A core with a first shell layer of Al2O3Layer, the second shell layer is modified C60A layer; modification C60Layer is at C60Carrying a carboxyl group thereon. 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 composite material with the structure promotes alpha-AlH3And (3) thermal stability.
The preparation method comprises the following steps:
the microstructure is shown in fig. 2. The synthesis process comprises the following steps: (1) from fullerene (C)60) Preparation methodSex C60(ii) a (2) Modification C60With alpha-AlH3Preparation of alpha-AlH3/Al2O3/C60A double shell structure compound;
cleaning alpha-AlH with dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3Core/shell materials of construction, alpha-AlH3/Al2O3Core/shell structure material and modified C60Stirring and dispersing in a toluene/tetrahydrofuran mixed solvent to obtain the alpha-AlH3/Al2O3/C60A double shell structured composite.
For example, the concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min.
For example, alpha-AlH3/Al2O3Core/shell structure material and modified C60The mass ratio of (A) to (B) is 5: 1; the volume ratio of toluene to tetrahydrofuran in the toluene/tetrahydrofuran mixed solvent is 2; the stirring and dispersing time is 4-12 h.
Modification C60The preparation method comprises the following steps:
collecting 170mg of 4-carboxybenzaldehyde and 150mg of C60And 90mg sarcosine in turn in 50ml chlorobenzene; refluxing the chlorobenzene solution at 135 ℃ for 16h under nitrogen atmosphere; the solvent component in the product was removed by rotary evaporation to obtain a dark brown powder, which was then dispersed in a toluene/tetrahydrofuran mixed solvent (v/v ═ 2), and separated by silica gel column chromatography to obtain brown modified C60And (3) sampling.
With alpha-AlH3By contrast, the alpha-AlH synthesized by the method3/Al2O3/C60The thermal stability of the compound with a double-shell structure is obviously improved, and C in the compound structure60The content is less than 1%. alpha-AlH of the invention3/Al2O3/C60The 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/Al2O3/C60The double-shell structure compound can be used as solid propellant fuel, the preparation process of the double-shell structure is carried out at normal temperature, and the preparation method is safe, reliable and suitable forFor large-scale production.
Example 1: alpha-AlH3/Al2O3/C60And (3) synthesizing a double-shell structure compound:
(1) modification C60The synthesis of (2):
collecting 170mg of 4-carboxybenzaldehyde and 150mg of C60And 90mg sarcosine in turn in 50ml chlorobenzene; refluxing the chlorobenzene solution at 135 ℃ for 16h under nitrogen atmosphere; the solvent component in the product was removed by rotary evaporation to obtain a dark brown powder, which was then dispersed in a toluene/tetrahydrofuran mixed solvent (v/v ═ 2), and separated by silica gel column chromatography to obtain brown modified C60And (3) sampling.
Modification C is apparent from the IR spectrum of FIG. 160The peak having a characteristic of C ═ O indicates that the structure contains a carboxyl group.
(2)α-AlH3/Al2O3/C60Synthesis of double-shell structure compound
First, the alpha-AlH is washed by a dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3A core/shell structural material; taking 20mg of modified C in the step (1)60Dispersing in toluene/tetrahydrofuran (v/v ═ 2) mixed solvent, and collecting alpha-AlH3/Al2O3Adding the core/shell structure material (100mg), stirring and dispersing for 4-12 h, filtering and collecting light yellow powder. The data of the relation between the concentration of dilute hydrochloric acid, the cleaning time and the thickness of the first shell layer are specifically researched and shown in the table 1:
TABLE 1
α-AlH3/Al2O3/C60And (3) characterizing the structure and the thermal stability of the double-shell structure compound:
synthetic alpha-AlH3/Al2O3/C60The TEM image of the double-shell structure composite is shown in FIG. 2, the double-shell boundary of the composite is clear, and the alpha-AlH is arranged from the inside to the outside of the particle3，Al2O3Layer and modification C60And (3) a layer. Wherein, alpha-AlH3Some of them were observed as lattice diffraction fringes, with a pitch of 0.32nm, corresponding to the pitch of their (012) crystal planes. The middle part of the dotted line is Al2O3Layer, wherein tiny black spots are visible in TEM image and distributed on the outermost layer, and the black spots are modified C60And agglomerated particles thereof.
Thermal stability characterization experiments were performed under vacuum at 60 ℃, as shown in fig. 3: 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/Al2O3/C60The thermal stability of the compound with the double-shell structure is obviously higher than that of alpha-AlH3/Al2O3。
Thermal stability characterization experiments were performed under vacuum at 60 ℃, as shown in fig. 4: thermal stability, measured as percent decomposition, with greater Al at the same constant temperature2O3alpha-AlH of layer thickness3/Al2O3Has better thermal stability.
FIG. 5 is a view of alpha-AlH3/Al2O3With alpha-AlH3/Al2O3/C60XRD pattern of the double-shell structure composite from which modification C can be seen60The layer does not change alpha-AlH3/Al2O3The crystal structure of (a).
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 (10)
1. alpha-AlH3/Al2O3/C60The double-shell structure compound is characterized in that the 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 Al2O3Layer, the second shell layer is modified C60A layer;
modification C60Layer is C60A material layer formed by carrying carboxyl.
2. alpha-AlH according to claim 13/Al2O3/C60The double-shell structure compound is characterized in that 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.
3. alpha-AlH according to claim 1 or 23/Al2O3/C60A double shell structure complex characterized by alpha-AlH3/Al2O3/C60The preparation method of the double-shell structure compound comprises the following steps:
cleaning alpha-AlH with dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3Core/shell materials of construction, alpha-AlH3/Al2O3Core/shell structure material and modified C60Stirring and dispersing in a toluene/tetrahydrofuran mixed solvent to obtain the alpha-AlH3/Al2O3/C60A double shell structured composite.
4. alpha-AlH according to claim 33/Al2O3/C60The double-shell structure compound is characterized in that the concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min.
5. alpha-AlH according to claim 33/Al2O3/C60A double shell structure complex characterized by alpha-AlH3/Al2O3Core/shell structure material and modified C60The mass ratio of (A) to (B) is 5: 1; the volume ratio of toluene to tetrahydrofuran in the toluene/tetrahydrofuran mixed solvent is 2; the stirring and dispersing time is 4-12 h.
6. alpha-AlH according to claim 33/Al2O3/C60The compound with a double-shell structure is characterized in that the modified C60The preparation method comprises the following steps:
collecting 170mg of 4-carboxybenzaldehyde and 150mg of C60And 90mg sarcosine in turn in 50ml chlorobenzene; refluxing the chlorobenzene solution at 135 ℃ for 16h under nitrogen atmosphere; the solvent component in the product was removed by rotary evaporation to obtain a dark brown powder, which was then dispersed in a toluene/tetrahydrofuran mixed solvent (v/v ═ 2), and separated by silica gel column chromatography to obtain brown modified C60And (3) sampling.
7. alpha-AlH3/Al2O3/C60The method for synthesizing the double-shell structure compound is characterized by comprising the following steps of:
cleaning alpha-AlH with dilute hydrochloric acid solution3Obtaining alpha-AlH3/Al2O3Core/shell materials of construction, alpha-AlH3/Al2O3Core/shell structure material and modified C60Stirring and dispersing in a toluene/tetrahydrofuran mixed solvent to obtain the alpha-AlH3/Al2O3/C60A double shell structured composite.
8. alpha-AlH according to claim 73/Al2O3/C60The method for synthesizing the double-shell structure compound is characterized in that the concentration of the dilute hydrochloric acid solution is 5-12V%, and the cleaning time is 6-7 min;
α-AlH3/Al2O3core/shell structure material and modified C60The mass ratio of (A) to (B) is 5: 1; the volume ratio of toluene to tetrahydrofuran in the toluene/tetrahydrofuran mixed solvent is 2; the stirring and dispersing time is 4-12 h.
9. alpha-AlH according to claim 7 or 83/Al2O3/C60The method for synthesizing the compound with the double-shell structure is characterized in that the modified C60The preparation method comprises the following steps:
collecting 170mg of 4-carboxybenzaldehyde and 150mg of C60And 90mg sarcosine in turn in 50ml chlorobenzene; refluxing the chlorobenzene solution at 135 ℃ for 16h under nitrogen atmosphere; the solvent component in the product was removed by rotary evaporation to obtain a dark brown powder, which was then dispersed in a toluene/tetrahydrofuran mixed solvent (v/v ═ 2), and separated by silica gel column chromatography to obtain brown modified C60And (3) sampling.
10. alpha-AlH according to any one of claims 1 to 63/Al2O3/C60Use of a double shell structure composite for the preparation of a solid propellant fuel.
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| CN112441863A (en) * | 2020-11-27 | 2021-03-05 | 湖北航天化学技术研究所 | ADN/AlH3Composite microspheres, preparation method and solid propellant containing microspheres |
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| CN112441863B (en) * | 2020-11-27 | 2022-04-12 | 湖北航天化学技术研究所 | ADN/AlH3Composite microspheres, preparation method and solid propellant containing microspheres |
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