CN112209344B - Method for removing alpha' crystal form aluminum trihydride - Google Patents
Method for removing alpha' crystal form aluminum trihydride Download PDFInfo
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- CN112209344B CN112209344B CN202010932924.0A CN202010932924A CN112209344B CN 112209344 B CN112209344 B CN 112209344B CN 202010932924 A CN202010932924 A CN 202010932924A CN 112209344 B CN112209344 B CN 112209344B
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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
- C01B6/34—Purification; Stabilisation
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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
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The invention provides a method for removing alpha' crystal form aluminum trihydride, which comprises the following steps: taking aluminum trihydride to be purified, adding a solvent and uniformly mixing under an inert drying atmosphere; step two, transferring the mixed liquid uniformly mixed in the step one into a reaction kettle, sealing the reaction kettle, heating the reaction kettle to 100-160 ℃, and reacting at constant temperature; and step three, naturally cooling and filtering after the reaction is finished to obtain a product, namely the pure-phase alpha crystal form aluminum trihydride. The method of the invention can completely and thoroughly remove the alpha 'crystal form aluminum trihydride, and the finally obtained product has high purity which is all the alpha crystal form, and the alpha' crystal form can not be detected in the finally obtained product. The method of the invention uses less solvent, the reaction device is simple and easy to operate, and the obtained product has no alpha' crystal form aluminum trihydride. The method is mainly used for removing the alpha' crystal form aluminum trihydride.
Description
Technical Field
The invention belongs to the field of preparation of high-activity materials, relates to aluminum trihydride, and particularly relates to a method for removing alpha' crystal form aluminum trihydride.
Background
α-AlH 3 The hydrogen storage material is a binary covalent hydride, the mass hydrogen storage can reach 10.08 percent, the volume hydrogen storage is 0.148Kg/L (2 times of the liquid hydrogen density), the hydrogen storage material can be used as a hydrogen storage material due to higher hydrogen storage capacity, and in addition, the hydrogen storage material is a high-energy additive which is hopefully applied to a solid propellant formula due to higher combustion heat and specific impulse. According to theoretical calculations, AlH is used 3 The specific impulse of the solid propellant can be increased by at least 100N.s.kg instead of aluminum powder -1 And the temperature of the combustion chamber and the ejected gas is lower than that of aluminum powder-containing propellant AlH 3 Releases 10% of its own weight of H during decomposition 2 Effectively reducing the average molecular weight of the fuel gas, therefore, AlH 3 High-energy additives as solid propellants have become the focus of researchers at home and abroad.
α-AlH 3 Is AlH 3 The seven crystal forms (alpha, alpha', beta, gamma, epsilon, delta and zeta) have the most stable thermodynamic property, and are the only crystal form with application prospect in the propellant formula. However, the generation of alpha ' crystal form aluminum trihydride is often mixed in the preparation process of the alpha 0 crystal form aluminum trihydride, the alpha ' crystal form causes the thermal stability of the alpha crystal form aluminum trihydride to be poor, and the AlH is caused by the existence of the alpha ' impurity crystal form 3 The decomposition is accelerated under the condition of room temperature storage, the friction sensitivity of the sample is increased, particularly the influence on the static sensitivity is particularly obvious, and the alpha crystal form AlH has better crystal form 3 Compared with the prior art, the difference of E50 is 5-10 times. The influence on the sensitivity of propellant slurry is more obvious, and AlH with poorer crystal form is added 3 The impact sensitivity and the friction sensitivity of the propellant slurry are increased rapidly, and the requirement of charging is difficult to meet. Li Lei et al, Hubei research institute of space and chemical technology, propose to adopt the flotation method to remove the impurity crystal form, this method needs to adopt a large amount of flotation agents oleic acid, linoleic acid, linolenic acid, etc., and the stratification limit is difficult to control, the operating unit is more tedious. Therefore, it is very desirable to remove the alpha' form of aluminum trihydride from the alpha form of aluminum trihydride by an efficient method.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for removing alpha 'crystal form aluminum trihydride, and solve the technical problem that the alpha' crystal form aluminum trihydride is not completely removed in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for removing alpha' crystal form aluminum trihydride, the method comprising the steps of:
taking aluminum trihydride to be purified, adding a solvent and uniformly mixing under an inert drying atmosphere;
step two, transferring the mixed liquid uniformly mixed in the step one into a reaction kettle, sealing the reaction kettle, heating the reaction kettle to 100-160 ℃, and reacting at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished, and obtaining a product, namely the pure-phase alpha crystal form aluminum trihydride.
The invention also has the following technical characteristics:
the uniform mixing is realized by ultrasonic wave.
The solvent is toluene, cyclohexane or benzene.
The mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 0.5 g-1.0 g: 15ml to 18 ml.
The reaction kettle is put in an oven to be heated.
The constant temperature reaction time is 6-10 h.
Specifically, the method comprises the following steps:
taking aluminum trihydride to be purified, adding a solvent, and uniformly mixing by ultrasonic waves in an inert dry atmosphere;
the solvent is toluene, cyclohexane or benzene;
the mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 0.5 g-1.0 g: 15ml to 18 ml;
step two, transferring the mixed liquid uniformly mixed in the step one to a reaction kettle, sealing the reaction kettle, placing the reaction kettle in a drying oven, heating to 100-160 ℃, and reacting for 6-10 h at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished, and obtaining a product, namely the pure-phase alpha crystal form aluminum trihydride.
Preferably, the method is carried out according to the following steps:
taking aluminum trihydride to be purified, adding a solvent toluene in an inert drying atmosphere, and uniformly mixing by ultrasonic waves;
the mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 0.8 g: 16ml of the solution;
step two, transferring the mixed liquid uniformly mixed in the step one to a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, heating to 140 ℃, and reacting for 8 hours at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished to obtain a product, namely the pure-phase alpha crystal form aluminum trihydride.
Compared with the prior art, the invention has the following technical effects:
the method of the invention (I) can completely and thoroughly remove the alpha 'crystal form aluminum trihydride, the finally obtained product has high purity which is all alpha crystal form, and the alpha' crystal form can not be detected in the finally obtained product.
The method of the invention has the advantages of small solvent amount, simple reaction device and easy operation, and the obtained product has no alpha' crystal form aluminum trihydride. The method is mainly used for removing the alpha' crystal form aluminum trihydride.
Drawings
FIG. 1 is an XRD pattern of aluminum trihydride to be purified.
FIG. 2 is an XRD pattern of the product of the present invention after removal of the alpha' form of aluminum trihydride, i.e., the XRD pattern of pure phase alpha form of aluminum trihydride.
The present invention will be explained in further detail with reference to examples.
Detailed Description
In the invention, the structure and phase composition of a sample are determined by X-ray diffraction (XRD) analysis, a Japanese physical D/MAX-2400 type X-ray powder diffractometer is adopted, and an X-ray source is Cu K α Wavelength of light
The tube voltage is 40KV, the tube current is 80mA, the scanning range 2 theta is 3-90 degrees, and the step length is 0.02 degree.
In the invention, the aluminum trihydride to be purified is alpha crystal form aluminum trihydride containing alpha' crystal form.
The present invention is not limited to the following embodiments, and equivalent changes made on the basis of the technical solutions of the present invention fall within the scope of the present invention.
Example 1:
this example presents a process for removing the aluminum trihydride in the α' form, carried out according to the following steps:
taking aluminum trihydride to be purified, adding a solvent toluene, and uniformly mixing by ultrasonic waves in an inert drying atmosphere;
the aluminum trihydride to be purified has a purity of 99.0 wt.%, i.e., contains 1.0 wt.% of the α' crystalline form aluminum trihydride.
The mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 0.8 g: 16ml of the solution;
step two, transferring the mixed liquid uniformly mixed in the step one to a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, heating to 140 ℃, and reacting for 8 hours at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished, and obtaining a product, namely the pure-phase alpha crystal form aluminum trihydride.
And (3) analyzing the purity of the product:
FIG. 1 is an XRD pattern of aluminum trihydride to be purified, which pattern is such that α -AlH appears except at 27.70 °, 38.55 °, 40.54 °, 46.11 °, 49.76 °, 57.06 °, 63.00 °, 66.01 °, 67.96 °, 72.24 °, 73.74 °, 82.51 °, 86.03 °, 87.50 ° of 2 θ 3 The characteristic diffraction peak shows alpha' -AlH at 2 theta of 15.74 degrees, 26.98 degrees and 42.19 degrees 3 Characteristic diffraction peaks.
FIG. 2 is an XRD pattern of the product of the invention after the removal of the alpha' crystal form aluminum trihydride, i.e. a pure phase alpha crystal form aluminum trihydride XRD pattern, which shows that alpha-AlH appears only at the positions of 27.70 degrees, 38.55 degrees, 40.54 degrees, 46.11 degrees, 49.76 degrees, 57.06 degrees, 63.00 degrees, 66.01 degrees, 67.96 degrees, 72.24 degrees, 73.74 degrees, 82.51 degrees, 86.03 degrees and 87.50 degrees of 2 theta 3 Characteristic diffraction peaks and no other impurity peaks appear.
The analysis from fig. 1 and 2 shows that the alpha' form of aluminum trihydride can be completely removed using the process of this example.
Example 2:
this example shows a process for removing aluminum trihydride in the α' form, which is carried out according to the following steps:
taking aluminum trihydride to be purified, adding a solvent toluene in an inert drying atmosphere, and uniformly mixing by ultrasonic waves;
the aluminum trihydride to be purified has a purity of 99.0 wt.%, i.e., contains 1.0 wt.% of aluminum trihydride in the α' crystal form.
The mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 0.5 g: 15 ml;
step two, transferring the mixed liquid uniformly mixed in the step one to a reaction kettle, sealing the reaction kettle, placing the reaction kettle in a drying oven, heating to 100 ℃, and reacting for 10 hours at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished to obtain a product, namely the pure-phase alpha crystal form aluminum trihydride.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 3:
this example presents a process for removing the aluminum trihydride in the α' form, carried out according to the following steps:
taking aluminum trihydride to be purified, adding a solvent toluene, and uniformly mixing by ultrasonic waves in an inert drying atmosphere;
the aluminum trihydride to be purified has a purity of 99.0 wt.%, i.e., contains 1.0 wt.% of the α' crystalline form aluminum trihydride.
The mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 1.0 g: 18 ml;
step two, transferring the mixed liquid uniformly mixed in the step one into a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, heating to 160 ℃, and reacting for 6 hours at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished, and obtaining a product, namely the pure-phase alpha crystal form aluminum trihydride.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 4:
this example shows a method for removing α 'form aluminum trihydride, which is substantially the same as the method for removing α' form aluminum trihydride of example 1 except that the solvent in this example is equal amount of cyclohexane.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 5:
this example shows a method for removing alpha 'form aluminum trihydride, which is substantially the same as the method for removing alpha' form aluminum trihydride of example 1 except that the solvent in this example is an equal amount of benzene.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 6:
this example shows a method for removing α ' crystal form aluminum trihydride, which is substantially the same as the method for removing α ' crystal form aluminum trihydride in example 1, except that the purity of aluminum trihydride to be purified in this example is 99.1 wt.%, i.e., 0.9 wt.% of α ' crystal form aluminum trihydride is contained.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 7:
this example shows a method for removing α ' form aluminum trihydride, which is substantially the same as the method for removing α ' form aluminum trihydride of example 1 except that the purity of aluminum trihydride to be purified in this example is 99.2 wt.%, i.e., it contains 0.8 wt.% of α ' form aluminum trihydride.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 8:
this example shows a method for removing α ' form aluminum trihydride, which is substantially the same as the method for removing α ' form aluminum trihydride of example 1 except that the purity of aluminum trihydride to be purified in this example is 99.5 wt.%, i.e., it contains 0.5 wt.% of α ' form aluminum trihydride.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Example 9:
this example shows a method for removing α ' form aluminum trihydride, which is substantially the same as the method for removing α ' form aluminum trihydride of example 1 except that the purity of aluminum trihydride to be purified in this example is 99.9 wt.%, i.e., it contains 0.1 wt.% of α ' form aluminum trihydride.
The product purity analysis of this example is essentially the same as example 1, indicating that alpha' form aluminum trihydride can be completely removed using the method of this example.
Claims (1)
1. A method for removing alpha' crystal form aluminum trihydride, characterized in that the method is carried out according to the following steps:
taking aluminum trihydride to be purified, adding a solvent toluene in an inert drying atmosphere, and uniformly mixing by ultrasonic waves;
the mass volume ratio of the aluminum trihydride to be purified to the solvent is as follows: 0.8 g: 16ml of the solution;
step two, transferring the mixed liquid uniformly mixed in the step one to a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, heating to 140 ℃, and reacting for 8 hours at constant temperature;
and step three, naturally cooling and filtering after the reaction is finished to obtain a product, namely the pure-phase alpha crystal form aluminum trihydride.
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| US10435297B2 (en) * | 1999-06-16 | 2019-10-08 | Ardica Technologies, Inc. | Crystallization and stabilization in the synthesis of microcrystalline alpha alane |
| US6984746B2 (en) * | 2004-04-05 | 2006-01-10 | Alliant Techsystems Inc. | Method for the production of α-alane |
| CN106957047B (en) * | 2017-05-27 | 2019-03-29 | 河南纳宇新材料有限公司 | A kind of rotating crystal method of three aluminum hydrides |
| CN106986306B (en) * | 2017-05-27 | 2019-03-29 | 河南纳宇新材料有限公司 | A kind of preparation method of high-purity α-three aluminum hydride |
| CN109734053B (en) * | 2019-03-26 | 2022-03-01 | 哈尔滨工业大学 | Aluminum trihydride preparation method based on recycling of ether solvent |
| CN110550607B (en) * | 2019-09-12 | 2021-06-11 | 湖北航天化学技术研究所 | alpha-AlH 3 flotation method and application thereof |
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| AlH3热分解释氢机理研究进展;蔚明辉;《固体火箭技术》;20200415;全文 * |
| 三氢化铝乙醚配合物的稳定性及其固相转晶制备α-三氢化铝(英文);朱朝阳等;《应用化学》;20191231(第009期);全文 * |
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