CN102826510A - Synthesis method of metal deuterium storage material AlD3 powder - Google Patents
Synthesis method of metal deuterium storage material AlD3 powder Download PDFInfo
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- CN102826510A CN102826510A CN2012103579708A CN201210357970A CN102826510A CN 102826510 A CN102826510 A CN 102826510A CN 2012103579708 A CN2012103579708 A CN 2012103579708A CN 201210357970 A CN201210357970 A CN 201210357970A CN 102826510 A CN102826510 A CN 102826510A
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Abstract
The invention relates to a synthesis method of metal deuterium storage material AlD3 powder, and in particular relates to a synthesis method of AlD3, aiming at solving the technical problems that the existing synthesis method of AlH3 is strict for test operation requirements, the synthesized AlH3 is low in hydrogen storage content, and similar metal deuterium compounds are low in deuterium storage content and energy supply. The synthesis method comprises the following steps of: under the anhydrous condition, mixing AlCl3 with absolute ether solution of LiAlD4; then, adding a crystallization additive LiBH4 into the mixed solution; and drying under the vacuum condition to obtain the product AlD3. The synthesis method is simple in operation method; and the synthesized AlD3 powder is single in crystal form, high in deuterium storage content (about 15-20%) and more in energy supply, thus being an ideal metal deuterium storage material of high-energy solid propellants, solid-liquid hybrid propellants, composite propellants and the like, and being applied to fields of rocket propellants and scientific research.
Description
Technical field
The present invention relates to AlD
3Compound method.
Background technology
The developing direction of solid rocket propellant; Be to use composite solidpropellant; Compare with liquid propellant and hybrid propellant, SP all has superiority at aspects such as safety performance, unfailing performance, storge quality and low costs, and composite solidpropellant generally is made up of oxygenant, sizing agent, fuel and additive; Fuel is as the important component part in the composite solidpropellant; Play the effect that energy is provided, therefore the research to fuel in the composite solidpropellant seems particularly important, because AlH
3Excellent in performance, since the seventies, countries such as the U.S., Russia and Europe all begin with AlD
3Isotopic compound AlH
3The composite solidpropellant that acts as a fuel is studied.The existing patent No. is 201110176732 Chinese invention patent " catalyzer directed control LiH and AlCl
3The synthetic AlH of reaction
3Method ", this compound method avoids taking place side reaction through the level of response with tertiary amine control aluminum chloride and aluminum hydride, and is strict to test operation, be difficult for carrying out, though and this compound method reduced cost, the AlH that obtains through this compound method
3, hydrogen-storage amount is about 10%, and hydrogen-storage amount is not high, similar metal storage deuterate MgD
2Storage deuterium amount be about about 14%; Storage deuterium amount is not high yet; With being not enough to satisfy the raising along with weapon tactics index such as all kinds of strategy and tactics guided missiles, space vehicles, guided missile space vehicle and kinetic energy interception weapon are to the needs of composite solidpropellant fuel-efficient storage deuterium and energy supply.
AlD
3Belong to a kind of in the fuel, have toxicity little, contain that the deuterium amount is high, the combustion heat is high, can produce advantages such as gas, be desired metallic storage deuterium material as high-energy solid propellant, hybrid propellant, compositepropellent etc., up to now, relevant AlD
3Report seldom, synthetic rarely have the people to attempt especially, so for AlD
3Research very broad application prospect is arranged.
Summary of the invention
The present invention will solve existing AlH
3Compound method strict to test operation, and synthetic AlH
3Hydrogen-storage amount is not high, and similar metal storage deuterate storage deuterium amount is not high, the technical problem that energy supply is low, and a kind of metal storage deuterium materials A lD is provided
3The compound method of powder.
Metal storage deuterium materials A lD of the present invention
3The compound method of powder is carried out according to the following steps:
One, presses AlCl
3And LiAlD
4Mol ratio be 1: (2 ~ 4), AlCl
3And LiBH
4Mol ratio be 1: (0.5 ~ 10) takes by weighing AlCl
3, LiAlD
4And LiBH
4By anhydrous AlCl
3With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous AlCl
3Be dissolved in the anhydrous diethyl ether, obtain AlCl
3Solution; By anhydrous LiAlD
4With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous LiAlD
4Be dissolved in the anhydrous diethyl ether, obtain LiAlD
4Solution; By anhydrous LiBH
4With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous LiBH
4Be dissolved in the anhydrous diethyl ether, obtain LiBH
4Solution;
Two, the AlCl that step 1 is obtained
3Solution and LiAlD
4Solution mixes, and stirs 2 ~ 3min, and being heated to temperature then is 15 ~ 35 ℃, reaction 10 ~ 60min, and still aging again 1 ~ 6h filters then, obtains filtrating;
Three, the LiBH that step 1 is obtained
4Solution joins in the filtrating that step 2 obtains, and is under 15 ~ 30 ℃ of conditions in temperature, behind reaction 10 ~ 60min, filters, and is that vacuum-drying 4 ~ 6h obtains powder under 30 ~ 90 ℃ the condition in temperature with the solid formation that obtains;
Four, the powder that step 3 is obtained heats 1 ~ 6h in temperature is 60 ~ 80 ℃ oil bath, then with the anhydrous ether solution washing, under temperature was 30 ~ 90 ℃ condition, vacuum-drying 4 ~ 6h obtained AlD again
3Powder.
Metal storage deuterium materials A lD of the present invention
3The compound method of powder is carried out under anhydrous condition, will use AlCl earlier
3And LiAlD
4Anhydrous ether solution mix, add crystallization auxiliary LiBH then
4, dry under vacuum condition again, obtain product A lD
3Powder through the adding of LiBH4, can be controlled single crystal form β-AlD
3Generation, convenient change brilliant, synthetic metal storage deuterium materials A lD
3The powder inclusion-free, purity is high, and simple to operate, is swift in response, and productive rate can reach 85% ~ 95%, and productive rate is high, the AlD that is obtained by compound method of the present invention
3, storage deuterium amount is 15% ~ 20%, than existing metal storage hydrogen compound AlH as metal storage deuterium material
3Hydrogen-storage amount improved 5% ~ 10%, than similar metal storage deuterate MgD
2, storage deuterium amount has improved 0.7 ~ 5.7% approximately, though compare with metal storage deuterate LiD; Both have close storage deuterium amount, but it is very little with rate again to react the material that contains Li of generation by LiD, does not calculate economically; Do not meet the requirement of Green Chemistry, so the AlD that the present invention obtains
3Because it is high to have storage deuterium amount, the advantage that energy supply is big has satisfied the high-energy needs of guided missile space vehicle and kinetic energy interception weapon to composite solidpropellant fuel.The AlD that while compound method of the present invention obtains
3Also having combustion heat height, can produce advantages such as gas, is the desired metallic storage deuterium material as high-energy solid propellant, hybrid propellant, compositepropellent etc., aspect rocket propellant, has a wide range of applications.
Description of drawings
Fig. 1 is the AlD of test one
3The PND spectrogram and the β-AlD of powder
3Crystalline PND spectrogram comparison diagram, wherein a is the AlD of test one
3The PND curve of powder, b are β-AlD
3Crystalline PND curve;
Fig. 2 is the AlD of test one
3The SR-PXD spectrogram and the β-AlD of powder
3Crystalline SR-PXD spectrogram comparison diagram, wherein a is the AlD of test one
3The SR-PXD curve of powder, b are β-AlD
3Crystalline SR-PXD curve.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the metal storage deuterium materials A lD of this embodiment
3The compound method of powder is carried out according to the following steps:
One, presses AlCl
3And LiAlD
4Mol ratio be 1: (2 ~ 4), AlCl
3And LiBH
4Mol ratio be 1: (0.5 ~ 10) takes by weighing AlCl
3, LiAlD
4And LiBH
4By anhydrous AlCl
3With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous AlCl
3Be dissolved in the anhydrous diethyl ether, obtain AlCl
3Solution; By anhydrous LiAlD
4With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous LiAlD
4Be dissolved in the anhydrous diethyl ether, obtain LiAlD
4Solution; By anhydrous LiBH
4With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous LiBH
4Be dissolved in the anhydrous diethyl ether, obtain LiBH
4Solution;
Two, the AlCl that step 1 is obtained
3Solution and LiAlD
4Solution mixes, and stirs 2 ~ 3min, and being heated to temperature then is 15 ~ 35 ℃, reaction 10 ~ 60min, and still aging again 1 ~ 6h filters then, obtains filtrating;
Three, the LiBH that step 1 is obtained
4Solution joins in the filtrating that step 2 obtains, and is under 15 ~ 30 ℃ of conditions in temperature, behind reaction 10 ~ 60min, filters, and is that vacuum-drying 4 ~ 6h obtains powder under 30 ~ 90 ℃ the condition in temperature with the solid formation that obtains;
Four, the powder that step 3 is obtained heats 1 ~ 6h in temperature is 60 ~ 80 ℃ oil bath, then with the anhydrous ether solution washing, under temperature was 30 ~ 90 ℃ condition, vacuum-drying 4 ~ 6h obtained AlD again
3Powder.
The compound method of the metal storage deuterium materials A lD3 powder of this embodiment is carried out under anhydrous condition, will use AlCl earlier
3And LiAlD
4Anhydrous ether solution mix, add crystallization auxiliary LiBH then
4, dry under vacuum condition again, obtain product A lD
3Powder through the adding of LiBH4, can be controlled single crystal form β-AlD
3Generation, convenient change brilliant, synthetic metal storage deuterium materials A lD
3The powder inclusion-free, purity is high, and simple to operate, is swift in response, and productive rate can reach 85% ~ 95%, and productive rate is high, the AlD that is obtained by the compound method of this embodiment
3, storage deuterium amount is 15% ~ 20%, than existing metal storage hydrogen compound AlH as metal storage deuterium material
3Hydrogen-storage amount improved 5% ~ 10%, than similar metal storage deuterate MgD
2, storage deuterium amount has improved 0.7 ~ 5.7% approximately, though compare with metal storage deuterate LiD; Both have close storage deuterium amount, but it is very little with rate again to react the material that contains Li of generation by LiD, does not calculate economically; Do not meet the requirement of Green Chemistry, so the AlD that this embodiment obtains
3Because it is high to have storage deuterium amount, the advantage that energy supply is big has satisfied the high-energy needs of guided missile space vehicle and kinetic energy interception weapon to composite solidpropellant fuel.The AlD that the compound method of this embodiment of while obtains
3Also having combustion heat height, can produce advantages such as gas, is the desired metallic storage deuterium material as high-energy solid propellant, hybrid propellant, compositepropellent etc., aspect rocket propellant, has a wide range of applications.
Embodiment two: what this embodiment and embodiment one were different is: the anhydrous AlCl in the step 1
3With the mol ratio of anhydrous diethyl ether be 1: (10 ~ 15), anhydrous LiAlD
4With the mol ratio of anhydrous diethyl ether be 1: (10 ~ 15), anhydrous LiBH
4With the mol ratio of anhydrous diethyl ether be 1: (10 ~ 15), other step and parameter are different with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is: the AlCl in the step 2
3And LiAlD
4Mol ratio be 1:3, other step and parameter are different with embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one to three is: the Heating temperature in step 2 and the step 3 is 20 ~ 30 ℃; Be 20 ~ 40min heat-up time; Still aging again 1.5 ~ 5.5h, other step and parameter are different with one of embodiment one to three.
Embodiment five: what this embodiment was different with one of embodiment one to four is: the Heating temperature in step 2 and the step 3 is 25 ℃; Be 30min heat-up time; Still aging again 2h, other step and parameter are different with one of embodiment one to four.
Embodiment six: what this embodiment was different with one of embodiment one to five is: the AlCl in the step 3
3And LiBH
4Mol ratio be 1: (2 ~ 6), other step and parameter are different with one of embodiment one to five.
Embodiment seven: what this embodiment was different with one of embodiment one to six is: the vacuum-drying temperature in the step 3 is 35 ℃, vacuum-drying time 5h, and other step and parameter are different with one of embodiment one to six.
Embodiment eight: what this embodiment was different with one of embodiment one to seven is: the vacuum-drying temperature in the step 3 is 35 ℃; Oil bath temperature in vacuum-drying time 5h step 3 and the step 4 is 65 ℃; Be 2h heat-up time, and other step and parameter are different with one of embodiment one to seven.
Embodiment nine: what this embodiment was different with one of embodiment one to eight is: the oil bath temperature in step 3 and the step 4 is 65 ℃, and be 2h heat-up time, and other step and parameter are different with one of embodiment one to eight.
With following verification experimental verification beneficial effect of the present invention:
The compound method of the metal storage deuterium materials A lD3 powder of test one, this test formula is carried out according to the following steps: one, press AlCl
3And LiAlD
4Mol ratio be 1:3, AlCl
3And LiBH
4Mol ratio be 1:4, take by weighing AlCl
3, LiAlD
4And LiBH
4By anhydrous AlCl
3With the mol ratio of anhydrous diethyl ether be 1:12, with anhydrous AlCl
3Be dissolved in the anhydrous diethyl ether, obtain AlCl
3Solution; By anhydrous LiAlD
4With the mol ratio of anhydrous diethyl ether be 1:12, with anhydrous LiAlD
4Be dissolved in the anhydrous diethyl ether, obtain LiAlD
4Solution; By anhydrous LiBH
4With the mol ratio of anhydrous diethyl ether be 1:12, with anhydrous LiBH
4Be dissolved in the anhydrous diethyl ether, obtain LiBH
4Solution;
Two, the AlCl that step 1 is obtained
3Solution and LiAlD
4Solution mixes, and stirs 3min, and being heated to temperature then is 25 ℃, reaction 30min, and still aging again 2h filters then, obtains filtrating;
Three, the LiBH that step 1 is obtained
4Solution joins in the filtrating that step 2 obtains, and is under 25 ℃ of conditions in temperature, behind the reaction 30min, filters, and is that vacuum-drying 5h obtains powder under 35 ℃ the condition in temperature with the solid formation that obtains;
Four, the powder that step 3 is obtained heats 3h in temperature is 65 ℃ oil bath, then with the anhydrous ether solution washing, under temperature was 35 ℃ condition, vacuum-drying 5h obtained AlD again
3Powder.
The metal storage deuterium materials A lD of this test
3The compound method of powder is carried out under anhydrous condition, will use AlCl earlier
3And LiAlD
4Anhydrous ether solution mix, add crystallization auxiliary LiBH then
4, dry under vacuum condition again, obtain product A lD
3Powder through the adding of LiBH4, can be controlled single crystal form β-AlD
3Generation, convenient change brilliant, synthetic metal storage deuterium materials A lD
3The powder inclusion-free, purity is high, and simple to operate, is swift in response, and productive rate can reach 95%, and productive rate is high, the AlD that is obtained by the compound method of this test
3, storage deuterium amount is 18.1%, than existing metal storage hydrogen compound AlH as metal storage deuterium material
3Hydrogen-storage amount improved 8% approximately, than similar metal storage deuterate MgD
2, storage deuterium amount has improved 4% approximately, though compare with metal storage deuterate LiD; Both have close storage deuterium amount, but it is very little with rate again to react the material that contains Li of generation by LiD, does not calculate economically; Do not meet the requirement of Green Chemistry, so the AlD that this test obtains
3Because it is high to have storage deuterium amount, the advantage that energy supply is big has satisfied the high-energy needs of guided missile space vehicle and kinetic energy interception weapon to composite solidpropellant fuel.The AlD that the compound method of this test simultaneously obtains
3Also having combustion heat height, can produce advantages such as gas, is the desired metallic storage deuterium material as high-energy solid propellant, hybrid propellant, compositepropellent etc., aspect rocket propellant, has a wide range of applications.
Test two, to testing the AlD that obtains
3Powder carries out neutron powder diffraction (PND) test, and test is carried out according to the following steps:
With test one AlD that obtains
3Powder is placed on the JEEP II reactor drum on the PUS equipment, is under 22 ℃ the anhydrous condition in temperature, carries out the PND test, obtains testing one AlD
3The PND spectrogram and the β-AlD of powder
3Crystalline PND spectrogram comparison diagram, as shown in Figure 1, wherein the PUS equipment purchase is from Norway Kjeller company; The test neutron current is the neutron current of 1.5553 dusts for the wavelength that from the focal monochromator of Ge (511), obtains.
Can find out AlD by Fig. 1
3Diffraction peak has appearred in the PND curve of powder when 87.07 °, 92.93 °, 179.99 °, 180.00 ° and 136.83 °, contrast β-AlD
3Crystalline PND spectrogram is explained β-AlD
3Crystal is synthetic by successfully, and on the curve except above-mentioned diffraction peak, do not have other diffraction peaks; Proof test one synthetic efficient metal storage deuterium materials A lD3 powder; Impurity is few, and purity is high, in addition; The curve diffraction peak intensity is high, explains that test one synthetic efficient metal storage deuterium materials A lD3 powder crystallization property is good.
Test three, to testing the AlD that obtains
3Powder carries out synchrotron radiation X ray (SR-PXD) test, and test is carried out according to the following steps:
With test one AlD that obtains
3Powder is placed on the synchrotron radiation X ray appearance that model is BM01B, is under 22 ℃ the anhydrous condition in temperature, carries out the SR-PXD test, obtains testing one AlD
3The SR-PXD spectrogram and the β-AlD of powder
3Crystalline SR-PXD spectrogram comparison diagram, as shown in Figure 2, wherein testing tool is bought from the ESRF of Grenoble, France company; The test X ray is the X ray from 0.50059 dust that obtains from Si (111).
Can find out AlD by Fig. 2
3Diffraction peak has appearred in the SR-PXD curve of powder when 5.5970 °, 10.7645 °, 11.1755 °, 12.8375 °, 13.9915 °, 16.8320 ° and 18.2010 °, contrast β-AlD
3Crystalline SR-PXD spectrogram further specifies β-AlD
3Crystal is synthetic by successfully.
Claims (9)
1. metal stores up deuterium materials A lD
3The compound method of powder is characterized in that AlD
3Compound method carry out according to the following steps:
One, presses AlCl
3And LiAlD
4Mol ratio be 1: (2 ~ 4), AlCl
3And LiBH
4Mol ratio be 1: (0.5 ~ 10) takes by weighing AlCl
3, LiAlD
4And LiBH
4By anhydrous AlCl
3With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous AlCl
3Be dissolved in the anhydrous diethyl ether, obtain AlCl
3Solution; By anhydrous LiAlD
4With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous LiAlD
4Be dissolved in the anhydrous diethyl ether, obtain LiAlD
4Solution; By anhydrous LiBH
4With the mol ratio of anhydrous diethyl ether be 1: (5 ~ 20), with anhydrous LiBH
4Be dissolved in the anhydrous diethyl ether, obtain LiBH
4Solution;
Two, the AlCl that step 1 is obtained
3Solution and LiAlD
4Solution mixes, and stirs 2 ~ 3min, and being heated to temperature then is 15 ~ 35 ℃, reaction 10 ~ 60min, and still aging again 1 ~ 6h filters then, obtains filtrating;
Three, the LiBH that step 1 is obtained
4Solution joins in the filtrating that step 2 obtains, and is under 15 ~ 30 ℃ of conditions in temperature, behind reaction 10 ~ 60min, filters, and is that vacuum-drying 4 ~ 6h obtains powder under 30 ~ 90 ℃ the condition in temperature with the solid formation that obtains;
Four, the powder that step 3 is obtained heats 1 ~ 6h in temperature is 60 ~ 80 ℃ oil bath, then with the anhydrous ether solution washing, under temperature was 30 ~ 90 ℃ condition, vacuum-drying 4 ~ 6h obtained AlD again
3Powder.
2. metal storage deuterium materials A lD according to claim 1
3Compound method, it is characterized in that the anhydrous AlCl in the step 1
3With the mol ratio of anhydrous diethyl ether be 1: (10 ~ 15), anhydrous LiAlD
4With the mol ratio of anhydrous diethyl ether be 1: (10 ~ 15), anhydrous LiBH
4With the mol ratio of anhydrous diethyl ether be 1: (10 ~ 15).
3. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the AlCl in the step 2
3And LiAlD
4Mol ratio be 1:3.
4. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the Heating temperature in step 2 and the step 3 is 20 ~ 30 ℃, and be 20 ~ 40min heat-up time, still aging again 1.5 ~ 5.5h.
5. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the Heating temperature in step 2 and the step 3 is 25 ℃, and be 30min heat-up time, still aging again 2h.
6. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the AlCl in the step 3
3And LiBH
4Mol ratio be 1: (2 ~ 6).
7. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the AlCl in the step 3
3And LiBH
4Mol ratio be 1:4.
8. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the vacuum-drying temperature in the step 3 is 35 ℃, vacuum-drying time 5h.
9. metal storage deuterium materials A lD according to claim 1 and 2
3The compound method of powder is characterized in that the oil bath temperature in step 3 and the step 4 is 65 ℃, and be 3h heat-up time.
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Cited By (3)
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| CN104176751A (en) * | 2014-07-02 | 2014-12-03 | 北京理工大学 | Method for preparing aluminum trideuteride by high/medium/low-temperature pressurization direct process |
| CN112210818A (en) * | 2020-08-31 | 2021-01-12 | 北京理工大学 | Method for preparing single-crystal metal deuteride by movable zone melting |
| CN115215295A (en) * | 2022-06-29 | 2022-10-21 | 理道新材(北京)科技有限公司 | α-LiAlD 4 And method for preparing the same |
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| 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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| 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104176751A (en) * | 2014-07-02 | 2014-12-03 | 北京理工大学 | Method for preparing aluminum trideuteride by high/medium/low-temperature pressurization direct process |
| CN104176751B (en) * | 2014-07-02 | 2015-11-25 | 北京理工大学 | A kind of senior middle school low temperature pressurization direct method prepares the method for three deuterate aluminium |
| CN112210818A (en) * | 2020-08-31 | 2021-01-12 | 北京理工大学 | Method for preparing single-crystal metal deuteride by movable zone melting |
| CN112210818B (en) * | 2020-08-31 | 2021-07-20 | 北京理工大学 | Method for preparing single-crystal metal deuteride by movable zone melting |
| CN115215295A (en) * | 2022-06-29 | 2022-10-21 | 理道新材(北京)科技有限公司 | α-LiAlD 4 And method for preparing the same |
| CN115215295B (en) * | 2022-06-29 | 2023-08-22 | 理道新材(北京)科技有限公司 | α-LiAlD 4 And a method for preparing the same |
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| CN102826510B (en) | 2015-04-08 |
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