CN103754821A - Method of promoting coordinate alanate and ammonium salt to react by solvent to prepare hydrogen - Google Patents

Method of promoting coordinate alanate and ammonium salt to react by solvent to prepare hydrogen Download PDF

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CN103754821A
CN103754821A CN201410010880.0A CN201410010880A CN103754821A CN 103754821 A CN103754821 A CN 103754821A CN 201410010880 A CN201410010880 A CN 201410010880A CN 103754821 A CN103754821 A CN 103754821A
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ammonium salt
aluminum hydride
hydrogen
coordination aluminum
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CN103754821B (en
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陈云贵
王小炼
吴朝玲
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Sichuan University
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
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Abstract

The invention relates to a method of promoting coordinate alanate and ammonium salt to react by a solvent to prepare hydrogen. The chemical formula of the coordinate alanate is M(AlH4)m, wherein M is an alkali metal or alkaline earth capable of forming coordinate hydride, and m is the valence of the alkali metal or alkaline earth; the chemical formula of ammonium salt is (NH4)nX, wherein X is an acidic group and n is the valence of the acidic group. The method comprises the following steps: adding the coordinate alanate, the ammonium slat and the solvent into a reactor to be mixed, thus accelerating reaction of the coordinate alanate and the ammonium slat by the solvent, wherein the molar ratio of the coordinate alanate to the ammonium slat is (0.38-4.55):1, and the use level of the solvent is 0.4-100L/mol of the coordinate alanate. According to the method, the coordinate alanate is just contacted with the ammonium salt without heating, and the solvent provides the reaction environment, so that reaction can be carried to generate hydrogen. The method can efficiently release hydrogen under a condition of not providing extra energy sources.

Description

Utilize solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing
Technical field
The invention belongs to coordination aluminum hydride and ammonium salt reaction hydrogen producing technology field, particularly coordination aluminum hydride and ammonium salt do not heat with low temperature under react the method for hydrogen manufacturing.
Background technology
Storing hydrogen is one of main difficult technical of current hydrogen economy transition.At present, hydrogen storage technology mainly contains three kinds: high-pressure gaseous storage hydrogen, low-temperature liquefaction storage hydrogen and solid-state storage hydrogen, with respect to high-pressure gaseous storage hydrogen and low-temperature liquefaction storage hydrogen, the solid state hydrogen storing mode that forms sosoloid or hydride by the interaction of hydrogen and storeroom, because it has higher security and energy density, is the most promising a kind of storing hydrogen technology.During solid state hydrogen stores, the hydrogen storage material of lightweight heavy body, as hydroborate, alanate, nitrogen hydride and amino borane compound etc., theoretical hydrogen storage capability is all more than 5.0wt%, be hopeful most to meet the requirement of USDOE to on-board hydrogen storage system, but not yet have a kind of comprehensive hydrogen storage property (mainly comprise volume and weight hydrogen-storage density, inhale hydrogen discharging temperature, speed for hydrogen absorbing and releasing, cyclical stability and material cost) of material can meet practical requirement at present.This is because this type of hydrogen storage material is when as hydrogen source, hydrogen desorption method mostly is the dehydrogenation of solid-phase thermal solution, at heating condition, make hydrogen discharge to be used as hydrogen source, but they need 100 ℃ of above hot conditionss mostly, and there is the problems such as kinetics is slow, while using as hydrogen storage material, need to provide extra thermal source, energy efficiency is low, can not meet vehicle-mounted and mobile practical requirement completely.
Have at present about be heated to certain temperature with the solids composition that contains some suitable coordination aluminum hydride and ammonium salt and cause the research that solid state reaction generation hydrogen occurs between component, as United States Patent (USP) (U.S.1973,3,734,863; U.S.1975,3,862,052; U.S.1976,3,977,990; U.S.1976,3,931,395; U.S.1977,4,022,795; U.S.1980,4,231,891; U.S.1982,4,341,65) introduced when alkali/alkaline earth metal hydride and ammonium salt are heated to 150 ℃ and can produce hydrogen.Composite alkali aluminum hydride (the MAlH that and for example mol ratio is 1:1 4, M=Li or Na) and NH 4cl carries out solid state reaction when being heated to 170 ℃ can produce hydrogen (H.Zhang, Y.S.Loo, H.Geerlings, J.Lin and W.S.Chin, International Journal of Hydrogen Energy2010,35,176-180.).The solid-phase thermal solution dehydrogenation of these hydrogen storage materials all needs to be heated to comparatively high temps, economical and practical not.
Summary of the invention
The object of the invention is to mostly need for existing solid state hydrogen storing technology the deficiency of high temperature ability hydrogen desorption, a kind of method of utilizing solvent to impel basic metal or alkaline-earth metal coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing is provided, this method can be under the condition that additional energy source is not provided efficient release hydrogen.
The method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing of the present invention, the chemical formula of coordination aluminum hydride is M (AlH 4) m, wherein M is basic metal or the alkaline-earth metal that can form complex hydrides, and m is the valency of described basic metal or alkaline-earth metal, and the chemical formula of ammonium salt is (NH 4) nx, wherein X is acidic-group, n is the valency of acidic-group, the method is that coordination aluminum hydride, ammonium salt and solvent are added in reactor and mixed mutually, by solvent, accelerate reacting of coordination aluminum hydride and ammonium salt, wherein, the mol ratio of coordination aluminum hydride and ammonium salt is (0.38～4.55): 1, and the consumption of solvent is 0.4L/mol～100L/mol coordination aluminum hydride.
The method does not need heating, as long as coordination aluminum hydride contacts with ammonium salt, and has solvent that reaction environment is provided, and generation hydrogen can react.
The above-mentioned method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, the temperature of reaction of coordination aluminum hydride and ammonium salt is chosen in-40 ℃～85 ℃ according to the main range of application of the method (on-board hydrogen source, compact power, low temperature hydrogen supply), and the working temperature of this temperature range and hydrogen fuel cell adapts.
The above-mentioned method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, the consumption of solvent is 1～10L/mol coordination aluminum hydride preferably.
The above-mentioned method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, the selection face of solvent is wider, as long as dissolving at least partly basic metal or alkaline-earth metal coordination aluminum hydride and ammonium salt, and do not form strong chemical bond with basic metal or alkaline-earth metal coordination aluminum hydride and ammonium salt, the solvent that also can not be consumed in desorption process all can.Described solvent can be organic solvent, comprises ether, aldehyde, alcohol, ketone, amine, heterogeneous ring compound, ester, Organohalogen compounds or its mixture, can be also aqueous solvent, as water, liquid nitrogen, ionic liquid or its mixture.The preferred tetrahydrofuran (THF) of described solvent (THF), ether (Et 2o), at least one in glycol dimethyl ether (DME).When using two or more solvent, their proportioning can be any proportioning.
The above-mentioned method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, described coordination aluminum hydride is LiAlH 4, NaAlH 4, KAlH 4, Mg (AlH 4) 2, Ca (AlH 4) 2in at least one, be preferably LiAlH 4or/and NaAlH 4.When the coordination aluminum hydride of selecting two or more is during as raw material, their proportioning can be any proportioning.
The above-mentioned method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, described ammonium salt is NH 4f, NH 4cl, NH 4br, NH 4nO 3, (NH 4) 2cO 3, NH 4hCO 3, (NH 4) 2sO 4, NH 4hSO 4in at least one, preferably NH 4f, NH 4cl, (NH 4) 2cO 3, (NH 4) 2sO 4in at least one.When selecting two or more ammonium salts as raw material, their proportioning can be any proportioning.
The above-mentioned method of utilizing solvent to impel coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, adds the order of solvent and reactant unrestricted.
Compared with prior art, the present invention has following beneficial effect:
1, the method for the invention even more just can be reacted the NH of Heat of Formation poor stability under low temperature at normal temperature by the coordination aluminum hydride that adds solvent and make Heat stability is good and ammonium salt 4alH 4, and NH 4alH 4and degradation production NH 3alH 3, NH 2alH 2at normal temperature, even more just can continue to decompose under low temperature to emit a large amount of hydrogen, whole process does not need to provide additional energy source, is specially adapted to the working temperature of-40～85 ℃, and theory is stored up hydrogen weight and can be reached 4.5wt%(and see embodiment).The method of the invention is save energy not only, and solved solid hydrogen storage material and need to just can put the poor difficult problem of hydrogen and hydrogen desorption kinetics at comparatively high temps, on-board hydrogen source and compact power for Hydrogen Fuel-cell Vehicles have very large practicality and commercial value, for the low temperature hydrogen supply difficult problem facing at present, also can solve well, can meet as the demand of cold district automobile fuel battery simultaneously.
2, the coordination aluminum hydride using in the method for the invention and ammonium salt are stable at normal temperatures, are convenient to store and carry coordination aluminum hydride M (AlH 4) min LiAlH 4, NaAlH 4, KAlH 4, Mg (AlH 4) 2and Ca (AlH 4) 2, the rich content of contained element in the earth's crust, ammonium salt (NH 4) nnH in X 4f, NH 4cl and (NH 4) 2sO 4, production technology maturation, cheap, the range of choice of solvent is large, easily from market, obtains low price, and only work to provide reaction environment, can not consume, especially low boiling point solvent, is easy to make it separation with reaction product by intensification or vacuum pump, can realize recycle, thereby the method for the invention is easy to implement, good in economic efficiency, be suitable for large-scale promotion application.
3, in the method for the invention, impel the solvent that reaction occurs can play heat buffering simultaneously, the heat producing in absorption reaction process, reduces thermosteresis, improves energy utilization rate.
Accompanying drawing explanation
Fig. 1 be in embodiment 1 hydrogen release high-volume with time chart.
Fig. 2 be in embodiment 2 hydrogen release high-volume with time chart.
Fig. 3 be in embodiment 3 hydrogen release high-volume with time chart.
Fig. 4 be in embodiment 4 hydrogen release high-volume with time chart.
Fig. 5 be in embodiment 5 hydrogen release high-volume with time chart.
Fig. 6 be in embodiment 6 hydrogen release high-volume with time chart.
Fig. 7 be in embodiment 7 hydrogen release high-volume with time chart.
Fig. 8 be in embodiment 8 hydrogen release high-volume with time chart.
Fig. 9 be in embodiment 9 hydrogen release high-volume with time chart.
Figure 10 be in embodiment 10 hydrogen release high-volume with time chart.
Figure 11 be in embodiment 11 hydrogen release high-volume with time chart.
Figure 12 be in embodiment 12～17 hydrogen release high-volume with time chart.
Embodiment
Below by embodiment, the method for the invention is described further.
In following examples, LiAlH 4and NaAlH 4purity is respectively 95%, 90%, all from the Sigma-Aldrich(manufacturer's of St. Louis title); NH 4f, NH 4cl, (NH 4) 2sO 4be analytical pure, from Chengdu Ke Long chemical reagent factory; THF, Et 2o, DME are analytical pure, from Chengdu Ke Long chemical reagent factory.Described coordination aluminum hydride and ammonium salt raw material are the conventional existence form under its natural condition, i.e. powder or particulate state.
In following examples, solvent impels the temperature of coordination aluminum hydride and ammonium salt reaction to be its working temperature during as hydrogen manufacturing or hydrogen source of laboratory condition Imitating; The account form of storage hydrogen weight is the hydrogen of generation and the weight percent of coordination aluminum hydride used and ammonium salt, unit represents with wt%, during due to reaction, solvent can not consume, and has therefore adopted Chu Qing field hydrolytic hydrogen production to calculate the method for storing up hydrogen weight, does not consider the weight of solvent.
Embodiment 1
By 0.005mol LiAlH 4with 0.005mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 1:1) pack in flask, adding 10mL DME(solvent load is 2L/mol LiAlH 4), under 85 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 1, reaction produced the hydrogen of about 6.71wt% in 60 minutes, the hydrogen of the raw about 6.90wt% of common property in 120 minutes.
Embodiment 2
By 0.005mol LiAlH 4with 0.005mol NH 4cl(LiAlH 4with NH 4the mol ratio of Cl is 1:1) pack in flask, add 10mL Et 2o(solvent load is 2L/mol LiAlH 4), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 2, reaction produced the hydrogen of about 5.08wt% in 90 minutes, the hydrogen of the raw about 5.29wt% of common property in 180 minutes.
Embodiment 3
By 0.005mol LiAlH 4and 0.005mol (NH 4) 2sO 4(LiAlH 4with (NH 4) 2sO 4mol ratio be 1:1) pack in flask, adding 10mL THF(solvent load is 2L/mol LiAlH 4), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 3, produce the hydrogen of about 3.56wt% in 15 minutes, continue reaction and substantially no longer including hydrogen and produce.
Embodiment 4
By 0.005mol NaAlH 4with 0.005mol NH 4f(NaAlH 4with NH 4the mol ratio of F is 1:1) pack in flask, adding 50mL THF(solvent load is 10L/mol NaAlH 4), under-40 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 4, produce the hydrogen of about 2.78wt% in 180 minutes, after 120 minutes, hydrogen desorption kinetics is significantly slack-off.
Embodiment 5
By 0.005mol LiAlH 4with 0.013mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 0.38:1) pack in flask, then to add 10mL THF(solvent load be 2L/mol LiAlH 4), under 0 ℃ of stirring, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 5, in 90 minutes, produce the hydrogen of about 4.34wt%.
Embodiment 6
By 0.023mol LiAlH 4with 0.005mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 4.55:1) pack in flask, then to add 10mL THF(solvent load be 0.43L/mol LiAlH 4), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 6, in 60 minutes, produce the hydrogen of about 4.39wt%.
Embodiment 7
By 0.0005mol LiAlH 4with 0.0005mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 1:1) pack in flask, then to add 50mL THF(solvent load be 100L/mol LiAlH 4), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 7, produced the hydrogen of about 3.40wt% in 60 minutes, and hydrogen desorption kinetics comparatively steadily fast, but hydrogen desorption kinetics after 60 minutes is slower, the hydrogen of the raw about 4.08wt% of common property during by 180 minutes.
Embodiment 8
By 0.005mol LiAlH 4with 0.005mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 1:1) pack in flask, then to add 5mL THF(solvent load be 1L/mol LiAlH 4), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 8, produce the hydrogen of about 5.44wt% in 120 minutes, continue reaction and substantially no longer including hydrogen and produce.
Embodiment 9
By 0.005mol LiAlH 4with 0.005mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 1:1) pack in flask, then add 10mL THF and Et 2(consumption of mixed solvent is 2L/mol LiAlH to the mixed solvent of O 4, wherein the consumption of THF is 1.98L/mol LiAlH 4, Et 2the consumption of O is 0.0198L/mol LiAlH 4, THF and Et in mixed solvent 2the volume ratio of O is 100:1), under 40 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in Figure 9, in 60 minutes, produce the hydrogen of about 7.83wt%.
Embodiment 10
The NaAlH that is 0.005mol by mole total amount 4and LiAlH 4mixture (NaAlH 4with LiAlH 4mol ratio be 1:100) and 0.005mol NH 4f packs in flask, then to add 10mL THF(solvent load be 2L/mol coordination aluminum hydride), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in figure 10, in 60 minutes, produce the hydrogen of about 7.84wt%.
Embodiment 11
By 0.005mol LiAlH 4with mole total amount NH that is 0.005mol 4f and NH 4mixture (the NH of Cl 4f and NH 4the mol ratio of Cl is 100:1) pack in flask, then to add 10mL THF(solvent load be 2L/mol LiAlH 4), under 25 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.As shown in figure 11, in 60 minutes, produce the hydrogen of about 7.85wt%.
Embodiment 12
By 0.005mol LiAlH 4with 0.005mol NH 4f(LiAlH 4with NH 4the mol ratio of F is 1:1) pack in flask, then to add 10mL THF(solvent load be 2L/mol LiAlH 4), under-40 ℃ of stirrings, react, adopt draining water gathering of gas law to collect hydrogen.
Embodiment 13
Be that with the difference of embodiment 12 temperature of reaction is-20 ℃.
Embodiment 14
Be that with the difference of embodiment 12 temperature of reaction is 0 ℃.
Embodiment 15
Be that with the difference of embodiment 12 temperature of reaction is 25 ℃.
Embodiment 16
Be that with the difference of embodiment 12 temperature of reaction is 40 ℃.
Embodiment 17
Be that with the difference of embodiment 12 temperature of reaction is 60 ℃.
In embodiment 12～17, the relation of hydrogen burst size and time as shown in figure 12, reaction power association is along with temperature of reaction raises and accelerates, when temperature of reaction is more than 0 ℃, in 90 minutes, can approach and put hydrogen completely, produce the hydrogen of about 7.80wt%,-40 and-20 ℃ also can put hydrogen, in 180 minutes, produce respectively the hydrogen of about 3.11wt% and 5.70wt%.

Claims (10)

1. utilize solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, the chemical formula of described coordination aluminum hydride is M (AlH 4) m, wherein M is basic metal or the alkaline-earth metal that can form coordination aluminum hydride, and m is the valency of described basic metal or alkaline-earth metal, and the chemical formula of described ammonium salt is (NH 4) nx, wherein X is acidic-group, n is the valency of acidic-group, it is characterized in that coordination aluminum hydride, ammonium salt and solvent to add in reactor and mix mutually, coordination aluminum hydride and the ammonium salt generation hydrogen that can react, wherein, the mol ratio of coordination aluminum hydride and ammonium salt is (0.38～4.55): 1, and the consumption of solvent is 0.4L/mol～100L/mol coordination aluminum hydride.
2. utilize according to claim 1 solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, the temperature of reaction that it is characterized in that coordination aluminum hydride and ammonium salt is-40 ℃～85 ℃.
3. according to utilizing solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing described in claim 1 or 2, the consumption that it is characterized in that described solvent is 1L/mol～10L/mol coordination aluminum hydride.
4. according to utilizing solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing described in claim 1 or 2, it is characterized in that described solvent is ether solvent.
5. utilize according to claim 4 solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, it is characterized in that described solvent is at least one in tetrahydrofuran (THF), ether, glycol dimethyl ether.
6. according to utilizing solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing described in claim 1 or 2, it is characterized in that described coordination aluminum hydride is LiAlH 4, NaAlH 4, KAlH 4, Mg (AlH 4) 2, Ca (AlH4) 2in at least one.
7. utilize according to claim 3 solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, it is characterized in that described coordination aluminum hydride is LiAlH 4, NaAlH 4, KAlH 4, Mg (AlH 4) 2, Ca (AlH4) 2in at least one.
8. utilize according to claim 7 solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, it is characterized in that described coordination aluminum hydride is LiAlH 4or/and NaAlH 4.
9. according to utilizing solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing described in claim 1 or 2, it is characterized in that described ammonium salt is NH 4f, NH 4cl, NH 4br, NH 4nO 3, (NH 4) 2cO 3, NH 4hCO 3, (NH 4) 2sO 4, NH 4hSO 4in at least one.
10. utilize according to claim 9 solvent to impel the method for coordination aluminum hydride and ammonium salt reaction hydrogen manufacturing, it is characterized in that described ammonium salt is NH 4f, NH 4cl, (NH 4) 2cO 3, (NH 4) 2sO 4in at least one.
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