CN101734622A - Preparation method of hydrogen storage material of Li-Al-H complex hydride - Google Patents
Preparation method of hydrogen storage material of Li-Al-H complex hydride Download PDFInfo
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- CN101734622A CN101734622A CN200910156910A CN200910156910A CN101734622A CN 101734622 A CN101734622 A CN 101734622A CN 200910156910 A CN200910156910 A CN 200910156910A CN 200910156910 A CN200910156910 A CN 200910156910A CN 101734622 A CN101734622 A CN 101734622A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000001257 hydrogen Substances 0.000 title claims abstract description 39
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 39
- 150000004678 hydrides Chemical class 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000011232 storage material Substances 0.000 title abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000010936 titanium Substances 0.000 claims abstract description 6
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 abstract 4
- 150000004820 halides Chemical class 0.000 abstract 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 abstract 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 description 20
- 229910000103 lithium hydride Inorganic materials 0.000 description 20
- 229910010082 LiAlH Inorganic materials 0.000 description 14
- 238000003860 storage Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000003701 mechanical milling Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000012916 structural analysis Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- -1 lithium aluminum hydride Chemical compound 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a hydrogen storage material of Li-Al-H complex hydride, which comprises the following steps of: (1) mixing powdery high-purity Al, powdery high-purity LiH and a catalyst evenly under the protection of inert gas, wherein the mole ratio of the Al to the LiH is 1:1 or 1:3, the weight percent of the catalyst relative to the powder mixture of the Al and the LiH is 0-5%, and the catalyst is arbitrary one or arbitrary several of titanium, the halide of the titanium or the halide of cerium; (2) adding the powder mixture, a hard grinding ball and anhydrous tetrahydrofuran liquid into a ball milling tank; (3) introducing high-purity hydrogen gas into the sealed ball milling tank, wherein the pressure of the hydrogen gas is 5-15MPa; (4) carrying out mechanical ball milling for 5-15h; and (5) then, controlling the temperature of the ball milling tank at 60-70 DEG C and then carrying out vacuum pumping on the ball milling tank to remove tetrahydrofuran so as to obtain the hydrogen storage material. The invention has the advantages of no need for high temperature and high pressure, high utilization rate of raw materials, no generation of a by-product, simple operation, low cost and good safety.
Description
Technical field
The invention belongs to technical field of function materials, specifically is a kind of preparation method of coordinate hydride hydrogen-storing material.
Background technology
Along with the countries in the world rapid economy development, human society constantly increases the demand of the energy.Human society has caused energy shortage and two significant problems of environmental pollution to depending on unduly of fossil oil, and this forces people to remove to develop new clean energy.Because hydrogen has outstanding advantages such as products of combustion cleaning, resource be unlimited, Hydrogen Energy is considered to the important secondary clean energy of new millennium.And the storage of hydrogen is the Hydrogen Energy key in application.In recent years, the fuel cell car fast development, people have proposed very high requirement for automobile-used hydrogen storage system, and the target that International Energy Agency (IEA) proposes is the weight hydrogen-storage density greater than 5%, the volume hydrogen-storage density is greater than 50kgH
2/ m
3, and the target that USDOE (DOE) proposes is that the weight hydrogen-storage density is not less than 6.5%.Utilize the solid-state storage hydrogen mode of hydrogen storage material and H-H reaction generation hydride, because its distinctive security is considered to the most promising vehicle-mounted storage hydrogen mode with relative higher volume hydrogen-storage density.But the weight hydrogen-storage amount of traditional metal hydride is generally lower, and the reversible hydrogen storage capacity generally is lower than 2wt%, can't satisfy the requirement of application.
With NaAlH
4And Na
3AlH
6For the coordinate hydride hydrogen-storing material of representative because its higher weight hydrogen storage capability (NaAlH
4The theoretical weight hydrogen storage capability be 5.6%) be subjected to broad research in recent years.And Li is the lightest metallic element, and therefore, the Li-Al-H complex hydrides has the weight hydrogen storage capability higher than Na-Al-H complex hydrides, wherein, and LiAlH
4And Li
3AlH
6The theoretical weight hydrogen storage capability be respectively 10.5% and 11.1%, be a kind of tool hydrogen storage material with broad prospects for development, but they synthetic difficult, cost is high.
Wherein, LiAlH
4Main synthetic method have: 1) under high temperature, High Pressure Hydrogen condition that LiH, Al and H-H reaction is synthetic; 2) it is synthetic lithium hydride and aluminum trichloride (anhydrous) to be carried out following reaction in ether:
Above-mentioned synthetic method 1) shortcoming is to need high temperature, condition of high voltage, poor stability, cost height.Synthetic method 2) following shortcoming is arranged: when the reaction beginning, will add a small amount of lithium aluminum hydride as initiator; 3/4ths lithium hydride is converted into inexpensive lithium chloride in the reaction; Reaction has by product LiCl to generate, and need separate etc.
And Li
3AlH
6The preparation of complex hydrides generally need be adopted two-step approach, promptly earlier synthetic LiAlH
4, again by LiAlH
4Carrying out following reaction with LiH synthesizes:
LiAlH
4+2LiH→Li
3AlH
6 (2)
Summary of the invention
The new preparation method who the purpose of this invention is to provide a kind of Li-Al-H coordinate hydride hydrogen-storing material.
The present invention realizes that the technical scheme that above-mentioned purpose is taked is: the preparation method of this Li-Al-H coordinate hydride hydrogen-storing material mainly comprises the steps:
(1) under protection of inert gas, high-purity Al powder, LiH powder and powder catalyst are carried out uniform mixing, the mol ratio of described Al powder and LiH powder is 1: 1 or 1: 3, described catalyzer is 0～5% with respect to the weight percent of the powdered mixture of Al and LiH, described catalyzer be the halogenide of titanium, titanium or cerium halid any or appoint several;
(2) in ball grinder, add powdered mixture, hard abrading-ball and anhydrous tetrahydrochysene instep that step (1) the obtains liquid of muttering, then with this ball grinder sealing;
(3) feed high-purity hydrogen in the ball grinder after sealing, hydrogen pressure is 5～15MPa;
(4) ball grinder is placed carry out mechanical ball milling on the ball mill, the ball milling time is 5～15h;
(5) after ball milling is finished, the temperature of ball grinder is controlled at 60～70 ℃, the back vacuumizes the removal so that the tetrahydrochysene instep is muttered with vacuum pump to ball grinder, obtain described Li-Al-H coordinate hydride hydrogen-storing material.
Further, the present invention is in described step (2), and the anhydrous tetrahydrochysene instep liquid phase of muttering is 8～10 milliliters for the add-on of the powdered mixture of every gram Al and LiH; The mass ratio of the powdered mixture of described hard abrading-ball and described Al and LiH is 60～120: 1.
Further, the present invention also comprise between described step (2) and (3) with vacuum pump to the sealing after ball grinder outgas to remove the step of described rare gas element.
Compared with prior art, the invention has the beneficial effects as follows: (1) is compared with the high-temperature high-pressure chemical synthesis method, and the present invention prepares LiAlH
4Method can at room temperature carry out, security is good, energy consumption is low; (2) compare with the aluminum trichloride (anhydrous) reaction synthesis method with adopting lithium hydride, the present invention prepares LiAlH
4Method in lithium hydride utilization ratio height, no coupling product generate, need not to separate, simple to operate, cost is low; (3) the present invention can be by LiH and the synthetic Li of Al one step ball milling
3AlH
6, simple to operate, cost is low.
Description of drawings
Fig. 1 is the embodiment of the invention 1 synthetic LiAlH
4The X ray diffracting spectrum of complex hydrides.
Fig. 2 is the embodiment of the invention 2 synthetic LiAlH
4The hydrogen curve is put in the temperature programming of complex hydrides.
Fig. 3 is the embodiment of the invention 3 synthetic Li
3AlH
6The X ray diffracting spectrum of complex hydrides.
Fig. 4 is the embodiment of the invention 3 synthetic Li
3AlH
6The hydrogen desorption kinetics curve of complex hydrides.
Embodiment
Because raw material Li H that preparation Li-Al-H complex hydrides is used and Li-Al-H complex hydrides are easy and water and oxygen generation oxidizing reaction, involved raw material weighing and transfer in Li-Al-H complex hydrides preparation process, and in the structure of complex hydrides and performance test process involved sample weighing and shift and all in the atmosphere of rare gas element (for example high-purity argon), carry out.
In being filled with the glove box of high-purity argon gas, high-purity Al powder and LiH powder are pressed 1: 1 mol ratio uniform mixing, the powder gross weight is about 2 grams.The powdered mixture that obtains is put into sealable ball grinder with the hard abrading-ball, add 20 milliliters of anhydrous tetrahydrochysene insteps (THF) organic liquid of muttering, then ball grinder is sealed.In order to remove the trace water that the THF organic liquid may exist, before joining ball grinder, THF THF is handled and filters (following each embodiment is identical) with reguline metal calcium.Feed high-purity hydrogen (purity is 99.9999%) in the ball grinder after sealing, hydrogen pressure is 10MPa.For making the hydrogen purity in the ball grinder higher, can before feeding high-purity hydrogen, outgas to remove original rare gas element to ball grinder with vacuum pump.Then ball grinder is placed and carry out mechanical ball milling on the ball mill.Wherein, the hard abrading-ball is 90: 1 with the ratio (being ratio of grinding media to material) of the quality of high-purity Al powder and LiH powdered mixture, and the rotating speed of ball mill is 350rpm, and the ball milling time is 10 hours.After ball milling is finished, the temperature of ball grinder is controlled at 60～70 ℃, the back vacuumizes the removal so that the tetrahydrochysene instep is muttered with vacuum pump to ball grinder, can obtain LiAlH
4Coordinate hydride hydrogen-storing material.
The coordinate hydride hydrogen-storing material that adopts X-ray diffraction (XRD) to analyze obtaining carries out structural analysis.For guaranteeing sample and air insulated in XRD test analysis process, XRD specimen support has sealable protective guard (down together).Fig. 1 is synthetic LiAlH
4The XRD figure spectrum of complex hydrides.Analytical results shows, contains 70% LiAlH in the sample
4, the main chemical reactions that takes place in the mechanical milling process is as follows:
In being filled with the glove box of high-purity argon gas, high-purity Al powder and LiH powder are pressed 1: 1 mol ratio uniform mixing, the powder gross weight is about 2 grams.The employing metallic titanium powder is a catalyzer, and the addition of metallic titanium powder accounts for 2.5% of Al and LiH powdered mixture gross weight.Raw material powder mixture and catalyzer are put into sealable ball grinder with the hard abrading-ball, add 20 milliliters of anhydrous THF organic liquids of handling through calcium, then ball grinder is sealed.Ball grinder after the sealing is outgased to remove original rare gas element with vacuum pump, feed high-purity hydrogen (purity is 99.9999%) then, hydrogen pressure is 15MPa.Ball grinder placed carry out mechanical ball milling on the ball mill.Wherein, ratio of grinding media to material is 60: 1, and the rotating speed of ball mill is 350rpm, and the ball milling time is 15 hours.After ball milling is finished, the temperature of ball grinder is controlled at 60～70 ℃, the back vacuumizes the removal so that the tetrahydrochysene instep is muttered with vacuum pump to ball grinder, can obtain LiAlH
4Coordinate hydride hydrogen-storing material.Sample is carried out the temperature programmed control heating put the hydrogen test, the Heating temperature scope is heated to 400 ℃ by room temperature, and heat-up rate is 1 ℃/min.Fig. 2 is that the hydrogen curve is put in the heating of sample temperature programmed control.The result shows that the material hydrogen desorption capacity (weight percent) of preparation is reached for 6.31%, and initial hydrogen discharging temperature is about 120 ℃.
In being filled with the glove box of high-purity argon gas, high-purity Al powder and LiH powder are pressed 1: 3 mol ratio uniform mixing, the powder gross weight is about 1.5 grams.Add TiF
3And CeF
3As catalyzer, TiF
3And CeF
3Addition all account for 2.5% of Al and LiH powdered mixture gross weight.Raw material powder mixture and catalyzer are put into sealable ball grinder with the hard abrading-ball, add 12 milliliters of anhydrous THF organic liquids of handling through calcium, then ball grinder is sealed.Ball grinder after the sealing is outgased to remove original rare gas element with vacuum pump, feed high-purity hydrogen (purity is 99.9999%) then, hydrogen pressure is 5MPa.Ball grinder placed carry out mechanical ball milling on the ball mill.Wherein, ratio of grinding media to material is 120: 1, and the rotating speed of ball mill is 350rpm, and the ball milling time is 5 hours.After ball milling is finished, the temperature of ball grinder is controlled at 60～70 ℃, the back vacuumizes the removal so that the tetrahydrochysene instep is muttered with vacuum pump to ball grinder, can obtain Li
3AlH
6Coordinate hydride hydrogen-storing material.The coordinate hydride hydrogen-storing material that adopts X-ray diffraction (XRD) to analyze obtaining carries out structural analysis, and Fig. 3 is synthetic Li
3AlH
6The XRD figure spectrum of complex hydrides.Analytical results shows, contains the Li more than 90% in the sample
3AlH
6, the main chemical reactions that takes place in the mechanical milling process is as follows:
To synthetic Li
3AlH
6The complex hydrides sample adopts " constant volume pressure differential method " to put the hydrogen test, and Fig. 4 is that sample is put the hydrogen curve under 300 ℃ of conditions.The result shows that the hydrogen desorption capacity (weight percent) of prepared material under 300 ℃ of conditions is 3.28%.
Claims (3)
1. the preparation method of a Li-Al-H coordinate hydride hydrogen-storing material is characterized in that comprising the steps:
(1) under protection of inert gas, high-purity Al powder, LiH powder and powder catalyst are carried out uniform mixing, the mol ratio of described Al powder and LiH powder is 1: 1 or 1: 3, described catalyzer is 0～5% with respect to the weight percent of the powdered mixture of Al and LiH, described catalyzer be the halogenide of titanium, titanium or cerium halid any or appoint several;
(2) in ball grinder, add powdered mixture, hard abrading-ball and anhydrous tetrahydrochysene instep that step (1) the obtains liquid of muttering, then with this ball grinder sealing;
(3) feed high-purity hydrogen in the ball grinder after sealing, hydrogen pressure is 5～15MPa;
(4) ball grinder is placed carry out mechanical ball milling on the ball mill, the ball milling time is 5～15h;
(5) after ball milling is finished, the temperature of ball grinder is controlled at 60～70 ℃, the back vacuumizes the removal so that the tetrahydrochysene instep is muttered with vacuum pump to ball grinder, obtain described Li-Al-H coordinate hydride hydrogen-storing material.
2. the preparation method of Li-Al-H coordinate hydride hydrogen-storing material according to claim 1 is characterized in that: in described step (2), the anhydrous tetrahydrochysene instep liquid phase of muttering is 8～10 milliliters for the add-on of the powdered mixture of every gram Al and LiH; The mass ratio of the powdered mixture of described hard abrading-ball and described Al and LiH is 60～120: 1.
3. the preparation method of Li-Al-H coordinate hydride hydrogen-storing material according to claim 1 and 2 is characterized in that: also comprise between described step (2) and (3) with vacuum pump to the sealing after ball grinder outgas to remove the step of described rare gas element.
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|---|---|---|---|
| CN200910156910A CN101734622A (en) | 2009-12-24 | 2009-12-24 | Preparation method of hydrogen storage material of Li-Al-H complex hydride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920973A (en) * | 2010-09-02 | 2010-12-22 | 浙江大学 | Method for preparing porous aluminum diboride |
| CN102167286A (en) * | 2011-03-23 | 2011-08-31 | 浙江大学 | Multi-element light-weight coordination hydride hydrogen-storing material as well as preparation method and application thereof |
| CN102167284A (en) * | 2011-03-23 | 2011-08-31 | 浙江大学 | Light-metal composite hydrogen storage material and preparation method thereof |
| CN111498799A (en) * | 2020-06-09 | 2020-08-07 | 世能氢电科技有限公司 | Metal alanate composite hydrogen storage material and preparation method thereof |
-
2009
- 2009-12-24 CN CN200910156910A patent/CN101734622A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920973A (en) * | 2010-09-02 | 2010-12-22 | 浙江大学 | Method for preparing porous aluminum diboride |
| CN102167286A (en) * | 2011-03-23 | 2011-08-31 | 浙江大学 | Multi-element light-weight coordination hydride hydrogen-storing material as well as preparation method and application thereof |
| CN102167284A (en) * | 2011-03-23 | 2011-08-31 | 浙江大学 | Light-metal composite hydrogen storage material and preparation method thereof |
| CN102167284B (en) * | 2011-03-23 | 2012-11-28 | 浙江大学 | Light-metal composite hydrogen storage material and preparation method thereof |
| CN111498799A (en) * | 2020-06-09 | 2020-08-07 | 世能氢电科技有限公司 | Metal alanate composite hydrogen storage material and preparation method thereof |
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Open date: 20100616 |