CN106957047B - A kind of rotating crystal method of three aluminum hydrides - Google Patents
A kind of rotating crystal method of three aluminum hydrides Download PDFInfo
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- CN106957047B CN106957047B CN201710390747.6A CN201710390747A CN106957047B CN 106957047 B CN106957047 B CN 106957047B CN 201710390747 A CN201710390747 A CN 201710390747A CN 106957047 B CN106957047 B CN 106957047B
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- 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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Abstract
The invention discloses a kind of rotating crystal methods of three aluminum hydrides, comprising the following steps: under dry nitrogen atmosphere, three aluminum hydrides is taken to be added in solvent, stirring filters and removes insoluble impurity, obtains three hydrogenation aluminum solutions；It is ultrasonically treated again；It is then rotated, obtains three aluminum hydride solid particles；Three aluminum hydride solid particles are placed in air, is then dissolved, filtered, rotated, product is dried in vacuo to obtain the final product.A kind of rotating crystal method of three aluminum hydride provided by the invention, can will be converted into higher α-three aluminum hydride of stability in three aluminum hydrides with three aluminum hydrides existing for β and γ crystal form, at the same remove the impurity aluminum in three aluminum hydrides and remaining with three aluminum hydrides existing for unstable crystal form.Rotating crystal method of the invention turns brilliant high-efficient, turns brilliant mild condition, easily operated control.The purity of α-three aluminum hydride obtained after turning brilliant can reach 99% or more, can be stabilized in air atmosphere.
Description
Technical field
The present invention relates to a kind of rotating crystal methods of three aluminum hydrides, particularly belong to energetic material preparation technical field.
Background technique
Three aluminum hydride (AlH3), it is binary covalent hydride, volume hydrogen storage is 0.148kg H2/ L (2 times of liquid hydrogen density
It is more), quality hydrogen storage reaches 10.08%, hydrogen storage content with higher.Use fuel in three aluminum hydrides substitution conventional solid propellant
Aluminium powder, solid propellant can generate more heats and gas, and can significantly improve the specific impulse value of solid propellant.With important
Application value in army.
Three aluminum hydrides have heterogeneity.Three non-solvated aluminum hydrides have seven kinds of different crystal forms, i.e. α-AlH3、β-AlH3、
γ-AlH3、δ-AlH3、ε-AlH3、θ-AlH3、α’-AlH3, wherein three aluminum hydrides are with α-AlH3、β-AlH3And γ-AlH3Three kinds
Based on the presence of crystal form.In this seven kinds of crystal forms, α-AlH3With most stable of structure, can be stabilized in air, and
Three aluminum hydride properties of other crystalline structures are active, can react in the moisture in air discharge hydrogen and heat in air
Amount.Wherein θ-AlH3、α’-AlH3Crystal form is extremely unstable, if removing not in time, the aluminum hydride of polymorphic mixing is in air easily
Cause spontaneous combustion.Higher three aluminum hydride of activity certainly will will cause the liter of propellant sensitivity as fuel applications in solid propellant
Height causes the reduction of the stability of solid propellant, therefore, how to obtain three aluminum hydrides that can be stabilized in air,
Be three aluminum hydrides as fuel applications in the main difficulty of solid propellant.Currently, the method that three aluminum hydrides are stablized in acquisition is main
There are two types of, it is the cladding deactivation method of three aluminum hydrides and turn brilliant deactivation method of three aluminum hydrides respectively.
The method that a kind of three aluminum hydrides of cladding passivation are described in 105565262 A of Chinese patent application publication number CN, tool
Gymnastics work is with bicyclic diene (DCPD) for polymerization reaction monomer, by home position polymerization reaction, is formed in three hydrogenation aluminium surfaces poly-
The homopolymer of dicyclopentadiene (pDCPD) or the clad of copolymer, to realize the passivation of the insulation blocking to three aluminum hydrides
Method.Clad used in this method is the non-class clad containing energy, is carried out with such non-clad containing energy to three aluminum hydrides blunt
Change processing also reduces three aluminum hydrides simultaneously and adds as high energy although playing the purpose being passivated to three aluminum hydrides
High energy flow characteristic when agent.Brower F M et al. goes out a kind of high temperature rotating crystal method of three aluminum hydrides reported in the article, specifically
Operation is that three aluminum hydrides that will synthesize heat under nitrogen atmosphere protection, when temperature reaches 100 DEG C or so, β and
Three aluminum hydrides of γ crystal form are gradually converted into three aluminum hydride of α type, after high temperature turns brilliant processing 50h, three hydrogenations of β and γ crystal form
The ratio that aluminium is converted into three aluminum hydride of type is 80%.Although this method can gradually convert α for three aluminum hydrides of β and γ crystal form
Three aluminum hydride of type, but conversion ratio is lower, takes a long time.Therefore, a kind of turn of brilliant high-efficient, three hydrogenations of easily operated control are studied
The rotating crystal method of aluminium, it appears particularly necessary.
Summary of the invention
To solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of rotating crystal method of three aluminum hydrides, turn crystalline substance
It is high-efficient, turn brilliant mild condition, easily operated control.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of rotating crystal method of three aluminum hydrides, comprising the following steps: under dry inert gas atmosphere, take three hydrogen of polymorphic
Change aluminium, be added in solvent, stirring filters and removes insoluble impurity, obtains three hydrogenation aluminum solutions；It is rotated after sonicated,
Obtain three aluminum hydride granular crystal objects；Three aluminum hydride granular crystal objects are placed in air, using natural air to gained crystalline substance
Type carries out rolling oxidation, further removes trace impurity to reach, and then adds solvent and carries out secondary dissolution, filtering, revolving,
Product is dried in vacuo to obtain the final product.
Further, the rotating crystal method of aforementioned three aluminum hydride, comprising the following steps: under dry inert gas atmosphere, take
Three aluminum hydride of polymorphic is added in solvent, stirs 20min~30min, filters and removes insoluble impurity, obtains three hydrogenation aluminum solutions；
2~4h of ultrasonic treatment is carried out again；It is then rotated, obtains three aluminum hydride granular crystal objects；By three aluminum hydride granular crystal objects
It is placed in 1~3h in air, solvent is then added and carries out secondary dissolution, filtering, revolving, product is dried in vacuo i.e.
?.
In the rotating crystal method of aforementioned three aluminum hydride, the supersonic frequency of ultrasonic treatment is 50kHz~130kHz.It is cleaned by ultrasonic pond
Power is 150W.
In the rotating crystal method of aforementioned three aluminum hydride, it is 30%~50%RH's that three aluminum hydride granular crystal objects, which are placed in humidity,
In air.Three obtained aluminum hydride granular crystal objects are laid in glass surface ware, can remove other than α-three aluminum hydride with
Three aluminum hydrides existing for the unstable crystal form of δ, ε, θ and α ' four kind.
In the rotating crystal method of aforementioned three aluminum hydride, the mass volume ratio of polymorphic three aluminum hydrides and solvent are as follows: 5~10g ︰
200~400mL.
In the rotating crystal method of aforementioned three aluminum hydride, solvent is tetrahydrofuran or ether.Promote three aluminum hydrides in a solvent
Solubility, can further promote three aluminum hydrides turns brilliant rate.
In the rotating crystal method of aforementioned three aluminum hydride, product is subjected to vacuum drying and refers to that in vacuum degree be 320~490mmHg
Dry 2~5h under conditions of with 50~70 DEG C, finally obtains α-three aluminum hydride that purity is 99.9%.
It is used in the present invention and three aluminum hydride solid particles is placed in humidity for that can remove in the air of 30%~50%RH
Go α-three aluminum hydride three aluminum hydrides existing for the unstable crystal form of ' four kind with δ, ε, θ and α in addition.If humidity is too low, it is remaining not
Stable crystal form reacts slowly with water vapor in air, takes a long time.The excessively high reaction of humidity is very fast, and release heat is more, it is possible to create
Open fire causes chain reaction, there is certain risk.
Cell parameter between different crystal forms is different, when phase co-conversion it is required activation energy magnitude it is also different, need at this time
Change offer energy value by adjusting supersonic frequency.Therefore comprehensively consider, the supersonic frequency of final choice ultrasonic treatment of the present invention
Rate is 50kHz~130kHz, can be with the successful conversion between effective guarantee crystal form.
Two parts (quality A) will be divided into untreated three aluminum hydride of a batch, the crystalline substance being primarily present in three aluminum hydrides at this time
Type has α, β and γ, and three aluminum hydrides of portion are directly put in the air of 30%-50%RH, makes three hydrogenation existing for β and γ crystal form
Aluminium reacts completely with air, is filtered and recrystallizes after being dissolved in tetrahydrofuran or ether later, obtains the α that quality is B
Three aluminum hydrides, then quality is that the quality of β and γ in three aluminum hydrides of A is calculated as A-B.Another three aluminum hydride is by the method for the invention
It is C that tri- aluminum hydride quality of α is obtained after processing, is calculated as C-B from the quality that β and γ transformation of crystal is tri- aluminum hydride of α, turning brilliant efficiency can
Pass through formula C-B/A-B.It is computed, is up to 90% or more using the brilliant efficiency that turns of rotating crystal method of the present invention.
The presence of three aluminum hydride of β and γ crystal form makes three aluminum hydrides unstable in order to prevent in conventional method, mostly adopts
The passivation protection mode for taking cladding makes three aluminum hydride outer surfaces wrap up layer protecting film.Packet in addition to using energetic material on a small quantity
Mode is covered, most method for coating all there are problems that the averaged energy levels of three aluminum hydrides can be reduced.It will not in the present invention
Three aluminum hydride of stable crystal form is converted into three aluminum hydride of stable crystal form, and same matter energy will not change, and energy response will not
It changes.So that the method for the present invention three aluminum hydride obtained not only has characteristic stable under air atmosphere, simultaneously
The method of the present invention also has the advantages that not changing three aluminum hydride energy responses.
The invention has the beneficial effects that: a kind of rotating crystal method of three aluminum hydrides provided by the invention, it can be by three hydrogenations
It is converted into higher α-three aluminum hydride of stability with three aluminum hydrides existing for β and γ crystal form in aluminium, while being removed in three aluminum hydrides
Impurity aluminum and remaining with three aluminum hydrides existing for unstable crystal form.Rotating crystal method of the invention turns brilliant high-efficient, turns crystal bar
Part is mild, easily operated control.The purity of α-three aluminum hydride obtained after turning brilliant can reach 99% or more, can be in air atmosphere
In be stabilized.Compared to the conventional cladding passivation protection of three aluminum hydrides, not only had using the present invention three aluminum hydride obtained
There is characteristic stable under air atmosphere, while also having the advantages that not changing three aluminum hydride energy responses.The method of the present invention technique
Simply, easily operated control, institute is Ke Xunhuanliyong using solvent, and cost is relatively low.
Specific embodiment
The present invention will be further described below in conjunction with specific embodiments.
Agents useful for same is commercial product in the present invention.
Embodiment 1
A kind of rotating crystal method of three aluminum hydrides, comprising the following steps: under dry inert gas atmosphere, take three hydrogen of polymorphic
Change aluminium to be added in solvent, solvent is tetrahydrofuran, the mass volume ratio of polymorphic three aluminum hydrides and solvent are as follows: 5g ︰ 400mL is stirred
20min is mixed, filters and removes insoluble impurity, obtain three hydrogenation aluminum solutions；Ultrasonic treatment 2h, supersonic frequency 130kHz are carried out again；
It is then rotated, obtains three aluminum hydride granular crystal objects；It is 30%RH's that three aluminum hydride granular crystal objects, which are placed in humidity,
3h in air then adds solvent and carries out secondary dissolution, filtering, revolving, in vacuum degree is 490mmHg, 70 DEG C by product
Under the conditions of dry 2h up to three aluminum hydride 4.2g.X-ray diffraction test is carried out to brilliant three obtained aluminum hydrides are turned, as the result is shown institute
Obtaining α-three aluminum hydride proportion in three aluminum hydrides is 99.9%.
Embodiment 2
A kind of rotating crystal method of three aluminum hydrides, comprising the following steps: under dry inert gas atmosphere, take three hydrogen of polymorphic
Change aluminium to be added in solvent, solvent is ether, the mass volume ratio of polymorphic three aluminum hydrides and solvent are as follows: 10g ︰ 200mL, stirring
30min filters and removes insoluble impurity, obtains three hydrogenation aluminum solutions；Ultrasonic treatment 4h, supersonic frequency 50kHz are carried out again；Then
It is rotated, obtains three aluminum hydride granular crystal objects；Three aluminum hydride granular crystal objects are placed in the air that humidity is 50%RH
Middle 1h, then add solvent carry out it is secondary dissolution, filtering, revolving, by product vacuum degree be 320mmHg, 50 DEG C of condition
Lower dry 5h is up to three aluminum hydride 8.6g.X-ray diffraction test is carried out to brilliant three obtained aluminum hydrides are turned, as the result is shown gained three
α-three aluminum hydride proportion is 99.1% in aluminum hydride.
Embodiment 3
A kind of rotating crystal method of three aluminum hydrides, comprising the following steps: under dry inert gas atmosphere, take three hydrogen of polymorphic
Change aluminium to be added in solvent, solvent is tetrahydrofuran, the mass volume ratio of polymorphic three aluminum hydrides and solvent are as follows: 8g ︰ 300mL is stirred
25min is mixed, filters and removes insoluble impurity, obtain three hydrogenation aluminum solutions；Ultrasonic treatment 3h, supersonic frequency 100kHz are carried out again；
It is then rotated, obtains three aluminum hydride granular crystal objects；It is 40%RH's that three aluminum hydride granular crystal objects, which are placed in humidity,
2h in air then adds solvent and carries out secondary dissolution, filtering, revolving, in vacuum degree is 395mmHg, 60 DEG C by product
Under the conditions of dry 3.5h up to three aluminum hydride 7.1g.X-ray diffraction test is carried out to brilliant three obtained aluminum hydrides are turned, as the result is shown
α-three aluminum hydride proportion is 99.9% in three aluminum hydride of gained.
Embodiment 4
A kind of rotating crystal method of three aluminum hydrides, comprising the following steps: under dry inert gas atmosphere, take three hydrogen of polymorphic
Change aluminium to be added in solvent, solvent is ether, the mass volume ratio of polymorphic three aluminum hydrides and solvent are as follows: 6g ︰ 250mL, stirring
22min filters and removes insoluble impurity, obtains three hydrogenation aluminum solutions；Ultrasonic treatment 2.5h, supersonic frequency 120kHz are carried out again；
It is then rotated, obtains three aluminum hydride granular crystal objects；It is 35%RH's that three aluminum hydride granular crystal objects, which are placed in humidity,
2.5h in air, then add solvent carry out it is secondary dissolution, filtering, revolving, by product vacuum degree be 430mmHg, 65 DEG C
Under conditions of dry 2.5h up to three aluminum hydride 5.2g.X-ray diffraction test is carried out to brilliant three obtained aluminum hydrides are turned, is as a result shown
Show that α-three aluminum hydride proportion is 99.5% in three aluminum hydrides of gained.
Embodiment 5
A kind of rotating crystal method of three aluminum hydrides, comprising the following steps: under dry inert gas atmosphere, take three hydrogen of polymorphic
Change aluminium to be added in solvent, solvent is tetrahydrofuran, the mass volume ratio of polymorphic three aluminum hydrides and solvent are as follows: 9g ︰ 350mL is stirred
27min is mixed, filters and removes insoluble impurity, obtain three hydrogenation aluminum solutions；Ultrasonic treatment 3.5h, supersonic frequency 80kHz are carried out again；
It is then rotated, obtains three aluminum hydride granular crystal objects；It is 45%RH's that three aluminum hydride granular crystal objects, which are placed in humidity,
1.5h in air, then add solvent carry out it is secondary dissolution, filtering, revolving, by product vacuum degree be 380mmHg, 55 DEG C
Under conditions of dry 4h up to three aluminum hydride 8.2g.X-ray diffraction test is carried out to brilliant three obtained aluminum hydrides are turned, as the result is shown
α-three aluminum hydride proportion is 99.2% in three aluminum hydride of gained.
Claims (6)
1. a kind of rotating crystal method of three aluminum hydrides, it is characterised in that: the following steps are included: being taken under dry inert gas atmosphere
Three aluminum hydride of polymorphic is added in solvent, stirs 20min~30min, filters and removes insoluble impurity, obtains three hydrogenation aluminum solutions；
2~4h of ultrasonic treatment is carried out again；It is then rotated, obtains three aluminum hydride granular crystal objects；By three aluminum hydride granular crystal objects
It is placed in 1~3h in air, solvent is then added and carries out secondary dissolution, filtering, revolving, product is dried in vacuo i.e.
?.
2. the rotating crystal method of three aluminum hydride according to claim 1, it is characterised in that: the supersonic frequency of the ultrasonic treatment
For 50kHz~130kHz.
3. the rotating crystal method of three aluminum hydride according to claim 1, it is characterised in that: three aluminum hydride granular crystal objects are placed
In the air that humidity is 30%~50%RH.
4. the rotating crystal method of three aluminum hydride according to claim 1, it is characterised in that: three aluminum hydride of polymorphic and solvent
Mass volume ratio are as follows: 5~10g ︰, 200~400mL.
5. the rotating crystal method of three aluminum hydride according to claim 1, it is characterised in that: the solvent is tetrahydrofuran or second
Ether.
6. the rotating crystal method of three aluminum hydride according to claim 1, it is characterised in that: product is carried out vacuum drying and is referred to
Dry 2~5h under conditions of vacuum degree is 320~490mmHg and 50~70 DEG C.
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| CN109775663B (en) * | 2019-03-26 | 2022-11-04 | 哈尔滨工业大学 | Effective preservation method of aluminum trihydride etherate |
| CN112209344B (en) * | 2020-09-08 | 2022-08-19 | 西安近代化学研究所 | Method for removing alpha' crystal form aluminum trihydride |
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| RU2175637C2 (en) * | 1999-02-08 | 2001-11-10 | Российский Федеральный Ядерный Центр - Всероссийский Научно-Исследовательский Институт Экспериментальной Физики | Method of increasing thermal stability of aluminum hydride upon storage |
| CN102320569A (en) * | 2011-06-28 | 2012-01-18 | 哈尔滨工业大学 | Method for directionally controlling the reaction of LiH and AlCl3 with catalyst to synthesize A1H3 |
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