CN104016302B - A kind of rare earth alloy slurries hydrogen-storing device and hydrogen storage method thereof - Google Patents
A kind of rare earth alloy slurries hydrogen-storing device and hydrogen storage method thereof Download PDFInfo
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- CN104016302B CN104016302B CN201410239807.0A CN201410239807A CN104016302B CN 104016302 B CN104016302 B CN 104016302B CN 201410239807 A CN201410239807 A CN 201410239807A CN 104016302 B CN104016302 B CN 104016302B
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Abstract
The invention discloses a kind of rare earth alloy slurries hydrogen-storing device and hydrogen storage method thereof; This device comprises hydrogen source bottle 1, pipeline 2, also comprise autoclave 3, hydrogen storehouse 4, thermocouple 6, agitating device 7, on autoclave 3, be provided with hydrogen source and be filled with interface 31, exhaust outlet 32, vacuum drawn interface 33, charge door 34 and discharging opening 35, thermocouple is arranged in autoclave, and described hydrogen storehouse, hydrogen source are filled with on mouth, exhaust outlet, vacuum drawn interface and are respectively arranged with Pressure gauge or pressure sensor; The step of the method: vacuumize → priming reaction → making of → charging slurries → hydrogen abstraction reaction → detection → discharging; Its advantage is, solve preferably pipeline blockage that solid rare earth alloy hydrogen storage technology causes and the container problem such as break, it releases hydrogen efficiency deficiency on the low side to have overcome liquid storage hydrogen, by the adjusting of slurries middle rare earth alloy and organic solvent, change rare earth alloy slurries system performance, provide battery material for making large-capacity and high-performance battery.
Description
Technical field:
The present invention relates to a kind of energy storage device and energy storage method of battery material, relate in particular to the storage hydrogen of terres rares battery materialDevice and hydrogen storage method thereof are specifically a kind of rare earth alloy slurries hydrogen-storing device and hydrogen storage method thereof.
Background technology:
Along with the day by day exhausted of the resource such as Global Oil, coal and the raising day by day to environmental protection requirement, national governments have dropped intoSubstantial contribution is developed new clean energy resource, and wherein Hydrogen Energy is to have an optimistic view of the most and the new forms of energy of tool potentiality, and various countries scholar generally believes21 century will be Hydrogen Energy century, and propose the new ideas of " hydrogen economy ". Hydrogen is a kind of complete free of contamination desirable energy and material,There is unit mass heat higher than high-energy-density more than gasoline twice. But in Hydrogen Energy Application and Development, its range of application expandsLarge to the energy, chemical industry, electronics, aerospace, military affairs and civilian various aspects. Wherein, in Ni-MH battery and fuel cell, obtainThe most widely application. Ni-MH battery and fuel cell are the first-selected power of novel electric vehicle, along with electric environment protecting and mixing are movedThe marketization of power automobile, has proposed the requirement of large-capacity and high-performance to Ni-MH battery and fuel cell, hydrogen storage material is also carried simultaneouslyRequirements at the higher level are gone out. Known to the applicant, current high performance rare earth is the fabulous storage hydrogen of manufacturing Ni-MH battery and fuel cellMaterial. But, for how by hydrogen energy storage in rare earth alloy, become the battery material of large-capacity and high-performance, be thisThe great research and development problem of the jumbo rare earth hydrogen storage battery of industry exploitation high-performance material. The hydrogen of rare earth storage at present mainly contains solidRare earth alloy storage hydrogen (also claiming hydride hydrogen-storing or alloy storage hydrogen) and liquid storage hydrogen mode: solid rare earth storage hydrogen, this rare earthHydrogen bearing alloy, normally adopts grinding technique, offers user by collecting with packaging with the form of dry powder. Because this storage hydrogen closesGold battery material is a kind of Powdered, exists the easy expansion of volume often to cause pipeline blockage and container to break, and has the capacity of heat transmission poorEtc. problem. And liquid storage hydrogen is temperature required higher owing to adding dehydrogenation reaction, the actual hydrogen efficiency of releasing is on the low side, thereby exists cost highThe problem that hydrogen utilization rate is low.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of rare earth alloy slurries hydrogen-storing device and hydrogen storage method thereof, this storage hydrogen dressPut and method can solve simple solid rare earth alloy hydrogen storage battery material in engineering application because alloy pulverization and volumetric expansion are madeThe problems such as the pipeline blockage becoming and container break, and it is temperature required higher owing to adding dehydrogenation reaction to overcome liquid storage hydrogen, actual releasingThe deficiency that hydrogen efficiency is on the low side.
One of technical solution of the present invention is, a kind of rare earth alloy slurries liquid hydrogen-storing device with following structure is provided,This device comprises hydrogen source bottle, pipeline, it is characterized in that, also comprises autoclave, hydrogen storehouse, thermocouple, agitating device, instituteOn the autoclave of stating, be provided with hydrogen source and be filled with interface, exhaust outlet, vacuum drawn interface, charge door and discharging opening, describedThermocouple is arranged in autoclave, and described hydrogen storehouse, hydrogen source are filled with on mouth, exhaust outlet, vacuum drawn interface and are respectively arranged withPressure gauge or pressure sensor.
As technique scheme supplement and perfect, the present invention also has following feature and advantage:
In described thermocouple 6, connect an AD converter I. AD converter is set, and is mainly in order can enough to connect with computerConnect.
Described agitating device 7 connects an AD converter II. AD converter is set, and is mainly in order can enough to connect with computerConnect.
The pressure sensor connecting on described hydrogen storehouse is pressure sensor I.
It is pressure sensor II that described hydrogen source is filled with mouthful pressure sensor connecting.
The pressure sensor that described exhaust outlet connects is pressure sensor III.
The pressure sensor that described vacuum drawn interface connects is pressure sensor IV.
Described pressure sensor I, II, III, IV and AD converter I and AD converter II are by I/O interface and calculatingMachine connects. Arranging like this, is mainly to realize computer controlled automatic operation.
Two of technical solution of the present invention is to utilize above-mentioned rare earth alloy slurries hydrogen-storing device to store up rare earth alloy slurriesThe method of hydrogen. The method comprises the steps:
(1) charging: rare earth alloy material powder is added in autoclave;
(2) vacuumize: autoclave is vacuumized;
(3) priming reaction: be filled with high-purity hydrogen in autoclave, rare earth alloy is repeatedly lived under the effect of hydrogenChange reaction;
(4) make slurries: in autoclave, add toluene, and start mixer raw material in still is stirred, make in still rareSoil alloy raw material forms slurries;
(5) hydrogen abstraction reaction: be heated to 250-350 DEG C in autoclave, stir and constantly to reactor supplemental hydrogen simultaneously constantlyGas, makes slurries constantly carry out hydrogen abstraction reaction;
(6) detect: the product after above-mentioned steps hydrogen abstraction reaction is sampled to detection;
(7) discharging: detect and reach standard-required, get final product discharging.
The present invention has the following advantages:
The present invention has not only solved the pipe that solid rare earth alloy hydrogen storage technology causes because of alloy pulverization and volumetric expansion in engineering applicationProblem that road is stopped up and container breaks etc., overcoming liquid, to store up hydrogen temperature required higher owing to adding dehydrogenation reaction, and it is actual that to release hydrogen efficiency on the low sideDeficiency, by the adjusting of slurries middle rare earth alloy and organic solvent, changed rare earth alloy slurries system performance, make its storage hydrogenAmount greatly improves, and provides battery material for making large-capacity and high-performance battery.
Brief description of the drawings:
Fig. 1 is rare earth alloy slurries hydrogen-storing device structural representation of the present invention.
Shown in figure: 1, hydrogen source bottle, 2, pipeline, 3, autoclave, 31, hydrogen source is filled with interface, 32, exhaust outlet,33, vacuum drawn interface, 34, charge door, 35, discharging opening, 4, hydrogen storehouse, 5, computer, 51, I/O interface, 6,Thermocouple, 61, AD converter I, 7, agitating device, 71, AD converter II, 81, pressure sensor I, 82, pressureSensor II, 83, pressure sensor III, 84, pressure sensor IV.
Detailed description of the invention:
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
As shown in Figure 1, a kind of rare earth alloy slurries liquid hydrogen-storing device, this device comprises hydrogen source bottle 1, pipeline 2, its feature existsIn, also comprise an autoclave 3, hydrogen storehouse 4, thermocouple 6, agitating device 7. Described agitating device 7 be by motor andPaddle forms, and described paddle is put 7 and entered in autoclave 3. On described autoclave 3, being provided with hydrogen source is filled withInterface 31, exhaust outlet 32, vacuum drawn interface 33 and charge door 34 and discharging opening 35, described thermocouple 6 is arranged on heightPress in reactor 3, described hydrogen storehouse 4 is connected with Pressure gauge or pressure sensor I81, and described hydrogen source is filled with mouth 31 and is connected with pressurePower table or pressure sensor II82, described exhaust outlet 32 is connected with Pressure gauge or pressure sensor III83, described vacuum drawnInterface 33 is connected with Pressure gauge or pressure sensor IV84. In described thermocouple 6, connect AD converter I61. Described stirsMix device 7 and connect AD converter II71. Described pressure sensor I, II, III, IV and AD converter I and AD conversionDevice III is connected with computer 5 by I/O interface 51.
Two of technical solution of the present invention is to utilize above-mentioned rare earth alloy slurries hydrogen-storing device to store up rare earth alloy slurriesThe method of hydrogen. The method comprises the steps:
(1) charging: rare earth alloy material powder is added in autoclave;
(2) vacuumize: autoclave is vacuumized;
(3) priming reaction: be filled with high-purity hydrogen in autoclave, rare earth alloy is repeatedly lived under the effect of hydrogenChange reaction; Requiring hydrogen purity is 99.99%; Add after hydrogen, make still internal pressure rise to 5.0-5.5Mpa;
(4) make slurries: in autoclave, add toluene, and start mixer raw material in still is stirred, make in still rareSoil alloy raw material forms slurries; The addition of toluene is to be 1 by the mass ratio of rare earth alloy powder and toluene: 2.5-3, stirring turnsSpeed is not less than 1000r.P.m;
(5) hydrogen abstraction reaction: heat by thermocouple, make reaction under high pressure temperature in the kettle rise to 250-350 DEG C, stir simultaneously constantly andConstantly, to reactor hydrogen make-up, make slurries constantly carry out hydrogen abstraction reaction; Require speed of agitator to be not less than 1000r.P.m;
(6) detect: the product after above-mentioned steps hydrogen abstraction reaction is sampled to detection; Quality requirement is the slurries rare earth in reactorAlloy is fully inhaled hydrogen to saturation state;
(7) discharging: reach standard-required, get final product discharging.
Embodiment
The present embodiment is to operate under computer controlled automatic:
(1) charging: take 10 kilograms of rare earth alloy material powders and add autoclave;
(2) vacuumize: by computer control evacuator, to autoclave extracting vacuum; Make to be in autoclave trueDummy status;
(3) activation: by computer controlled hydrogen manufacturing storehouse, be slowly filled with high-purity hydrogen in autoclave, hydrogen purity requirement is99.99%; Add after hydrogen, still internal pressure increases, and is 5.0Mpa by computer control still internal pressure, makes rare earth alloy powderProduce priming reaction with hydrogen;
(4) make slurries: be the ratio of 1: 2.5 in mass ratio, take 25 kilograms of toluene. Toluene is added in autoclave,It is under 1000r.P.m. condition that mixing speed is set on computers, and starts mixer raw material in still is stirred, and makes in stillRaw material after activation and toluene form slurries;
(5) hydrogen abstraction reaction: after slurries fully activate in still, it is 300 DEG C that reactor temperature is set on computers, stirs speedDegree, under 1000r.P.m. condition, continues to reactor hydrogen make-up, makes slurries constantly carry out hydrogen abstraction reaction;
(6) detect: the product after above-mentioned steps hydrogen abstraction reaction is sampled to detection; Quality requirement is that the slurries in reactor are abundantInhale hydrogen to saturation state; As undesirable, then proceed hydrogenation reaction, until meet the requirements;
(7) discharging: reach standard-required, get final product discharging.
Claims (2)
1. a method for rare earth alloy slurries storage hydrogen, is characterized in that, the method comprises the steps:
(1) charging: rare earth alloy material powder is added in autoclave;
(2) vacuumize: autoclave is vacuumized;
(3) priming reaction: be filled with high-purity hydrogen in autoclave, rare earth alloy is repeatedly lived under the effect of hydrogenChange reaction;
(4) make slurries: in autoclave, add toluene, and start mixer raw material in still is stirred, make in still rareSoil alloy raw material forms slurries, the described quantity to adding toluene in autoclave with rare earth alloy powder than the quality of tolueneThan being 1: 2.5-3;
(5) hydrogen abstraction reaction: be heated to 250-350 DEG C in autoclave, stir and constantly to reactor supplemental hydrogen simultaneously constantlyGas, makes slurries constantly carry out hydrogen abstraction reaction;
(6) detect: the product after above-mentioned steps hydrogen abstraction reaction is sampled to detection;
(7) discharging: detect and reach standard-required, get final product discharging.
2. the method for a kind of rare earth alloy slurries storage hydrogen as claimed in claim 1, is characterized in that, step (4) is made slurriesAnd stirring in step (5) hydrogen abstraction reaction, its speed of agitator is not less than 1000r.P.m.
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| CN108131563B (en) * | 2017-11-22 | 2020-05-26 | 北京有色金属研究总院 | Metal hydride hydrogen storage tank with spiral structure |
| CN113200515A (en) * | 2021-04-19 | 2021-08-03 | 有研工程技术研究院有限公司 | Hydrogen slurry material for storing and transporting hydrogen at normal temperature and normal pressure and hydrogen storage method |
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| CN1111280C (en) * | 2000-06-07 | 2003-06-11 | 信息产业部电子第十八研究所 | Complex test device and test method for mixed rare earth hydrogen storage alloy hydrogenizing property |
| JP4403499B2 (en) * | 2003-06-13 | 2010-01-27 | 株式会社豊田中央研究所 | Hydrogen storage material |
| CN101823692B (en) * | 2010-04-20 | 2012-03-14 | 浙江大学 | Reversible hydrogen adsorption and desorption method using piperidine as media and device |
| CN201815306U (en) * | 2010-09-14 | 2011-05-04 | 浙江大学 | Device utilizing aromatic compound to continuously absorb and emit hydrogen |
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