CN112921341A - Efficient reaction system for coupling small molecular catalytic oxidation and hydrogen production - Google Patents
Efficient reaction system for coupling small molecular catalytic oxidation and hydrogen production Download PDFInfo
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Abstract
The invention discloses a high-efficiency micromolecule catalytic oxidation and hydrogen production coupled reaction system, which comprises an electrolytic cell and a two-electrode coupled reaction mechanism, wherein the two-electrode coupled reaction mechanism comprises a hydrogen precipitation cathode and a No. I micromolecule oxidation anode which are respectively connected with the positive electrode and the negative electrode of a No. I external power supply; the device also comprises an oxygen reduction reaction mechanism and a proton exchange membrane, wherein the oxygen reduction reaction mechanism comprises an oxygen reduction cathode and a small molecular oxidation anode II which are respectively connected with the anode and the cathode of the external power supply II; the proton exchange membrane is arranged between the hydrogen evolution cathode and the I-type small molecule oxidation anode, and the interior of the electrolytic cell is divided into a I-type electrolytic area and a II-type electrolytic area; no. I electrolysis district and No. II electrolysis district fill electrolyte. The invention realizes high hydrogen yield and biomass oxidation rate and improves energy conversion efficiency.
Description
Technical Field
The invention belongs to the technical field of biomass catalytic conversion and chemical engineering, and particularly relates to a high-efficiency reaction system for coupling small-molecule catalytic oxidation and hydrogen production.
Background
Due to the increased environmental pollution and the consumption of fossil fuels, there is a need to find eco-friendly renewable energy sources. Hydrogen energy is one of the most desirable alternative energy carriers due to its clean, sustainable and renewable advantages. Conventional routes to large scale production of hydrogen include steam reforming of methane and coal gasification to produce hydrogen and conversion of water to hydrogen (H)2) The former process releases a large amount of carbon dioxide, which is the most important greenhouse gas. And the latter catalytically produces H by water decomposition2Although a promising and environmentally sustainable way of production, there are still drawbacks: for example, due to the slow kinetics of the anodic Oxygen Evolution Reaction (OER), considerable overpotentials are often required to produce hydrogen at appreciable rates. There have been many recent studies that have shown that this limitation can be overcome by coupling the traditional OER with the Hydrogen Evolution Reaction (HER) with a more facile oxidation of small molecules. Numerous research works have demonstrated that the introduction of molecules such as methanol, ethanol, hydrazine, 5-hydroxymethylfurfural, and urea, etc., can increase the efficiency of energy conversion.
In the last decade, researchers have made a lot of research work to find excellent biomass small-molecule oxidation reaction (BOR) electrocatalysts, and through doping, anion replacement, defect engineering, etc., the kinetics of the catalyst reaction is improved, and many electrocatalysts such as alloys, metal oxides, sulfides, phosphides, nitrides, etc., with excellent performance and low cost are obtained. However, although these catalysts show excellent catalytic conversion performance of biomass, with the conventional two-electrode (BOR-HER) coupled system, due to the inevitable competition of OER in the aqueous electrolyte, the biomass oxidation reaction can only be operated at a low potential with a relatively low current density, and thus the reaction rate and conversion efficiency are greatly reduced, failing to meet the requirements of industrial production.
Disclosure of Invention
The invention aims to overcome the defect of the existing method for catalytically producing H by water decomposition2The system has the defects, and the aim is to provide a reaction system for coupling the high-efficiency small-molecule catalytic oxidation and hydrogen production.
The invention is realized by the following technical scheme:
a reaction system for coupling high-efficiency micromolecule catalytic oxidation with hydrogen production comprises an electrolytic cell and a two-electrode coupling reaction mechanism, wherein the two-electrode coupling reaction mechanism comprises a hydrogen precipitation cathode and a No. I micromolecule oxidation anode which are respectively connected with the anode and the cathode of a No. I external power supply; the device also comprises an oxygen reduction reaction mechanism and a proton exchange membrane, wherein the oxygen reduction reaction mechanism comprises an oxygen reduction cathode and a small molecular oxidation anode II which are respectively connected with the anode and the cathode of the external power supply II; the proton exchange membrane is arranged between the hydrogen evolution cathode and the I-type small molecule oxidation anode, and the interior of the electrolytic cell is divided into a I-type electrolytic area and a II-type electrolytic area; no. I electrolysis district and No. II electrolysis district fill electrolyte.
In the technical scheme, the electrolyte filled in the No. I electrolysis region is alkaline electrolyte; the electrolyte filled in the No. II electrolysis area is alkaline electrolyte added with biomass micromolecules.
In the technical scheme, the hydrogen evolution cathode and the oxygen reduction cathode are commercial Pt/C electrodes.
In the technical scheme, the hydrogen evolution cathode, the I small molecular oxidation anode, the oxygen reduction cathode and the II small molecular oxidation anode are immersed in the electrolyte.
In the technical scheme, the No. I small molecular oxidation anode and the No. II small molecular oxidation anode are hydrotalcite nanosheet array electrodes.
The invention has the beneficial effects that:
the invention provides a micromolecule capable of realizing high-efficiency biomassThe catalytic oxidation and hydrogen production coupled reaction system introduces an oxygen reduction reaction system (ORR) into a traditional two-electrode (BOR-HER) coupled reaction system, simultaneously realizes high hydrogen yield and biomass oxidation rate, avoids energy consumption caused by competition of oxygen precipitation reaction, and improves energy conversion efficiency. Compared with the reaction of the traditional two-electrode (BOR-HER) coupled reaction system, the high value-added oxidation product and H2The yield is respectively improved by 68 times and 46 times, and the system can be driven by using a 3V solar cell, thereby proving the super practicability.
Drawings
FIG. 1 is a schematic structural diagram of a reaction system for coupling high-efficiency small-molecule catalytic oxidation and hydrogen production;
FIG. 2 is a graph showing the variation of the content of substances in the process of oxidizing biomass micromolecules 5-hydroxymethylfurfural by using a reaction system coupling efficient micromolecule catalytic oxidation and hydrogen production in example 2 of the present invention;
FIG. 3 is a graph of data comparing the yields of 2, 5-furandicarboxylic acid (FDCA) from a system constructed in example 2 of the present invention and a conventional two-electrode system;
FIG. 4 is a graph of data comparing hydrogen production for a system constructed in accordance with example 2 of the present invention with a conventional two-electrode system.
Wherein:
1 electrolytic cell
2 hydrogen evolution cathode
3I small molecular oxidation anode
4 proton exchange membrane
5I external power supply
6 oxygen reduction cathode
No. 7 II small molecule oxidation anode
8 II external power supply
No. 9I electrolysis zone
No. 10 II electrolysis zone.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical scheme of the invention better understood by those skilled in the art, the technical scheme of the high-efficiency small-molecule catalytic oxidation and hydrogen production coupled reaction system of the invention is further described by combining the drawings of the specification and through a specific implementation mode.
Example 1
As shown in fig. 1, a high-efficiency reaction system for coupling small-molecule catalytic oxidation with hydrogen production comprises an electrolytic cell 1 and a two-electrode coupling reaction mechanism, wherein the two-electrode coupling reaction mechanism comprises a hydrogen evolution cathode (HER)2 and a No. i small-molecule oxidation anode (BOR)3 which are respectively connected with the positive electrode and the negative electrode of a No. i external power supply 5; the device also comprises an oxygen reduction reaction mechanism and a proton exchange membrane 4, wherein the oxygen reduction reaction mechanism comprises an oxygen reduction cathode (ORR)6 and a small molecular oxidation anode (BOR)7 which are respectively connected with the anode and the cathode of a No. II external power supply 8; the proton exchange membrane 4 is arranged between the hydrogen evolution cathode 2 and the I-type small molecular oxidation anode 3, and divides the interior of the electrolytic cell 1 into a I-type electrolytic area 9 and a II-type electrolytic area 10; no. I electrolysis zone 9 and No. II electrolysis zone 10 are filled with electrolyte.
The electrolyte filled in the No. I electrolysis region 9 is alkaline electrolyte; the electrolyte filled in the No. II electrolysis area 10 is alkaline electrolyte added with biomass micromolecules.
The hydrogen evolution cathode 2 and the oxygen reduction cathode 6 are commercial Pt/C electrodes.
The hydrogen separation cathode 2, the I small molecular oxidation anode 3, the oxygen reduction cathode 6 and the II small molecular oxidation anode 7 are immersed in the electrolyte.
The electrolytic tank 1 is a glass electrolytic tank.
The No. I small molecular oxidation anode 3 and the No. II small molecular oxidation anode 7 are cobalt-iron hydrotalcite nanosheet array electrodes.
The preparation method of the hydrotalcite nanosheet array electrode comprises the following steps:
respectively carrying out ultrasonic treatment on the foamed nickel of the conductive substrate for 10min by using absolute ethyl alcohol, acetone and deionized water, and removing impurities on the surface;
(ii) preparation of 0.5mg/mL cobalt nitrate (Co (NO)3)2) 0.25mg/mL ferrous sulfate (FeSO)4) 50mL of the mixed salt solution is used as an electrolyte solution;
and (iii) in the electrolyte solution prepared in the step (i), taking a saturated calomel electrode as a reference electrode and a platinum wire as a counter electrode, directly growing a ferrocobalt hydrotalcite nanosheet array on the foamed nickel by using a potentiostatic method, setting the potential of electrochemical synthesis to be-1V, setting the synthesis time to be 100s, and setting the synthesis temperature to be 25 ℃.
In the embodiment, biomass micromolecules 5-hydroxymethylfurfural (5-HMF) are oxidized to obtain 2, 5-furandicarboxylic acid (FDCA) with huge application potential, and hydrogen is efficiently produced at the same time.
In this embodiment, the voltage of the external power supply 5 i is 1V; the voltage of the external power supply 8 No. II is 2V; the No. I small molecular oxidation anode 3 and the No. II small molecular oxidation anode 7 both adopt cobalt-iron hydrotalcite nanosheet array electrodes; the alkaline electrolyte filled in the No. I electrolysis region 9 is 1.0M KOH aqueous solution; electrolytic zone II, 10, was filled with electrolyte as a 1.0M aqueous KOH solution containing 50mM 5-HMF.
For further proving the effect of the system of the present invention, as a comparison, a conventional two-electrode (BOR-HER) coupled system reaction is constructed, the electrode material and the electrolyte are used, and the voltage selection is the same as that of the reaction system coupling the high-efficiency small-molecule catalytic oxidation and hydrogen production in this embodiment.
Under the above conditions, the reaction system of the present embodiment, which couples the high-efficiency small-molecule catalytic oxidation and hydrogen production, is operated for about 30 minutes, the electrolyte in the reaction process is collected, the content of substances in the electrolyte in the reaction process is analyzed by using high performance liquid chromatography HPLC, and the conversion rate and selectivity of the product are calculated.
As shown in fig. 2, as the reaction proceeds, 5-hydroxymethylfurfural (5-HMF) is gradually oxidized in the system to obtain a final product 2, 5-furandicarboxylic acid (FDCA), and after the reaction is finished, 5-hydroxymethylfurfural (5-HMF) is completely converted into the product 2, 5-furandicarboxylic acid (FDCA), no other by-product is generated, and the conversion rate and the selectivity are both greater than 99%.
As shown in FIGS. 3 and 4, the 2, 5-furandimethanol of the system constructed in this example was reacted during the same reaction timeThe yield of acid (FDCA) and hydrogen is far greater than that of the traditional two-electrode (BOR-HER) coupling system, and the high value-added oxidation products and H2The yield is improved by 68 times and 46 times respectively.
Example 2
Based on example 1, this example oxidizes small molecule furfuryl alcohol to obtain furoic acid, while efficiently producing hydrogen.
In this embodiment, the voltage of the external power supply 5 i is 1V; the voltage of the external power supply 8 No. II is 2V; the No. I micromolecular oxidation anode 3 and the No. II micromolecular oxidation anode 7 both adopt cobalt-aluminum hydrotalcite nanosheet array electrodes; the alkaline electrolyte filled in the No. I electrolysis region 9 is 1.0M KOH aqueous solution; electrolytic zone II, 10, was filled with electrolyte as a 1.0M aqueous KOH solution containing 10mM furfuryl alcohol.
Example 3
Based on example 1, this example oxidizes small-molecule benzyl alcohol to obtain benzoic acid, and simultaneously produces hydrogen gas with high efficiency.
In this embodiment, the voltage of the external power supply 5 i is 1V; the voltage of the external power supply 8 No. II is 2V; the No. I small molecular oxidation anode 3 and the No. II small molecular oxidation anode 7 both adopt nickel iron hydrotalcite nanosheet array electrodes; the alkaline electrolyte filled in the No. I electrolysis region 9 is 1.0M KOH aqueous solution; electrolytic zone II, 10, was filled with electrolyte as a 1.0M aqueous KOH solution containing 10mM benzyl alcohol.
The working principle of the invention is as follows:
in the novel system, the No. I electrolysis area uses alkaline electrolyte, and the No. II electrolysis area uses alkaline electrolyte added with small molecules. After the external power supply is electrified, the surface of a Hydrogen Evolution (HER) cathode in the No. I electrolysis area is subjected to water molecule reduction to form hydrogen reaction, the water molecules produce hydrogen through electrons transmitted by an external circuit, and meanwhile, protons are transmitted to the No. II electrolysis area through a proton exchange membrane. The No. II electrolysis area is a core component of the system, wherein, biomass micromolecule oxidation reaction and oxygen precipitation reaction occur on the surface of the No. I micromolecule oxidation anode, and meanwhile, micromolecule oxidation reaction and oxygen precipitation reaction occur on the surface of the No. II micromolecule oxidation anode in the No. II electrolysis area. In the No. I small molecular oxidation anodeOxygen generated on the surfaces of the electrode and the II small-molecule oxidation anode is reduced on the surface of an oxygen reduction cathode (ORR), and an intermediate product HO generated by reduction is generated2Further participate in the small molecule oxidation reaction on the surface of the small molecule oxidation anode, thereby improving the oxidation efficiency and avoiding O2Energy loss due to precipitation.
Compared with the existing small molecule oxidation technology, the novel system designed by the invention has the following advantages:
the traditional small molecule oxidation process needs high temperature, high pressure and addition of external oxygen, and meanwhile, a reactor required by the reaction has a complex structure, consumes energy and time, and has low efficiency, low reaction selectivity and low substrate conversion rate. The novel system is carried out at normal temperature and normal pressure, does not need to add an oxidant, has small applied voltage, high reaction selectivity and high substrate conversion rate.
(ii) compared with the traditional two-electrode (BOR-HER) coupled system reaction, the novel system designed by the invention has high hydrogen and high value-added micromolecule production rate and high energy utilization efficiency, more economically utilizes the oxygen byproduct generated in the reaction process, and realizes that the oxygen atoms in the water are completely added into the biomass molecules instead of O2The form of (A) is separated out.
(iii) the novel system designed by the invention can be driven by solar energy to stably operate, so that the conversion of the solar energy into hydrogen energy and chemicals with high added values is realized, and the practicability is high.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (5)
1. A reaction system for coupling high-efficiency micromolecule catalytic oxidation with hydrogen production comprises an electrolytic cell (1) and a two-electrode coupling reaction mechanism, wherein the two-electrode coupling reaction mechanism comprises a hydrogen precipitation cathode (2) and a No. I micromolecule oxidation anode (3) which are respectively connected with the anode and the cathode of a No. I external power supply (5);
the method is characterized in that: the device also comprises an oxygen reduction reaction mechanism and a proton exchange membrane (4), wherein the oxygen reduction reaction mechanism comprises an oxygen reduction cathode (6) and a small molecular oxidation anode (7) which are respectively connected with the anode and the cathode of a No. II external power supply (8); the proton exchange membrane (4) is arranged between the hydrogen evolution cathode (2) and the I-type small molecule oxidation anode (3), and divides the interior of the electrolytic cell (1) into a I-type electrolytic area (9) and a II-type electrolytic area (10); the No. I electrolysis area (9) and the No. II electrolysis area (10) are filled with electrolyte.
2. The efficient small-molecule catalytic oxidation and hydrogen production coupled reaction system of claim 1, characterized in that: the electrolyte filled in the No. I electrolysis region (9) is alkaline electrolyte; the electrolyte filled in the No. II electrolysis area (10) is alkaline electrolyte added with biomass micromolecules.
3. The efficient small-molecule catalytic oxidation and hydrogen production coupled reaction system of claim 1, characterized in that: the hydrogen evolution cathode (2) and the oxygen reduction cathode (6) are commercial Pt/C electrodes.
4. The efficient small-molecule catalytic oxidation and hydrogen production coupled reaction system of claim 1, characterized in that: the hydrogen separation cathode (2), the I small molecular oxidation anode (3), the oxygen reduction cathode (6) and the II small molecular oxidation anode (7) are immersed in the electrolyte.
5. The efficient small-molecule catalytic oxidation and hydrogen production coupled reaction system of claim 1, characterized in that: the No. I small molecular oxidation anode (3) and the No. II small molecular oxidation anode (7) are cobalt-iron hydrotalcite nanosheet array electrodes.
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