CN108910956A - A method of soft magnetism mangano-manganic oxide is produced using aniline reduction electrolytic manganese anode mud - Google Patents
A method of soft magnetism mangano-manganic oxide is produced using aniline reduction electrolytic manganese anode mud Download PDFInfo
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- CN108910956A CN108910956A CN201810783429.0A CN201810783429A CN108910956A CN 108910956 A CN108910956 A CN 108910956A CN 201810783429 A CN201810783429 A CN 201810783429A CN 108910956 A CN108910956 A CN 108910956A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/244—Preparation by double decomposition of ammonium salts with sulfates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a kind of methods using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide, include the following steps：S1 adds the broken slurrying of water mill in Manganese anode slime；S2 imports manganese slurry in the reaction kettle with cooling device；Aniline is added in manganese slurry in S3；Manganese slurry is heated to 90~130 degrees Celsius, the benzoquinone after collecting vaporization by S4；S5 obtains slicker solder slag and manganese sulfate solution by manganese slurry by filter press separating and filtering；Manganese sulfate solution is controlled at 15~50 degrees Celsius, ammonium hydrogen carbonate is added in manganese sulfate solution, obtains manganese carbonate and ammonium sulfate by S6；S7, evaporation ammonium sulfate recycling ammonium sulfate do agricultural fertilizer, and by manganese carbonate, calcining obtains solid-state mangano-manganic oxide in 830~1000 celsius temperatures after deionized water is washed, by solid-state mangano-manganic oxide after crushing or sand milling, it is washed with deionized, dries, obtain finished product mangano-manganic oxide.
Description
Technical field
The present invention relates to a kind of methods using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide, belong to
The technology for producing field of mangano-manganic oxide.
Background technique
When being electrolysed manganese sulfate, there is a manganese metal and the earth of positive pole, manganese metal is used as the deep processing of manganese, and the earth of positive pole its mainly
Ingredient is MnO2, and containing valuable metals such as lead, tin, antimony, it is generally industrially regarded into pyrolusite raw material, using iron powder reducing
Method, ferrous sulfate reduction leaching process, two mines roasting water seaoning or two mine One-step production manganese sulfates.But no matter which kind of side used
Method, because solid reductant is added, the leaching quantity of slag after soaking manganese is larger, causes the tenors such as lead, tin, the antimony in slag lower, returns
It is big to receive difficulty, cost recovery is high, and without economic significance, therefore current domestic production producer is substantially by the way of landfill
Reason, leads to the wasting of resources and environmental pollution.
Summary of the invention
Soft magnetism mangano-manganic oxide is produced using aniline reduction electrolytic manganese anode mud the object of the present invention is to provide a kind of
Method, manganese, benzoquinone have not only been recycled using this method, but also recycled the lead etc. in the earth of positive pole to the greatest extent to have
Valence element, while perfectly solving the Manganese anode slime bring wasting of resources of electrolytic manganese manufacturer and problem of environmental pollution.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A method of soft magnetism mangano-manganic oxide being produced using aniline reduction electrolytic manganese anode mud, is included the following steps：
S1 adds water slurrying in Manganese anode slime；Below levigate extremely -120 mesh of Manganese anode slime；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Solid-to-liquid ratio (guaranteeing the initial acid concentrations being added in 400~500g/l) and manganese dioxide content, are added according to manganese dioxide content
Sulfuric acid solution (dosage of sulfuric acid be theoretical amount 1~2 times)；
S3, by reactor temperature control at 30 degrees Celsius hereinafter, manganese slurry in aniline is added, after having added aniline,
It is reacted 2~10 hours under normal temperature state；
MnO2+C6H7N+H2SO4→MnSO4+C6H4O2+H2O
Manganese slurry is heated to 90~130 degrees Celsius by S4, and the benzoquinone after collecting vaporization, temperature is too low, and benzoquinone is not
It can vaporize completely, the excessively high benzoquinone of temperature will appear coking phenomenon, both will affect the rate of recovery of benzoquinone, using this
The rate of recovery of method benzoquinone is up to 97% or more；
S5, by manganese slurry be cooled to 55 degrees Celsius or less (temperature is excessively high, in ammonium hydroxide with when ammonium hydroxide volatilization loss it is larger),
Ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 5~7, and (under this pH condition, the impurity other than manganese is deposited in solid form
), by manganese slurry by filter press separating and filtering, obtain slicker solder slag (lead, tin the rate of recovery can achieve 99% or more) and sulfuric acid
Manganese solution；
MeSO4+(NH4)2S→MeS+(NH4)2SO4, Me indicates the heavy metals such as lead in this chemical formula.
Manganese sulfate solution is controlled at 15~50 degrees Celsius, ammonium hydrogen carbonate is added in manganese sulfate solution, obtains carbonic acid by S6
Manganese and ammonium sulfate；
MnSO4+NH4HCO3→MnCO3+(NH)2SO4+CO2
S7, evaporation ammonium sulfate recycling ammonium sulfate do agricultural fertilizer, by manganese carbonate after deionized water is washed 830~
In 1000 celsius temperatures calcining obtain solid-state mangano-manganic oxide, by solid-state mangano-manganic oxide after crushing or frosted, spend from
Sub- water washing dries to obtain finished product mangano-manganic oxide.
MnCO3→Mn3O4+CO2
In a kind of method using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide above-mentioned, the step
Rapid S5 further includes following methods：The manganese sulfate solution is collected, ammonium sulfide solution is added in manganese sulfate solution, removes manganese sulfate
Heavy metal in solution.MeSO4+(NH4)2S→MeS+(NH4)2SO4, Me indicates the heavy metals such as lead in this chemical formula.
In a kind of method using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide above-mentioned, the step
Rapid S1 further includes following methods：Manganese anode slime particle is milled to -120 mesh hereinafter, then adding water slurrying.
In a kind of method using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide above-mentioned, the manganese
The Manganese anode slime generated when the earth of positive pole is electrolytic manganese.
In a kind of method using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide above-mentioned, by aniline
Be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry.
Compared with prior art, lead, tin, the antimony etc. in the original earth of positive pole are remained after benzoquinone of the present invention, manganese are recovered, in slag
Element and a small amount of manganese, because the quantity of slag significantly tails off, therefore in slag, slicker solder antimony content significantly increases and by enriching and recovering.The technique is at one stroke
Three, manganese, benzoquinones are not only recycled, but also recycled the valuable elements such as the lead in the earth of positive pole to the greatest extent, while perfect
Solve the Manganese anode slime bring wasting of resources of electrolytic manganese manufacturer and problem of environmental pollution.
The present invention is further illustrated With reference to embodiment.
Specific embodiment
The embodiment of the present invention 1：A kind of side using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide
Method includes the following steps：
S1 adds water slurrying in Manganese anode slime, and Manganese anode slime is levigate to -120 mesh；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Sulfuric acid solution is added according to manganese dioxide content in solid-to-liquid ratio and manganese dioxide content；Guarantee the initial acid concentrations being added in 400g/
L, the dosage of sulfuric acid are 1 times of theoretical amount；
Reactor temperature is controlled at 30 degrees Celsius, aniline is added in manganese slurry, after having added aniline, in room temperature by S3
Reacted 2 hours under state, by aniline be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry；
Manganese slurry is heated to 90 degrees Celsius, the benzoquinone after collecting vaporization by S4；
Manganese slurry is cooled to 55 degrees Celsius, ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 5, manganese slurry is passed through by S5
Filter press separating and filtering obtains slicker solder slag and manganese sulfate solution, collects the manganese sulfate solution, sulphur is added in manganese sulfate solution
Change ammonium salt solution, removes the heavy metals such as the lead in manganese sulfate solution；
S6, by manganese sulfate solution control at 15 degrees Celsius, ammonium hydrogen carbonate is added in manganese sulfate solution, obtain manganese carbonate and
Ammonium sulfate；
S7, evaporation ammonium sulfate recycling ammonium sulfate do agricultural fertilizer, manganese carbonate are taken the photograph after deionized water is washed 850
Calcining obtains solid-state mangano-manganic oxide in family name's degree high temperature, by solid-state mangano-manganic oxide after being sanded, is washed with deionized, and dries
Obtain finished product mangano-manganic oxide.
Embodiment 2：A method of using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide, including with
Lower step：
Then plus water slurrying S1, the Manganese anode slime particle generated when by electrolytic manganese are milled to -150 mesh,；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Sulfuric acid solution is added according to manganese dioxide content in solid-to-liquid ratio and manganese dioxide content；Guarantee the initial acid concentrations being added in 500g/
L, the dosage of sulfuric acid are 2 times of theoretical amount；
Reactor temperature is controlled at 20 degrees Celsius, aniline is added in manganese slurry, after having added aniline, in room temperature by S3
Reacted 10 hours under state, by aniline be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry；
Manganese slurry is heated to 130 degrees Celsius, the benzoquinone after collecting vaporization by S4；
Manganese slurry is cooled to 45 degrees Celsius, ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 7, manganese slurry is passed through by S5
Filter press separating and filtering obtains slicker solder slag and manganese sulfate solution, collects the manganese sulfate solution, sulphur is added in manganese sulfate solution
Change ammonium salt solution, removes the heavy metals such as the lead in manganese sulfate solution；
S6, by manganese sulfate solution control at 50 degrees Celsius, ammonium hydrogen carbonate is added in manganese sulfate solution, obtain manganese carbonate and
Ammonium sulfate；
S7, evaporation ammonium sulfate recycling ammonium sulfate does agricultural fertilizer, by manganese carbonate 1000 after deionized water is washed
Calcining obtains solid-state mangano-manganic oxide in celsius temperature, after crushed by solid-state mangano-manganic oxide, is washed with deionized, and dries
It is dry, obtain finished product mangano-manganic oxide.
Embodiment 3：A method of using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide, including with
Lower step：
Then plus water slurrying S1, the Manganese anode slime particle generated when by electrolytic manganese are milled to -160 mesh,；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, detection manganese slurry
Sulfuric acid solution is added according to manganese dioxide content in solid-to-liquid ratio and manganese dioxide content；Guarantee the initial acid concentrations being added in 430g/
L, the dosage of sulfuric acid are 1.4 times of theoretical amount；
Reactor temperature is controlled at 25 degrees Celsius, aniline is added in manganese slurry, after having added aniline, in room temperature by S3
Reacted 7 hours under state, by aniline be no more than in reaction kettle controlled at controlling value, aniline is added in manganese slurry；
Manganese slurry is heated to 110 degrees Celsius, the benzoquinone after collecting vaporization by S4；
Manganese slurry is cooled to 35 degrees Celsius, ammonium hydroxide is added in manganese slurry, the pH value that manganese is starched is adjusted to 6, manganese slurry is passed through by S5
Filter press separating and filtering obtains slicker solder slag and manganese sulfate solution, collects the manganese sulfate solution, sulphur is added in manganese sulfate solution
Change ammonium salt solution, removes the heavy metals such as the lead in manganese sulfate solution；
S6, by manganese sulfate solution control at 30 degrees Celsius, ammonium hydrogen carbonate is added in manganese sulfate solution, obtain manganese carbonate and
Ammonium sulfate；
S7, evaporation ammonium sulfate recycling ammonium sulfate do agricultural fertilizer, manganese carbonate are taken the photograph after deionized water is washed 900
Calcining obtains solid-state mangano-manganic oxide in family name's degree high temperature, by solid-state mangano-manganic oxide after being sanded, is washed with deionized, and dries
Obtain finished product mangano-manganic oxide.
Claims (6)
1. a kind of method using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide, which is characterized in that including
Following steps：
S1 adds water slurrying in Manganese anode slime；
S2 imports manganese slurry in the reaction kettle with cooling device, measures the volume of manganese slurry in reaction kettle, the solid-liquid of detection manganese slurry
Than with manganese dioxide content, according to manganese dioxide content be added sulfuric acid solution；
S3 controls reactor temperature at 30 degrees Celsius hereinafter, aniline is added in manganese slurry, after having added aniline, in room temperature
It is reacted 2~10 hours under state；
Manganese slurry is heated to 90~130 degrees Celsius, the benzoquinone after collecting vaporization by S4；
S5, by manganese slurry be cooled to 55 degrees Celsius hereinafter, manganese slurry in ammonium hydroxide is added, by manganese starch pH value be adjusted to 5~7, manganese is starched
By filter press separating and filtering, slicker solder slag and manganese sulfate solution are obtained；
S6, by manganese sulfate solution control at 15~50 degrees Celsius, ammonium hydrogen carbonate is added in manganese sulfate solution, obtain manganese carbonate and
Ammonium sulfate；
S7, evaporation ammonium sulfate recycling ammonium sulfate does agricultural fertilizer, by manganese carbonate 830~1000 after deionized water is washed
Calcining obtains solid-state mangano-manganic oxide in celsius temperature, by solid-state mangano-manganic oxide after crushing or sand milling, uses deionized water
Washing, drying, obtains finished product mangano-manganic oxide.
2. a kind of side using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide according to claim 1
Method, which is characterized in that the step S5 further includes following methods：The manganese sulfate solution is collected, is added in manganese sulfate solution
Ammonium sulfide solution removes the heavy metal in manganese sulfate solution.
3. a kind of side using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide according to claim 1
Method, which is characterized in that the step S1 further includes following methods：Manganese anode slime particle is milled to -120 mesh hereinafter, then adding
Water slurrying.
4. a kind of side using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide according to claim 1
Method, which is characterized in that the Manganese anode slime that the Manganese anode slime generates when being electrolytic manganese.
5. a kind of side using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide according to claim 1
Method, which is characterized in that further include following methods in the step S3：By aniline be no more than reaction kettle in controlled at control
Aniline is added in manganese slurry value processed.
6. a kind of side using aniline reduction electrolytic manganese anode mud production soft magnetism mangano-manganic oxide according to claim 1
Method, which is characterized in that further include following methods in the step S2：The solid-to-liquid ratio and manganese dioxide content for detecting manganese slurry, according to
Sulfuric acid solution is added in manganese dioxide content；Guarantee the initial acid concentrations being added in 400~500g/l, the dosage of sulfuric acid is theoretical amount
1~2 times.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115011799A (en) * | 2022-07-13 | 2022-09-06 | 重庆上甲电子股份有限公司 | Method for producing soft magnetic trimanganese tetroxide by using electrolytic manganese anode slime |
| CN115259230A (en) * | 2022-07-13 | 2022-11-01 | 重庆上甲电子股份有限公司 | Impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching |
| CN116835971A (en) * | 2023-07-12 | 2023-10-03 | 华东师范大学 | Method for preparing high saturation magnetic induction density manganese-zinc ferrite material by using manganese waste residues and zinc waste residues |
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| CN101348280A (en) * | 2008-09-09 | 2009-01-21 | 湖南东方锰业集团股份有限公司 | Method for preparing electronic grade non-selenium manganomanganic oxide from dialogite |
| CN101698513A (en) * | 2009-11-03 | 2010-04-28 | 鄢冬子 | Method for preparing high-purity trimanganese tetroxide |
| CN103789551A (en) * | 2014-02-18 | 2014-05-14 | 广西大学 | Method for preparing manganese sulfate electrolyte and recycling lead by using electrolytic manganese anode mud |
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| CN1121049A (en) * | 1994-10-18 | 1996-04-24 | 冶金工业部长沙矿冶研究院 | Method for producing high-purity manganese carbonate by using pyrolusite |
| CN1126246A (en) * | 1994-10-28 | 1996-07-10 | 北京矿冶研究总院 | Arylamine reduction leaching method for marine manganese nodule |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115011799A (en) * | 2022-07-13 | 2022-09-06 | 重庆上甲电子股份有限公司 | Method for producing soft magnetic trimanganese tetroxide by using electrolytic manganese anode slime |
| CN115259230A (en) * | 2022-07-13 | 2022-11-01 | 重庆上甲电子股份有限公司 | Impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching |
| CN115259230B (en) * | 2022-07-13 | 2023-04-18 | 重庆上甲电子股份有限公司 | Impurity removal method for producing trimanganese tetroxide for soft magnetism from electrolytic manganese anode mud by utilizing molten acid leaching |
| CN116835971A (en) * | 2023-07-12 | 2023-10-03 | 华东师范大学 | Method for preparing high saturation magnetic induction density manganese-zinc ferrite material by using manganese waste residues and zinc waste residues |
| CN116835971B (en) * | 2023-07-12 | 2024-02-27 | 华东师范大学 | Method for preparing high saturation magnetic induction density manganese-zinc ferrite material by using manganese waste residues and zinc waste residues |
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Application publication date: 20181130 |