CN103588171B - Circulate under a kind of Li-N-H of realization system microwave and put the method for hydrogen fast - Google Patents
Circulate under a kind of Li-N-H of realization system microwave and put the method for hydrogen fast Download PDFInfo
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Abstract
The present invention relates to one and realize Li-N-H(LiH+LiNH
2) put the method for hydrogen under system microwave fast, the method adopts that in Li-N-H, add mass percent be 5 ~ 35%LiBH
4; Be LiH and LiNH of 1:1 by mol ratio
2powder and massfraction are the LiBH of 5 ~ 35%
4powder is under the protection of rare gas element after ball milling mixing, and being placed in frequency is 2.45GHz multimode field pattern microwave oven, and under certain power, this material can be rapidly heated and put hydrogen.The invention has the advantages that LiBH
4with LiNH
2solid solution phase (LiNH is generated in mechanical milling process
2) x (LiBH
4) (1-x), this solid solution phase is both as catalysis phase, and again as inhaling ripple phase, and absorbing property is better than LiBH
4, thus realize Li-N-H system and be rapidly heated under microwave and put hydrogen.
Description
Technical field
The present invention relates to hydrogen storage material technical field, particularly relate to a kind of realize coordinate hydride hydrogen-storing material microwave under put the method for hydrogen fast.The invention belongs to hydrogen storage material preparation technology and applied technical field.
Background technology
Along with being on the rise of environmental pollution and petering out of fossil energy, development new forms of energy become the urgent demand in countries in the world.Clean as one, the free of contamination green energy resource of Hydrogen Energy, causes the great interest of people.The applicable key issue of restriction hydrogen is safe and reliable hydrogen storage technology.Hydrogen storage technology is mainly divided into gaseous state to store up hydrogen, liquid storage hydrogen and solid-state storage hydrogen.Solid-state storage hydrogen because of its security and hydrogen-storage density high and studied widely.In solid-state hydrogen storage material, metal nitrogen base hydride is advantages such as capacity is high, reversible hydrogen adsorption and desorption performance is good and being favored because having.By LiH+LiNH
2the Li-N-H system of composition is the Typical Representative of metal nitrogen base hydride hydrogen storage system, and its reversible hydrogen adsorption and desorption capacity is 6.5wt.%, but its hydrogen discharging temperature and hydrogen desorption kinetics performance await further improvement.Current investigator, mainly through adding catalyzer, the approach such as cation-modified, makes its hydrogen discharging performance be improved, but its hydrogen discharging temperature is still higher than the temperature requirement of fuel cell use.Because the heat conductivility of Li-N-H system is poor, usually adopt traditional type of heating, its heat-up rate is comparatively slow, and observable index is comparatively large, seriously limits its practical application.
Microwave is the hertzian wave of a kind of range of frequency at 300 MHz to 300 GHz.When being in the material in microwave field and containing microwave absorbing medium, the energy that substance absorbs microwave carries out conducting self-heating.This type of heating is called microwave heating.Microwave heating is a kind of brand-new heat energy technology, and compared with traditional heating, microwave heating has the features such as heating efficiency is high, rate of heating fast, selectivity heating, globality heating; In addition, microwave heating also has catalyzed chemical reaction, reduces chemical reaction temperature, for chemical reaction creates the more favorably non-thermal effect such as thermodynamic condition.
In order to improve the hydrogen discharging performance of Li-N-H system, the present invention proposes a kind of Li-N-H of realization system and circulates under microwave and put the method for hydrogen fast.Add in Li-N-H system and can play the medium that katalysis can absorb again microwave, realize Li-N-H system by microwave heating and put hydrogen fast, in conjunction with the cycle performance that Li-N-H system is good, by the practical application of favourable promotion Li-N-H system hydrogen storage material.
Summary of the invention
Circulate under the object of this invention is to provide a kind of Li-N-H of realization system microwave and put the method for hydrogen fast.The method is simple, has both overcome the problem of Li-N-H system heat conductivility difference, has improve heating efficiency, facilitates again the hydrogen desorption kinetics performance of Li-N-H system.
To achieve these goals, the present invention adopts following technical scheme:
Circulate under realizing Li-N-H system microwave and put a method for hydrogen fast, it is characterized in that, at Li-N-H(mol ratio LiH:LiNH
2=1:1) in add a small amount of LiBH
4; LiBH
4content and Li-N-H content by mass percentage, LiBH
4content be 5 ~ 35%; There is following step:
A. LiH powder is taken by certain proportioning, LiNH
2powder, LiBH
4powder, powder LiH and LiNH
2mol ratio be 1:1, LiBH
4the mass percentage content of powder is 5 ~ 35%.Above-mentioned raw materials is placed in ball mill fully mix, ball material weight ratio in ball mill is 30:1, and the powder that namely every 1 g is heavy needs the abrading-ball that 30 g are heavy, and the speed of mainshaft of ball mill is 200 revs/min, countershaft rotating speed is-400 revs/min, and wherein "-" expression turns to contrary; Ball-milling Time is 2 ~ 4h, and ball milling 10-30 minute has a rest 1-30 minute; For preventing Powder Oxidation, carry out in the canned sample of sample weighing, ball milling and the glove box of sampling all under Ar atmosphere protection;
B. uniform for above-mentioned ball milling sample is shifted in microwave tube type oven, vacuumize and pass into high-purity argon gas protection, opening microwave power supply, power 400-3000W, sample is rapidly heated, and in 5 minutes, sample temperature can rise to more than 400 DEG C, makes Li-N-H system put hydrogen completely;
C. sample after ball milling is heated under microwave less than 300 DEG C carry out suction put hydrogen circulation, the LiBH in sample
4with LiNH
2reaction forms solid solution phase (LiNH
2)
x(LiBH
4)
(1-x), this solid solution phase is both as catalysis phase, and again as inhaling ripple phase, and absorbing property is better than LiBH
4, thus realize Li-N-H system and circulate under microwave and put hydrogen fast.
The microwave frequency adopted in above-mentioned steps b and c is 2.45GHz, and the field pattern of microwave is multimode field pattern.
Feature and the mechanism of the inventive method are as described below:
The present invention makes full use of the feature of microwave radiation, by adding LiBH
4as wave absorbing agent, achieve Li-N-H rapid temperature increases and put hydrogen rapidly under microwave action, both overcome heating efficiency in traditional heating mode low, heat the problems such as uneven, facilitate again the hydrogen desorption kinetics performance of Li-N-H system by the effect of microwave.The present invention makes full use of LiBH
4feature: LiBH during (1) ball milling
4play grinding aid effect, powder is mixed uniformly, and effectively can reduce the particle of Li-N-H; (2) LiBH
4with LiNH
2quaternary solid solution phase (LiNH is generated in mechanical milling process
2)
x(LiBH
4)
(1-x), N-H key is weakened, katalysis is played to the hydrogen of putting of Li-N-H system; (3) the quaternary solid solution phase (LiNH generated when microwave heating
2)
x(LiBH
4)
(1-x)again as inhaling ripple phase, compare LiBH
4there is better absorbing property, thus realize Li-N-H system and be rapidly heated under microwave and put hydrogen.This system is being put in hydrogen working cycle lower than 300 DEG C of microwave heatings, (LiNH
2)
x(LiBH
4)
(1-x)all the time deposit in the sample to which, thus realize Li-N-H system and can circulate to be rapidly heated under microwave and put hydrogen.And in practice, can also according to the demand by hydrogen amount, the power of adjustment microwave, thus change hydrogen discharging rate.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and remarkable advantage:
Under microwave radiation, Li-N-H system temperature rise rate is fast, and heating efficiency is high, under 400W power microwave, is such as heated to 250 DEG C of times used be only 100s, and traditional heating method reaches uniform temp and needs 1700s under 800W power.The hydrogen discharging rate of Li-N-H system under microwave improves a lot compared with under traditional heating mode, such as with the addition of 7.6wt%LiBH
4sample in common heating furnace, only have the H of 1.2wt% in 10 minutes at 250 DEG C
2release, and under microwave heating, have the H of 3.2wt%
2release.LiBH
4with LiNH
2quaternary solid solution phase (LiNH is generated in mechanical milling process
2)
x(LiBH
4)
(1-x)because decomposition temperature is 330 DEG C, ensure that sample is put in hydrogen working cycle in the suction lower than 300 DEG C and all can put hydrogen at rapid temperature increases under microwave.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1,2,3 and comparative example in sample heating curve comparison diagram in 400W power microwave stove.
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates before and after the microwave heating of the embodiment of the present invention 1 sample.
Fig. 3 is embodiment of the present invention Isosorbide-5-Nitrae, the microwave heating curve comparison diagram of 5 samples under different capacity.
Fig. 4 is that the embodiment of the present invention 6 sample is heated to 250 DEG C and the hydrogen desorption kinetics curve being incubated 30 minutes respectively in microwave oven and common heating furnace.
Fig. 5 is the embodiment of the present invention 7, the microwave heating curve comparison diagram under 8 sample 400W power.
Embodiment
After now specific embodiments of the invention being described in.Following examples do not form limitation of the invention.
embodiment 1
LiH powder (purity 98wt.%, Alfa-Aesar chemical reagent company limited) 0.238g, LiNH is taken by proportioning
2(purity 95wt.%, Alfa-Aesar chemical reagent company limited) 0.687g, LiBH
4powder (purity 95wt.%, Alfa-Aesar chemical reagent company limited) 0.076g, i.e. LiH and LiNH
2mol ratio be 1:1, LiBH
4mass percent be 7.6wt.%.Powder is placed in Pulverisette 4 planetary high-energy ball mill that goes at express speed fully to mix.For preventing sample oxidized, in Ar gas glove box, carry out the canned sample of ball milling.The ball grinder volume used is 80 cm
3, ratio of grinding media to material is 30:1 (adopting 30 g abrading-ball/1 g powders), and during ball milling, the rotating speed of main shaft is 200 revs/min, and countershaft rotating speed is-400 revs/min ("-" representative turns to contrary), and Ball-milling Time is 4h, grinds and within 10 minutes, has a rest 10 minutes.After ball milling, take 0.5g sample and be placed in BN crucible in glove box, then transferring to frequency is in the multimode field pattern microwave tube type oven of 2.45GHz, passes into purity >=99.999%(volume percent after vacuumizing) argon gas protect.Open microwave power supply, setting power is 400W, and sample is rapidly heated, and within 5 minutes, temperature rises to 773K, and its heating-rate curve as shown in Figure 1; And this sample is positioned in common stove and heats 30 minutes with 400W, temperature just rises to 100 DEG C; Fig. 2 is the XRD figure spectrum of this sample before microwave heating and after microwave heating to the highest temperature, and result shows that this sample puts hydrogen completely after microwave heating is raised to the highest temperature.
embodiment 2
LiH powder (purity 98wt.%, Alfa-Aesar chemical reagent company limited) 0.232g, LiNH is taken by proportioning
2(purity 95wt.%, Alfa-Aesar chemical reagent company limited) 0.668g, LiBH
4powder (purity 95wt.%, Alfa-Aesar chemical reagent company limited) 0.1g, i.e. LiH and LiNH
2mol ratio be 1:1, LiBH
4mass percent be 10wt.%.Powder is placed in Pulverisette 4 planetary high-energy ball mill that goes at express speed fully to mix.For preventing sample oxidized, in Ar gas glove box, carry out the canned sample of ball milling.The ball grinder volume used is 80 cm
3, ratio of grinding media to material is 30:1 (adopting 30 g abrading-ball/1 g powders), and during ball milling, the rotating speed of main shaft is 200 revs/min, and countershaft rotating speed is-400 revs/min ("-" representative turns to contrary), and Ball-milling Time is 4h, grinds and within 10 minutes, has a rest 10 minutes.After ball milling, take 0.5g sample and be placed in BN crucible in glove box, then transferring to frequency is in the multimode field pattern microwave tube type oven of 2.45GHz, passes into purity >=99.999%(volume percent after vacuumizing) argon gas protect.Open microwave power supply, setting power is 400W, the heating curve of sample as shown in Figure 1, the initial stage temperature rise rate of sample with containing 7.6wt.%LiBH
4basically identical, but in 10 minutes, sample temperature rises to 853K; From XRD result, sample puts hydrogen after being raised to the highest temperature completely.
embodiment 3
LiH powder (purity 98wt.%, Alfa-Aesar chemical reagent company limited) 0.224g, LiNH is taken by proportioning
2(purity 95wt.%, Alfa-Aesar chemical reagent company limited) 0.646g, LiBH
4powder (purity 95wt.%, Alfa-Aesar chemical reagent company limited) 0.13g, i.e. LiH and LiNH
2mol ratio be 1:1, LiBH
4mass percent be 13wt.%.Powder is placed in Pulverisette 4 planetary high-energy ball mill that goes at express speed fully to mix.For preventing sample oxidized, in Ar gas glove box, carry out the canned sample of ball milling.The ball grinder volume used is 80 cm
3, ratio of grinding media to material is 30:1 (adopting 30 g abrading-ball/1 g powders), and during ball milling, the rotating speed of main shaft is 200 revs/min, and countershaft rotating speed is-400 revs/min ("-" representative turns to contrary), and Ball-milling Time is 4h, grinds and within 10 minutes, has a rest 10 minutes.After ball milling, take 0.5g sample and be placed in BN crucible in glove box, then transferring to frequency is in the multimode field pattern microwave tube type oven of 2.45GHz, passes into purity >=99.999%(volume percent after vacuumizing) argon gas protect.Open microwave power supply, setting power is 400W, the heating-rate curve of sample as shown in Figure 1, its initial stage heat-up rate also with 10wt.%LiBH
4sample is consistent, but 10 minutes temperature can rise to 903K; From XRD result, sample puts hydrogen after being raised to the highest temperature completely.
embodiment 4
LiH powder (purity 98 wt.%, Alfa-Aesar chemical reagent company limited) 0.238g, LiNH is taken by proportioning
2(purity 95 wt.%, Alfa-Aesar chemical reagent company limited) 0.687g, LiBH
4powder (purity 95 wt.%, Alfa-Aesar chemical reagent company limited) 0.076g, i.e. LiH and LiNH
2mol ratio be 1:1, LiBH
4mass percent be 7.6wt.%.Powder is placed in Pulverisette 4 planetary high-energy ball mill that goes at express speed fully to mix.For preventing sample oxidized, in Ar gas glove box, carry out the canned sample of ball milling.The ball grinder volume used is 80 cm
3, ratio of grinding media to material is 30:1 (adopting 30 g abrading-ball/1 g powders), and during ball milling, the rotating speed of main shaft is 200 revs/min, and countershaft rotating speed is-400 revs/min ("-" representative turns to contrary), and Ball-milling Time is 4h, grinds and within 10 minutes, has a rest 10 minutes.After ball milling, take 0.5g sample and be placed in BN crucible in glove box, then transferring to frequency is in the multimode field pattern microwave tube type oven of 2.45GHz, passes into purity >=99.999%(volume percent after vacuumizing) argon gas protect.Open microwave power supply, setting power is 600W.The heating-rate curve of sample as shown in Figure 3, slightly fast than under 400W of its initial stage heat-up rate, within 5 minutes, namely temperature rises to 848K; From XRD result, sample puts hydrogen after being raised to the highest temperature completely.
embodiment 5
LiH powder (purity 98 wt.%, Alfa-Aesar chemical reagent company limited) 0.238g, LiNH is taken by proportioning
2(purity 95 wt.%, Alfa-Aesar chemical reagent company limited) 0.687g, LiBH
4powder (purity 95 wt.%, Alfa-Aesar chemical reagent company limited) 0.076g, i.e. LiH and LiNH
2mol ratio be 1:1, LiBH
4mass percent be 7.6wt.%.Powder is placed in Pulverisette 4 planetary high-energy ball mill that goes at express speed fully to mix.For preventing sample oxidized, in Ar gas glove box, carry out the canned sample of ball milling.The ball grinder volume used is 80 cm
3, ratio of grinding media to material is 30:1 (adopting 30 g abrading-ball/1 g powders), and during ball milling, the rotating speed of main shaft is 200 revs/min, and countershaft rotating speed is-400 revs/min ("-" representative turns to contrary), and Ball-milling Time is 4h, grinds and within 10 minutes, has a rest 10 minutes.After abundant mixing, take 0.5g sample and be placed in BN crucible in glove box, then transferring to frequency is in the multimode field pattern microwave tube type oven of 2.45GHz, passes into purity >=99.999%(volume percent after vacuumizing) argon gas protect.Open microwave power supply, setting power is 800W, and as shown in Figure 3, its initial stage heat-up rate is than the further quickening under 600W, and within 4 minutes, namely temperature rises to 973K for the heating-rate curve of sample; From XRD result, sample puts hydrogen after being raised to the highest temperature completely.
embodiment 6
The sample prepared by ball milling in embodiment 1 is placed in multimode field pattern microwave oven that frequency is 2.45GHz respectively and common heating furnace is heated to 250 DEG C and is incubated 30 minutes, its hydrogen desorption kinetics curve as shown in Figure 4, result show sample in common heating furnace in 30 minutes hydrogen desorption capacity only have 3.9wt.%, and corresponding hydrogen desorption capacity is 5 wt.% under microwave heating, hydrogen discharging rate significantly improves.
embodiment 7
Carried out by sample in embodiment 1 inhaling for 2 times in Sieverts device and put hydrogen circulation, hydrogen discharging temperature is 250 DEG C, and putting hydrogen initial pressure is 0.001MPa, and putting the hydrogen time is 2 hours; Inhaling hydrogen temperature is 250 DEG C, and hydrogenation pressure is 2MPa, and hydrogenation time is 1 hour.Sample after XRD result shows hydrogenation is mainly LiH, LiNH
2(LiNH
2)
x(LiBH
4)
(1-x).Sample after hydrogenation is placed in the multimode field pattern microwave oven that frequency is 2.45GHz, setting power is 400W, Fig. 5 is its heating-rate curve, and result shows, after hydrogenation, sample can be warming up to 783K in 7 minutes under microwave, realizes putting hydrogen completely fast.
embodiment 8
Carried out by sample in embodiment 1 inhaling for 5 times in Sieverts device and put hydrogen circulation, hydrogen discharging temperature is 250 DEG C, and putting hydrogen initial pressure is 0.001MPa, and putting the hydrogen time is 2 hours; Inhaling hydrogen temperature is 250 DEG C, and hydrogenation pressure is 2MPa, and hydrogenation time is 1 hour.After XRD result shows 5 circulations, the sample of hydrogenation is mainly LiH, LiNH
2(LiNH
2)
x(LiBH
4)
(1-x), sample after circulation 5 hydrogenation is placed in the multimode field pattern microwave oven that frequency is 2.45GHz, and setting power is 400W, Fig. 5 is its heating-rate curve, and result shows, after circulation hydrogenation, sample can be warming up to 793K in 10 minutes, realizes putting hydrogen completely fast.
comparative example
LiH powder (purity 98 wt.%, Alfa-Aesar chemical reagent company limited) 0.257g, LiNH is taken by proportioning
2(purity 95 wt.%, Alfa-Aesar chemical reagent company limited) 0.743g, i.e. LiH and LiNH
2mol ratio be 1:1.Powder is placed in the Pulverisette 4 planetary high-energy ball mill ball milling that goes at express speed.For preventing sample oxidized, in Ar gas glove box, carry out the canned sample of ball milling.The ball grinder volume used is 80 cm
3, ratio of grinding media to material is 30:1 (adopting 30 g abrading-ball/1 g powders), and during ball milling, the rotating speed of main shaft is 200 revs/min, and countershaft rotating speed is-400 revs/min ("-" representative turns to contrary), and Ball-milling Time is 4h, grinds and within 10 minutes, has a rest 10 minutes.After abundant ball milling, take 0.5g sample and be placed in BN crucible in glove box, then transferring to frequency is in the multimode field pattern microwave tube type oven of 2.45GHz, passes into purity >=99.999%(volume percent after vacuumizing) argon gas protect.Open microwave power supply, setting power is 400W.The heating-rate curve of sample as shown in Figure 1, the most promotion of sample temperature in 30 minutes to 393K, far below the decomposition hydrogen discharging temperature of Li-N-H system.
Claims (2)
1. circulate under realizing Li-N-H system microwave and put a method for hydrogen fast, it is characterized in that the method has following step:
A. LiH powder is taken by certain proportioning, LiNH
2powder, LiBH
4powder, powder LiH and LiNH
2mol ratio be 1:1, LiBH
4the total mass percentage composition that accounts for of powder is 5 ~ 35%; Above-mentioned raw materials is placed in ball mill fully mix, ball material weight ratio in ball mill is 30:1, and the powder that namely every 1g is heavy needs the abrading-ball that 30 g are heavy, and the speed of mainshaft of ball mill is 200 revs/min, countershaft rotating speed is-400 revs/min, and wherein "-" expression turns to contrary; Ball-milling Time is 2 ~ 4h, and ball milling 10-30 minute has a rest 1-30 minute; For preventing Powder Oxidation, carry out in the canned sample of sample weighing, ball milling and the glove box of sampling all under Ar atmosphere protection;
B. uniform for above-mentioned ball milling sample is shifted in microwave tube type oven, vacuumize and pass into high-purity argon gas protection, opening microwave power supply, power 400-3000W, sample is rapidly heated, and in 5 minutes, sample temperature can rise to more than 400 DEG C, makes Li-N-H system put hydrogen completely;
C. sample after ball milling is heated under microwave less than 300 DEG C carry out suction put hydrogen circulation, the LiBH in sample
4with LiNH
2reaction forms solid solution phase (LiNH
2)
x(LiBH
4)
(1-x), this solid solution phase is both as catalysis phase, and again as inhaling ripple phase, and absorbing property is better than LiBH
4, thus realize Li-N-H system and circulate under microwave and put hydrogen fast.
2. circulate under a kind of Li-N-H of realization system microwave according to claim 1 and put the method for hydrogen fast, it is characterized in that, the microwave frequency adopted in step b and c is 2.45GHz, and the field pattern of microwave is multimode field pattern.
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