CN114561658A - High-purity hydrogen peroxide and production method thereof - Google Patents
High-purity hydrogen peroxide and production method thereof Download PDFInfo
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- CN114561658A CN114561658A CN202210271443.9A CN202210271443A CN114561658A CN 114561658 A CN114561658 A CN 114561658A CN 202210271443 A CN202210271443 A CN 202210271443A CN 114561658 A CN114561658 A CN 114561658A
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- 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
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- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
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Abstract
The invention discloses high-purity hydrogen peroxide, wherein the TOC content of the hydrogen peroxide is lower than 1000 ppb. The invention also discloses a production method of the high-purity hydrogen peroxide, which adopts pure water and oxygen as raw materials and comprises an electrolysis process and a distillation process, wherein the electrolysis process adopts an oxide single wafer as an anode material of an electrolytic cell, a carbon-based material as a cathode material, neutral or alkaline electrolyte is added into the electrolytic cell, and after high-purity oxygen is introduced into a cathode, bias voltage is applied to the anode and the cathode of the electrolytic cell, so that the anode generates two-electron water oxidation reaction to generate hydrogen peroxide, and simultaneously the cathode generates oxygen reduction reaction to generate hydrogen peroxide. The invention has the beneficial effects that: the total organic carbon content in the high-purity hydrogen peroxide can be ignored, and inorganic impurities are efficiently removed through a distillation process, so that high-quality food-grade and reagent-grade hydrogen peroxide can be obtained; simple process flow and low production cost.
Description
Technical Field
The invention relates to the field of fine chemicals, in particular to food-grade and reagent-grade high-purity hydrogen peroxide and an electrochemical production method thereof.
Background
Hydrogen peroxide (aqueous 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 industrial production methods of hydrogen peroxide include a barium peroxide method, an ammonium persulfate method, an anthraquinone method, an isopropanol method, an oxygen cathode reduction method and the like. Among them, the anthraquinone process is the mainstream industrial production method at home and abroad at present, and the total production method isChemical reaction equation is H2+O2＝H2O2Its advantages are mature technology, high automation control, low cost and energy consumption of raw materials, and high adaptability to large-scale production.
The hydrogen peroxide is generally divided into industrial grade, food grade, reagent grade and electronic grade, and has corresponding specifications corresponding to typical impurity contents in national standards such as GB/T1616-2014, GB22216-2020, GB/T6684-2002, HG/T5736-2020 and the like. Wherein the food-grade, reagent-grade and electronic-grade hydrogen peroxide all belong to high-purity hydrogen peroxide without stabilizer. The content of hydrogen peroxide in the food-grade hydrogen peroxide is 35 wt% or 50 wt%, and the content of carcinogenic substances is clearly specified, for example, the nonvolatile matter content is required to be less than or equal to 60ppm, the typical metal ion content Fe is less than or equal to 0.5ppm, As is less than or equal to 1ppm, Pb is less than or equal to 2ppm, Sn is less than or equal to 10ppm, and the total organic carbon content TOC is less than or equal to 80 ppm. The hydrogen peroxide content of the reagent-grade hydrogen peroxide is 30 wt%, and the hydrogen peroxide can be subdivided into a high-purity grade, an analytical purity grade and a chemical purity grade, wherein the requirement of the chemical purity hydrogen peroxide on impurity content is similar to that of the food-grade hydrogen peroxide, the high-purity grade hydrogen peroxide has higher requirement, specifically, the nonvolatile content is less than or equal to 25ppm, the typical metal ion content Fe is less than or equal to 0.1ppm, the As is less than or equal to 0.5ppm, and the Pb/Cu/Ni is less than or equal to 20 ppb. At present, the food-grade and reagent-grade hydrogen peroxide is obtained by taking industrial-grade hydrogen peroxide produced by an anthraquinone method as a raw material and purifying the raw material by using technologies such as rectification, ion exchange resin, membrane separation, supercritical extraction, adsorption, recrystallization and the like (application and purification technologies of food-grade hydrogen peroxide, namely, lygod, dawn, rochan, and food-grade hydrogen peroxide, namely, 626-629 page of 2006).
Besides relying on a purification technology, the method for directly improving the purity of the synthesized hydrogen peroxide raw material is also an important way for obtaining high-purity hydrogen peroxide. An electrochemical method for generating two-electron water oxidation reaction on bismuth vanadate monocrystal anode catalyst, which is called bismuth vanadate method or monocrystal electrocatalysis method for short, hopefully provides hydrogen peroxide raw material with low cost and high purity (according to the document, the patent name of inventor Living applied is 'an electrolysis method for producing high-purity hydrogen peroxide and hydrogen with low cost', and the patent application number is '201610567960.5' Chinese invention patent application). Another electrochemical method that utilizes a two-electron oxygen reduction reaction on a cathodic catalyst, namely the oxygen cathodic reduction method, also promises to provide a low-cost, high-purity Hydrogen Peroxide feedstock (according to the literature: Gustaaf Goor et al, Hydrogen Peroxide in Ullmann's Encyclopedia of Industrial Chemistry, Wiley-VCH, Weinheim, Germany, 2019).
Compared with the anthraquinone method, the raw materials (water and oxygen) required by the bismuth vanadate method and the oxygen cathode reduction method are low in price, sufficient in supply and good in purity controllability, so that the purity of the produced hydrogen peroxide is higher. However, the electrochemical method has technical disadvantages, such as low added value of hydrogen gas precipitated from the cathode by the bismuth vanadate method, and the need of using noble metal platinum for the anode by the oxygen cathode reduction method. If the advantages of the raw materials of the electrochemical method can be fully exerted, the technical disadvantages of the anode of the oxygen cathode reduction method or the cathode of the bismuth vanadate method can be solved, and the production cost can be further reduced, the electrochemical method is hopeful to replace the anthraquinone method to produce the hydrogen peroxide raw material with higher quality, and the purification cost of the high-purity hydrogen peroxide can be effectively reduced.
Disclosure of Invention
The invention aims to provide high-purity hydrogen peroxide for producing food grade and reagent grade hydrogen peroxide and a production method thereof on the basis of a bismuth vanadate method and an oxygen cathode reduction method aiming at the defects of the prior art.
In order to achieve the above purpose, the technical solution adopted by the present invention to solve the above technical problems is: a high-purity hydrogen peroxide solution contains TOC (total organic carbon) less than 1000ppb, and is controlled to 1-1000 ppb. Furthermore, the evaporation residue is less than 5 ppm: na is less than 1000ppb, other metal ions are less than 100ppb, and the requirements on TOC and corresponding pollutant content of the existing food-grade hydrogen peroxide are improved by nearly 100 times.
A process for preparing high-purity hydrogen peroxide used to prepare food-class or reagent-class hydrogen peroxide from pure water and high-purity oxygen includes such steps as electrolyzing and distilling, fully combining the advantages of bismuth vanadate method and oxygen cathode reduction method, and preparing single crystal oxide wafer as anode and carbon substrateAdding neutral or alkaline electrolyte as cathode material into an electrolytic cell, introducing high-purity oxygen into the cathode, and applying bias voltage to the anode and cathode of the electrolytic cell to make the anode generate 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 general chemical reaction equation is O2+2H2O→2H2O2。
The neutral or alkaline electrolyte consists of pure water (secondary water or tertiary water, according to analytical laboratory water GB/T6682-2008) and high-purity electrolyte K2CO3Or Na2CO3Not less than 3N, and the pH value is 7-13.
The high-purity oxygen is industrial high-purity oxygen (more than or equal to 3N) or cheap oxygen with the purity of more than or equal to 90 percent prepared by an oxygen generator.
The oxide single crystal wafer is the same as or similar to an anode material used by a 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 composition 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.
Preferably, the oxide single crystal wafer is a doped bismuth vanadate single crystal, and the chemical component is Bi1-xSnxV1-yByO4(0<x is less than or equal to 0.04 and y is less than or equal to 0.2), wherein B is +4/+6 valence metal cation or a mixed component thereof, the electrode efficiency can be improved, and the generation of impurities can be reduced.
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 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 distillation process comprises two physical separation processes of evaporation and rectification, wherein after electrolysis in an electrolytic bath is finished, electrolyte (the hydrogen peroxide content is 0.5 wt% -2 wt%) in an anode region and a cathode region is collected, nonvolatile matters including electrolyte and metal ions are removed in an evaporator through a reduced pressure evaporation process to obtain high-purity low-concentration hydrogen peroxide, and then redundant moisture is separated in a rectifying tower through a reduced pressure rectification process to obtain food-grade or reagent-grade hydrogen peroxide with the expected concentration.
Organic materials such as ABS plastics, chlorinated polyvinyl chloride (CPVC), Fluororubber (FKM), High Density Polyethylene (HDPE), meltable Polytetrafluoroethylene (PFA), polypropylene (PP-363), Polytetrafluoroethylene (PTFE), polyvinyl chloride (PVC) and the like are used as linings in the electrolytic cell, the evaporator and the rectifying tower.
The invention has the beneficial effects that: compared with the existing preparation process of the food-grade and reagent-grade hydrogen peroxide, the process adopts high-purity water and high-purity oxygen with relatively low cost as raw materials, the total organic carbon content in the prepared high-purity hydrogen peroxide can be ignored, inorganic impurities and most of metal impurities are removed efficiently through a mature distillation process, and the high-quality food-grade and reagent-grade hydrogen peroxide can be obtained; the process flow is simple, the production cost is low, and the method has potential industrial application value.
Drawings
FIG. 1 is a flow chart of the production method of high-purity hydrogen peroxide according to the present invention.
Wherein 111 is pure water, and 112 is electrolyte (K)2CO3Or Na2CO3) 113 is oxygen, 114 is electrolyte (H)2O2Content 0.5-2 wt%), 115 is H2O2The solution (low concentration and high purity) 116 is high-purity hydrogen peroxide, 121 is distilled pure water, and 122 is evaporation residual liquid.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1: method for producing food grade/chemical purity/analytical pure hydrogen peroxide
In this example, the electrolyzer, evaporator and rectifying column in the production facility were lined with meltable polytetrafluoroethylene PFA. The electrolytic cell adopts a doped bismuth vanadate single crystal as an anode material, a graphite/carbon black/polytetrafluoroethylene compound as a cathode material, and the cathode and the anode are isolated by a proton exchange membrane. The evaporator adopts a falling film evaporator, and the rectifying tower adopts a primary rectifying device. The applied bias voltage was 2.5V, and the current density at the time of electrolysis was 0.25A/cm2。
The production flow is shown in figure 1, the electrolyte flows through the electrolytic bath to generate electrolytic reaction, the introduced high-purity oxygen 113 generates oxygen reduction reaction at the cathode to obtain hydrogen peroxide, and the anode generates two electron water oxidation reactions to also obtain the hydrogen peroxide; when the hydrogen peroxide concentration reaches 1 wt%, the electrolyte 114 containing hydrogen peroxide in the cathode chamber and the anode chamber is subjected to subsequent reduced pressure evaporation, the high-concentration evaporation residual liquid 122 is refluxed to the electrolyte for recycling, and the evaporated low-concentration high-purity H is recycled2O2Introducing the solution 115 into a rectifying tower for low-pressure rectification; and refluxing the rectified pure water 121 to an electrolytic bath, and packaging the rectified high-purity hydrogen peroxide 116. Wherein, the process conditions of the vacuum evaporation and the low-pressure rectification are as follows: the pressure is 0.1-0.6atm, and the temperature is 50-100 ℃. Preferably, the process conditions of the reduced pressure evaporation are as follows: the pressure is 0.4atm and the temperature is 70 ℃.
The analysis of the contents of organic matters and inorganic matters in the high-purity hydrogen peroxide 116 shows that: h2O235.0wt％；TOC<500 ppb; evaporation of residue<2ppm, typical metal ion content: na (Na)<100ppb of other metal ions<50ppb, and all indexes exceed the index requirements of food-grade hydrogen peroxide, chemical pure hydrogen peroxide and even analytical pure hydrogen peroxide.
Example 2: production method of high-quality hydrogen peroxide
In the embodiment, the pure water 111 adopts secondary water which conforms to the analysis laboratory water GB/T6682-; the oxygen 113 is industrial high-purity oxygen (more than or equal to 3N), and the electrolyte 112 is Na2CO3(≥99.99％)。
The production flow and the process parameters are the same as or similar to those of the example 1. The organic and inorganic matter contents of the obtained high-purity hydrogen peroxide 116 were analyzed, and the results were: h2O2 30.0wt％；TOC<100 ppb; evaporation of residue<1ppm, typical metal ion content: na (Na)<50ppb of other metal ions<20ppb, all indexes meet the index requirements of high-quality hydrogen peroxide.
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 (9)
1. A high-purity hydrogen peroxide is characterized in that: the TOC content is less than 1000 ppb.
2. The method for producing high-purity hydrogen peroxide according to claim 1, wherein the method comprises the following steps: adopting pure water and oxygen as raw materials, and comprising an electrolysis process and a distillation process; the electrolytic process adopts an oxide single crystal wafer as an anode material of an electrolytic cell, a carbon-based material as a cathode material, neutral or alkaline electrolyte is added into the electrolytic cell, and after high-purity oxygen is introduced into a cathode, bias voltage is applied to the anode and the cathode of the electrolytic cell, so that the anode generates two electron water oxidation reactions to generate hydrogen peroxide, and meanwhile, the cathode generates an oxygen reduction reaction to generate the hydrogen peroxide.
3. The method for producing high-purity hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the neutral or alkaline electrolyte consists of two-level or three-level pure water and electrolyte K with the purity more than or equal to 3N2CO3Or Na2CO3The pH value range of the composition is 7-13.
4. The method for producing high-purity hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the oxygen is high-purity oxygen with the industrial use of more than or equal to 3N or oxygen with the purity of more than or equal to 90 percent prepared by an oxygen generator.
5. The method for producing high-purity hydrogen peroxide according to claim 1, wherein the method comprises the following steps: 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.
6. The method for producing high-purity hydrogen peroxide according to claim 5, wherein the method comprises the following steps: the chemical composition 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, B is +4/+6 valence metal cation or a mixed component thereof, x is more than or equal to 0, and y is less than or equal to 0.2.
7. The electrolytic process of claim 2, wherein: the carbon-based material is a graphite/carbon black/polytetrafluoroethylene composite, an oxidized or doped carbon material, or a carbon-based single-atom catalyst.
8. The method for producing high-purity hydrogen peroxide according to claim 1, wherein the method comprises the following steps: the distillation process comprises two physical separation processes of evaporation and rectification, electrolyte in an anode region and a cathode region is collected after electrolysis in an electrolytic cell is completed, nonvolatile matters including electrolyte and metal ions are removed in an evaporator through a reduced pressure evaporation process to obtain hydrogen peroxide with high purity and low concentration, and then redundant moisture is separated in a rectification tower through a reduced pressure rectification process.
9. The method for producing high-purity hydrogen peroxide according to claim 7, wherein the method comprises the following steps: ABS, CPVC, FKM, HDPE, PFA, PP-363, PTFE and PVC are used as linings in the electrolytic cell, the evaporator and the rectifying tower.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB316919A (en) * | 1928-05-04 | 1929-08-06 | Ig Farbenindustrie Ag | Improvements in or relating to the manufacture of hydrogen peroxide by cathodic reduction of oxygen |
| JPH08310803A (en) * | 1995-05-18 | 1996-11-26 | Mitsubishi Gas Chem Co Inc | Production of refined hydrogen peroxide |
| US6004449A (en) * | 1998-02-09 | 1999-12-21 | Boeing North American, Inc. | Method of operating electrolytic cell to produce highly concentrated alkaline 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 |
| CN113371683A (en) * | 2020-12-16 | 2021-09-10 | 惠州市宙邦化工有限公司 | Production method of electronic-grade hydrogen peroxide |
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- 2022-03-18 CN CN202210271443.9A patent/CN114561658A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB316919A (en) * | 1928-05-04 | 1929-08-06 | Ig Farbenindustrie Ag | Improvements in or relating to the manufacture of hydrogen peroxide by cathodic reduction of oxygen |
| JPH08310803A (en) * | 1995-05-18 | 1996-11-26 | Mitsubishi Gas Chem Co Inc | Production of refined hydrogen peroxide |
| US6004449A (en) * | 1998-02-09 | 1999-12-21 | Boeing North American, Inc. | Method of operating electrolytic cell to produce highly concentrated alkaline 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 |
| CN113371683A (en) * | 2020-12-16 | 2021-09-10 | 惠州市宙邦化工有限公司 | Production method of electronic-grade hydrogen peroxide |
Non-Patent Citations (1)
| Title |
|---|
| XINJIAN SHI 等: ""Light-Driven BiVO4–C Fuel Cell with Simultaneous Production of H2O2"", 《ADVANCED ENERGY MATERIALS》 * |
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