CN114672824A - Electrolytic method for producing high-purity hydrogen peroxide - Google Patents
Electrolytic method for producing high-purity hydrogen peroxide Download PDFInfo
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- CN114672824A CN114672824A CN202210208635.5A CN202210208635A CN114672824A CN 114672824 A CN114672824 A CN 114672824A CN 202210208635 A CN202210208635 A CN 202210208635A CN 114672824 A CN114672824 A CN 114672824A
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Abstract
The invention discloses an electrolysis method for producing high-purity hydrogen peroxide, which adopts an oxide single crystal wafer as an anode material of an electrolytic cell and a carbon-based material as a cathode material, adds neutral or alkaline electrolyte into the electrolytic cell, applies bias voltage on the anode and the cathode of the electrolytic cell after oxygen is introduced into the cathode, leads the anode to generate two-electron water oxidation reaction to generate hydrogen peroxide, and leads the cathode to generate oxygen reduction reaction to generate the hydrogen peroxide. Compared with the prior art, the method replaces the proton reduction reaction generated at the cathode with the two-electron oxygen reduction reaction, directly converts hydrogen into hydrogen peroxide, and solves the storage and utilization problems of the byproduct hydrogen; the single target product hydrogen peroxide is synchronously generated at the anode and the cathode, so that the added value of the product is greatly improved; the two-electron oxygen reduction reaction is utilized to further reduce the external bias voltage and improve the utilization efficiency of electric energy.
Description
Technical Field
The invention relates to the technical field of hydrogen peroxide preparation, in particular to an electrolysis method for producing high-purity hydrogen peroxide by using ultrapure water and oxygen as raw materials.
Background
The aqueous hydrogen peroxide solution is commonly called hydrogen peroxide, is an important chemical raw material, has the characteristics of cleanness and no pollution, and is widely applied to the industries of printing and dyeing, papermaking, environmental protection, food, chemical synthesis, semiconductors and the like. The hydrogen peroxide is generally classified into industrial grade, food grade, reagent grade and electronic grade, wherein the ultra-clean high-purity electronic grade hydrogen peroxide is one of indispensable key materials in the micro-processing and manufacturing process of semiconductor technology, is mainly used in the working procedures of grinding, oxidation, etching, cleaning and the like in chip manufacturing, and the electrical property, reliability and yield of an integrated circuit are seriously influenced by the purity of the ultra-clean high-purity electronic grade hydrogen peroxide.
Industrial production methods of hydrogen peroxide include a barium peroxide method, an ammonium persulfate method (electrolytic method), an anthraquinone method, an isopropanol method, an oxygen cathode reduction method, and the like. Wherein, the anthraquinone process is the mainstream industrial production method at home and abroad at present, and the total chemical reaction equation is H2 + O2 = H2O2(ii) a Its advantages are mature technology, high automation control, low cost and energy consumption of raw material, and high purity of product. At present, the electronic grade hydrogen peroxide is obtained by taking industrial grade hydrogen peroxide produced by an anthraquinone method as a raw material and then deeply purifying by using technologies such as rectification, ion exchange resin, membrane separation, supercritical extraction and the like. The oxygen cathode reduction method is an electrochemical method, and the anode generates oxygen evolution reaction (4 OH) under the strong alkaline condition ‒→ O2 + 2H2O + 4e ‒) The cathode undergoes two-electron oxygen reduction reaction (2O)2 + 2H2O + 4e ‒→ 2HO2 ‒+ 2OH‒) The total chemical reaction equation is O2 + 2OH‒→ 2HO2 ‒Or O2 + 2H2O → 2H2O2(ii) a Its advantages are high current efficiency, small-scale production, and high catalytic activity of Pt and RuO2And the cost is high, and the produced hydrogen peroxide has poor stability (according to the literature, Gustaaf Goor)et al., Hydrogen Peroxide in Ullmann's Encyclopedia of Industrial Chemistry, Wiley-VCH, Weinheim, Germany, 2019）。
In another electrochemical method, bismuth vanadate single crystal is adopted as an anode material to enhance the catalytic activity and selectivity of the water oxidation reaction to the maximum extent, and a nickel-based alloy is adopted as a cathode material; under the alkaline condition, the anode generates two-electron water oxidation reaction (2H)2O → H2O2 + 2H+ + 2e ‒) The cathode generates hydrogen evolution reaction (2H)+ + 2e ‒→ H2) The total chemical reaction equation is 2H2O → H2O2 + H2(ii) a The water anodizing method takes bismuth vanadate single crystal as a core catalyst and can be called as a bismuth vanadate method or a single crystal electrocatalysis method; its advantages are high current efficiency, low cost and high purity of product, and low added value of hydrogen generated from cathode and inconvenience for storage and utilization (according to the patent application in "an electrolytic method for producing high-purity hydrogen peroxide and hydrogen at low cost", China patent application No. 201610567960.5).
Compared with the anthraquinone method, the oxygen cathode reduction method and the bismuth vanadate method have the advantages that the raw materials (water and oxygen) needed by the oxygen cathode reduction method and the bismuth vanadate method are low in price, sufficient in supply and good in purity controllability, so that the produced hydrogen peroxide is higher in purity, and if the method is used for replacing industrial-grade hydrogen peroxide produced by the anthraquinone method, the purification cost of electronic-grade hydrogen peroxide can be effectively reduced. If the advantages of the raw materials of the electrochemical method can be fully exerted and the technical disadvantages of the anode of the oxygen cathode reduction method or the cathode of the bismuth vanadate method can be solved, so that the production cost is further reduced, the electrochemical method is hopefully substituted for the anthraquinone method to become the mainstream industrial production method of the hydrogen peroxide.
Disclosure of Invention
The invention aims to provide an electrolysis method for producing high-purity hydrogen peroxide on the basis of comprehensively considering the advantages and the disadvantages of an oxygen cathode reduction method and a bismuth vanadate method.
In order to achieve the above purpose, the technical solution adopted by the present invention to solve the above technical problems is: an electrolytic method for producing high-purity hydrogen peroxide adopts single crystal oxide wafer as anode material of electrolytic bath and carbon-based material as cathode materialAdding neutral or alkaline electrolyte as cathode material into the electrolytic tank, introducing oxygen into the cathode, and applying bias voltage to the anode and cathode of the electrolytic tank to make the anode produce two-electron water oxidation reaction to generate hydrogen peroxide (2H) 2O → H2O2 + 2H+ + 2e ‒) While the cathode undergoes oxygen reduction reaction to produce hydrogen peroxide (O)2 + 2H+ + 2e ‒→ H2O2) The total chemical reaction equation is O2 + 2H2O → 2H2O2。
The oxide single crystal wafer is the same as or similar to the anode material used by the bismuth vanadate method, and can be a crystal face of doped bismuth vanadate single crystal {111}, {110}, {112}, {100} and the like or a crystal face of doped zinc oxide single crystal {0001 }.
The chemical component of the doped bismuth vanadate single crystal is (Bi)1-xAx)(V1-yBy)O4Wherein A is vacancy, +1/+2/+3 valence metal cation or a mixed component thereof, and B is +4/+6 valence metal cation or a mixed component thereof, wherein x is more than or equal to 0, and y is less than or equal to 0.2.
The chemical components of the doped zinc oxide single crystal are Ga: ZnO.
The + 1-valent metal cation is Li, Na, K and the like; the + 2-valent metal cation is Mg, Ca, Sr, Zn and the like; the + 3-valent metal cation is Ga, In, Sc, Y or other rare earth elements and the like; the + 4-valent metal cation is Ti or Ge and the like; the + 6-valent metal cation is W, Mo or the like.
The pH value of the neutral or alkaline electrolyte is 7-13.
The oxygen is low-cost oxygen with the purity of 90% prepared by the oxygen generator.
The carbon-based material is the same as or similar to the cathode material used in the oxygen cathode reduction method, and may be a graphite/carbon black/polytetrafluoroethylene composite, an oxidized or doped carbon material, a carbon-based single-atom catalyst, or the like.
The single crystal wafer of the oxide is fixed on a conductive film of conductive glass.
The external bias voltage is 1.8-2.5V, and the current density during electrolysis is 0.01-0.3A/cm2。
And collecting the electrolyte in the anode and cathode regions after the electrolysis is finished, and obtaining the hydrogen peroxide solution after the evaporation and concentration treatment.
The beneficial effects of the invention are: compared with a bismuth vanadate method, the method replaces proton reduction reaction generated at the cathode with two-electron oxygen reduction reaction, directly converts hydrogen into hydrogen peroxide, and solves the storage and utilization problems of byproduct hydrogen; under the condition of 1.8-2.5V external bias voltage, a single target product hydrogen peroxide is synchronously generated at the anode and the cathode, so that the added value of products is greatly improved; the two-electron oxygen reduction reaction is utilized to further reduce the external bias voltage, improve the utilization efficiency of electric energy and have important industrial application value.
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FIG. 1 is a schematic view of an electrolytic cell used in the present invention.
In the reference numerals, 111 is an anode, 112 is a cathode, 113 is a proton exchange membrane, and 121 is an applied forward bias.
Detailed Description
The present invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention as claimed.
An electrolytic method for producing high-purity hydrogen peroxide is based on the electrolytic cell configuration shown in FIG. 1, wherein an anode 111 and a cathode 112 are respectively arranged on the cell wall of the electrolytic cell, and a proton exchange membrane 113 is arranged between the anode 111 and the cathode 112 in the electrolytic cell. The anode 111 uses a single crystal oxide wafer as an anode material, and the cathode uses a carbon-based material as a cathode material. Adding neutral or alkaline electrolyte into the electrolytic cell, introducing oxygen into the cathode 112, and applying a forward bias 121 to the anode 111 and the cathode 112 of the electrolytic cell to allow the anode 111 to perform two-electron water oxidation reaction to generate hydrogen peroxide (2H)2O → H2O2 + 2H+ + 2e ‒) While the cathode 112 undergoes an oxygen reduction reaction to produce hydrogen peroxide (O)2 + 2H++ 2e ‒→ H2O2) The total chemical reaction equation is O2 + 2H2O → 2H2O2. Wherein the single crystal oxide wafer in the anode 111 is fixed on a conductive film of conductive glass. The conductive glass consists of a glass substrate and a conductive film attached to the glass substrate, and can be ITO glass, FTO glass or the like. An oxygen inlet is provided at the cell wall corresponding to the cathode 112, which is in communication with the carbon-based material on the cathode 112 to facilitate efficient introduction of the oxygen required for the reaction.
The production of 1 ton of 30% hydrogen peroxide is described in further detail below.
By doping with bismuth vanadate<111>The single chip is used as an anode of the electrolytic cell, the commercial graphite/carbon black/polytetrafluoroethylene composite is used as a cathode of the electrolytic cell, and the effective areas of the single chip and the commercial graphite/carbon black/polytetrafluoroethylene composite are all 10 m2(ii) a The applied bias voltage was 2.5V, and the current intensity per unit area was 0.3A/cm2(ii) a Performing high-purity ethanol by 90% at cathode, and performing high-purity ethanol by oxygen plant (oxygen yield 14 Nm)3And/h) is provided. The production of the hydrogen peroxide requires 622 kilowatts of hours and takes about 8 hours, as estimated by the current conversion efficiency of 100% of the anode and 90% of the cathode, without considering the energy consumption of the oxygen generator. If the power of the oxygen generator is 18 kW, the power consumption for producing the hydrogen peroxide is about 766 kilowatt-hour.
If the bismuth vanadate method is adopted to produce the hydrogen peroxide and the byproduct hydrogen gas with the thickness of 200 Nm3The required power consumption is 1322 kwh and the required time is about 16 hours (according to the Chinese patent application with patent application No. 201610567960.5, named as "an electrolytic method for producing high-purity hydrogen peroxide and hydrogen at low cost").
Compared with a bismuth vanadate method, the method directly converts hydrogen into hydrogen peroxide, solves the storage and utilization problems of the byproduct hydrogen, shortens the production time, improves the electric energy utilization efficiency, and greatly improves the added value of products.
The above description is only a preferred embodiment of the present invention, but not intended to limit the scope of the invention, and all simple equivalent changes and modifications made in the claims and the description of the invention are within the scope of the invention.
Claims (8)
1. An electrolytic process for producing high purity hydrogen peroxide, characterized by: the method comprises the steps of adopting an oxide single crystal wafer as an anode material of an electrolytic cell, adopting a carbon-based material as a cathode material, adding neutral or alkaline electrolyte into the electrolytic cell, introducing oxygen into a cathode, and applying bias voltage to the anode and the cathode of the electrolytic cell to enable the anode to generate two-electron water oxidation reaction to generate hydrogen peroxide, and simultaneously enabling the cathode to generate oxygen reduction reaction to generate hydrogen peroxide.
2. An electrolytic process for producing high purity hydrogen peroxide according to claim 1, wherein: the oxide single crystal wafer is a doped bismuth vanadate single crystal {111}, {110}, {112}, {100} crystal face or a doped zinc oxide single crystal {0001} crystal face.
3. An electrolytic process for producing high purity hydrogen peroxide according to claim 2, wherein: the carbon-based material is a graphite/carbon black/polytetrafluoroethylene compound, an oxidized or doped carbon material or a carbon-based single-atom catalyst.
4. An electrolytic process for producing high purity hydrogen peroxide in accordance with claim 1 in which: the oxygen introduced into the cathode is oxygen with the purity of 90% prepared by the oxygen generator.
5. An electrolytic process for producing high purity hydrogen peroxide in accordance with claim 1 in which: the pH value of the neutral or alkaline electrolyte is 7-13.
6. An electrolytic process for producing high purity hydrogen peroxide in accordance with claim 2 in which: the single crystal wafer of the oxide is fixed on a conductive film of conductive glass.
7. An electrolytic process for producing high purity hydrogen peroxide in accordance with claim 1 in which: the external bias voltage is 1.8-2.5V, and the current density during electrolysis is 0.01-0.3A/cm2。
8. An electrolytic process for producing high purity hydrogen peroxide according to claim 1, wherein: and collecting the electrolyte in the anode and cathode regions after the electrolysis is finished, and obtaining the hydrogen peroxide solution through evaporation and concentration treatment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990610A (en) * | 2022-07-13 | 2022-09-02 | 郑州大学 | Method for preparing functionalized carbon material through in-situ oxidation, prepared carbon material and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6004449A (en) * | 1998-02-09 | 1999-12-21 | Boeing North American, Inc. | Method of operating electrolytic cell to produce highly concentrated alkaline hydrogen peroxide |
| CN106086922A (en) * | 2016-07-19 | 2016-11-09 | 李国岭 | A kind of utilize solar energy low-cost production hydrogen peroxide and the electrolytic method of hydrogen |
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- 2022-03-04 CN CN202210208635.5A patent/CN114672824A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6004449A (en) * | 1998-02-09 | 1999-12-21 | Boeing North American, Inc. | Method of operating electrolytic cell to produce highly concentrated alkaline hydrogen peroxide |
| CN106086922A (en) * | 2016-07-19 | 2016-11-09 | 李国岭 | A kind of utilize solar energy low-cost production hydrogen peroxide and the electrolytic method of hydrogen |
Non-Patent Citations (2)
| Title |
|---|
| SARA R. KELLY等: "ZnO As an Active and Selective Catalyst for Electrochemical Water Oxidation to Hydrogen Peroxide", 《ACS CATAL》, vol. 9, pages 4593 * |
| XINJIAN SHI等: "Light-Driven BiVO4–C Fuel Cell with Simultaneous Production of H2O2", 《ADVANCED ENERGY MATERIALS》, vol. 8, no. 23, pages 1 - 9 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114990610A (en) * | 2022-07-13 | 2022-09-02 | 郑州大学 | Method for preparing functionalized carbon material through in-situ oxidation, prepared carbon material and application thereof |
| CN114990610B (en) * | 2022-07-13 | 2023-06-13 | 郑州大学 | Method for preparing functionalized carbon material by in-situ oxidation, prepared carbon material and application thereof |
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