CN114606517A - High-quality raw material for producing ultra-pure electronic grade hydrogen peroxide and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-quality raw material for producing ultra-pure electronic grade hydrogen peroxide, which is hydrogen peroxide meeting SEMI G2 standard and prepared by an electrolysis process and a distillation process. The invention also discloses a preparation method of the high-quality raw material for producing the ultra-pure electronic grade hydrogen peroxide, which comprises the preparation steps of an electrolysis process and a distillation process. The invention has the beneficial effects that: high-purity water and high-purity oxygen with relatively low cost are used as raw materials, the total organic carbon content in the prepared hydrogen peroxide can be ignored, inorganic impurities are removed efficiently through a mature distillation process, and a high-quality hydrogen peroxide raw material meeting the SEMI G2 standard is obtained and is used as a raw material for producing higher-purity electronic grade hydrogen peroxide; the preparation process flow is relatively simple, and the high-quality raw material has lower comprehensive production cost than that of the preparation of the electronic grade hydrogen peroxide by directly purifying the industrial grade hydrogen peroxide, and has important industrial application value.
Description
Technical Field
The invention relates to the field of wet electronic chemicals, in particular to a high-quality raw material capable of producing ultra-pure electronic grade hydrogen peroxide in an ultra-purification process and a preparation 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. 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＝H2O2The method has the advantages of mature technology, high automation control degree, low raw material cost and energy consumption, suitability for large-scale production, and the defects of raw material supply bottleneck, complex production process and more organic impurities, inorganic impurities and mechanical impurities in the product.
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. The electronic grade hydrogen peroxide has extremely high requirements on impurity content, and can be further subdivided into five grades according to the standard SEMI C30-0218 of the International society for semiconductor and materials. The highest grade SEMI G5 (< 10ppt) was about 4 orders of magnitude higher than the lowest grade SEMI G1 (< 100ppb) for individual metal ion content, which was about 3 orders of magnitude higher than commercial grade hydrogen peroxide produced by the anthraquinone process (. about.100 ppm).
At present, most of the food grade, reagent grade and electronic grade hydrogen peroxide is obtained by using industrial grade hydrogen peroxide produced by anthraquinone Method as raw material and further using techniques such as rectification, ion exchange resin, membrane separation, supercritical extraction, adsorption, crystallization, etc. to deeply purify (refer to James A. Cook Jr. and Henry C. Stevens, Purification of hydrogen peroxide, US Patent 3617219,1971; John H. Boughton et al, Manufacture of high purity hydrogen peroxide by using conversion reactions, US Patent 4879043,1989; Helmut Honig and Sieged Geiged, Method for conversion of hydrogen peroxide for microorganisms, US Patent 5232680,1993; gelki Shimowa, Yoghiki, Minissuang and series, sea water and sea water, moisture and moisture reaction, moisture and moisture content 3632, the preparation method of electronic grade hydrogen peroxide is summarized in chemical industry and engineering technology, volume 35, 2 nd phase, pages 65-68, 2014). For ultra-pure electronic grade hydrogen peroxide such as SEMI G3, SEMI G4 and SEMI 5, the more advanced anthraquinone process is used to produce higher purity industrial grade hydrogen peroxide as raw material to reduce the overall production cost (Hisashi Sakaitani et al, Method for producing hydrogen peroxide, US Patent 7601323,2009).
The Hydrogen-oxygen direct synthesis method can be used to prepare higher purity Hydrogen peroxide, and may be used as an alternative raw material for producing electronic grade chemicals (Ricardo Abej Lo n et al, Hydrogen peroxide object direct synthesis as alternative raw material for ultra-purification process to product electronic grade Chemical, Journal of Chemical Technology & Biotechnology,2016,91: 1136-1148). An electrochemical method for generating two-electron water oxidation reaction on bismuth vanadate single-crystal anode catalyst, which is called bismuth vanadate method or single-crystal 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 Ling 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 and the direct hydrogen-oxygen synthesis method, the bismuth vanadate method and the oxygen cathode reduction method have the advantages of low price of required raw materials (water and oxygen), sufficient supply and good purity controllability, so that the produced hydrogen peroxide has higher purity. 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 ultra-pure electronic grade hydrogen peroxide can be effectively reduced.
Disclosure of Invention
The invention aims to provide a high-quality raw material for producing ultra-pure electronic grade hydrogen peroxide based on a bismuth vanadate method and an oxygen cathode reduction method aiming at the defects of the prior art.
The second purpose of the invention is to provide a preparation method of high-quality raw materials for producing ultra-pure electronic grade hydrogen peroxide.
In order to achieve the above purpose, the technical solution adopted by the present invention to solve the above technical problems is: a high-quality raw material for producing ultra-pure electronic grade hydrogen peroxide is prepared by an electrolysis process and a distillation process, can be a high-quality raw material with typical impurity content equivalent to or lower than that of the electronic grade hydrogen peroxide meeting the SEMI G2 standard, and can be used for producing the electronic grade hydrogen peroxide meeting the SEMI G3, G4 and G5 standards or higher in ultra-purification process.
A preparation method of a high-quality raw material for producing ultra-pure electronic grade hydrogen peroxide comprises the steps of an electrolysis process and a distillation process, wherein the electrolyte after the electrolysis process is subjected to distillation process treatment, the electrolysis process combines the advantages of a bismuth vanadate method and an oxygen cathode reduction method, an oxide single crystal wafer is used as an anode material of an electrolytic cell, a carbon-based material is used as a cathode material, a neutral or alkaline electrolyte is added into the electrolytic cell, and after oxygen is introduced into the cathode, a bias voltage is applied to the anode and the cathode of the electrolytic cell, so that the anode is subjected to two-electron water oxidation reaction to generate hydrogen peroxide (2H)2O→H2O2+2H++2e-) While the cathode is subjected to oxygen reduction reaction to generate hydrogen peroxide (O)2+2H++2e-→H2O2) General chemical (II)The reaction equation is O2+2H2O→2H2O2. The distillation process comprises two physical separation processes of evaporation and rectification. The prepared product is a high-quality raw material with typical impurity content equivalent to or lower than that of SEMI G2 electronic grade hydrogen peroxide, and can be used for producing the SEMI G3, G4, G5 or higher-purity electronic grade hydrogen peroxide in an ultra-pure process.
The neutral or alkaline electrolyte consists of electronic grade water (EW-I, EW-II or EW-III according to GB/T11446.1-2013) or water for analytical laboratories (primary water, secondary water or tertiary water according to GB/T6682-2008) and high-purity electrolyte K2CO3Or Na2CO3Not less than 99.9 percent, and the pH value range is 7-13, thereby ensuring the stability of the generated hydrogen peroxide.
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.
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 oxygen is industrial oxygen with the purity of more than or equal to 99.9 percent or cheap oxygen with the purity of more than or equal to 90 percent prepared by an oxygen generator.
The external bias voltage is 1.8-2.5V, and the current density during electrolysis is 0.01-0.3A/cm2。
The distillation process comprises two physical separation processes of evaporation and rectification. After the electrolysis is finished, electrolyte (the hydrogen peroxide content is 0.5 wt% -2 wt%) in the anode region and the cathode region is collected, nonvolatile matters including electrolyte and metal ions are removed in an evaporator through an evaporation process to obtain a high-purity low-concentration hydrogen peroxide solution, and then redundant moisture is separated in a rectifying tower through a reduced pressure rectification process to obtain the hydrogen peroxide solution with the expected concentration (the content of single metal ions is less than 10ppb, and the content of total organic carbon is less than 200ppb), so that the requirements of SEMI G2 are met.
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 selected organic lining materials have excellent chemical stability, thermal stability, hydrogen peroxide friendliness and the like, and do not initiate hydrogen peroxide decomposition is the most important index.
The invention has the beneficial effects that: high-purity water and high-purity oxygen with relatively low cost are used as raw materials, the total organic carbon content in the prepared hydrogen peroxide can be ignored, inorganic impurities are efficiently removed through a mature distillation process, and the high-quality hydrogen peroxide raw material which meets the SEMI G2 standard is obtained and used as a raw material for producing higher-purity hydrogen peroxide; the preparation process flow is relatively simple, and the high-quality raw material has lower comprehensive production cost than the electronic grade hydrogen peroxide (SEMI G2) prepared by directly purifying the industrial grade hydrogen peroxide, and has important industrial application value.
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: production apparatus and parameters
The production device comprises an electrolytic bath, an evaporator and a rectifying tower, and meltable polytetrafluoroethylene is adopted in the electrolytic bath, the evaporator and the rectifying towerEnrafluoroethylene (PFA) as an inner liner. Preferably, the thickness of the liner is in the range of 0.5-5 mm. Most preferably, the thickness of the liner is in the range of 0.8 to 1mm, which is effective in preventing decomposition of hydrogen peroxide while ensuring economy and reliability. 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 is preferably a falling film evaporator, and the rectifying tower adopts a primary rectifying tower. The applied bias voltage was 2.3V, and the current density during electrolysis was 0.15A/cm2。
Example 2: high-quality hydrogen peroxide raw material meeting SEMI G2 requirement
Based on the production device and the process parameters of example 1, the raw materials adopted in this example are: na (Na)2CO3(99.9%) analysis of the laboratory water secondary water (conductivity. ltoreq.0.1 mS/m, evaporation residue. ltoreq.1.0 mg/L); the pH of the electrolyte is 9.5; o is2Cheap oxygen with the purity more than or equal to 90 percent is prepared by the oxygen generator. Electrolyzing and distilling to obtain hydrogen peroxide raw material.
The content analysis of organic matters and inorganic matters is carried out on the hydrogen peroxide raw material, and the result is as follows: h2O2 30.5wt％；TOC<500 ppb; evaporation of residue<0.1 mg/L; content of single metal ion:<10 ppb. The hydrogen peroxide raw material basically meets the SEMI G2 electronic grade hydrogen peroxide standard.
Example 3: high-quality hydrogen peroxide raw material meeting SEMI G2 requirement
Based on the production device and the process parameters of example 1, the raw materials adopted in this example are: na (Na)2CO3(99.9%), electronic grade water (resistivity ≥ 12M Ω. M, TOC)<200ppb, and the content of single metal ions is less than or equal to 5 ppb); the pH of the electrolyte is 9.5; o is2As high purity oxygen (99.999%). Electrolyzing and distilling to obtain hydrogen peroxide raw material.
The content analysis of organic matters and inorganic matters is carried out on the hydrogen peroxide raw material, and the result is as follows: h2O2 31.0wt％；TOC<100 ppb; content of single metal ion: na (Na)<10ppb of other metal ions<2 ppb. Except that the content of Na ions in the hydrogen peroxide raw material is slightly over standard, the other raw materials all meet or even exceed the SEMI G2 electronic grade hydrogen peroxide standard.
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 (10)
1. A high-quality raw material for producing ultra-pure electronic grade hydrogen peroxide is characterized in that: is hydrogen peroxide prepared by an electrolysis process and a distillation process.
2. The high-quality feedstock for the production of ultrapure electronic-grade hydrogen peroxide of claim 1, wherein: the hydrogen peroxide is hydrogen peroxide meeting the SEMI G2 standard.
3. The method for preparing high-quality raw materials for producing ultrapure electronic grade hydrogen peroxide according to claim 1 or 2, wherein: the preparation method comprises the steps of an electrolysis process and a distillation process, wherein the electrolyte after the electrolysis process is treated by the distillation process, the electrolysis process adopts an oxide single chip as an anode material of an electrolytic cell, a carbon-based material is used as a cathode material, neutral or alkaline electrolyte is added into the electrolytic cell, and after 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 meanwhile, the cathode generates oxygen reduction reaction to generate hydrogen peroxide; the distillation process comprises two physical separation processes of evaporation and rectification.
4. The method for preparing a high-quality raw material for producing ultrapure electronic-grade hydrogen peroxide according to claim 3, wherein the method comprises the following steps: the neutral or alkaline electrolyte is prepared from electronic grade water or analysis laboratory water and high-purity electrolyte K2CO3Or Na2CO3The pH value range of the composition is 7-13.
5. The method for preparing a high-quality raw material for producing ultrapure electronic-grade hydrogen peroxide according to claim 3, wherein the method comprises the following steps: the oxide single crystal wafer is a crystal face of a doped bismuth vanadate single crystal {111}, {110}, {112}, {100} and the like or a crystal face of a doped zinc oxide single crystal {0001 }.
6. The method for preparing a high-quality raw material for producing ultrapure electronic-grade hydrogen peroxide according to claim 3, wherein the method comprises the following steps: the carbon-based material is a graphite/carbon black/polytetrafluoroethylene composite, an oxidized or doped carbon material, or a carbon-based single-atom catalyst.
7. The method for preparing a high-quality raw material for producing ultrapure electronic-grade hydrogen peroxide according to claim 3, wherein the method comprises the following steps: the oxygen is industrial oxygen with the purity of more than or equal to 99.9 percent or oxygen with the purity of more than or equal to 90 percent prepared by an oxygen generator.
8. The method for preparing a high-quality raw material for producing ultrapure electronic-grade hydrogen peroxide according to claim 3, wherein the method comprises the following steps: the external bias voltage is 1.8-2.5V, and the current density during electrolysis is 0.01-0.3A/cm2。
9. The method for preparing a high-quality raw material for producing ultrapure electronic-grade hydrogen peroxide according to claim 3, wherein the method comprises the following steps: after the electrolysis is finished, electrolyte in the anode region and the cathode region is collected, nonvolatile matters including electrolyte and metal ions are removed in an evaporator through a reduced pressure evaporation process to obtain a high-purity and low-concentration hydrogen peroxide solution, and then redundant moisture is separated in a rectifying tower through a reduced pressure rectification process to obtain the hydrogen peroxide solution with the content of single metal ions less than 10ppb and the content of total organic carbon less than 200 ppb.
10. The preparation method of the high-quality raw material for producing the ultrapure electronic grade hydrogen peroxide according to claim 3, wherein: ABS plastics, chlorinated polyvinyl chloride, fluororubber, high-density polyethylene, meltable polytetrafluoroethylene, polypropylene, polytetrafluoroethylene or polyvinyl chloride are used as linings in the electrolytic cell, the evaporator and the rectifying tower.
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| CN115259097A (en) * | 2022-08-24 | 2022-11-01 | 菏泽市巨丰新能源有限公司 | Hydrogen peroxide solution purification production system |
Citations (15)
| 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 |
| GB473342A (en) * | 1936-04-09 | 1937-10-11 | George Zotos | Improvements in the manufacture of hydrogen peroxide |
| GB627249A (en) * | 1945-07-11 | 1949-08-04 | Buffalo Electro Chem Co | Improvements in or relating to the distillation of hydrogen peroxide |
| GB1466990A (en) * | 1973-06-20 | 1977-03-16 | Kernforschungsanlage Juelich | Process for the preparation of hydrogen peroxide |
| JPH07118002A (en) * | 1993-08-30 | 1995-05-09 | Katayama Chem Works Co Ltd | Method for producing hydrogen peroxide and device therefor |
| JPH08310803A (en) * | 1995-05-18 | 1996-11-26 | Mitsubishi Gas Chem Co Inc | Production of refined hydrogen peroxide |
| JPH09184085A (en) * | 1995-12-28 | 1997-07-15 | Permelec Electrode Ltd | Production of hydrogen peroxide |
| US5670028A (en) * | 1994-11-22 | 1997-09-23 | Ube Industries, Ltd. | Process for preparing high purity hydrogen peroxide aqueous solution |
| US6004449A (en) * | 1998-02-09 | 1999-12-21 | Boeing North American, Inc. | Method of operating electrolytic cell to produce highly concentrated alkaline hydrogen peroxide |
| CN1293641A (en) * | 1999-02-08 | 2001-05-02 | 大赛璐化学工业株式会社 | Process for producing hydrogen peroxide |
| CN101454483A (en) * | 2005-06-30 | 2009-06-10 | 阿克佐诺贝尔公司 | Electrosynthesis of hydrogen peroxide |
| US20120148482A1 (en) * | 2010-12-08 | 2012-06-14 | Shanghai Huayi Microelectronic Material Co., Ltd. | Method for producing ultra-pure aqueous hydrogen peroxide solution |
| CN105951117A (en) * | 2016-07-19 | 2016-09-21 | 李国岭 | Electrolysis method for producing high-purity hydrogen peroxide and hydrogen with low cost |
| US20200173045A1 (en) * | 2017-08-23 | 2020-06-04 | The Board Of Trustees Of The Leland Stanford Junior University | N- and O-Doped Carbon with High Selectivity for Electrochemical H2O2 Production in Neutral Condition |
| CN113172234A (en) * | 2021-04-13 | 2021-07-27 | 南开大学 | Preparation method of carbon-based single-atom electrocatalyst |
-
2022
- 2022-03-18 CN CN202210270345.3A patent/CN114606517A/en active Pending
Patent Citations (15)
| 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 |
| GB473342A (en) * | 1936-04-09 | 1937-10-11 | George Zotos | Improvements in the manufacture of hydrogen peroxide |
| GB627249A (en) * | 1945-07-11 | 1949-08-04 | Buffalo Electro Chem Co | Improvements in or relating to the distillation of hydrogen peroxide |
| GB1466990A (en) * | 1973-06-20 | 1977-03-16 | Kernforschungsanlage Juelich | Process for the preparation of hydrogen peroxide |
| JPH07118002A (en) * | 1993-08-30 | 1995-05-09 | Katayama Chem Works Co Ltd | Method for producing hydrogen peroxide and device therefor |
| US5670028A (en) * | 1994-11-22 | 1997-09-23 | Ube Industries, Ltd. | Process for preparing high purity hydrogen peroxide aqueous solution |
| JPH08310803A (en) * | 1995-05-18 | 1996-11-26 | Mitsubishi Gas Chem Co Inc | Production of refined hydrogen peroxide |
| JPH09184085A (en) * | 1995-12-28 | 1997-07-15 | Permelec Electrode Ltd | Production of 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 |
| CN1293641A (en) * | 1999-02-08 | 2001-05-02 | 大赛璐化学工业株式会社 | Process for producing hydrogen peroxide |
| CN101454483A (en) * | 2005-06-30 | 2009-06-10 | 阿克佐诺贝尔公司 | Electrosynthesis of hydrogen peroxide |
| US20120148482A1 (en) * | 2010-12-08 | 2012-06-14 | Shanghai Huayi Microelectronic Material Co., Ltd. | Method for producing ultra-pure aqueous hydrogen peroxide solution |
| CN105951117A (en) * | 2016-07-19 | 2016-09-21 | 李国岭 | Electrolysis method for producing high-purity hydrogen peroxide and hydrogen with low cost |
| US20200173045A1 (en) * | 2017-08-23 | 2020-06-04 | The Board Of Trustees Of The Leland Stanford Junior University | N- and O-Doped Carbon with High Selectivity for Electrochemical H2O2 Production in Neutral Condition |
| CN113172234A (en) * | 2021-04-13 | 2021-07-27 | 南开大学 | Preparation method of carbon-based single-atom electrocatalyst |
Non-Patent Citations (2)
| Title |
|---|
| XINJIAN SHI等: "Light-Driven BiVO4–C Fuel Cell with Simultaneous Production of H2O2", 《ADVANCED ENERGY MATERIALS》 * |
| 桑志远等: "碳基非金属纳米材料用于二电子氧 还原制备过氧化氢的研究进展", 《新型碳材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115259097A (en) * | 2022-08-24 | 2022-11-01 | 菏泽市巨丰新能源有限公司 | Hydrogen peroxide solution purification production system |
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