CN111422928A - Nickel deposition method without impurity brought in laterite-nickel ore leaching solution - Google Patents
Nickel deposition method without impurity brought in laterite-nickel ore leaching solution Download PDFInfo
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- CN111422928A CN111422928A CN202010286751.XA CN202010286751A CN111422928A CN 111422928 A CN111422928 A CN 111422928A CN 202010286751 A CN202010286751 A CN 202010286751A CN 111422928 A CN111422928 A CN 111422928A
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- nickel
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- precipitation
- liquid
- laterite
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 99
- 238000002386 leaching Methods 0.000 title claims abstract description 23
- 239000012535 impurity Substances 0.000 title claims abstract description 14
- 238000000151 deposition Methods 0.000 title claims description 15
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 238000001556 precipitation Methods 0.000 claims abstract description 31
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 14
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 230000000694 effects Effects 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000004064 recycling Methods 0.000 claims abstract description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000011504 laterite Substances 0.000 claims abstract description 4
- 229910001710 laterite Inorganic materials 0.000 claims abstract description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000011630 iodine Substances 0.000 claims description 5
- 229910052740 iodine Inorganic materials 0.000 claims description 5
- 239000012527 feed solution Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001425 magnesium ion Inorganic materials 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- BXNFVPMHMPQBRO-UHFFFAOYSA-N magnesium nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Mg++].[Ni++] BXNFVPMHMPQBRO-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- -1 sulfur ions Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a nickel precipitation method without impurity brought in from a laterite-nickel ore leaching solution, which is characterized by comprising the following steps: 1) heating feed liquid to 40-90 ℃ under a stirring state by taking laterite nickel ore leaching liquid with nickel sulfate and magnesium sulfate as main components as a raw material; 2) adding magnesium oxide into the heated feed liquid to precipitate nickel until the pH value of the feed liquid is 7.5-9 to obtain a nickel precipitation liquid; 3) stirring and aging the nickel precipitation solution for 60-240min at the rotation speed of 100 plus 200 rpm, filtering and separating to obtain a nickel hydroxide product, wherein the filtrate is the solution after nickel precipitation; 4) returning the liquid after nickel precipitation to the step 1) for recycling. The characteristics of alkalinity and activity of active magnesium oxide are effectively utilized, a high-grade nickel hydroxide product is obtained, the nickel precipitation effect is good, the product purity is as high as 35-45%, especially, in the nickel precipitation process, only active magnesium oxide which is the same as magnesium ions except nickel in the laterite-nickel ore leaching solution is used for nickel precipitation, so that the feed liquid elements are simple, the subsequent impurity removal difficulty and cost are reduced, the resource utilization rate is high, the production water is recycled, and no discharge is generated.
Description
Technical Field
The invention relates to a method for separating and purifying metal ions from a hydrometallurgical solution, in particular to a method for precipitating nickel hydroxide from a laterite nickel ore wet leaching impurity-removed solution, and belongs to the technical field of hydrometallurgy.
Background
In the hydrometallurgy process, valuable elements and associated elements are inevitably leached or dissolved at the same time and enter a leachate system, so that the leachate is separated, extracted and purified again by means or methods such as chemical precipitation, solvent extraction, membrane separation, electrolytic deposition and the like to obtain the required valuable elements and associated elements, and the resource utilization rate is improved.
In the prior art, in the process of extracting nickel from laterite-nickel ore by a wet method, nickel is a main recovered element, other elements such as iron and magnesium have low value, and in the process of comprehensive recovery treatment, various factors such as cost increase, comprehensive treatment difficulty increase, resource waste and the like are caused due to unreasonable process or lack of process technology, and the like, so that nickel has to be abandoned. However, with the progress and development of production technology and the change of the current situations of resource exhaustion, high ecological environment requirement and the like, the comprehensive utilization of valuable resources becomes a trend of continuous development of enterprises, and is also a new way for the enterprises to increase economic benefits. The main element, namely nickel, in the laterite-nickel ore leaching solution is mostly recovered by an alkaline method and a sulfuration method, the obtained products are nickel hydroxide, nickel carbonate and nickel sulfide, nickel precipitating agents adopted in the recovery process mainly comprise nickel carbonate, sodium hydroxide, lime, sodium sulfide, hydrogen sulfide and the like, and other impurities can be brought into nickel precipitating liquid together when the nickel precipitating agents are used for precipitating the nickel, so that the subsequent comprehensive treatment is not facilitated, wherein calcium and sodium ions can greatly influence the recovery of magnesium, new calcium salt and sodium salt are generated at the same time, the subsequent treatment cost is increased, and the economic benefit is reduced. The hydrogen sulfide used in the sulfuration method not only has tight control, but also can generate great pollution to water, and the removal of sulfur ions increases the treatment cost. The methods bring new problems due to the limited reuse of production water, high cost of outward discharge treatment and the like, so that the production recycling of enterprises is difficult to realize.
Disclosure of Invention
The invention aims to recover the main element nickel, simultaneously introduce no new impurities, reduce the separation steps and cost, comprehensively recover associated valuable metals and completely recycle production water, and provides an impurity-free nickel precipitation method.
The invention is completed by the following technical scheme: a nickel deposition method without impurity brought in from a laterite-nickel ore leaching solution is characterized by comprising the following steps:
1) heating feed liquid to 40-90 ℃ under a stirring state by taking laterite nickel ore leaching liquid with nickel sulfate and magnesium sulfate as main components as a raw material;
2) adding magnesium oxide into the heated feed liquid obtained in the step 1) to precipitate nickel until the pH value of the feed liquid is 7.5-9, so as to obtain a nickel precipitation liquid;
3) stirring and aging the nickel precipitation solution obtained in the step 2) for 60-240min at the rotation speed of 100 plus 200 rpm, filtering and separating to obtain a nickel hydroxide product, wherein the filtrate is the solution after nickel precipitation;
4) returning the liquid after nickel deposition in the step 3) to the step 1) for recycling.
The laterite-nickel ore leaching solution in the step 1) is a feed solution for removing impurities from the laterite-nickel ore leaching solution, the pH value of the feed solution is 4.5-6, the nickel content is 2.5-8 g/L, the magnesium content is 25-60 g/L, the iron content is less than 0.001 g/L, and other impurity elements are less than 0.0001 g/L.
The magnesium oxide in the step 2) is active magnesium oxide with the activity of 80-120 (mgI 2/100 gMgO) expressed by an iodine absorption value, the MgO content is more than 88%, the specific surface area is 5-20m and n/g, the specific volume is 6-8.5ml/g, and the average grain diameter is less than 2 mm.
The nickel hydroxide obtained in the step 3) contains 35-45% of nickel.
The nickel content in the nickel-precipitated liquid obtained in the step 3) is less than 0.001 g/L, and the nickel precipitation rate reaches 99.98%.
The chemical reaction formula of the magnesium oxide nickel deposition is as follows:
the invention has the following advantages and effects: by adopting the technical scheme, the characteristics of alkalinity and activity of the active magnesium oxide are effectively utilized, the nickel ions are effectively precipitated to obtain a high-grade nickel hydroxide product, the nickel precipitation effect is good, the product purity is high, more importantly, no new element or ion is introduced in the nickel precipitation process, the active magnesium oxide which is the same as the magnesium ions except the nickel in the laterite-nickel ore leaching solution is only used for precipitating the nickel, the original element in the feed liquid is simple, the subsequent impurity removal difficulty and the impurity removal cost are reduced, and the comprehensive recovery of the elements is facilitated. The nickel content of the nickel hydroxide product is up to 35-45%, and the nickel hydroxide product is a high-quality nickel sulfate production raw material and is an ideal environment-friendly nickel precipitation method.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The laterite-nickel ore leaching solution of the embodiment comprises the main components of 2.52 g/L nickel, 25.3 g/L magnesium, less than 0.001 g/L iron and 4.5 pH value, and is prepared by the following steps:
1) heating the laterite-nickel ore leaching solution with the pH value of 4.5 to 40 ℃ under a stirring state;
2) adding MgO of more than 88% and activity expressed by iodine absorption value of 80 (mgI) into the heated feed liquid in the step 1)2100g of MgO), 5 m/g of specific surface area, 6ml/g of specific volume and magnesium oxide with the average grain diameter less than 2mm until the pH value is 7.5 to obtain nickel precipitation liquid;
3) stirring and aging the nickel precipitation solution obtained in the step 2) for 60min at the rotating speed of 100 r/min, filtering and separating to obtain a nickel hydroxide product with the nickel grade of 35.2%, wherein the filtrate is a nickel precipitation solution, the nickel content of the filtrate is 0.0005 g/L, and the nickel precipitation rate reaches 99.98%;
4) returning the liquid after nickel deposition in the step 3) to the step 1) for recycling.
Example 2
The laterite-nickel ore leaching solution of the embodiment comprises the main components of 7.96 g/L nickel, 59.7 g/L magnesium, less than 0.001 g/L iron and a pH value of 5.94, and is prepared by the following steps:
1) heating the laterite-nickel ore leaching solution with the pH value of 5.94 to 90 ℃ under a stirring state;
2) adding MgO of more than 88% and activity represented by an iodine absorption value of 120 (mgI) into the heated feed liquid in the step 1)2/100g MgO), 20 m/g specific surface area, 8.5ml/g specific volume and magnesium oxide with average grain diameter less than 2mm until the pH value is 9, and obtaining nickel precipitation liquid;
3) stirring and aging the nickel precipitation solution obtained in the step 2) for 240min at the rotating speed of 200 r/min, filtering and separating to obtain a nickel hydroxide product with the nickel grade of 44.92%, wherein the filtrate is the solution after nickel precipitation, the nickel content of the filtrate is 0.0002 g/L, and the nickel precipitation rate reaches 99.98%;
4) returning the liquid after nickel deposition in the step 3) to the step 1) for recycling.
Example 3
The main components of the leaching impurity-removed liquid of the laterite-nickel ore are 5.6 g/L nickel, 46.8 g/L magnesium, less than 0.001 g/L iron and 5.23 pH value, and the leaching impurity-removed liquid is prepared by the following steps:
1) heating the laterite-nickel ore leaching solution with the pH value of 5.23 to 70 ℃ under a stirring state;
2) adding MgO of more than 88% and activity represented by iodine absorption value of 100 (mgI) into the heated feed liquid in the step 1)2100g of MgO), 10 m/g of specific surface area, 7.5ml/g of specific volume and magnesium oxide with the average grain diameter less than 2mm until the pH value is 8.3 to obtain nickel precipitation liquid;
3) stirring and aging the nickel precipitation solution obtained in the step 2) for 120min at the rotating speed of 150 r/min, filtering and separating to obtain a nickel hydroxide product with the nickel grade of 43.88%, wherein the filtrate is the nickel precipitation solution, the nickel content of the filtrate is 0.0003 g/L, and the nickel precipitation rate reaches 99.98%;
4) returning the liquid after nickel deposition in the step 3) to the step 1) for recycling.
Claims (5)
1. A nickel deposition method without impurity brought in from a laterite-nickel ore leaching solution is characterized by comprising the following steps:
1) heating feed liquid to 40-90 ℃ under a stirring state by taking laterite nickel ore leaching liquid with nickel sulfate and magnesium sulfate as main components as a raw material;
2) adding magnesium oxide into the heated feed liquid obtained in the step 1) to precipitate nickel until the pH value of the feed liquid is 7.5-9, so as to obtain a nickel precipitation liquid;
3) stirring and aging the nickel precipitation solution obtained in the step 2) for 60-240min at the rotation speed of 100 plus 200 rpm, filtering and separating to obtain a nickel hydroxide product, wherein the filtrate is the solution after nickel precipitation;
4) returning the liquid after nickel deposition in the step 3) to the step 1) for recycling.
2. The nickel precipitating method according to claim 1, wherein the lateritic nickel ore leaching solution of the step 1) is a feed solution for removing impurities from the lateritic nickel ore leaching solution, the feed solution has a pH value of 4.5-6, nickel content of 2.5-8 g/L, magnesium content of 25-60 g/L, iron content of less than 0.001 g/L, and other impurity elements of less than 0.0001 g/L.
3. The nickel deposition method of claim 1, wherein the magnesium oxide in step 2) is activated magnesium oxide having an activity of 80-120 (mgI 2/100g MgO) as indicated by an iodine absorption value, an MgO content of > 88%, a specific surface area of 5-20 m/g, an apparent specific volume of 6-8.5ml/g, and an average particle size of < 2 mm.
4. The method according to claim 1, wherein the nickel hydroxide obtained in step 3) contains 35-45% nickel.
5. The nickel deposition method according to claim 1, wherein the nickel deposition solution of step 3) has a nickel content of less than 0.001 g/L and a nickel deposition rate of 99.98%.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113846217A (en) * | 2021-09-28 | 2021-12-28 | 贵州中伟资源循环产业发展有限公司 | Nickel hydroxide and preparation method thereof |
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US20020031463A1 (en) * | 1997-08-01 | 2002-03-14 | Centaur Nickel Pty Limited | Selective precipitation of nickel and cobalt |
CN102876892A (en) * | 2012-10-30 | 2013-01-16 | 杭州蓝普水处理设备有限公司 | Method for leaching nickel and cobalt form low-iron and high-magnesium and high-iron and low-magnesium laterite-nickel ore by using waste dilute sulphuric acid |
CN102874852A (en) * | 2012-09-28 | 2013-01-16 | 广西银亿科技矿冶有限公司 | High-activity magnesite powder and manufacturing method thereof and method for reclaiming nickel cobalt from laterite nickel ores |
CN103074493A (en) * | 2013-02-20 | 2013-05-01 | 广西银亿科技矿冶有限公司 | Application of brucite to recovery of nickel cobalt |
CN105296744A (en) * | 2015-10-26 | 2016-02-03 | 广西银亿再生资源有限公司 | Method for laterite-nickel ore resourceful treatment and comprehensive recycling |
-
2020
- 2020-04-13 CN CN202010286751.XA patent/CN111422928A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US20020031463A1 (en) * | 1997-08-01 | 2002-03-14 | Centaur Nickel Pty Limited | Selective precipitation of nickel and cobalt |
CN102874852A (en) * | 2012-09-28 | 2013-01-16 | 广西银亿科技矿冶有限公司 | High-activity magnesite powder and manufacturing method thereof and method for reclaiming nickel cobalt from laterite nickel ores |
CN102876892A (en) * | 2012-10-30 | 2013-01-16 | 杭州蓝普水处理设备有限公司 | Method for leaching nickel and cobalt form low-iron and high-magnesium and high-iron and low-magnesium laterite-nickel ore by using waste dilute sulphuric acid |
CN103074493A (en) * | 2013-02-20 | 2013-05-01 | 广西银亿科技矿冶有限公司 | Application of brucite to recovery of nickel cobalt |
CN105296744A (en) * | 2015-10-26 | 2016-02-03 | 广西银亿再生资源有限公司 | Method for laterite-nickel ore resourceful treatment and comprehensive recycling |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN113846217A (en) * | 2021-09-28 | 2021-12-28 | 贵州中伟资源循环产业发展有限公司 | Nickel hydroxide and preparation method thereof |
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Application publication date: 20200717 |