CN113526547A - Preparation method of sulfur poisoning resistant solid oxide fuel cell anode material - Google Patents
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- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
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Abstract
The invention relates to a preparation method of an anti-sulfur poisoning solid oxide fuel cell anode material, which belongs to a layered perovskite oxide, wherein the structural general formula of an active component is AxLn1‑ xTiO4(x is more than or equal to 0 and less than 0.3, ALTO, wherein A represents alkali metal ions, Ln represents rare earth metal ions), tetrabutyl titanate and citric acid are firstly selected to be dissolved in water, corresponding nitrate of A and Ln are added to prepare aqueous solution, excessive glycine is added to prepare active component impregnation liquid, and the impregnation liquid is dropwise added to Sm0.2Ce0.8O2And (SDC) roasting the anode framework at 400 ℃ until the mass of active components accounts for 20-50% of the framework, and finally carrying out high-temperature treatment for 0.5-2 hours to obtain the sulfur poisoning resistant solid oxide fuel cell anode material ALTO/SDC. The alkali metal ions and the layered structure in the composite anode material can adsorb water to form surface hydroxyl, and the surface hydroxyl is formedCan react with sulfur in fuel to generate sulfur dioxide for desorption, thereby inhibiting sulfur poisoning and solving the problem that the anode of the solid oxide fuel cell is easily poisoned by sulfur-containing impurities.
Description
Technical Field
The invention relates to a solid oxide fuel cell anode material, a preparation method and application thereof, in particular to a sulfur poisoning resistant layered perovskite oxide, and a preparation method and application thereof.
Background
The fuel cell is an energy conversion device, can directly convert chemical energy in fuel into electric energy, and has the characteristics of high conversion efficiency, cleanness, no pollution and the like, wherein the Solid Oxide Fuel Cell (SOFC) also has the characteristics of diversified fuels, full solid structure, no need of noble metal and the like. The solid oxide fuel cell can directly use methane as fuel, the main component of natural gas and biomass gas is methane, but when the natural gas or methane is directly used as fuel gas, the anode is subjected to serious sulfur poisoning phenomenon, although the sulfur content can be reduced by pretreatment, the sulfur content is difficult to reach below 50ppm due to technical and cost reasons, and for the solid oxide fuel cell, sulfide with the content higher than 10ppm can cause irreversible poisoning. Therefore, improving the sulfur poisoning resistance of the anode is a difficult and hot problem for commercializing the solid oxide fuel cell.
At present, the research focus for solving the problem of sulfur poisoning is to develop novel anodes, such as using noble metal catalysts, some noble metals have high sulfur poisoning resistance, but the noble metals limit the large-scale application of the noble metals due to the problems of high cost, low storage capacity, stability and the like. Perovskite-like materials such as La0.75Sr0.25Cr0.5Mn0.5O3-δ、Sr2Mg1- xMnxMoO6-δAnd the like, but the structural stability or the electrocatalytic activity of the perovskite materials cannot meet the requirement of high-concentration hydrogen sulfide.
Therefore, it is particularly necessary to develop a sulfur-resistant anode which is low in cost, has excellent catalytic activity and stability, and is simple to prepare. The anode catalyst prepared by the invention contains high-concentration H2S fuel shows excellent electrocatalytic performance and long-term stability, and harmful gas H in fuel gas2S not only does not poison the anode catalyst, but also promotes the reaction to H2Electrocatalytic capacity of. The alkali metal ions and the layered structure in the composite anode material can adsorb water to form surface hydroxyl which can be mixed with fuelSulfur dioxide is generated by the sulfur reaction and is desorbed, so that the sulfur poisoning of the anode material is inhibited, and the problem that the anode of the solid oxide fuel cell is easily poisoned by sulfur-containing impurities is possibly thoroughly solved.
Disclosure of Invention
The invention provides a preparation method of a sulfur poisoning resistant solid oxide fuel cell anode material, which comprises the following specific steps:
1) selecting tetrabutyl titanate, adding a certain amount of citric acid monohydrate and deionized water, and uniformly stirring;
2) selecting nitrates corresponding to A and Ln, adding the nitrates into the mixed solution prepared in the step 1) according to a certain proportion, and uniformly stirring;
3) adding excessive glycine into the aqueous solution prepared in the step 2) to prepare an active component impregnation solution;
4) dripping the dipping liquid prepared in the step 3) into the SDC-based anode framework, roasting for 30 minutes at 400 ℃, repeating for many times until the mass of the active component accounts for 20-50% of the framework, and finally performing high-temperature treatment to obtain the ALnTiO4A solid oxide fuel cell anode material resistant to sulfur poisoning as an active component.
Preferably, the preferable molar ratio of tetrabutyl titanate to citric acid monohydrate in the step 1) is 1: 0.5-1.
Preferably, in the step 2), the element a is one or a combination of Na, Li and K, and the element Ln is one or a combination of La, Pr, Nd, Gd, Y, Sm, Eu and Lu.
Preferably, in the step 2), the molar ratio of A to Ln to Ti is (1.1-1.5) to 1: 1.
Preferably, in the step 3), the molar ratio of (A + Ln + Ti) to glycine is 1: 0.5-1.5.
Preferably, in the step 4), the high-temperature range is 750-1000 ℃, and the treatment time is 0.5-3 hours.
Compared with the prior art, the method for preparing the sulfur poisoning resistant solid oxide fuel cell anode material has the following beneficial effects:
(1) the invention provides a fuel cell anode active material which is easy to prepare, low in cost, and excellent in catalytic performance and stability due to the close combination of an active substance and an SDC-based framework, wherein the influence of sulfur-containing impurities on a fuel cell anode is inhibited by the special layered configuration of a layered perovskite oxide.
(2) The invention introduces alkali metal with low melting point into the solid oxide fuel cell, solves the characteristic that the alkali metal is volatile under the high temperature condition, and solves the problem of sulfur poisoning under the high temperature condition by utilizing the characteristic that the alkali metal absorbs water and is dissociated into surface hydroxyl.
(3) The invention provides a fuel cell anode, which introduces the combustion improver glycine, reduces the sintering temperature and the particle size of the material, improves the catalytic activity of the material, and keeps excellent stability in the fuel containing high-concentration hydrogen sulfide.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is the XRD pattern of the product NLTO powder of the present invention calcined at 800 deg.C for 1 hour, the SDC mechanically mixed with NLTO and calcined at 800 deg.C for 1 hour and the SDC powder;
FIG. 2 is an XRD spectrum of the product NLTO powder of the first embodiment of the invention calcined at 800 ℃ for 1 hour;
FIG. 3 is an XPS spectrum of a product NLTO powder of the first embodiment of the present invention calcined at 800 ℃ for 1 hour;
FIG. 4 shows carbon dioxide temperature programmed desorption (CO) of NLTO product in accordance with an embodiment of the present invention2-TPD) profile;
FIG. 5 shows a water-programmed temperature desorption (H) of the product NLTO according to the present invention2O-TPD) spectrum;
FIG. 6 is SEM images of a SDC framework a) and NLTO/SDC anode material b) of a product of the embodiment of the invention, and TEM images and energy spectrum images of the NLTO/SDC anode material;
FIG. 7 shows a fuel cell at H made of NLTO/SDC as a product of an embodiment of the present invention2Voltage-current and power-current graphs in (1);
FIG. 8 shows a product NLTO/SDC system according to an embodiment of the present inventionThe fuel cell thus obtained contained 1000ppm of H2H of S2Voltage-current and power-current graphs in (1);
FIG. 9 shows fuel cell at 800 deg.C H made of NLTO/SDC as a product of one embodiment of this invention2And contains 1000ppm of H2H of S2EIS diagram in (1);
FIG. 10 shows a fuel cell made of a product NLTO/SDC of an example of the present invention containing 1000ppm H2H of S2A medium stability test result;
FIG. 11 is a comparison of XRD pattern and standard pattern of NYTO product of example two of the present invention after calcination at different temperatures for different times;
FIG. 12 is a comparison of the XRD pattern of NGTO, a product of example two of the present invention, after calcination at different temperatures for different times, with a standard pattern.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The first embodiment is as follows:
0.05mol of tetrabutyl titanate and 0.025mol of citric acid monohydrate are weighed and added with a small amount of deionized water to prepare an aqueous solution. Weighing 0.05mol of NaNO3And 0.05mol of La (NO)3)3·6H2Dissolving O in deionized water to obtain water solution. And mixing the two aqueous solutions, adding 0.075mol of glycine, and dissolving to obtain an active component impregnation liquid. Dripping the prepared dipping liquid into an SDC-based anode framework, roasting for 30 minutes at 400 ℃, repeating for many times until the mass of active components accounts for 20 percent of the framework, and finally carrying out high-temperature treatment at 750 ℃ or 800 ℃ for 0.5 hour or 1 hour to obtain NaLaTiO4(NLTO) solid oxide fuel cell anode material NLTO/SDC resistant to sulfur poisoning as an active component.
Mixing NLTO/SDC with commercial cathode material Ba0.5Sr0.5Co0.8Fe0.2O3-δThe fuel cell sheet was prepared and tested, wherein the effective area of the cell was 0.45cm2. During the electrochemical test, the anode is introduced with 1000ppm H2H of S2As fuel, the flow rate was 80mL/min, and the cathode was directly exposed to air. The prepared cell was tested for current-voltage (I-V) curves using a four-probe mode from an electrochemical workstation (Keithley 2420). Electrochemical Impedance (EIS) was measured using Solartron 1287 and Solartron 1260A at 10mV stimulation voltage in open circuit from 100kHz to 0.1 Hz.
Example two
0.05mol of tetrabutyl titanate and 0.04mol of citric acid monohydrate are weighed and added with a small amount of deionized water to prepare an aqueous solution. 0.065mol LiNO was weighed3And 0.05mol of Y (NO)3)3·6H2Dissolving O in deionized water to obtain water solution. And mixing the two aqueous solutions, adding 0.15mol of glycine, and dissolving to obtain an active component impregnation solution. Dripping the obtained impregnation liquid into SDC-based anode framework, roasting for 30 minutes at 400 ℃, repeating for many times until the mass of active components accounts for 30 percent of the framework, and finally performing high-temperature treatment for 2 hours or 3 hours at 1000 ℃ to obtain NaYTiO4(NYTO) sulfur poisoning resistant solid oxide fuel cell anode material NYTO/SDC as active component.
EXAMPLE III
0.05mol of tetrabutyl titanate and 0.05mol of citric acid monohydrate are weighed and added with a small amount of deionized water to prepare an aqueous solution. Weighing 0.065mol of KNO3And 0.05mol of Gd (NO)3)3·6H2Dissolving O in deionized water to obtain water solution. And mixing the two aqueous solutions, adding 0.225mol of glycine, and dissolving to obtain an active component impregnation liquid. Dripping the prepared dipping solution into an SDC-based anode framework, roasting for 30 minutes at 400 ℃, repeating for many times until the mass of active components accounts for 50 percent of the framework, and finally performing high-temperature treatment at 1000 ℃ for 2 hours or 3 hours to obtain NaGdTiO4(NGTO) sulfur poisoning resistant solid oxide fuel cell anode material NGTO/SDC as an active component.
While the invention has been described with respect to the preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of sulfur poisoning resistant solid oxide fuel cell anode material with a general formula of ALnTiO4/Sm0.2Ce0.8O2(ALTO/SDC, wherein A represents one or more alkali metal ions, and Ln represents one or more rare earth metal ions). The method is characterized by comprising the following specific steps:
1) selecting tetrabutyl titanate, adding a certain amount of citric acid monohydrate and deionized water, and uniformly stirring;
2) selecting nitrates corresponding to A and Ln, adding the nitrates into the mixed solution prepared in the step 1) according to the corresponding proportion of the chemical formula of the target product, and uniformly stirring;
3) adding excessive glycine into the aqueous solution prepared in the step 2) to prepare an active component impregnation solution;
4) dripping the dipping liquid prepared in the step 3) into the SDC-based anode framework, roasting for 30 minutes at 400 ℃, repeating for many times until the mass of the active component accounts for 20-50% of the framework, and finally performing high-temperature treatment to obtain the ALnTiO4A solid oxide fuel cell anode material resistant to sulfur poisoning as an active component.
2. The method for preparing the sulfur poisoning resistant solid oxide fuel cell anode material according to claim 1, wherein the molar ratio of tetrabutyl titanate to citric acid monohydrate in the step 1) is 1: 0.5-1.
3. The method for preparing the anode material of the solid oxide fuel cell resistant to sulfur poisoning according to claim 1, wherein in the step 2), the element A is preferably one or a combination of Na, Li and K, and the element Ln is preferably one or a combination of La, Pr, Nd, Gd, Y, Sm, Eu and Lu.
4. The method for preparing the anode material of the solid oxide fuel cell resistant to sulfur poisoning as claimed in claim 1, wherein in the step 2), the molar ratio of A: Ln: Ti is (1.1-1.5): 1: 1.
5. The method for preparing the anode material of the solid oxide fuel cell resistant to sulfur poisoning according to claim 1, wherein in the step 3), the molar ratio of (A + Ln + Ti) to glycine is 1: 0.5-1.5.
6. The method for preparing the sulfur poisoning resistant solid oxide fuel cell anode material according to claim 1, wherein in the step 4), the high temperature is 750 to 1000 ℃ and the processing time is 0.5 to 3 hours.
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Citations (5)
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| CN1597097A (en) * | 2004-08-30 | 2005-03-23 | 南京大学 | Preparation method of high specific surface tantalate and niobate photo catalyst |
| US20130045437A1 (en) * | 2011-08-18 | 2013-02-21 | Fanglin Chen | Sulfur-Tolerant Anode Material for Direct Hydrocarbon Solid Oxide Fuel Cells |
| US20180019478A1 (en) * | 2016-07-14 | 2018-01-18 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | Strontium magnesium molybdenum oxide material having double perovskite structure and method for preparing the same |
| CN110429285A (en) * | 2019-07-15 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | A kind of SOFC anode electrode and preparation method thereof with sulfur resistance |
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- 2021-06-02 CN CN202110616288.5A patent/CN113526547A/en active Pending
Patent Citations (5)
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| CN1597097A (en) * | 2004-08-30 | 2005-03-23 | 南京大学 | Preparation method of high specific surface tantalate and niobate photo catalyst |
| US20130045437A1 (en) * | 2011-08-18 | 2013-02-21 | Fanglin Chen | Sulfur-Tolerant Anode Material for Direct Hydrocarbon Solid Oxide Fuel Cells |
| US20180019478A1 (en) * | 2016-07-14 | 2018-01-18 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | Strontium magnesium molybdenum oxide material having double perovskite structure and method for preparing the same |
| CN110429285A (en) * | 2019-07-15 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | A kind of SOFC anode electrode and preparation method thereof with sulfur resistance |
| CN112844486A (en) * | 2021-01-29 | 2021-05-28 | 南京工程学院 | For CO2Chemically fixed high-stability catalyst ZIF-8/CeO2Composite material and preparation method thereof |
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