CN108179288A - A kind of chemical industry metallurgical method for separating of wulfenite - Google Patents
A kind of chemical industry metallurgical method for separating of wulfenite Download PDFInfo
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- CN108179288A CN108179288A CN201711456327.XA CN201711456327A CN108179288A CN 108179288 A CN108179288 A CN 108179288A CN 201711456327 A CN201711456327 A CN 201711456327A CN 108179288 A CN108179288 A CN 108179288A
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- Prior art keywords
- molybdenum
- lead
- sodium
- wulfenite
- concentrate
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Classifications
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/08—Preparation by double decomposition
- C01D9/10—Preparation by double decomposition with ammonium nitrate
-
- 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
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
Abstract
The present invention is a kind of chemical metallurgical method that molybdenum and lead are produced to lead concentrate and molybdenum concentrate with wulfenite of the chemical constitution symbiosis in same molecule by chemical sorting, by the use of vulcanized sodium saturated solution as lead agent is divided to be reacted with the wulfenite of pulverizing and jevigating, molybdenum is made to become the big sodium molybdate of solubility and enters solution, lead is then stranded in slag as insoluble compound vulcanized lead as artificial lead concentrate, and molybdenum and lead is enable to be totally separated from.Again using ammonium nitrate as molybdenum precipitation agent, in strong acidic environment(PH value is adjusted with nitric acid)Metathesis reaction is carried out with the sodium molybdate in solution, molybdenum is made to become ammonium molybdate precipitation separation.After separation of solid and liquid, molybdenum concentrate is made through expansion drying calcination in solid phase ammonium molybdate;Liquid phase is sodium nitrate solution, byproduct sodium nitrate is made through the crystallization of triple effect thin film evaporation, the drying of sulphur stateization, each section of tail gas scripture formula absorption plant absorbs qualified discharge with limewash, and absorbing liquid makees vulcanized sodium adapted water.
Description
Technical field
The present invention is a kind of by the wulfenite of molybdenum and lead with chemical constitution symbiosis in same molecule(PbMoO4)Pass through
Chemical sorting produces the chemical industry metallurgical technique of preparing of lead concentrate and molybdenum concentrate.
Background technology
In nature, molybdenum and lead form wulfenite with chemical constitution symbiosis in same molecule(PbMoO4).Using
Traditional selects smelting means(Gravity treatment, flotation, magnetic separation etc.)Can not detach lead and molybdenum therein.For a long time, a large amount of color molybdenum lead
Ore deposit is only used as lead ore and carries out smelting lead.This traditional way, not only the rate of recovery of lead is low, and value ratio lead is made to exceed decades of times
Strontium molybdate in vain abandon in slag.The present invention applies advanced chemical industry metallurgical technology, has successfully carried out the chemistry of wulfenite
Sorting, enables the molybdenum and lead separation and concentration completely and economically in wulfenite, and realized industrialization production, obtains very
Good economic benefit and social benefit.
Invention content
The technical problem to be solved by the present invention is to:A kind of molybdenum by wulfenite is provided and lead is kept completely separate enrichment and produces
The chemical sorting method of the chemical industry metallurgical of molybdenum concentrate and lead concentrate.Concrete scheme is to divide lead agent with breaking with vulcanized sodium saturated solution work
Wulfenite after comminution is thin is reacted, and molybdenum is made to become the big sodium molybdate of solubility and enters solution, lead is then used as chemical combination hard to tolerate
Object vulcanized lead, which is stranded in slag, is used as artificial lead concentrate.Again using ammonium nitrate as molybdenum precipitation agent, molybdenum is made to become ammonium molybdate precipitation separation.
Liquid phase is sodium nitrate, concentrated crystallization recycling byproduct sodium nitrate.Molybdenum concentrate is made through drying, calcination in ammonium molybdate.This scheme
Key has the following:
1st, select vulcanized sodium as lead agent is divided, using saturation sodium sulfide solution as the leachant of molybdenum, with it is broken, levigate after color molybdenum
Lead ore carries out metathesis reaction, and molybdenum becomes the very big sodium molybdate of solubility and enters solution, and lead is then stagnant for insoluble compound vulcanized lead
It stays in slag, becomes artificial lead concentrate.Enable to be switched " off " molybdenum and lead after strand to detach well.
PbMoO4+Na2S→Na2MoO4+Pb2S↓
2nd, ammonium nitrate is selected molybdenum to be made to become the ammonium molybdate Precipitation of solubility very little, mother in strong acid environment as molybdenum precipitation agent
Liquid is sodium nitrate solution, can condensing crystallizing, drying, recycling byproduct sodium nitrate.
Na2MoO4+2NH4NO3→(NH4)2MoO4↓+2Na2NO3
Ammonium nitrate is selected to have four as the principle of molybdenum precipitation agent:First, the ammonium molybdate precipitation separation of reaction generation solubility very little;Two
It is that the oxidation of ammonium nitrate avoids appraising at the current rate for molybdenum and generates heteropolyacid salt in the reaction, is only settled out with high price ammonium molybdate;Third,
The ammonium molybdate of generation is easily at low temperature(≥180℃)With regard to that can decompose, dilute releasing moisture and N2↑、H2↑, molybdenum concentrate MoO is made3:
(NH4)2MoO4 ≜ MoO3+3H2↑+N2↑+H2O
Fourth, reaction mother liquor is sodium nitrate, concentration, crystallization, dried recovered obtain the pair of the raw material ammonium nitrate higher value than addition
Product sodium nitrate.
3rd, control ammonium molybdate carries out calcination at a temperature of 190-250 DEG C and the molybdenum concentrate for meeting national standard is made.
4th, select triple effect thin film evaporation crystallizer efficient, reliable as the device of disposing mother liquor sodium nitrate.
The realization step of the present invention:
1st, wulfenite is broken, levigate:
It is centimetre block size that wulfenite is crushed in jaw crusher, levigate to -100 in overflow-type wet ball mill
≥95Wt%
2nd, the leaching of molybdenum is reacted with the separation of lead:
In the stirring of A3 steel bands, the reaction kettle heated.Through levigate wulfenite ore pulp in first pumping, it is molten to add vulcanized sodium saturation
Molten molybdenum is carried out under liquid heating stirring divides lead to react.Control condition is:
Mo:Na2S=1:1.3~1.5(It gives money as a gift base meter)
(Gu Mo):Liquid(Saturation Na2S): 1:2~2.5
Reaction temperature:80~90 DEG C
Mixing speed:90n/min
Reaction time:1.5~2h
Separation of solid and liquid is carried out in plate and frame filter press, and is washed to neutrality.Slag is artificial lead concentrate, and liquid is sodium molybdate solution, is washed
Water is returned with sodium sulphate water.
3rd, the precipitation reaction of molybdenum:
The precipitation reaction of molybdenum is carried out in the heating of lining acid-proof ceramic tile band, the reaction kettle stirred.Sodium molybdate solution is put into, with nitric acid tune
Whole pH value adds in ammonium nitrate, ammonium molybdate precipitation reaction is carried out under heating stirring to strong acid.Control condition is:
Mo:NH4NO3=1:1.3~1.5(Butt meter)
Ph value of reaction:1.0~1.5
Mixing speed:90n/min
Reaction temperature:Slightly boiling
Reaction time:30~40min
Separation of solid and liquid is carried out in corrosion resistant plate and frame filter press, and is washed solid to neutral.Solid phase is ammonium molybdate, and liquid phase is sodium nitrate
Mother liquor.Wash water is returned to be used with vulcanized sodium.
4th, molybdenum concentrate processed is decomposed in ammonium molybdate drying:
Ammonium molybdate calcination is dried in stainless steel flash dryer, molybdenum concentrate product, 200 ± 10 DEG C of drying temperature is made.
5th, mother liquid evaporation, crystallization, dry sodium nitrate byproduct processed:
Mother liquor is evaporated crystallization in stainless steel triple effect thin film evaporator, is then done on stainless steel fluidization vibrating dryer
It is dry, byproduct sodium nitrate is made.Drying temperature:100±10℃.
6th, the literary formula device processing of exhaust gas:
Each stage tail gas is reacted, using literary formula negative pressure absorbing device, with limewash sorption enhanced qualified discharge, absorbing liquid is incorporated to leaching
Molybdenum reacts.
The beneficial effects of the invention are as follows:
Since the molybdenum in wulfenite and lead symbiosis are in lead molybdate(PbMoO4)In same molecular formula, using traditional selecting and smelting technology
(Gravity treatment, flotation, magnetic separation etc.)Can not detach molybdenum and lead therein.A large amount of wulfenite is only used as lead ore progress for a long time
Smelting lead.This traditional way, not only lead recovery is low, and the strontium molybdate that value ratio lead is made to exceed decades of times is abandoned in slag in vain
In.The present invention applies advanced chemical industry metallurgical technology, has successfully carried out the chemical sorting of wulfenite, has made in wulfenite
It is lead concentrate and molybdenum concentrate that lead and molybdenum, which are able to separation and concentration completely and economically,.The present invention has also carried out Comprehensive utilization, female
Liquid is recycled as sodium nitrate byproduct, does not generate waste residue, waste liquid.Tail gas is using advanced literary formula device processing, qualified discharge.
Example one:Yunnan government office wulfenite sorts molybdenum concentrate and lead concentrate processed
First, wulfenite Principle components analysis:
Ingredient | Pb | Mo | W | V | CaO |
Content(%) | 15.97 | 7.33 | 2.18 | 3.63 | 16.31 |
2nd, main processes:
Mineral crush, roughing takes off mud scum, wet type fine grinding, and leaching molybdenum takes off lead, and ammonium sinks molybdenum, flashes calcination molybdenum concentrate, mother liquor concentrations
Crystallizing and drying recycles sodium nitrate.Each section of tail gas clean-up processing.
3rd, technological condition:
1st, the levigate condition of mineral:Mineral are broken for a centimeter block, roughing desliming in eddy flow machine, levigate in wet type overflow ball mill
Granularity is -100 mesh >=95Wt%
2nd, leaching molybdenum takes off leads part:Mo:Na2S=1:1.5 (butt meters)
Gu(Ore deposit):Liquid(Saturation Na2S)=1:2.5
Mixing speed:90n/min
Reaction temperature:85±5℃
Reaction time:2h
Tail gas clean-up:Saturated limewater
3rd, ammonium sinks molybdenum condition:Mo:NH4NO3=1:1.5 (butt meters)
Ph value of reaction:1.0±0.1
Mixing speed:90n/min
Reaction temperature:Slightly boiling
Reaction time:40min
4th, calcination condition is flashed:Flash calcination temperature:200±10℃
5th, mother liquor sodium nitrate recycling condition:Triple effect thin film evaporation:Negative pressure, slightly boiling
Sulphur state drying temperature:100±10℃
4th, products obtained therefrom quality and metal recovery rate:
1st, lead concentrate:Quality:Containing Pb38.6%, containing Mo 0.23%, metal recovery rate:91.37%
2nd, molybdenum concentrate:Quality
Ingredient | Mo | SiO2 | As | Sb | Sn | W | Pb | CaO |
Content(%) | 52.31 | 0.021 | 0.0011 | 0.011 | 0.0001 | 0.018 | 0.31 | 1.76 |
Metal recovery rate:83.86%
3rd, sodium nitrate:Quality
Ingredient | Na2NO3 | H2O | NaNO2 | Ca(NO2)2 | Fe |
Content(%) | 98.21 | 1.63 | 0.078 | 0.18 | 0.0031 |
Example two, Yunnan paper plant wulfenite sort molybdenum concentrate and lead concentrate processed
First, wulfenite Principle components analysis
Ingredient | Pb | Mo | W | V | CaO |
Content(%) | 11.56 | 6.37 | 2.04 | 2.38 | 16.31 |
2nd, main processes:
Mineral crush, roughing takes off mud scum, wet type fine grinding, and leaching molybdenum takes off lead, and ammonium sinks molybdenum, flashes calcination molybdenum concentrate, mother liquor concentrations
Crystallizing and drying recycles sodium nitrate.Each section of tail gas clean-up processing.
3rd, technological condition:
1st, the levigate condition of mineral:Mineral are broken for a centimeter block, roughing desliming in eddy flow machine, levigate grain in wet type overflow ball mill
It spends for -100 mesh >=95Wt%
2nd, leaching molybdenum takes off leads part:Mo:Na2S=1:1.4 (butt meters)
Gu(Ore deposit):Liquid(Saturation Na2S)=1:2.5
Mixing speed:90n/min
Reaction temperature:85±5℃
Reaction time:2h
Tail gas clean-up:Saturated limewater
3rd, ammonium sinks molybdenum condition:Mo:NH4NO3=1:1.5 (butt meters)
Ph value of reaction:1.0±0.1
Mixing speed:90n/min
Reaction temperature:Slightly boiling
Reaction time:40min
4th, calcination condition is flashed:Flash calcination temperature:200±10℃
5th, mother liquor sodium nitrate recycling condition:Triple effect thin film evaporation:Negative pressure, slightly boiling
Sulphur state drying temperature:100±10℃
4th, products obtained therefrom quality and metal recovery rate:
1. lead concentrate quality:Containing 0.19% metal recovery rates 89.43% containing Mo of Pb 36.31%
2. molybdenum concentrate quality:
Ingredient | Mo | SiO2 | As | Sb | Sn | W | Pb | CaO |
Content(%) | 51.86 | 0.076 | / | / | 0.0033 | 0.023 | 0.28 | 2.13 |
Metal recovery rate:81.26%
3rd, sodium nitrate quality:
Ingredient | NaNO3 | H2O | NaNO2 | Ca(NO2)2 | Fe |
Content(%) | 98.03 | 1.89 | 0.038 | 0.073 | 0.0048 |
Example three:Henan Luan Zhou wulfenites sort molybdenum concentrate and lead concentrate processed
One:Wulfenite Principle components analysis:
Ingredient | Pb | Mo | W | V | CaO |
Content(%) | 10.61 | 4.87 | 1.43 | 2.13 | 23.31 |
Two:Main processes:Mineral crush, roughing takes off mud scum, wet type fine grinding, and leaching molybdenum takes off lead, ammonium sinks molybdenum, flashes calcination
Molybdenum concentrate processed, mother liquor concentrations crystallizing and drying recycling sodium nitrate.Each section of tail gas clean-up processing.
Three:Technological condition:
1st, mineral materials comminution:Mineral are broken for a centimeter block, roughing desliming in eddy flow machine, levigate grain in wet type overflow ball mill
It spends for -100 mesh >=95Wt%
2nd, leaching molybdenum takes off leads part:Gu(Ore deposit):Liquid(Saturation Na2S)=1:2.3
Mixing speed:90n/min
Reaction temperature:85±5℃
Reaction time:2h
Tail gas clean-up:Saturated limewater.
3rd, ammonium sinks molybdenum condition:Mo:NH4NO3=1:1.5 (butt meters)
Ph value of reaction:1.0±0.1
Mixing speed:90n/min
Reaction temperature:Slightly boiling
Reaction time:40min
4th, calcination condition is flashed:Flash calcination temperature:200±10℃
5th, mother liquor sodium nitrate recycling condition:Triple effect thin film evaporation:Negative pressure, slightly boiling
Sulphur state drying temperature:100±10℃
Four:Products obtained therefrom quality and metal recovery rate:
1. lead concentrate:Quality:Containing 0.21% metal recovery rates 86.31% containing Mo of Pb 35.87%
2. molybdenum concentrate quality:
Ingredient | Mo | SiO2 | As | Sb | Sn | W | Pb | CaO |
Content(%) | 52.37 | 0.0031 | 0.019 | 0.093 | / | 0.036 | 0.16 | 2.98 |
Metal recovery rate:78.83%
3. sodium nitrate quality:
Ingredient | NaNO3 | H2O | NaNO2 | Ca(NO2)2 | Fe |
Content(%) | 98.33 | 1.69 | 0.069 | 0.21 | 0.0019 |
Claims (7)
1. a kind of chemical industry metallurgical method for separating of wulfenite, feature is to divide lead using saturation sodium sulfide solution as leaching molybdenum
Agent with it is broken, levigate after wulfenite reacted, molybdenum is made to become the big sodium molybdate of solubility and enters solution, lead is then indissoluble
Compound vulcanized lead is detained in slag, becomes artificial lead concentrate, molybdenum and lead are relatively completely separated, then using ammonium nitrate as heavy molybdenum
Agent, using nitric acid regulation system as molybdenum in strong acid environment, is made to become ammonium molybdate precipitation separation, solid phase ammonium molybdate is through dry calcination system
Molybdenum concentrate is obtained, the concentrated crystallization of liquid phase, dry obtained byproduct sodium nitrate, system tail gas text formula device is absorbed with limewash to be returned
It returns and is used with vulcanized sodium.
2. a kind of chemical industry metallurgical method for separating of wulfenite according to claim, feature are;Mineral through grinding,
Wet-milling is granularity -100 >=95Wt%.
3. a kind of chemical industry metallurgical method for separating of wulfenite according to claim, feature are;Ore deposit through wet-milling
Starch A3 steel bands stirring, heating reaction kettle in, with saturation vulcanized sodium make molybdenum leachant carry out leaching molybdenum lead is divided to react, control strip
Part is:Material ratio:Mo:Na2S=1:1.3~1.5(It gives money as a gift base meter);Mixing speed:90n/min;Reaction temperature:80~90 DEG C;
Reaction time:1.5~2h carries out separation of solid and liquid in plate and frame filter press after the completion of reaction, and washs to neutrality, and slag is artificial lead
Concentrate, liquid are sodium molybdate solution, and wash water is returned with sodium sulphate water.
4. a kind of chemical industry metallurgical method for separating of wulfenite according to claim, feature are;In lining acid resistant porcelain
The precipitation reaction of molybdenum is carried out in the stirring of brick band, the reaction kettle heated, is put into sodium molybdate solution, pH value is adjusted to strong acid ring with nitric acid
Border adds in ammonium nitrate, ammonium molybdate precipitation reaction, control condition is carried out under heating stirring:Mo:NH4NO3=1:1.3~1.5(Butt
Meter), ph value of reaction:1.0-1.5, mixing speed:90n/min, reaction temperature:Slightly boiling, reaction time:30-40min has reacted
Cheng Hou carries out separation of solid and liquid in corrosion resistant plate and frame filter press, and washes solid extremely neutrality, and solid phase is ammonium molybdate, and liquid phase is nitric acid
Mother liquid of sodium, wash water are returned with vulcanized sodium water.
5. a kind of chemical industry metallurgical method for separating of wulfenite according to claim, feature are;Ammonium molybdate is not
Decomposition is dried in rust steel flash dryer and produces molybdenum concentrate product, dry calcination temperature is 200 ± 10 DEG C.
6. a kind of chemical industry metallurgical method for separating of wulfenite according to claim, feature are;Mother liquor is in stainless
Condensing crystallizing is evaporated in steel triple effect thin film evaporator, then nitric acid is produced in drying on stainless steel sulphur state vibrating dryer
Sodium byproduct, drying temperature are 100 ± 10 DEG C.
7. a kind of chemical industry metallurgical method for separating of wulfenite according to claim, feature are;Soak molybdenum, heavy molybdenum and
The tail gas of dry calcination each process is carried out processing by the use of literary formula device using limewash as absorbent and reaches discharge, and absorbing liquid is incorporated to
Soak molybdenum.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1074486A (en) * | 1992-01-18 | 1993-07-21 | 戴元宁 | The chemical sorting method of wulfenite |
CN101050486A (en) * | 2007-05-15 | 2007-10-10 | 中南大学 | Method for classifying wulfenite |
CN103981379A (en) * | 2014-06-04 | 2014-08-13 | 北京矿冶研究总院 | Clean extraction method of wulfenite |
CN104152687A (en) * | 2014-07-19 | 2014-11-19 | 罗侣旦 | Production process for extracting elements such as aluminum, vanadium, molybdenum and nickel from black shale |
CN105463217A (en) * | 2015-11-25 | 2016-04-06 | 中南大学 | Treatment method for high-phosphorus high-molybdenum complex scheelite |
CN107298462A (en) * | 2017-07-03 | 2017-10-27 | 信丰华锐钨钼新材料有限公司 | A kind of method of the high purity molybdate from rough sodium molybdate solution |
-
2017
- 2017-12-28 CN CN201711456327.XA patent/CN108179288A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1074486A (en) * | 1992-01-18 | 1993-07-21 | 戴元宁 | The chemical sorting method of wulfenite |
CN101050486A (en) * | 2007-05-15 | 2007-10-10 | 中南大学 | Method for classifying wulfenite |
CN103981379A (en) * | 2014-06-04 | 2014-08-13 | 北京矿冶研究总院 | Clean extraction method of wulfenite |
CN104152687A (en) * | 2014-07-19 | 2014-11-19 | 罗侣旦 | Production process for extracting elements such as aluminum, vanadium, molybdenum and nickel from black shale |
CN105463217A (en) * | 2015-11-25 | 2016-04-06 | 中南大学 | Treatment method for high-phosphorus high-molybdenum complex scheelite |
CN107298462A (en) * | 2017-07-03 | 2017-10-27 | 信丰华锐钨钼新材料有限公司 | A kind of method of the high purity molybdate from rough sodium molybdate solution |
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Application publication date: 20180619 |