CN108083230A - A kind of preparation method of three aluminum hydride of high-quality - Google Patents
A kind of preparation method of three aluminum hydride of high-quality Download PDFInfo
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- CN108083230A CN108083230A CN201810030889.6A CN201810030889A CN108083230A CN 108083230 A CN108083230 A CN 108083230A CN 201810030889 A CN201810030889 A CN 201810030889A CN 108083230 A CN108083230 A CN 108083230A
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- aluminum hydride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Hydrogen, Water And Hydrids (AREA)
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Abstract
A kind of preparation method of three aluminum hydride of high-quality, includes the following steps：Under protective gas protection, three aluminum hydrides and organic amine and toluene solvant are fully reacted, it is three aluminum hydride of high-quality to filter dried solid product.It solves the problems such as uneven current common three aluminum hydrides size distribution, Luan Jing, glomerocryst phenomenon is serious, hole and crackle are more, there is preferable application prospect in solid propellant, catalyst, hydrogen storage material and fuel cell etc..
Description
Technical field
The invention belongs to technical field of material, more particularly to a kind of preparation method of three aluminum hydride of high-quality.
Background technology
Three aluminum hydride (AlH3) there is high hydrogen content (theoretical value 10.08%), there is the combustion heat compared with aluminium powder
It is high, flame temperature is low, into gas it is good the advantages that, be considered as the high-energy fuel for most having development potentiality, in solid propellant field quilt
It places high hopes, while also there is preferable application prospect in fields such as hydrogen storage material, fuel cell, catalyst.
But it is more etc. that common three aluminum hydride is commonly present uneven size distribution, Luan Jing, glomerocryst phenomenon serious, hole and crackle
Problem limits its extensive use, therefore, seeks three aluminum hydride of high-quality (epigranular, few surface defects, structural integrity etc.)
Preparation method be engaged in three aluminum hydride correlative studys work institute it is in the urgent need to address the problem of.
The content of the invention
In view of the deficiencies of the prior art, the present invention is intended to provide a kind of preparation method of three aluminum hydride of high-quality.
The technical scheme is that a kind of preparation method of three aluminum hydride of high-quality, concretely comprises the following steps：In protectiveness gas
Under body protection, organic amine is added in into common three aluminum hydride, adds toluene solvant, then heating, return stirring, afterwards quickly
It filters, filtered solid product is heated under vacuum to get to three aluminum hydride of high-quality.
Further, above-mentioned protective gas is the mixing of one or more of nitrogen, argon gas, helium.
Further, the amount that above-mentioned organic amine adds in is calculated as 0.1 times -15 times of three aluminum hydrides by the amount of substance.
Further, the amount that above-mentioned toluene solvant adds in is 0.5 times -20 times of the organic amine added in by volume.
Further, above-mentioned heating, the heating temperature of the operation to flow back are between 25 DEG C -65 DEG C, the time of return stirring
For 2h-20h.
Further, above-mentioned organic amine includes trimethylamine, N, N- dimethyl amines, N, N- diethyl methyl amines and N- methyl pyrroles
One or more in pyrrolidone.
Further, the time that above-mentioned filtered solid product heats under vacuum is 1h-20h.
Three aluminum hydride of high-quality that the present invention is prepared by chemical method has epigranular, few surface defects, structural integrity
The characteristics of waiting, can be efficiently applied to solid propellant, catalyst, hydrogen storage material and fuel cell etc..Producer of the present invention
Method is simple, production cost is low and safe and reliable.
Description of the drawings
From the detailed description below in conjunction with the accompanying drawings to the embodiment of the present invention, of the invention these and/or other aspects and
Advantage will become clearer and be easier to understand, wherein：
Attached drawing 1 is the scanning electron microscopy of three aluminum hydride of high-quality and common three aluminum hydride prepared by the embodiment of the present invention 1
The scanning electron microscope diagram that the comparison of mirror figure, wherein Fig. 1 (a) are amplified for the 400X of common three aluminum hydride, Fig. 1 (b) is common
The scanning electron microscope diagram of the 6000X amplifications of three aluminum hydrides；Fig. 1 (c) is three aluminum hydride of high product prepared by the embodiment of the present invention 1
400X magnified sweep electron microscope pictures, Fig. 1 (d) is that the 23990X of three aluminum hydride of high product prepared by the embodiment of the present invention 1 is put
Expose thoroughly electron microscope picture.
Fig. 2 is the infrared spectrum of three aluminum hydride of high-quality prepared by the embodiment of the present invention.
Specific embodiment
In order to which those skilled in the art is made to more fully understand the present invention, with reference to the accompanying drawings and detailed description to this hair
It is bright to be described in further detail.Here it is to be noted that it in the accompanying drawings, identical reference numeral imparting is substantially had
The component of same or like 26S Proteasome Structure and Function, and will omit on their repeated description.
Embodiment 1
Under helium protection, the N of 25mL is added in into common three aluminum hydrides of 0.2g, N- dimethyl amine solution adds
100mL toluene solvants, at 45 DEG C, return stirring 8h, then rapid filtration under suction, heated under vacuum of the solid product at 45 DEG C
5h is to get to three aluminum hydride of high-quality.
Embodiment 2
Under nitrogen protection, the N of 50mL is added in into common three aluminum hydrides of 0.5g, N- diethyl methyl amine solution adds
200mL toluene solvants, at 50 DEG C, return stirring 6h, then rapid filtration under suction, heated under vacuum of the solid product at 40 DEG C
6h is to get to three aluminum hydride of high-quality.
Fig. 2 is the infrared spectrum of three aluminum hydride of high-quality prepared by the embodiment of the present invention, as seen from Figure 2, high-quality
Three aluminum hydrides possess all characteristic feature absworption peaks of three aluminum hydrides, and free from admixture peak shows prepared by three aluminum hydride of high-quality
Cheng Zhong, does not introduce impurity, and purity is very high.Therefore, three aluminum hydride of high-quality is successfully prepared.
Fig. 1 is the scanning electron microscope diagram of three aluminum hydride of high-quality prepared by the embodiment of the present invention and common three aluminum hydride
Comparison, as seen from Figure 1, compared with common three aluminum hydride, epigranular, the shape of three aluminum hydride of high-quality are regular, basic
Without Luan Jing glomerocrysts phenomenon, surface is smooth, hole and crack defect are less, therefore the surface texture integrality of three aluminum hydride of high-quality
Common three aluminum hydride is superior to particle size uniformity.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.In the case of without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes will be apparent from for the those of ordinary skill in art field.Therefore, protection scope of the present invention should
This is subject to the protection scope in claims.
Claims (7)
1. a kind of preparation method of three aluminum hydride of high-quality, which is characterized in that the method is：
Under protective gas protection, organic amine is added in into common three aluminum hydride, adds toluene solvant, then heated, return
Stream stirring, afterwards rapid filtration under suction heat filtered solid product under vacuum to get to three aluminum hydride of high-quality.
2. preparation method as described in claim 1, which is characterized in that the protective gas is nitrogen, in argon gas, helium
One or more mixing.
3. preparation method as described in claim 1, which is characterized in that the amount that the organic amine adds in is calculated as three by the amount of substance
0.1 times -15 times of aluminum hydride.
4. preparation method as claimed in claim 3, which is characterized in that the amount that the toluene solvant adds in is by volume addition
0.5 times -20 times of organic amine.
5. preparation method as described in claim 1, which is characterized in that the heating, the heating temperature of the operation to flow back are 25
Between DEG C -65 DEG C, the time of return stirring is 2h-20h.
6. preparation method as described in claim 1, which is characterized in that the organic amine includes trimethylamine, N, N- dimethyl second
Amine, N, the one or more in N- diethyl methyl amines and N-Methyl pyrrolidone.
7. preparation method as described in claim 1, which is characterized in that the filtered solid product adds under vacuum
The time of heat is 1h-20h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810030889.6A CN108083230B (en) | 2018-01-12 | 2018-01-12 | Preparation method of high-quality aluminum trihydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810030889.6A CN108083230B (en) | 2018-01-12 | 2018-01-12 | Preparation method of high-quality aluminum trihydride |
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| Publication Number | Publication Date |
|---|---|
| CN108083230A true CN108083230A (en) | 2018-05-29 |
| CN108083230B CN108083230B (en) | 2020-03-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810030889.6A Active CN108083230B (en) | 2018-01-12 | 2018-01-12 | Preparation method of high-quality aluminum trihydride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019507A (en) * | 2018-09-03 | 2018-12-18 | 黎明化工研究设计院有限责任公司 | A method of improving three aluminium hydride thermostabilisations |
| CN111994871A (en) * | 2020-08-04 | 2020-11-27 | 湖北航天化学技术研究所 | Synthesis method of alpha-aluminum trihydride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006556A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Regeneration method of aluminum trihydride |
-
2018
- 2018-01-12 CN CN201810030889.6A patent/CN108083230B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006556A (en) * | 2015-08-24 | 2016-10-12 | 湖北航天化学技术研究所 | Regeneration method of aluminum trihydride |
Non-Patent Citations (2)
| Title |
|---|
| DAVID LACINA ET AL.: "Regeneration of aluminium hydride using dimethylethylamine", 《ENERGY ENVIRONMENTAL SCIENCE》 * |
| 万剑等: "有机胺控制AlCl3与LiH合成AlH3的研究", 《四川兵工学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019507A (en) * | 2018-09-03 | 2018-12-18 | 黎明化工研究设计院有限责任公司 | A method of improving three aluminium hydride thermostabilisations |
| CN109019507B (en) * | 2018-09-03 | 2021-11-05 | 黎明化工研究设计院有限责任公司 | Method for improving thermal stability of aluminum trihydride |
| CN111994871A (en) * | 2020-08-04 | 2020-11-27 | 湖北航天化学技术研究所 | Synthesis method of alpha-aluminum trihydride |
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| Publication number | Publication date |
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| CN108083230B (en) | 2020-03-27 |
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