CN114108024B - Coal-based sacrificial electrode and preparation method and application thereof - Google Patents
Coal-based sacrificial electrode and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a coal-based sacrificial electrode and a preparation method and application thereof. The preparation method of the coal-based sacrificial electrode comprises the following steps: (1) Forming a mixture of raw materials comprising 2-8 parts by weight of coal, 1-6 parts by weight of alkali-activated biomass and 0.5-5 parts by weight of graphite; (2) pressing and molding the mixture to obtain a raw material; (3) And carbonizing the raw material at 600-1000 ℃ in an inert atmosphere to obtain the coal-based sacrificial electrode. The coal-based sacrificial electrode prepared by the method can improve the durability of the electrode on the premise of keeping low energy consumption for hydrogen production by water electrolysis.
Description
Technical Field
The invention relates to a coal-based sacrificial electrode and a preparation method and application thereof.
Background
Hydrogen is considered to be a novel non-polluting energy carrier. The heat generated per mass of hydrogen is much higher than that of coal, oil and natural gas of the same mass. Compared with the traditional thermochemical hydrogen production technology, the water electrolysis hydrogen production technology has the advantages of no pollution, high purity of the produced hydrogen and the like. However, the hydrogen production by electrolyzing water has the disadvantages of low efficiency, large energy consumption and the like.
CN112795948A discloses a method for producing hydrogen by electrolyzing coal water slurry by using a graphite felt electrode. The method comprises the following steps: (1) Sequentially crushing, grinding and screening raw coal to ensure that the granularity is less than 200 meshes to obtain refined coal powder; (2) Adding the refined coal powder and iron ions into an acid solution to obtain a coal water slurry mixture; (3) The graphite felt is used as an anode, a cathode is matched, and the water-coal-slurry mixture is used as an electrolyte to form an electrochemical reaction device for electrolyzing the water-coal-slurry to prepare hydrogen. The method forms coal into water-coal-slurry, and realizes the reduction of the electrode potential in the water electrolysis process through the collision between carbon particles and an anode plate or the collision between the carbon particles and an oxidizing group. The reaction process involves the diffusion of particles in the slurry, the generation of oxidizing groups at the electrode and the transfer in the electrolyte, which results in that the coal water slurry can obtain lower electrode potential than the electrolyzed water only at low current density, and the reduction of the electrode potential is difficult to achieve at high current density.
CN113388857A discloses a method for preparing an integral sacrificial anode for hydrogen production by electrolyzing water by utilizing wood fiber biomass. The method comprises the following steps: (1) Crushing and screening wood fiber biomass to a required granularity; (2) Performing hot alkali liquor activation on the raw material obtained in the step (1) to remove lignin and hemicellulose; (3) Filtering and washing the sample obtained in the step (2) to obtain a biomass raw material after alkali activation; (4) Fully mixing the biomass raw material subjected to alkali activation with conductive particles, an electrocatalyst and a binder to obtain a mixture; (5) Adding deionized water into the mixture, and then pressing and molding in a mold to obtain an electrode green body; (6) Carrying out pyrolysis carbonization on the electrolytic green body to obtain an electrode mature blank; and (7) shaping the electrode mature blank to obtain a final electrode. The electrode obtained by the method has low strength, and the loss of the anode sheet in the electrolytic process is large, so that the energy consumption for hydrogen production is high.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a coal-based sacrificial electrode for hydrogen production by water electrolysis, where the coal-based sacrificial electrode prepared by the method can reduce energy consumption for hydrogen production by water electrolysis, and has good durability. Another object of the present invention is to provide a coal-based sacrificial electrode. Still another object of the present invention is to provide an application of the coal-based sacrificial electrode in hydrogen production by water electrolysis.
The technical purpose is realized by the following technical scheme.
On one hand, the invention provides a preparation method of a coal-based sacrificial electrode, which comprises the following steps:
(1) Forming a mixture of raw materials comprising 2-8 parts by weight of coal, 1-6 parts by weight of alkali-activated biomass and 0.5-5 parts by weight of graphite;
(2) Pressing and molding the mixture to obtain a raw material;
(3) And carbonizing the raw material at 600-1000 ℃ in an inert atmosphere to obtain the coal-based sacrificial electrode.
According to the preparation method of the invention, preferably, the coal is selected from one of lignite or bituminous coal, and the biomass is lignocellulose biomass.
According to the preparation method of the present invention, preferably, the coal is deashed coal washed with 10 to 25wt% of hydrochloric acid;
activating the biomass for 1-8 h at 60-100 ℃ by using a sodium hydroxide solution to obtain the biomass after alkali activation.
According to the preparation method of the present invention, preferably, in the step (1), raw materials including coal, biomass after alkali activation, graphite and water are mixed to obtain a mixed solution; and drying the mixed solution to obtain a mixture.
According to the preparation method of the invention, preferably, the stirring speed in the mixing process is 200-1000 r/min, and the mixing time is 12-36 h; the drying temperature is 70-140 ℃, and the drying time is 4-80 h.
According to the preparation method of the present invention, preferably, the compression molding is performed on a tablet press, and in the step (2), the compression molding is performed on the tablet press, and the tablet compression strength is 1 to 15MPa.
According to the production method of the present invention, preferably, in the step (3), the inert atmosphere is an argon atmosphere.
According to the preparation method of the present invention, preferably, the flow rate of the inert gas is 100 to 300mL/min; the heating rate from room temperature to carbonization temperature is 5-20 ℃/min.
In another aspect, the invention provides a coal-based sacrificial electrode prepared by the above method.
In another aspect, the invention provides an application of the coal-based sacrificial electrode prepared by the method in hydrogen production by water electrolysis, wherein the temperature is 25 ℃ and the current density is 50mA/cm 2 The durability of the sacrificial electrode is more than 4h by adopting a constant current electrolysis test.
The invention constructs the sacrificial electrode by taking coal, alkali-activated biomass and graphite as raw materials in proper proportion, and improves the durability of the sacrificial electrode on the premise of keeping lower energy consumption for hydrogen production by water electrolysis.
Detailed Description
The present invention is described in more detail below, but the present invention is not limited thereto.
< preparation method of coal-based sacrificial electrode >
The preparation method of the coal-based sacrificial electrode comprises the following steps: (1) a step of forming a mixture; (2) a step of molding; and (3) carbonizing. As described in detail below.
Step of Forming the mixture
A feedstock comprising coal, alkali-activated biomass, and graphite is formed into a mixture. The coal-based sacrificial anode can be obtained by co-molding and co-pyrolysis by using acid-washed coal, alkali-activated biomass and graphite in a proper ratio as raw materials, using coal as a carbon source, using graphite as conductive particles and using alkali-activated biomass as a binder.
In the invention, the using amount of the coal after acid washing is 2 to 8 parts by weight; preferably 3 to 7 parts by weight; more preferably 4 to 6 parts by weight. Therefore, sufficient carbon source can be provided, the oxidation reaction is ensured to be carried out, and the coal-based sacrificial electrode with proper pore structure and strength can be obtained, so that the energy consumption of hydrogen production by water electrolysis is reduced, and the durability of the electrode is improved.
In the present invention, the coal is preferably one of lignite or bituminous coal. According to one embodiment of the invention, the coal is Mongolian Hu Shuotu bituminous coal. The particle size of the coal may be 200 to 400 mesh. The coal has proper carbon content and volatile content, and is favorable for forming a coal-based sacrificial electrode with proper pore structure and strength.
And (3) carrying out acid washing treatment on the coal to obtain the acid-washed coal. Specifically, the coal is washed and delimed with 10 to 25wt% hydrochloric acid to obtain the acid-washed coal. Preferably, the concentration of hydrochloric acid is 15 to 20wt%. This can eliminate the effect of the mineral component on the sacrificial anode performance.
In the invention, the amount of the biomass after alkali activation is 1 to 6 parts by weight; preferably 2 to 5 parts by weight; more preferably 3 to 4 parts by weight. Therefore, the coal-based sacrificial electrode has proper strength and a proper pore structure, so that the energy consumption of hydrogen production by water electrolysis is reduced, and the durability of the electrode is improved.
In the present invention, the biomass is a lignocellulosic biomass. Preferably, the biomass is selected from one or more of corn stover, corn cobs, rice, pine wood. According to one embodiment of the invention, the biomass is corn stover. The particle size of the biomass can be 200-300 meshes. Thus, the strength of the sacrificial electrode can be ensured, and the durability of the sacrificial electrode can be improved. The coal, the corn stalks and the graphite are jointly used as raw materials, the coal is cheaper and more easily obtained compared with biomass, and the durability of the electrode can be improved on the basis of lower energy consumption of hydrogen production by electrolyzing water by adding a proper amount of coal.
And (3) activating the biomass with alkaline liquor to obtain the biomass subjected to alkaline activation. The alkali solution may be sodium hydroxide solution. The concentration of the sodium hydroxide solution can be 0.5-5 wt%; preferably 1.5 to 2.5wt%. The mass ratio of the sodium hydroxide to the biomass can be (1-5) to 1; preferably 2:1. The activation temperature can be 60-100 ℃; preferably 70 to 90 ℃; more preferably 75 to 85 ℃. The activation time can be 1-8 h; preferably 2 to 6 hours; more preferably 3 to 5 hours. This can improve the binding properties of the biomass.
In the invention, the amount of graphite is 0.5-5 parts by weight; preferably 1 to 4 parts by weight; more preferably 2 to 3 parts by weight. The graphite may be white Cha Gan graphite. Thus being beneficial to increasing the conductivity of the coal-based sacrificial electrode, reducing the energy consumption of hydrogen production by water electrolysis and improving the durability of the electrode.
In the present invention, the raw materials may be mixed using an aqueous solution mixing method, a milling mixing method, or a mechanical mixing method to form a mixture. Preferably, an aqueous solution mixing method is employed. Specifically, raw materials comprising the coal after acid washing, the biomass after alkali activation, graphite and water are mixed to obtain a mixed solution; and drying the mixed solution to obtain a mixture. In certain embodiments, the feedstock consists of acid-washed coal, alkali-activated biomass, graphite, and water. The dosage of the water can be 2 to 5 times of the total volume of other raw materials; preferably 3 to 4 times.
The mixing can be carried out under stirring. The stirring speed can be 200-1000 r/min; preferably 400-800 r/min; more preferably 500 to 700r/min. The mixing time can be 12-36 h; preferably 20 to 30 hours; more preferably 22 to 27 hours. This facilitates the formation of a homogeneous mixed liquor.
The drying temperature can be 70-140 ℃; preferably 80 to 120 ℃; more preferably from 90 to 110 ℃. The drying time can be 40-80 h; preferably 50 to 70 hours; more preferably 55 to 65 hours.
Step of Forming
And pressing and molding the mixture to obtain the raw material. Compression molding may be performed on a tablet press. The tablet press may be an infrared tablet press. The tabletting strength can be 1-15 MPa; preferably 7 to 13MPa; more preferably 8 to 11MPa.
Step of carbonization
And carbonizing the raw material to obtain the coal-based sacrificial electrode.
The carbonization treatment is performed in an inert atmosphere. Preferably, the inert atmosphere is an argon atmosphere. The argon atmosphere can still keep inertia under the high-temperature condition, is favorable for carbonization, and improves the durability of the sacrificial electrode.
The carbonization temperature is 600-1000 ℃; preferably 700 to 950 ℃; more preferably 750 to 900 ℃. Thus being beneficial to improving the electrical property of the electrode and reducing the energy consumption of hydrogen production by electrolyzing water.
The temperature rise rate at which the carbonization temperature (for example, 600 to 1000 ℃) is raised from room temperature (for example, 25 ℃) may be 5 to 20 ℃/min; preferably 8-15 ℃/min; more preferably from 9 to 12 ℃/min.
The flow rate of the inert gas is 100-300 mL/min; preferably 150-250 mL/min; more preferably 200 to 250mL/min.
< electrode and use thereof >
The coal-based sacrificial electrode is prepared by the method.
The invention also provides application of the coal-based sacrificial electrode in water electrolysis. With platinum electrode (10X 0.1mm, effective area 2 cm) 2 ) Is the cathode. In Hg/Hg 2 SO 4 As a reference electrode. The coal-based sacrificial electrode (phi =13mm, half of which is immersed in electrolyte and has effective area1.33cm 2 ) As an anode. A water electrolysis hydrogen production system is constructed by adopting a east China electrochemical workstation (DH 7000) and a three-electrode H-type diaphragm electrolytic cell (the diaphragm is a Nafion 117 proton exchange membrane).
The test is carried out by adopting a linear sweep voltammetry under the conditions that the temperature is 25 ℃, the potential range is 0-2V and the sweep rate is 0.02V/s. The coal-based sacrificial electrode is 10mA/cm 2 The potential of (1) is less than 1000mV; preferably less than 960mV; more preferably 920 to 960mV. The coal-based sacrificial electrode is 50mA/cm 2 The potential at time is less than 1800mV; preferably less than 1750mV; more preferably 1650 to 1720mV.
The constant current electrolysis test is adopted, the test temperature is 25 ℃, and the current density is 50mA/cm 2 . The anode electrode is less than 2V; preferably less than 1.9V; more preferably 1.7 to 1.85V. The durability of the anode is more than 3h; preferably, greater than 4h.
Example 1
The Mongolian Hu Shuotu bituminous coal with the grain size of 200-400 meshes is subjected to deashing treatment by using 18wt% of hydrochloric acid to obtain the deashed bituminous coal. The corn straw with the grain diameter of 200-300 meshes is activated for 4 hours at 80 ℃ by adopting a sodium hydroxide solution with the mass fraction of 2 wt%. The mass ratio of the sodium hydroxide to the corn stalks is 2:1. Fully washing the activated solid sample by using deionized water to obtain biomass activated by alkali;
5 parts by weight of the coal after acid washing, 3 parts by weight of the biomass after alkali activation, and 2 parts by weight of Baiyin Chagan graphite were thoroughly mixed and ground. 0.2g of the above mixture was taken out and tabletted on a tabletting machine with a tabletting strength of 10MPa to obtain a raw material.
Carbonizing the raw material under the conditions of argon atmosphere and carbonization temperature of 800 ℃ to obtain the coal-based sacrificial electrode
Wherein the flow rate of argon is 200mL/min, and the heating rate is 10 ℃/min.
Comparative examples 1 to 3
The procedure of example 1 was repeated, except that the amounts of the acid-washed coal, the alkali-activated biomass, and the Bai Yincha dry graphite were as shown in table 1.
TABLE 1
Comparative example 4
The procedure of example 1 was repeated, except that the carbonization temperature was 400 ℃.
Examples of the experiments
With platinum electrode (10X 0.1mm, effective area 2 cm) 2 ) As cathode, hg/Hg 2 SO 4 As a reference electrode, the anode was used as shown in table 2, and a hydrogen production system by electrolysis of water was constructed using a east china electrochemical workstation (DH 7000) and a three-electrode H-type diaphragm electrolyzer (the diaphragm was Nafion 117 proton exchange membrane). The linear sweep voltammetry test (LSV test) and the constant current electrolysis test were performed separately.
The test conditions of the linear sweep voltammetry are as follows: the temperature is 25 ℃, the potential interval is 0-2V, and the scanning speed is 0.02V/s. Respectively obtaining the current-voltage curve of each system at 10mA/cm according to linear scanning 2 And 50mA/cm 2 The current density of (a) and the corresponding potential.
The constant current electrolysis test conditions were: the temperature is 25 ℃, and the current density is 50mA/cm 2 . The anode potential and time to failure were recorded. The failure criteria were: the anode electrode is immersed in the electrolyte and is completely oxidized to generate carbon dioxide; or the anode electrode is dissolved before the oxidation reaction is finished, so that the hydrogen production by water electrolysis cannot be carried out; and taking the time which is reached first by the two times as the failure time.
TABLE 2
Note: the effective area of the sacrificial electrode of example 1 was 1.33cm 2 Half immersed in the electrolyte;
the effective area of the Pt electrode is 2cm 2 。
As can be seen from Table 2, the sacrificial electrode material of comparative example 1, which does not contain coal, failed after 1.5 hours of electrolysis; the sacrificial electrode raw material of comparative example 2 does not contain biomass, and the sacrificial electrode raw material fails after 0.5h of electrolysis; while the electrolysis time of the sacrificial electrode of example 1 may reach 4 hours. The combination of coal and biomass can improve the durability of the sacrificial electrode, and the sacrificial electrolysis has lower potential, thereby reducing the energy consumption of hydrogen production by water electrolysis. Therefore, the sacrificial electrode greatly improves the durability on the basis of keeping lower energy consumption for hydrogen production by water electrolysis.
The consumption of the raw materials of the sacrificial electrode in the comparative example 3 is different from that of the sacrificial electrode in the embodiment 1, and the consumption of graphite in the raw materials is increased in the sacrificial electrode in the comparative example 3, so that the cost is increased, the energy consumption for hydrogen production by water electrolysis is increased, and the durability of the sacrificial electrode is reduced. It follows that the amounts of the components in the starting materials are not a routine choice.
The sacrificial electrolyte of comparative example 4 is carbonized at a lower temperature, which impairs the electrical properties of the sacrificial electrode.
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (8)
1. The preparation method of the coal-based sacrificial electrode is characterized by comprising the following steps:
(1) Forming a mixture of raw materials consisting of 4-6 parts by weight of coal, 3-4 parts by weight of biomass activated by alkali and 2-3 parts by weight of graphite; the coal is soft coal washed and deashed by 10 to 25 weight percent hydrochloric acid;
(2) Pressing and molding the mixture to obtain a raw material;
(3) Carbonizing the raw material in an argon atmosphere at the temperature of 700-950 ℃ to obtain a coal-based sacrificial electrode; the flow rate of argon gas is 100-300 mL/min; the heating rate from room temperature to carbonization temperature is 5-20 ℃/min.
2. The method of claim 1, wherein the biomass is a lignocellulosic biomass.
3. The method of claim 1, wherein:
activating the biomass for 1-8 h at 60-100 ℃ by using a sodium hydroxide solution to obtain the biomass after alkali activation.
4. The method according to claim 1, wherein in the step (1), raw materials consisting of coal, alkali-activated biomass, graphite and water are mixed to obtain a mixed solution; and drying the mixed solution to obtain a mixture.
5. The preparation method according to claim 4, wherein the stirring speed in the mixing process is 200-1000 r/min, and the mixing time is 12-36 h; the drying temperature is 70-140 ℃, and the drying time is 4-80 h.
6. The production method according to claim 5, wherein in the step (2), the compression molding is performed on a tablet press, and the tablet strength is 1 to 15MPa.
7. A coal-based sacrificial electrode, characterized in that it is prepared by the preparation method as claimed in any one of claims 1 to 6.
8. Use of the coal-based sacrificial electrode in the electrolysis of water to produce hydrogen according to claim 7, characterized in that the temperature is 25 ℃ and the current density is 50mA/cm 2 The durability of the sacrificial electrode is more than 4h.
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