CN111252733A - Preparation method of multi-element metal hydride - Google Patents
Preparation method of multi-element metal hydride Download PDFInfo
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- CN111252733A CN111252733A CN201811453111.2A CN201811453111A CN111252733A CN 111252733 A CN111252733 A CN 111252733A CN 201811453111 A CN201811453111 A CN 201811453111A CN 111252733 A CN111252733 A CN 111252733A
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- C—CHEMISTRY; METALLURGY
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Abstract
The application discloses a preparation method of multi-element metal hydride, which is characterized by comprising the following steps: mixing and roasting raw materials containing metal, alkali metal hydride and/or alkaline earth metal hydride to obtain the multi-element metal hydride. The method successfully prepares the alkali (earth) metal multi-element metal hydride, and has the advantages of simple and convenient operation, lower reaction temperature, lower hydrogen pressure required by the reaction, shorter time for synthesizing materials and higher product purity.
Description
Technical Field
The application relates to a preparation method of a multi-element metal hydride, belonging to the field of hydrogen storage materials.
Background
Metal hydrides have long been used primarily as reversible hydrogen storage materials. The first instance of the metal ternary hydride K was reported since 1964 by Knox et al2ReH9Until the eighties of the twentieth century, LaNi5H6And FeTiH2The hydrogen storage system is reported to show the characteristic of reversible hydrogen absorption and desorption, the multi-element metal hydride arouses the extensive interest of researchers and gradually and deeply researches, most of the multi-element metal hydrides have the properties of metal and hydride, and the understanding of the multi-element metal hydride is gradually deepened through the researches on a synthesis method, a diffraction method, a bonding mode and a crystal structure.
Solid phase synthesis is currently the most common method for preparing multi-element metal hydrides. The method uses the element simple substance or binary metal alloy or binary metal hydride as reactant, and adopts high enough hydrogen pressure and certain temperature condition to prepare the multielement metal hydride. Bronger and G.Auffermann report (W.Bronger and G.Auffer)mann, j. alloys comp, 1995,228,119) with Pd and NaH at a hydrogen pressure of up to 2500bar, heating to 770K to synthesize Na2PdH4(ii) a K.Kadir and D.Nor 'eus reports (K.Kadir and D.Nor' eus, Z.Phys.chem.NF.,1989,163,231) that Na was synthesized using Pd and NaH at a hydrogen pressure of up to 50bar, by heating to 643K2PdH2P.M ü ller et al (W.Bronger, K.Jansen, and P.M ü ller, J.less-Common Met.,1990,161,299) used Pd and CaH2Heating to 1123K under the hydrogen pressure of 300bar to synthesize CaPdH2。
Disclosure of Invention
According to one aspect of the application, the preparation method of the multi-element metal hydride is provided, and the method is simple to operate, low in price and easy to obtain raw materials, high in product purity, high in yield and environment-friendly.
The method uses metal and alkali (earth) metal hydride as raw materials, fully mixes reactants by a solid phase mechanical ball milling method, and then roasting the mixed solid reactants in a hydrogen atmosphere to obtain the alkali (earth) metal multi-element metal hydride. The method successfully prepares the alkali (earth) metal multi-element metal hydride, and has the advantages of simple and convenient operation, lower reaction temperature, lower hydrogen pressure required by the reaction, shorter time for synthesizing materials and higher product purity.
Specifically, the method comprises the steps of taking metal and alkali (earth) metal hydride as raw materials, fully mixing reactants by a solid-phase mechanical ball milling method, and roasting the mixed solid reactants in a hydrogen atmosphere to obtain the alkali (earth) metal multi-element metal hydride.
The preparation method of the multi-metal hydride is characterized by comprising the following steps: mixing and roasting raw materials containing metal, alkali metal hydride and/or alkaline earth metal hydride to obtain the multi-element metal hydride.
Optionally, the metal is selected from at least one of group VIIB, group VIIIB elements, group IB elements, group IIB elements.
Optionally, the metal is selected from at least one of Mn, Re, Fe, Co, Ni, Ru, Rh, Pd, Os, Ir, Pt, Cu, Zn.
Optionally, the alkali metal hydride and/or alkaline earth metal hydride is selected from LiH, NaH, KH, RbH, CsH, MgH2、CaH2、SrH2、BaH2At least one of (1).
Optionally, the molar ratio of the metal to the alkali metal hydride and/or alkaline earth metal cyanide is from 100:1 to 1: 100.
Alternatively, the upper or lower limit of the molar ratio of the metal to the alkali metal hydride and/or alkaline earth metal cyanide is selected from 90:1, 80:1, 50:1, 20:1, 10:1, 6:1, 5:1, 2:1, 1:2, 1:5, 1:6, 1:8, 1:10, 1:50, 1:80, or 1: 90.
Optionally, the mixing comprises ball milling.
Optionally, the ball milling comprises mechanical mixing or mechanical ball milling.
Optionally, the weight ratio of the grinding balls to the sample to be processed in the ball milling process is 1-100: 1.
Optionally, the ball milling time is 1-24 hours; the temperature range of ball milling is 0-100 ℃.
Optionally, the ball milling is performed under an inert atmosphere.
Optionally, the inert atmosphere comprises at least one of nitrogen and an inert gas.
Optionally, the inert gas is selected from argon, nitrogen or helium.
Optionally, the gas flow rate of the inert atmosphere in the ball milling process is 1-200 mL/min.
Optionally, the ball milling comprises mechanical mixing or mechanical ball milling on an automatic mechanical mill, a planetary ball mill, an oscillating ball mill, or a vibratory ball mill.
Optionally, the rotating speed of the planetary ball mill is 10-500 rpm.
Optionally, the oscillating frequency of the oscillating ball mill is 50-600 cycles/min.
Optionally, the rotation speed of the automatic powder mixing machine is 10-100 rpm.
Optionally, the ball milling is performed on an automatic mechanical powder mixer, a planetary ball mill, an oscillating ball mill, or a vibratory ball mill by mechanical mixing or mechanical ball milling; the grinding balls adopted in the ball milling treatment are one or more than two of stainless steel balls, tungsten carbide balls, corundum balls, agate balls or zirconia balls; the mechanical mixing or the mechanical ball milling is carried out under the protection of vacuum or inert atmosphere, and the inert atmosphere is one or more than two of nitrogen atmosphere, argon atmosphere or helium atmosphere.
Within the above ball milling condition parameters, mixing can be achieved. The specific parameters can be selected according to actual needs.
Optionally, the firing is performed in a hydrogen-containing atmosphere;
wherein the hydrogen pressure in the hydrogen-containing atmosphere is 1 to 100 bar.
The hydrogen-containing atmosphere is an atmosphere containing hydrogen.
Optionally, the roasting temperature is 100-800 ℃.
Optionally, the roasting temperature is 300-400 ℃.
Optionally, the upper temperature limit of the roasting is selected from 200 ℃, 300 ℃, 350 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃ or 800 ℃; the lower limit is selected from 100 deg.C, 200 deg.C, 300 deg.C, 350 deg.C, 400 deg.C, 500 deg.C, 600 deg.C or 700 deg.C.
Optionally, the temperature rise rate of the roasting is 1-10 ℃/min.
Optionally, the firing ramp rate is 5 ℃/min.
Optionally, the roasting time is 12-48 hours.
Optionally, the roasting time is 24-36 hours.
Optionally, the method comprises:
the method comprises the steps of taking metal and alkali metal hydride and/or alkaline earth metal hydride as raw materials, fully mixing the raw materials in a solid phase mechanical ball milling mode according to a proportion, and roasting a solid mixture subjected to ball milling under a hydrogen pressure condition to obtain the multi-element metal hydride.
As a specific embodiment, the method comprises:
1) under the condition of air isolation, a mixture of metal and alkali (earth) metal hydride is filled into a ball milling tank;
2) the mixture of metal and alkali (earth) metal hydride is uniformly mixed and ground by adopting a temperature control mechanical mixing or mechanical ball milling mode;
3) transferring the solid mixture obtained in the step 2) to a reactor, pumping to a vacuum state, and adding a certain hydrogen pressure;
4) heating the closed reactor in the step 3) to a certain temperature, maintaining the temperature for a period of time, cooling the reactor in a hydrogen atmosphere, and collecting a solid sample.
The synthesis method has the advantages of simple operation, low reaction temperature, low hydrogen pressure required by reaction, short time for synthesizing materials and high product purity.
The beneficial effects that this application can produce include:
the preparation method of the multi-element metal hydride is simple and convenient to operate, low in reaction temperature, low in hydrogen pressure required by reaction and short in material synthesis time.
Drawings
FIG. 1 is a ternary lithium palladium hydride compound (Li) synthesized from palladium and lithium hydride in example 12PdH2) X-ray powder diffraction pattern of (a).
FIG. 2 is a ternary sodium palladium hydride compound (Na) synthesized in example 2 using palladium and sodium hydride as raw materials2PdH2) X-ray powder diffraction pattern of (a).
FIG. 3 is a ternary potassium palladium hydride compound (K) synthesized in example 3 using palladium and potassium hydride as raw materials3PdH5) X-ray powder diffraction pattern of (a).
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
The analysis method in the examples of the present application is as follows:
x-ray powder diffraction phase analysis (XRD) an X' Pert PROX X-ray diffractometer from pananace (PANalytical) of the netherlands, Cu target, K α radiation source (λ ═ 0.15418nm), voltage 40KV, and current 40mA were used.
According to one embodiment of the present application, a method for synthesizing an alkali (earth) metal multi-metal hydride comprises: metal and different kinds of alkali (earth) metal hydrides are taken as raw materials, fully mixed and ground in a solid phase mechanical ball milling mode according to different proportions, and a solid mixture after ball milling is roasted under a certain hydrogen pressure condition to obtain different kinds of alkali (earth) metal multi-element metal hydrides; the molar ratio of the raw materials is as follows: metal: the alkali (earth) metal hydride is 100:1 to 1: 100.
Optionally, the metal is one or more of Mn, Re, Fe, Co, Ni, Ru, Rh, Pd, Os, Ir, Pt, Cu and Zn in the elements of groups VIIB, VIIIB, IB and IIB.
Optionally, the alkali (earth) metal hydride is LiH, NaH, KH, RbH, CsH, MgH2、CaH2、SrH2、BaH2And one or more of lanthanides.
Optionally, the solid phase synthesis reaction is mechanically mixed or mechanically ball milled on an automatic mechanical powder mixer, a planetary ball mill, a swing ball mill, or a vibratory ball mill; the grinding balls adopted in the ball milling treatment are one or more than two of stainless steel balls, tungsten carbide balls, corundum balls, agate balls or zirconia balls; the mechanical mixing or the mechanical ball milling is carried out under the protection of vacuum or inert atmosphere, and the inert atmosphere is one or more than two of nitrogen atmosphere, argon atmosphere or helium atmosphere.
Optionally, the weight ratio of the grinding ball to the sample is (1-100); the rotating speed of the planetary ball mill is 10-500rpm, the shimmying frequency of the oscillating ball mill is 50-600 weeks/minute, and the rotating speed of the automatic powder mixer is 10-100 rpm; the time of mechanical ball milling or mixing is 1-24 hours; the ball milling temperature range is 0-100 ℃.
Optionally, the inert atmosphere is argon, nitrogen or helium, and the gas flow rate is 1-200 mL/min.
Optionally, the roasting temperature is 100-800 ℃.
Optionally, the hydrogen pressure is 0 to 100 bar.
Example 1
In an argon glove box, 424mg of palladium powder (Pd) and 64mg of lithium hydride (LiH) are accurately weighed and placed in a self-made stainless steel ball milling tank. After the ball milling tank is closed, the ball milling tank is filled into a planetary ball mill, and the ball milling conditions are as follows: ball milling is carried out for 3 hours at the speed of 150rpm, the ball milling temperature is 30 ℃, the grinding balls are stainless steel balls, and the mass of the grinding balls and the mass of a sample are 20: 1. in an argon glove box, the mixture is placed in a self-made stainless steel reactor, vacuum pumping is carried out, a sample is heated to 300 ℃ under the hydrogen pressure of 10bar (the heating rate is 5 ℃/min), the temperature is kept for 36 hours, after cooling to the room temperature, the obtained sample is taken out and marked as # 1, and the obtained product is tested by an X-ray powder diffractometer as shown in figure 1. It can be seen from FIG. 1 that only Li was detected in the product2PdH2Phase, no phases of Pd and LiH starting materials were detected.
The multinary metal hydride is prepared by a similar process to that described above, except that: the roasting temperature is 100 deg.C, and the prepared sample is labeled as 1-1 #.
The multinary metal hydride is prepared by a similar process to that described above, except that: the roasting temperature is 800 ℃, and the prepared sample is marked as 1-2 #.
The multinary metal hydride is prepared by a similar process to that described above, except that: the hydrogen pressure was 100bar and the prepared sample was labeled 1-3 #.
The X-ray powder diffractometer test results for samples # 1-1 to # 1-3 are similar to those of fig. 1, and the conclusion is the same as above.
Example 2
In an argon glove box, 216mg of palladium powder (Pd) and 96mg of sodium hydride (NaH) were accurately weighed and placed in a self-made stainless steel ball-milling jar. And (3) sealing the ball milling tank, and then putting the ball milling tank into a planetary ball mill, wherein the ball milling condition is 150rpm for 3 hours, the ball milling temperature is 60 ℃, the grinding balls are stainless steel grinding balls, and the mass of the grinding balls and the sample is 20: 1. placing the obtained mixture in a self-made stainless steel reactor in an argon glove box, vacuumizing, heating the sample to 400 ℃ under the hydrogen pressure of 10bar (the heating rate is 5℃)Min) and kept at this temperature for 24 hours, after cooling to room temperature, the sample obtained is taken out, labelled # 2, and the product obtained is tested with an X-ray powder diffractometer, as shown in figure 2. From FIG. 2, it can be seen that only Na was detected in the product2PdH2Phase, no phase of Pd and NaH starting materials was detected.
The multinary metal hydride is prepared by a similar process to that described above, except that: the mass ratio of the palladium powder to the sodium hydride is 1:100, and the prepared sample is marked as 2-1 #.
The multinary metal hydride is prepared by a similar process to that described above, except that: the mass ratio of the palladium powder to the sodium hydride is 100:1, and the prepared sample is marked as 2-2 #.
The multinary metal hydride is prepared by a similar process to that described above, except that: the temperature of ball milling is 30 ℃, and the prepared sample is marked as 2-3 #.
The X-ray powder diffractometer test results for samples # 2-1 to # 2-3 are similar to fig. 2, and the conclusion is the same as above.
Example 3
212mg of palladium powder (Pd) and 240mg of potassium hydride (KH) are accurately weighed in an argon glove box and placed in a self-made stainless steel ball milling tank. And (3) sealing the ball milling tank, and then putting the ball milling tank into a planetary ball mill, wherein the ball milling condition is 150rpm for 3 hours, the ball milling temperature is 50 ℃, the grinding balls are stainless steel grinding balls, and the mass of the grinding balls and the sample is 20: 1. in an argon glove box, the mixture is placed in a self-made stainless steel reactor, vacuum pumping is carried out, a sample is heated to 350 ℃ under the hydrogen pressure of 15bar (the heating rate is 5 ℃/min), the temperature is kept for 36 hours, after cooling to the room temperature, the obtained sample is taken out and marked as # 3, and the obtained product is tested by an X-ray powder diffractometer, as shown in figure 3. It can be seen from FIG. 3 that only K was detected in the product3PdH5Phase, no phase of Pd and KH starting material was detected.
The multinary metal hydride is prepared by a similar process to that described above, except that: the mass ratio of the grinding ball to the sample is 1:1, and the prepared sample is marked as # 3-1.
The multinary metal hydride is prepared by a similar process to that described above, except that: the mass ratio of the grinding ball to the sample is 100:1, and the prepared sample is marked as # 3-2.
The X-ray powder diffractometer test results for samples # 3-1 to # 3-2 are similar to those of fig. 3, and the conclusion is the same as above.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A method for producing a multi-metal hydride, comprising: mixing and roasting raw materials containing metal, alkali metal hydride and/or alkaline earth metal hydride to obtain the multi-element metal hydride.
2. The method of claim 1, wherein the metal is selected from at least one of group VIIB, group VIIIB, group IB, group IIB;
preferably, the metal is selected from at least one of Mn, Re, Fe, Co, Ni, Ru, Rh, Pd, Os, Ir, Pt, Cu, Zn.
3. The process according to claim 1, characterized in that the alkali metal hydride and/or alkaline earth metal hydride is selected from LiH, NaH, KH, RbH, CsH, MgH2、CaH2、SrH2、BaH2At least one of (1).
4. The method according to claim 1, wherein the molar ratio of the metal to the alkali metal hydride and/or alkaline earth metal cyanide is 100:1 to 1: 100.
5. The method of claim 1, wherein the mixing comprises ball milling.
6. The method of claim 5, wherein the ball milling comprises mechanical mixing or mechanical ball milling;
preferably, the weight ratio of the grinding balls to the sample to be treated in the ball milling process is 1-100: 1;
preferably, the ball milling time is 1-24 hours; the temperature range of ball milling is 0-100 ℃.
7. The method of claim 5, wherein the ball milling is performed under an inert atmosphere;
preferably, the gas flow rate of the inactive atmosphere in the ball milling process is 1-200 mL/min.
8. The method of claim 5, wherein the ball milling comprises mechanical mixing or mechanical ball milling on an automatic mechanical mill, a planetary ball mill, an oscillating ball mill, or a vibratory ball mill;
preferably, the rotating speed of the planetary ball mill is 10-500 rpm;
preferably, the oscillating frequency of the oscillating ball mill is 50-600 weeks/min;
preferably, the rotating speed of the automatic powder mixing machine is 10-100 rpm.
9. The method of claim 1, wherein the firing is performed in a hydrogen-containing atmosphere;
wherein the hydrogen pressure in the hydrogen-containing atmosphere is 1-100 bar;
preferably, the roasting temperature is 100-800 ℃.
10. The method according to claim 1, characterized in that it comprises:
the method comprises the steps of taking metal and alkali metal hydride and/or alkaline earth metal hydride as raw materials, fully mixing the raw materials in a solid phase mechanical ball milling mode according to a proportion, and roasting a solid mixture subjected to ball milling under a hydrogen pressure condition to obtain the multi-element metal hydride.
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Citations (4)
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| CN1280527A (en) * | 1997-10-22 | 2001-01-17 | 魁北克水电公司 | Nahocomposites with activated interfaces prepared by mechanical grinding of magnesium hydrides and use for storing hydrogen |
| US6387152B1 (en) * | 1997-12-23 | 2002-05-14 | Gkss Forschungszentrum Geesthacht Gmbh | Process for manufacturing nanocrystalline metal hydrides |
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Application publication date: 20200609 |