CN110965077A - Preparation method of single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide - Google Patents
Preparation method of single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide Download PDFInfo
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Abstract
The invention provides a preparation method of a single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide, which comprises the following steps: s1, mixing absolute ethyl alcohol and BP2000 type conductive carbon black, and stirring uniformly; then, adding PTFE emulsion with solid content of 60% drop by drop, and mixing and stirring uniformly; the mass-volume ratio of the BP2000 type carbon black to the PTFE emulsion to the absolute ethyl alcohol is 1g:3g: 10-20 mL; s2, heating the mixture obtained in the step S1 in water bath, and stirring to form a paste; s3, removing excessive ethanol in the mixture obtained in the step S2; s4, pressing the mixture obtained in the step S3 into a sheet shape; s5, heating the mixture piece obtained in the step S4 to 320-360 ℃, preserving heat for 20-60min, and cooling to room temperature; s6, preparing the mixture sheet obtained in the step S5 into a required shape. The preparation method of the single-layer self-breathing high-efficiency hydrogen peroxide production cathode sheet has a simple preparation process, and greatly improves the current efficiency.
Description
Technical Field
The invention relates to a preparation method of a cathode sheet for efficiently producing hydrogen peroxide through single-layer self-respiration, belonging to the technical field of electrocatalytic synthesis.
Background
Hydrogen peroxide H2O2The hydrogen peroxide is also called as a cleaning oxidant, has wide application, can be used for bleaching textiles and paper products, is often used for manufacturing and processing food, minerals and petroleum products, and has great potential utilization value in the aspects of sewage treatment and water supply treatment. The decomposition reaction products of the hydrogen peroxide are oxygen and water, no harmful residue is generated in the decomposition process, and the hydrogen peroxide is an environment-friendly oxidant. However, hydrogen peroxide is expensive, not suitable for long-distance transportation, unstable, easy to decompose, and the like, so that the unit treatment cost is high in actual operation, and the application range of the catalytic oxidation of the electrolytic H2O2 is greatly limited.
The in-situ generation of hydrogen peroxide by cathodic electrochemical reduction of oxygen is a green and safe preparation method, and can avoid transportation and storage problems. Electrochemical cathodic reduction utilizes an oxygen two-electron reduction reaction to produce hydrogen peroxide, and the efficiency of hydrogen peroxide production depends mainly on cathode material selection and oxygen mass transfer rate. At present, most of the cathodes researched comprise a carbon felt cathode, an activated carbon fiber cathode, a graphite felt cathode, an air diffusion electrode and the like. The air diffusion electrode is generally composed of an air diffusion layer, a current conduction layer and a catalyst layer, wherein O2Is transferred in gaseous form to the catalytic layer via the air diffusion layer, so that its oxygen content can break through O in water2Limitation of solubility to produce H2O2In greater contentHigh.
The air diffusion electrode in the prior art generally consists of three layers, and the manufacturing process is complex and the current efficiency is not high. For example, the Chinese patent application with the application number of 201310698957.3 has the name: the invention relates to a configuration and a preparation method of an air diffusion cathode for efficiently producing hydrogen peroxide, wherein PTFE and carbon black are mixed and coated on a carbon fiber material to prepare the air diffusion cathode, and the current efficiency can only reach 80 percent at most; the invention is named as follows as Chinese patent application with application number 201610031999.5: the invention relates to a preparation method and application of a graphite-carbon black mixed air diffusion cathode sheet.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a single-layer self-breathing high-efficiency hydrogen peroxide production cathode sheet, which is simple in preparation process and greatly improves current efficiency.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide comprises the following steps:
s1, mixing absolute ethyl alcohol and BP2000 type conductive carbon black, and stirring uniformly; then, adding PTFE emulsion with solid content of 60% drop by drop, and mixing and stirring uniformly; the mass-volume ratio of the BP2000 type carbon black to the PTFE emulsion to the absolute ethyl alcohol is 1g:3g: 10-20 mL;
s2, heating the mixture obtained in the step S1 in water bath, and stirring to form a paste;
s3, removing excessive ethanol in the mixture obtained in the step S2;
s4, pressing the mixture obtained in the step S3 into a sheet shape;
s5, heating the mixture piece obtained in the step S4 to 320-360 ℃, preserving heat for 20-60min, and cooling to room temperature;
s6, preparing the mixture sheet obtained in the step S5 into a required shape.
The technical scheme of the invention is further improved by the following steps:
the typical particle size of the BP2000 type carbon black in step S1 is 15 nm.
In step S1, the mixture is mixed uniformly by ultrasonic stirring.
The time for stirring twice in the step S1 is 15-40 min.
The water bath heating temperature in the step S2 is 80-90 ℃, and the heating and stirring time is 20-40 min.
The step S3 of removing the excess ethanol is to roll the mixture using a roll press.
In step S4, the mixture is pressed into sheets by using a roller press, the distance between the roller presses is adjusted once each time the mixture is rolled, and the adjustment is performed according to the rule from large to small, and the distance for each adjustment is the same until the mixture is pressed to the required thickness.
The heating rate of the heating in step S5 is 5 + -1 deg.C/min.
In step S5, the mixture is heated using a muffle furnace.
According to the technical scheme provided by the invention, the preparation method of the single-layer self-breathing high-efficiency hydrogen peroxide production cathode sheet has simple steps, and only needs to mix and stir absolute ethyl alcohol, BP2000 type conductive carbon black and PTFE emulsion uniformly, heat the mixture into a paste, remove redundant ethyl alcohol in the paste, press the paste into a sheet shape, and heat the sheet to a certain temperature for sintering. The hydrogen peroxide cathode sheet prepared by the method is of a single-layer structure, the manufacturing process is simple, the single-layer structure is firmer, and the problems that the multi-layer structure is not firmly bonded and is easy to fall off can be solved. The invention selects BP2000 type ultrahigh conductive carbon black as the main material of the cathode sheet, and the specific surface area of the BP2000 type conductive carbon black can reach 1500m2The hydrogen peroxide can be effectively generated by the oxygen two-electron reaction due to the ultrahigh specific surface area, and the current efficiency is greatly improved. The liquid materials can be mixed from a microscopic angle by adopting an ultrasonic stirring method, the mixing degree is high, and the mixing is fine and sufficient. The mixture is heated more uniformly by continuously stirring during water bath heating.
Drawings
FIG. 1 is a schematic diagram of a self-breathing air cathode assembly in accordance with an embodiment of the present invention.
FIG. 2 is a graph showing the relationship between the current efficiency and the current magnitude under the blowing condition in the verification experiment according to the embodiment of the present invention.
FIG. 3 is a graph showing the relationship between the hydrogen peroxide concentration and the current level under the blowing condition in the verification experiment of the embodiment of the present invention.
FIG. 4 is a graph showing the relationship between the current efficiency and whether air is blown or not under the condition that the current is 50mA in the verification experiment according to the embodiment of the invention.
FIG. 5 is a flow chart illustrating the preparation of an embodiment of the present invention.
In the figure: 1. a breather pipe; 2. a cathode cavity; 3. a nut; 4. a wire; 5. a cathode plate.
Detailed Description
The invention is further illustrated below with reference to two examples:
as shown in fig. 5, the preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide in example 1 includes the following specific steps:
s1, mixing 1g of BP2000 type conductive carbon black with 10mL of absolute ethyl alcohol, and stirring for 15min by adopting ultrasonic; then 3g of PTFE emulsion with a solid content of 60% is added dropwise, and ultrasonic stirring is adopted while adding, wherein the stirring time is 15 min.
S2, heating the mixture obtained in the step S1 in water bath at 80 ℃, and continuously stirring for 40min to form a paste.
S3, putting the mixture obtained in the step S2 into a roller press, adjusting the distance between the roller press to be about 2mm, and repeatedly rolling for five times to remove the redundant ethanol.
S4, adjusting the spacing of the roller presses to be 0.5mm, rolling the mixture obtained in the step S3, reducing the spacing of the roller presses by 0.05mm each time, and rolling the mixture again until the mixture is pressed to be about 0.5mm in thickness. In each rolling process, the roller of the roller press is wiped by absolute ethyl alcohol, so that the roller is prevented from being adhered to the mixture in the shape of the rubber paste.
S5, putting the pressed mixture sheet obtained in the step S4 into a muffle furnace, heating to 330 +/-10 ℃, controlling the heating rate to be 5 +/-1 ℃/min, preserving the temperature for 20min, and naturally cooling to room temperature.
And S6, cutting the mixture sheet sintered in the step S5 into a circle with the diameter of about 1.8cm, and obtaining the required cathode sheet.
The preparation method of the single-layer self-breathing high-efficiency hydrogen peroxide production cathode sheet in the embodiment 2 comprises the following specific steps:
s1, mixing 1g of BP2000 type conductive carbon black with 20mL of absolute ethyl alcohol, and stirring for 40min by adopting ultrasonic; then 3g of PTFE emulsion with a solid content of 60% was added dropwise while stirring with ultrasound for 40 min.
S2, heating the mixture obtained in the step S1 in water bath at 90 ℃, and continuously stirring for 20min to form a paste.
S3, putting the mixture obtained in the step S2 into a roller press, adjusting the distance between the roller press to be about 2mm, and repeatedly rolling for five times to remove the redundant ethanol.
S4, adjusting the spacing of the roller presses to be 0.5mm, rolling the mixture obtained in the step S3, reducing the spacing of the roller presses by 0.05mm each time, and rolling the mixture again until the mixture is pressed to be about 0.25mm in thickness. In each rolling process, the roller of the roller press is wiped by absolute ethyl alcohol, so that the roller is prevented from being adhered to the mixture in the shape of the rubber paste.
S5, putting the mixture sheet pressed in the step S4 into a muffle furnace, heating to 340 plus or minus 10 ℃, controlling the heating rate to be 5 plus or minus 1 ℃/min, preserving the temperature for 60min, and naturally cooling to the room temperature.
And S6, cutting the mixture sheet sintered in the step S5 into a circle with the diameter of about 1.8cm, and obtaining the required cathode sheet.
In the two embodiments, the raw materials are ultrasonically mixed in the step S1, the mixed solution is stirred by the stirrer, the raw materials and the mixed solution act simultaneously, the liquid materials can be mixed from a microscopic angle, the mixing degree is high, and the mixing is fine and sufficient.
The prepared cathode plates are respectively assembled to form the self-breathing air cathode device according to the figure 1, firstly, the cathode plate 5 is arranged at the bottom of the cathode cavity 2, the cathode plate 5 is kept at the central position of the cathode cavity 2, the screw cap 3 is arranged on the top surface of the cathode plate 5, and the cathode plate 5 and the cathode cavity 2 are fixed by screwing the screw cap 3. One end of the lead 4 is contacted with the cathode sheet 5 at the bottom of the cathode cavity 2, and the middle part of the lead 4 is folded into a spiral shape and fixed in the cathode cavity 2. The vent pipe 1 is inserted from the top of the cathode cavity 2 and passes through the middle spiral part of the lead 4 until the bottom of the cathode cavity is above the cathode sheet 5.
In order to verify the high efficiency of the cathode sheet prepared by the method, the following experimental method is adopted to verify the high efficiency of the cathode sheet. 250mL of the suspension containing 50mM Na2SO4Electrolyte solution, adjusted to pH 7 at 1cm2The electrolysis experiment was carried out using the self-breathing cathode device assembled as described above as the cathode. The experimental results are shown in fig. 2, 3 and 4, fig. 2 is a graph of the current efficiency in the blowing state versus the current level, fig. 3 is a graph of the hydrogen peroxide concentration in the blowing state versus the current level, and fig. 4 is a graph of the current efficiency in the current of 50mA versus whether blowing is performed. Experimental results show that the prepared single-layer self-breathing cathode has higher current efficiency at 50mA, and the highest current efficiency can reach 92%. With increasing current, the current efficiency drops somewhat, but still above 80%. The concentration of hydrogen peroxide in the system is linearly increased along with time and reaches 105mg/L at 60min, thus reflecting the high efficiency and stability of the self-breathing cathode. It should be noted that although the above results are obtained under the condition of blowing air to the air cathode air side, as shown in the results of fig. 4, the highest current efficiency can still reach 90% when the air is not blown, so that the cathode sheet prepared by the invention has higher current efficiency and good stability.
The single-layer air diffusion cathode is prepared by mixing BP2000 type carbon black material with PTFE, mechanically rolling and sintering at high temperature, and the current efficiency can reach more than 92% at most. The preparation method is simple, when the cathode device is used for electrolysis, the aeration to the reaction solution is not needed, and the oxygen can diffuse into the solution from the gas phase through the cathode sheet for reaction.
The cathode sheet prepared by the method has strong mechanical property, and experiments prove that the cathode sheet does not generate cracks under the condition of being folded, the service life of the cathode sheet is long, and the cathode sheet is of a single-layer structure, so that the problems of infirm adhesion and easy falling of a multi-layer structure can be avoided, and the cathode sheet is firmer and more durable than the cathode sheet of the traditional multi-layer structure.
Claims (9)
1. A preparation method of a single-layer self-breathing cathode sheet capable of efficiently producing hydrogen peroxide is characterized by comprising the following steps:
s1, mixing absolute ethyl alcohol and BP2000 type conductive carbon black, and stirring uniformly; then, adding PTFE emulsion with solid content of 60% drop by drop, and mixing and stirring uniformly; the mass-volume ratio of the BP2000 type carbon black to the PTFE emulsion to the absolute ethyl alcohol is 1g:3g: 10-20 mL;
s2, heating the mixture obtained in the step S1 in water bath, and stirring to form a paste;
s3, removing excessive ethanol in the mixture obtained in the step S2;
s4, pressing the mixture obtained in the step S3 into a sheet shape;
s5, heating the mixture piece obtained in the step S4 to 320-360 ℃, preserving heat for 20-60min, and cooling to room temperature;
s6, preparing the mixture sheet obtained in the step S5 into a required shape.
2. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: the typical particle size of the BP2000 type carbon black in step S1 is 15 nm.
3. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: in step S1, the mixture is mixed uniformly by ultrasonic stirring.
4. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 2, is characterized by comprising the following steps: the time for stirring twice in the step S1 is 15-40 min.
5. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: the water bath heating temperature in the step S2 is 80-90 ℃, and the heating and stirring time is 20-40 min.
6. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: the step S3 of removing the excess ethanol is to roll the mixture using a roll press.
7. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: in step S4, the mixture is pressed into sheets by using a roller press, the distance between the roller presses is adjusted once each time the mixture is rolled, and the adjustment is performed according to the rule from large to small, and the distance for each adjustment is the same until the mixture is pressed to the required thickness.
8. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: the heating rate of the heating in step S5 is 5 + -1 deg.C/min.
9. The preparation method of the single-layer self-breathing cathode sheet capable of efficiently generating hydrogen peroxide according to claim 1, is characterized by comprising the following steps: in step S5, the mixture is heated using a muffle furnace.
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| CN115491698A (en) * | 2022-10-17 | 2022-12-20 | 天津大学 | Freely assembled H based on cathode unit group 2 O 2 Synthesis reactor |
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| KR20140073180A (en) * | 2012-12-06 | 2014-06-16 | 서울대학교산학협력단 | electrode assembly for hydrogen peroxide generation and Electrochemical system for hydrogen peroxide generation |
| CN108866569A (en) * | 2018-07-03 | 2018-11-23 | 青岛理工大学 | A kind of preparation method of teflon heat modification gas-diffusion electrode |
| CN110306203A (en) * | 2019-07-09 | 2019-10-08 | 郑州大学 | A kind of cathode generates the electrochemical appliance and method of the hydrogen peroxide organic wastewater of anode processing simultaneously |
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Patent Citations (3)
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| KR20140073180A (en) * | 2012-12-06 | 2014-06-16 | 서울대학교산학협력단 | electrode assembly for hydrogen peroxide generation and Electrochemical system for hydrogen peroxide generation |
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| CN110306203A (en) * | 2019-07-09 | 2019-10-08 | 郑州大学 | A kind of cathode generates the electrochemical appliance and method of the hydrogen peroxide organic wastewater of anode processing simultaneously |
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| HAIJIAN LUO ET AL: ""In situ electrosynthesis of hydrogen peroxide with an improved gas diffusion cathode by rolling carbon black and PTFE"", 《RSC ADVANCES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115491698A (en) * | 2022-10-17 | 2022-12-20 | 天津大学 | Freely assembled H based on cathode unit group 2 O 2 Synthesis reactor |
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