CN110760876A - For efficiently synthesizing H2O2Three-chamber reactor device - Google Patents

For efficiently synthesizing H2O2Three-chamber reactor device Download PDF

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Publication number
CN110760876A
CN110760876A CN201910762958.7A CN201910762958A CN110760876A CN 110760876 A CN110760876 A CN 110760876A CN 201910762958 A CN201910762958 A CN 201910762958A CN 110760876 A CN110760876 A CN 110760876A
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cathode
anode
power supply
chamber
direct current
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李楠
赵倩
安敬昆
吴玉
王鑫
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Tianjin University
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Tianjin University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/28—Per-compounds
    • C25B1/30—Peroxides
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms

Abstract

The invention discloses a method for efficiently synthesizing H2O2The three-chamber reactor device consists of an anode chamber and two cathode chambers, wherein the anode chamber and the cathode chambers are separated by a cation exchange membrane, the cathode is a manufactured carbon black-graphite-PTFE air diffusion cathode, the anode is a titanium/iridium dioxide composite metal plate which is vertically inserted into an anode tank, and the cathode is respectively fixed by two cathode fixing plates. The anode titanium/iridium dioxide composite metal plate is connected with the positive pole of a direct current power supply, and the two cathodes are both connected with the negative pole of the direct current power supply. The carbon black-graphite-PTFE air diffusion cathode selected by the device is a cathode, the anode is a titanium/iridium dioxide metal plate, the current efficiency can reach 100 percent, and the current efficiency is higher than that of a common reactorCurrent efficiency.

Description

For efficiently synthesizing H2O2Three-chamber reactor device
Technical Field
The invention relates to the field of electrochemical synthesis, in particular to a method for high-efficiency electricityCatalytic synthesis of H2O2The apparatus of (1).
Background
Hydrogen peroxide (H)2O2) Is an environmentally friendly strong chemical oxidant, and only water (H) is used in decomposition2O) and oxygen (O)2) The product does not produce harmful residue, and has wide application in pulp bleaching, textile and other manufacturing industries, electronic industry, waste water treatment, chemical oxidation (including large-scale propylene oxidation to produce propylene oxide), and the like.
Industrially, hydrogen peroxide is obtained by the Anthraquinone Oxidation (AO) process. However, this method is not considered to be a green and environmentally friendly production method because of large energy input, complicated steps, and much waste. Furthermore, the transportation, storage and handling of hydrogen peroxide present potential hazards and additional costs. O via the two-electron pathway of Oxygen Reduction Reaction (ORR)2Electrochemical reduction to H2O2For in situ production of H2O2Offering great potential. Carbon-based materials (such as activated carbon, fullerene, carbon nanotube, carbon aerogel, graphite, graphene, and the like) exist in various forms, including powder, fiber, aerogel, composite material, flake, monomer, tube, and the like, and are widely used as catalytic materials due to their advantages of large specific surface area, good electrical conductivity, corrosion resistance, high abundance, low price, and the like.
Currently, air breathing cathodes are a very promising form of cathode in electrochemical systems. The air breathing cathode consists of a hydrophobic Gas Diffusion Layer (GDL) exposed to air and a Catalytic Layer (CL) immersed in an electrolyte solution, wherein oxygen in the air can diffuse from the diffusion layer into the catalytic layer, and the oxygen is combined with hydrogen ions and reacts under the catalysis of active sites to generate H2O2。
Disclosure of Invention
The invention aims to solve the problems in the prior art and design a method for synthesizing H2O2The three-chamber reactor has simple structure and low manufacturing cost, and effectively improves H2O2The synthesis efficiency is improved.
The purpose of the invention is realized by the following technical scheme: for efficiently synthesizing H2O2The three-chamber reactor device consists of an anode chamber and two cathode chambers, wherein the anode chamber and the cathode chambers are separated by a cation exchange membrane.
The cathode is made of carbon black-graphite-PTFE air diffusion cathode, the anode is made of titanium/iridium dioxide composite metal plate and is vertically inserted into the anode tank, and the cathode is respectively fixed by two cathode fixing plates.
The anode titanium/iridium dioxide composite metal plate is connected with the positive electrode of a direct current power supply, and the two cathodes are connected with the negative electrode of the direct current power supply.
Three chambers were each filled with 200mL of sodium sulfate (Na)2SO4) And (3) an electrolyte.
The main body of the device is made of organic glass material
The cathode adopted by the device is a carbon black-graphite-PTFE air diffusion cathode which is composed of a diffusion layer, a catalyst layer and a steel mesh used as a current collector, wherein the catalyst layer and the diffusion layer are respectively formed by mixing graphite carbon black and carbon black powder with alcohol and PTFE, stirring the mixture into a paste shape, and rolling the paste onto two sides of the steel mesh.
The anode used in the device is a titanium/iridium dioxide plate with the length of 10cm, the width of 4cm and the thickness of 1 mm. Advantageous effects
1. The carbon black-graphite-PTFE air diffusion cathode is selected as the cathode, the titanium/iridium dioxide metal plate is used as the anode, and the current efficiency can reach 100 percent and is higher than that of a common reactor.
2. The system can control the concentration of the hydrogen peroxide by adjusting the current and the electrifying time, and is simple and convenient to operate.
3. The system has low cost, and the organic glass and the graphite-carbon black-PTFE air diffusion cathode are cheap and easy to obtain.
Drawings
FIG. 1 is a high efficiency synthesis of H2O2The structure of the three-chamber reactor is shown schematically.
Reference numerals: the device comprises a cathode chamber 1, a cathode 2, a cation exchange membrane 3, an anode chamber 4, an anode tank 5, a sampling port 6 and a cathode fixing plate 7.
Detailed Description
The invention is further described below with reference to the following figures and specific examples.
For efficiently synthesizing H2O2The main body of the three-chamber reactor device is made of organic glass materials and respectively consists of an anode chamber 4 (with the size of 10cm x 2cm) and two cathode chambers 1 (with the size of 10cm x 2cm), the anode chamber 4 and the cathode chambers 1 are separated by a cation exchange membrane 3, a manufactured carbon black-graphite-PTFE air diffusion cathode is selected as a cathode 2, a titanium/iridium dioxide composite metal plate (with the size of 4cm x 10cm x 1mm) is selected as an anode and vertically inserted into an anode groove 5 (with the size of 5cm x 1cm), and the cathode 2 is respectively fixed by two cathode fixing plates 7. When in use, the assembled reactor is connected with a direct current power supply, the anode titanium/iridium dioxide composite metal plate is connected with the anode of the direct current power supply, the two cathodes 2 are both connected with the cathode of the direct current power supply, and 200mL of sodium sulfate (Na) is respectively injected into the three chambers2SO4) The electrolyte controls the operation condition of the reactor by adjusting the current and the electrifying time, and samples are taken from the sampling port 6.
The common single-chamber reactor is a cylindrical chamber with the diameter of 3cm and the length of 4cm, the carbon black-graphite-PTFE air diffusion cathode is adopted as the cathode, a Pt sheet (1cm x 1cm) is adopted as the anode, and the distance between the cathode and the anode is 2 cm.
Example 1
200mL of Na with a concentration of 0.05M was injected into the anode chamber and the two cathode chambers, respectively2SO4Connecting the titanium/iridium dioxide composite metal plate with the positive electrode of a direct current power supply, connecting two cathodes with the negative electrode of the direct current power supply, turning on a power switch, adjusting the current to 70mA, operating for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration, H of two cathode compartments2O2The concentrations were 30mg/L and 25mg/L, and the current efficiency was 75%.
Example 2
Injecting water into the anode chamber and the two cathode chambers respectively200mL of 0.05M Na are added2SO4Connecting the titanium/iridium dioxide composite metal plate with the positive electrode of a direct current power supply, connecting two cathodes with the negative electrode of the direct current power supply, turning on a power switch, adjusting the current to 140mA, operating for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration, H of two cathode compartments2O2The concentrations were 71mg/L and 72mg/L, and the current efficiency was 96%.
Example 3
200mL of Na with a concentration of 0.05M was injected into the anode chamber and the two cathode chambers, respectively2SO4Connecting the titanium/iridium dioxide composite metal plate with the positive electrode of a direct current power supply, connecting two cathodes with the negative electrode of the direct current power supply, turning on a power switch, adjusting the current to 210mA, operating for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration, H of two cathode compartments2O2The concentrations were 120mg/L and 111mg/L, and the current efficiency was 100%.
Example 4
200mL of Na with a concentration of 0.05M was injected into the anode chamber and the two cathode chambers, respectively2SO4Connecting the titanium/iridium dioxide composite metal plate with the positive electrode of a direct current power supply, connecting two cathodes with the negative electrode of the direct current power supply, turning on a power switch, adjusting the current to 280mA, operating for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration, H of two cathode compartments2O2The concentrations were 131mg/L and 146mg/L, and the current efficiency was 94%.
Example 5
200mL of Na with a concentration of 0.05M was injected into the anode chamber and the two cathode chambers, respectively2SO4Connecting the titanium/iridium dioxide composite metal plate with the positive electrode of a direct current power supply, connecting two cathodes with the negative electrode of the direct current power supply, turning on a power switch, adjusting the current to 350mA, operating for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration, H of two cathode compartments2O2The concentrations were 167mg/L and 187mg/L, and the current efficiency was 95%.
Example 6
Into a common single-chamber reactor was injected 28mL of Na with a concentration of 0.05M2SO4Connecting a Pt sheet with the positive electrode of a direct current power supply, connecting the cathode with the negative electrode of the direct current power supply, turning on the direct current power supply, adjusting the current to 35mA, running for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration of H2O2The concentration was 173mg/L, and the current efficiency was 65%.
Example 7
Into a common single-chamber reactor was injected 28mL of Na with a concentration of 0.05M2SO4Connecting a Pt sheet with the positive electrode of a direct current power supply, connecting the cathode with the negative electrode of the direct current power supply, turning on the direct current power supply, adjusting the current to 70mA, running for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration of H2O2The concentration was 353mg/L and the current efficiency was 67%.
Example 8
Into a common single-chamber reactor was injected 28mL of Na with a concentration of 0.05M2SO4Connecting a Pt sheet with the positive electrode of a direct current power supply, connecting the cathode with the negative electrode of the direct current power supply, turning on the direct current power supply, adjusting the current to 105mA, running for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration of H2O2The concentration was 611mg/L, and the current efficiency was 77%.
Example 9
Into a common single-chamber reactor was injected 28mL of Na with a concentration of 0.05M2SO4Connecting a Pt sheet with the positive electrode of a direct current power supply, connecting the cathode with the negative electrode of the direct current power supply, turning on the direct current power supply, adjusting the current to 140mA, operating for 20min, and detecting H by using a potassium titanium oxalate spectrophotometry2O2Concentration of H2O2The concentration was 888mg/L, the current efficiency was 84%.
Example 10
Into a common single-chamber reactor was injected 28mL of Na with a concentration of 0.05M2SO4Electrolyte, connecting Pt sheet to positive electrode of DC power supply, connecting cathode to negative electrode of DC power supply, turning on DC power supply, and regulatingThe current is 175mA, after 20min of operation, H is detected by potassium titanium oxalate spectrophotometry2O2Concentration of H2O2The concentration was 1000mg/L and the current efficiency was 75%.
It should be understood that the embodiments and examples discussed herein are illustrative only and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this application and scope of the appended claims.

Claims (5)

1. For efficiently synthesizing H2O2The three-chamber reactor device is characterized by comprising an anode chamber and two cathode chambers, wherein the anode chamber and the cathode chambers are separated by a cation exchange membrane.
2. The process of claim 1 for the efficient synthesis of H2O2The three-chamber reactor device is characterized in that a cathode is a manufactured carbon black-graphite-PTFE air diffusion cathode, an anode is a titanium/iridium dioxide composite metal plate which is vertically inserted into an anode tank, and the cathode is respectively fixed by two cathode fixing plates.
3. The process of claim 1 for the efficient synthesis of H2O2The three-chamber reactor device is characterized in that the anode titanium/iridium dioxide composite metal plate is connected with the positive pole of a direct current power supply, and the two cathodes are both connected with the negative pole of the direct current power supply.
4. The process of claim 1 for the efficient synthesis of H2O2The three-chamber reactor device of (1), wherein 200mL of sodium sulfate (Na) was injected into each of the three chambers2SO4) And (3) an electrolyte.
5. The process of claim 1 for the efficient synthesis of H2O2The three-chamber reactor device is characterized in that the device main body is made of organic glass materials.
CN201910762958.7A 2019-08-19 2019-08-19 For efficiently synthesizing H2O2Three-chamber reactor device Pending CN110760876A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111979562A (en) * 2020-08-18 2020-11-24 天津大学 Plug-in capsule cathode and expandable efficient synthesis H2O2Reactor device
CN112048732A (en) * 2020-09-16 2020-12-08 天津大学 Continuous flow gallery type H based on plug-in capsule cathode2O2Synthesis reactor
CN113174605A (en) * 2021-03-04 2021-07-27 中山大学 Method for efficiently preparing hydrogen peroxide disinfectant

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CN101748422A (en) * 2008-12-19 2010-06-23 中国科学院大连化学物理研究所 Method for preparing alkaline hydrogen peroxide in situ
CN105696018A (en) * 2016-01-18 2016-06-22 天津大学 Preparation and application of graphite-carbon black mixed air diffusion cathode
CN105951117A (en) * 2016-07-19 2016-09-21 李国岭 Electrolysis method for producing high-purity hydrogen peroxide and hydrogen with low cost
CN107313068A (en) * 2016-04-26 2017-11-03 中国科学院大连化学物理研究所 A kind of electrochemical method of synthetic acidic hydrogen peroxide
CN207047325U (en) * 2017-07-21 2018-02-27 中山大学 A kind of stack electro synthesis reactor for efficiently preparing hydrogen peroxide
CN107849714A (en) * 2015-05-22 2018-03-27 西门子公司 The electrolysis system and restoring method that are used for electrochemistry and utilize carbon dioxide with proton donor unit
CN211394647U (en) * 2019-08-19 2020-09-01 天津大学 Three-chamber reactor device for efficiently synthesizing H2O2

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101748422A (en) * 2008-12-19 2010-06-23 中国科学院大连化学物理研究所 Method for preparing alkaline hydrogen peroxide in situ
CN107849714A (en) * 2015-05-22 2018-03-27 西门子公司 The electrolysis system and restoring method that are used for electrochemistry and utilize carbon dioxide with proton donor unit
CN105696018A (en) * 2016-01-18 2016-06-22 天津大学 Preparation and application of graphite-carbon black mixed air diffusion cathode
CN107313068A (en) * 2016-04-26 2017-11-03 中国科学院大连化学物理研究所 A kind of electrochemical method of synthetic acidic hydrogen peroxide
CN105951117A (en) * 2016-07-19 2016-09-21 李国岭 Electrolysis method for producing high-purity hydrogen peroxide and hydrogen with low cost
CN207047325U (en) * 2017-07-21 2018-02-27 中山大学 A kind of stack electro synthesis reactor for efficiently preparing hydrogen peroxide
CN211394647U (en) * 2019-08-19 2020-09-01 天津大学 Three-chamber reactor device for efficiently synthesizing H2O2

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111979562A (en) * 2020-08-18 2020-11-24 天津大学 Plug-in capsule cathode and expandable efficient synthesis H2O2Reactor device
CN111979562B (en) * 2020-08-18 2023-03-10 天津大学 Plug-in capsule cathode and expandable efficient synthesis H 2 O 2 Reactor device
CN112048732A (en) * 2020-09-16 2020-12-08 天津大学 Continuous flow gallery type H based on plug-in capsule cathode2O2Synthesis reactor
CN112048732B (en) * 2020-09-16 2023-08-01 天津大学 Continuous flow gallery type H based on plug-in type capsule cathode 2 O 2 Synthesis reactor
CN113174605A (en) * 2021-03-04 2021-07-27 中山大学 Method for efficiently preparing hydrogen peroxide disinfectant

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