CN111137858A - Composite material for hydrogen production by hydrolysis of magnesium hydride and preparation method thereof - Google Patents
Composite material for hydrogen production by hydrolysis of magnesium hydride and preparation method thereof Download PDFInfo
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- CN111137858A CN111137858A CN202010119607.7A CN202010119607A CN111137858A CN 111137858 A CN111137858 A CN 111137858A CN 202010119607 A CN202010119607 A CN 202010119607A CN 111137858 A CN111137858 A CN 111137858A
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- hydrolysis
- magnesium hydride
- hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/065—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents from a hydride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention belongs to the technical field of hydrogen storage, and particularly relates to a composite material for hydrogen production by hydrolysis of magnesium hydride and a preparation method thereof. The composite material is prepared by mixing magnesium hydride and chloride, wherein the mass ratio of the magnesium hydride to the anhydrous chloride is 1: 0.05 to 0.5. The composite material for hydrogen production by hydrolysis prepared by the invention is convenient to carry, and the hydrogen production operation is simple and controllable. The adding flow velocity of water is adjusted according to the flow requirement of the required hydrogen, the hydrogen discharging speed is adjustable and stable, high-pressure hydrogen is not generated during use, and the device is safe and convenient. The method utilizes the added catalyst anhydrous chloride such as anhydrous magnesium chloride and the like to dissolve and release heat when water is added to initiate magnesium hydride hydrolysis reaction, so that the reaction system is rapidly heated, and the hydrolysis of magnesium hydride is promoted; meanwhile, chloride dissolved in water can effectively etch Mg (OH) generated by hydrolysis2The contact between magnesium hydride and water is promoted, and the smooth proceeding of hydrolysis is ensured.
Description
Technical Field
The invention belongs to the technical field of hydrogen storage, and particularly relates to a composite material for hydrogen production by hydrolysis of magnesium hydride and a preparation method thereof.
Background
At present, the energy crisis and the environmental pollution problem are becoming more serious, energy conversion by replacing fossil energy with renewable energy is urgent. The hydrogen energy source, a clean and renewable secondary energy source, is considered as a core pillar in energy transformation. However, the development of hydrogen energy sources is limited by the lack of a sufficiently efficient and safe way of storing hydrogen.
In order to meet the application requirements of portable fuel cells, the corresponding in-situ hydrogen supply technology requires that the raw materials have higher hydrogen production capacity, and the hydrogen supply needs to be convenient and quick. Using magnesium hydride (MgH)2) The hydrolysis reaction can be used for conveniently and rapidly preparing hydrogen: MgH2+2H2O→Mg(OH)2+2H2The mass of the released hydrogen is 15.4% of that of the solid hydrogen storage material, and the hydrogen does not contain harmful gas impurities, can be directly used for a hydrogen fuel cell, and is an ideal hydrogen supply material. Therefore, much research has been conducted on the hydrolysis reaction of magnesium hydride.
However, the biggest problem of hydrogen production by hydrolysis of magnesium hydride is that the reaction speed of magnesium hydride and water is slow, and magnesium hydroxide generated by hydrolysis covers the surface of magnesium hydride, thus hindering the subsequent progress of hydrolysis reaction. Research has shown that the hydrolysis reaction of magnesium hydride is facilitated by adding a certain amount of chloride salt and heating the reaction system, so that the reaction device is usually maintained at 70 ℃ or above by external heating in the hydrogen production reaction by hydrolysis of magnesium hydride. But the addition of external heating increases the components of the hydrogen supply device, increases the weight of the whole system, reduces the hydrogen storage mass density of the magnesium hydride hydrolysis hydrogen supply system, and is not beneficial to the use of a mobile hydrogen fuel cell; secondly, the cost of the whole system is increased, and the portability is reduced.
Chinese patent application CN104555916A reports a method and apparatus for catalyzing hydrolysis of magnesium hydride by using magnesium chloride solution, in order to accelerate the hydrolysis reaction, firstly, the magnesium hydride is ball-milled for pre-activation, and secondly, the magnesium chloride solution is heated to 60 ℃ and then added into the magnesium hydride. The pretreatment additionally increases the cost and reduces the convenience of the pretreatment as a hydrogen supply source of the mobile hydrogen fuel cell.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a composite material for hydrogen production by hydrolysis of magnesium hydride and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the composite material for hydrogen production by hydrolysis of magnesium hydride is prepared by mixing magnesium hydride and chloride, wherein the mass ratio of the magnesium hydride to the anhydrous chloride is 1: 0.05 to 0.5.
Preferably, the anhydrous chloride of the present invention is selected from anhydrous MgCl2Anhydrous CaCl2Anhydrous AlCl3Anhydrous NiCl2One or more of them.
Preferably, the magnesium hydride and the anhydrous chloride are mixed by high-speed stirring, grinding or ball milling.
More preferably, the magnesium hydride hydrolysis hydrogen production composite material is applied to a normal pressure hydrolysis hydrogen production device, the normal pressure hydrolysis hydrogen production device comprises a water storage tank, a delivery pump and a reactor, and the reactor is a sealed container and is used for filling the magnesium hydride hydrolysis hydrogen production composite material; one end of the delivery pump is connected with the water storage tank, and the other end of the delivery pump is connected with the water inlet of the reactor; the gas outlet of the reactor is connected with the gas inlet of the dryer through a first hydrogen passage; the gas inlet and the gas outlet of the reactor are both positioned at the topmost end of the reactor, and the composite material for hydrogen production by hydrolysis of magnesium hydride is positioned at the bottom in the reactor.
More preferably, the dryer is a sealed container, the interior of the sealed container is filled with the drying agent, the bottom of the sealed container is provided with an exhaust port, and a second hydrogen passage is arranged on the exhaust port; the second hydrogen passage is connected to a hydrogen fuel cell.
More preferably, the water storage tank of the invention is used for storing the liquid required by hydrolysis, and the liquid is one or more of tap water, deionized water, river water, lake water and seawater.
More preferably, the reactor of the present invention is disposed upright or inclined.
More preferably, the delivery pump of the present invention is a peristaltic pump or a syringe pump.
More preferably, a flow meter is arranged at the water inlet of the reactor.
The invention relates to a preparation method of a composite material for hydrogen production by hydrolysis of magnesium hydride, which comprises the following preparation steps: mixing magnesium hydride and anhydrous chloride in proportion, dissolving the mixture in water for reaction, wherein the anhydrous chloride is selected from anhydrous MgCl2Anhydrous CaCl2Anhydrous AlCl3Anhydrous NiCl2One or more of them.
Compared with the prior art, the invention has the following advantages:
(1) the magnesium hydride is hydrolyzed into a high exothermic reaction, and the enthalpy change value of hydrogen release is-138.80 kJ/mol H2We have found that the magnesium hydride releases enough heat to maintain the reaction system at 70 ℃ and above after the hydrolysis reaction, so we can utilize the added catalyst anhydrous chloride such as anhydrous magnesium chloride to dissolve and release heat when adding water to initiate the magnesium hydride hydrolysis reaction, so as to heat the reaction system rapidly and promote the hydrolysis of magnesium hydride. Meanwhile, chloride dissolved in water can effectively etch Mg (OH) generated by hydrolysis2The contact between magnesium hydride and water is promoted, and the smooth proceeding of hydrolysis is ensured.
(2) The composite material of the invention has simple preparation process, easy operation and amplification and easy application.
(3) The composite material for preparing hydrogen by hydrolysis is convenient to carry, the hydrogen preparation operation is simple and controllable, and the added water can be deionized water or inorganic salt such as river water, lake water, seawater and the like. The water addition flow rate is adjusted according to the flow requirement of the required hydrogen. The hydrogen release speed can be adjusted and stable. The use does not have high-pressure hydrogen, and is safe and convenient.
Drawings
FIG. 1 is a graph showing the hydrogen evolution curve of the solid hydrolysis hydrogen production material in the process of producing hydrogen by adding water (the water adding rate is 6.8 mL/min) in example 1.
FIG. 2 is a graph showing hydrogen evolution during the process of producing hydrogen by adding water to the solid hydrolysis hydrogen production material of example 2 (water addition rate of 4 mL/min).
FIG. 3 is a graph showing the relationship between the hydrogen release rate and the water addition rate in the process of producing hydrogen by adding water to the solid hydrolysis hydrogen production material of example 3.
FIG. 4 is a graph showing hydrogen evolution during the process of producing hydrogen by adding water to the solid hydrolysis hydrogen production material of comparative example 1 (water addition rate of 6.8 mL/min).
FIG. 5 is a graph showing hydrogen evolution during the process of producing hydrogen by adding water to the solid hydrolysis hydrogen production material of comparative example 2 (water addition rate of 6.8 mL/min).
FIG. 6 is a diagram showing the structure of an apparatus for producing hydrogen by hydrolysis at atmospheric pressure according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
The invention relates to a composite material for hydrogen production by hydrolysis of magnesium hydride, which is a mixture of magnesium hydride and chloride, and is prepared by mixing magnesium hydride and anhydrous chloride, dissolving the mixture in water and reacting, wherein the mass ratio of the magnesium hydride to the anhydrous chloride is 1: 0.05 to 0.5.
Anhydrous chloride as catalyst, which may be one or more mixture of anhydrous chlorides, preferably anhydrous MgCl2Anhydrous CaCl2Anhydrous AlCl3Anhydrous NiCl2One or more of them.
The mixing method of the magnesium hydride and the anhydrous chloride can be high-speed stirring, grinding or ball milling and the like. In order to improve convenience and reduce cost, the magnesium hydride is stirred at high speed for 1 minute to be fully mixed with the catalyst anhydrous chloride. The mixed composite material is stored in a dry sealed container.
Example 1
Weighing 30g of magnesium hydride, adding 1.5 g of anhydrous magnesium chloride, placing the mixture in a high-speed stirrer, and mixing the mixture in a glove box for 1min to obtain the hydrolysis hydrogen production composite material.
The hydrolysis hydrogen release test is carried out on the composite material, tap water is added at a water adding speed of 6.8mL/min by utilizing a peristaltic pump, the hydrogen release speed is stable, the average speed is 1.2L/min, the hydrogen release amount is 47.3L, the hydrogen release conversion rate is 92.7% (calculated according to 30g of magnesium hydride), the mass hydrogen storage density is 13.4wt% (hydrogen release mass/total mass of a sample), and the hydrogen release curve chart in the process of preparing hydrogen by adding water is shown in figure 1.
Example 2
Weighing 30g of magnesium hydride, adding 6 g of anhydrous nickel chloride, placing the mixture in a high-speed stirrer, and mixing the mixture in a glove box for 1min to obtain the hydrolysis hydrogen production composite material.
And (3) carrying out hydrolysis hydrogen discharge test on the composite material, wherein tap water is added at a water adding speed of 4mL/min by using a peristaltic pump, the hydrogen discharge speed is stable, the average speed is 0.8L/min, the hydrogen discharge amount is 43.9L, the hydrogen discharge conversion rate is 86% (calculated according to 30g of magnesium hydride), and the mass hydrogen storage density is 10.9wt% (hydrogen discharge mass/total sample mass). The hydrogen discharge curve chart in the process of adding water to produce hydrogen is shown in figure 2.
Example 3
Weighing 30g of magnesium hydride, adding 15 g of anhydrous calcium chloride, placing the mixture in a high-speed stirrer, and mixing the mixture in a glove box for 1min to obtain the hydrolysis hydrogen production composite material.
And carrying out hydrolysis hydrogen discharge test on the composite material, and controlling the water adding speed by using a peristaltic pump to add tap water, wherein the water adding speed is respectively 0.85mL/min, 1.8 mL/min and 4mL/min, and the hydrogen discharge speed is respectively 0.3L/min, 0.44L/min and 0.8L/min. The graph of the relationship between the hydrogen release rate and the water adding rate in the process of adding water to prepare hydrogen is shown in figure 3.
Comparative example 1
Weighing 30g of magnesium hydride, adding 0.15 g of anhydrous magnesium chloride, placing the mixture in a high-speed stirrer, and mixing the mixture in a glove box for 1min to obtain the hydrolysis hydrogen production composite material.
The hydrolysis hydrogen release test is carried out on the composite material, tap water is added at a water adding speed controlled by a peristaltic pump, the water adding speed is 6.8mL/min, the mass hydrogen storage density is 14.0wt% (hydrogen release mass/total mass of a sample), the hydrogen release speed is uneven, and the hydrogen release kinetic property is poor. The hydrogen discharge curve chart in the process of adding water to produce hydrogen is shown in figure 4.
Comparative example 2
Weighing 30g of magnesium hydride, adding 18 g of anhydrous magnesium chloride, placing the mixture in a high-speed stirrer, mixing the mixture in a glove box for 1min to obtain a hydrolysis hydrogen production composite material, and performing a hydrolysis hydrogen production test on the composite material, wherein tap water is added at a water adding speed of 6.8mL/min by using a peristaltic pump, and the mass hydrogen storage density of the composite material is reduced to 8.9wt% (hydrogen production mass/total mass of a sample). The hydrogen discharge curve chart in the process of adding water to produce hydrogen is shown in figure 5.
The composite material for hydrogen production by hydrolysis prepared in examples 1 to 3 and comparative examples 1 to 2 was applied to hydrogen production by hydrolysis at normal pressure, and the apparatus for hydrogen production by hydrolysis at normal pressure was constructed by including a water storage tank 1, a transfer pump 2, a reactor 3 and a dryer 4, as shown in fig. 6.
The water storage tank 1 is used for storing water required by hydrolysis, and the added water can be tap water, deionized water, or inorganic salt solutions containing inorganic salts, such as river water, lake water, seawater and the like.
And one end of the delivery pump 2 is connected with a water source, the other end of the delivery pump is connected with a water inlet of the reactor 3, the effect is that water in the water storage tank flows into the reactor, and the flow rate of the delivered water is controlled by the delivery pump 2. The water adding amount and the water adding speed into the reactor 3 are controlled by the delivery pump 2, the flow is monitored by arranging a flow joint at the water inlet of the reactor 3, and the water adding speed are constant and can be adjusted within a certain range in cooperation, so that the requirements of an actual hydrogen fuel cell or other hydrogen-requiring equipment are met conveniently. In order to ensure constant and controllable water inlet rate, the delivery pump 2 can be a peristaltic pump or a syringe pump. The delivery pump 2 is powered by an external mobile battery. Because the water delivery speed is lower, the power requirement on the delivery pump 2 is lower, the voltage and the capacity of the required external mobile battery are both lower, and the weight of the whole hydrogen supply device cannot be increased excessively.
The reactor 3 is a sealed container and is used for filling the composite material 5 for hydrogen production by hydrolysis, the reactor is provided with a water inlet and an air outlet, and the water inlet is connected with the water outlet of the conveying pump 2; the outlet is connected to the inlet of the dryer 4 via a first hydrogen passage 6. The water inlet and the gas outlet of the reactor 3 are both positioned at the topmost end of the reactor 3, the composite material 5 for hydrogen production by hydrolysis is placed at the bottom in the reactor 3, the input water enters from top to bottom, and the hydrogen produced by hydrolysis is discharged from the gas outlet.
The dryer 4 is a sealed container and is provided with an air inlet and an air outlet, a drying agent is filled in the dryer and is used for absorbing a small amount of water vapor brought out by hydrogen generated by hydrolysis reaction, the air inlet is connected with the air outlet of the reactor 3 through a first hydrogen passage 6, the air outlet is arranged below the side surface of the dryer and is connected with a second hydrogen passage 7, and the second hydrogen passage 7 can be directly connected with a hydrogen fuel cell. Therefore, no hydrogen accumulation exists in the whole hydrogen production process, and a high-pressure device is not needed, so that no special pressure-resistant requirement is required on the material.
Wherein, the reactor 3 is arranged into a cylinder with the inner diameter of 6cm and the height of 20cm and is made of metal aluminum. The reactor was placed vertically and the water for the reaction was passed in from the top of the reactor. The peristaltic pump is powered by a section of 3.7V lithium battery. The water storage tank is a cylindrical plastic container with the inner diameter of 3cm and the height of 20 cm. The drying tube is a cylindrical plastic container with an inner diameter of 3cm and a height of 20cm, and desiccant anhydrous CaCl is filled in the drying tube2。
Claims (10)
1. The composite material for preparing hydrogen by hydrolyzing magnesium hydride is characterized by comprising the following components in parts by weight: the composite material is prepared by mixing magnesium hydride and chloride, wherein the mass ratio of the magnesium hydride to the anhydrous chloride is 1: 0.05 to 0.5.
2. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 1, characterized in that: the anhydrous chloride is selected from anhydrous MgCl2Anhydrous CaCl2Anhydrous AlCl3Anhydrous NiCl2One or more of them.
3. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 1, characterized in that: the magnesium hydride and the anhydrous chloride are mixed in a high-speed stirring, grinding or ball milling mode.
4. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 1, characterized in that: the magnesium hydride hydrolysis hydrogen production composite material is applied to a normal pressure hydrolysis hydrogen production device, the normal pressure hydrolysis hydrogen production device comprises a water storage tank (1), a delivery pump (2) and a reactor (3), and the reactor is a sealed container and is used for filling the magnesium hydride hydrolysis hydrogen production composite material (5); one end of the delivery pump is connected with the water storage tank, and the other end of the delivery pump is connected with the water inlet of the reactor; the gas outlet of the reactor (3) is connected with the gas inlet of the dryer through a first hydrogen passage (6); the gas inlet and the gas outlet of the reactor (3) are both positioned at the topmost end of the reactor, and the composite material for hydrogen production by hydrolysis of magnesium hydride is positioned at the bottom in the reactor.
5. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 4, wherein: the dryer (4) is a sealed container, a drying agent is filled in the dryer, an exhaust port is formed in the bottom of the dryer, and a second hydrogen passage (7) is formed in the exhaust port; the second hydrogen passage (7) is connected to a hydrogen fuel cell.
6. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 4, wherein: the water storage tank (1) is used for storing liquid required by hydrolysis, and the liquid is one or more of tap water, deionized water, river water, lake water and seawater.
7. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 4, wherein: the reactor (3) is vertically or obliquely arranged.
8. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 4, wherein: the delivery pump (2) is a peristaltic pump or an injection pump.
9. The composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 4, wherein: a flowmeter is arranged at the water inlet of the reactor (3).
10. A method for preparing the composite material for hydrogen production by hydrolysis of magnesium hydride according to claim 1, characterized in that: the preparation steps are as follows: proportionally mixing magnesium hydride with anhydrous chloride, dissolving in water, and reactionThe anhydrous chloride is selected from anhydrous MgCl2Anhydrous CaCl2Anhydrous AlCl3Anhydrous NiCl2One or more of them.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112357880A (en) * | 2020-11-12 | 2021-02-12 | 中南大学 | High-capacity hydrolysis hydrogen production material, preparation method and application thereof, and hydrogen production device |
| CN112794283A (en) * | 2020-12-31 | 2021-05-14 | 河南中氢动力研究院有限公司 | Seawater hydrogen production and desalination integrated equipment |
| CN113860255A (en) * | 2021-10-27 | 2021-12-31 | 世能氢电科技有限公司 | Method for effectively improving hydrogen production efficiency by hydrolyzing magnesium hydride and application thereof |
| CN114455541A (en) * | 2021-12-24 | 2022-05-10 | 世能氢电科技有限公司 | Magnesium hydride AB material capable of controlling hydrolysis to produce hydrogen and preparation method thereof |
| CN115072660A (en) * | 2022-06-14 | 2022-09-20 | 蓝海易氢动力(青岛)有限公司 | Magnesium hydride composite material, preparation method and application thereof, and hydrogen production method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113860255A (en) * | 2021-10-27 | 2021-12-31 | 世能氢电科技有限公司 | Method for effectively improving hydrogen production efficiency by hydrolyzing magnesium hydride and application thereof |
| CN114455541A (en) * | 2021-12-24 | 2022-05-10 | 世能氢电科技有限公司 | Magnesium hydride AB material capable of controlling hydrolysis to produce hydrogen and preparation method thereof |
| CN115072660A (en) * | 2022-06-14 | 2022-09-20 | 蓝海易氢动力(青岛)有限公司 | Magnesium hydride composite material, preparation method and application thereof, and hydrogen production method |
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Application publication date: 20200512 |