KR100912095B1 - 중공사막 필터를 이용한 이온 교환형 리튬 흡착제 및 그의제조 방법 - Google Patents
중공사막 필터를 이용한 이온 교환형 리튬 흡착제 및 그의제조 방법 Download PDFInfo
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- KR100912095B1 KR100912095B1 KR1020070117251A KR20070117251A KR100912095B1 KR 100912095 B1 KR100912095 B1 KR 100912095B1 KR 1020070117251 A KR1020070117251 A KR 1020070117251A KR 20070117251 A KR20070117251 A KR 20070117251A KR 100912095 B1 KR100912095 B1 KR 100912095B1
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- Prior art keywords
- membrane filter
- hollow fiber
- fiber membrane
- lithium
- ion exchange
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 87
- 239000003463 adsorbent Substances 0.000 title claims abstract description 77
- 239000012528 membrane Substances 0.000 title claims abstract description 74
- 238000005342 ion exchange Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims description 31
- 239000012510 hollow fiber Substances 0.000 claims abstract description 72
- 239000000843 powder Substances 0.000 claims abstract description 57
- 239000002243 precursor Substances 0.000 claims abstract description 48
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 34
- 229910002102 lithium manganese oxide Inorganic materials 0.000 claims abstract description 27
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 21
- 239000011029 spinel Substances 0.000 claims abstract description 21
- 238000010306 acid treatment Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 238000011049 filling Methods 0.000 claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 6
- 239000011572 manganese Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 150000002500 ions Chemical group 0.000 claims description 6
- 229910009343 Li1.33 Mn1.67 O4 Inorganic materials 0.000 claims description 3
- 229910018663 Mn O Inorganic materials 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 30
- 238000011084 recovery Methods 0.000 abstract description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 21
- 229910001416 lithium ion Inorganic materials 0.000 description 21
- 239000000243 solution Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 5
- 150000002642 lithium compounds Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- -1 manganese oxide compound Chemical class 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 150000002697 manganese compounds Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000013535 sea water Substances 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910018584 Mn 2-x O 4 Inorganic materials 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- LMDGMYBVQCPUTJ-UHFFFAOYSA-L lithium 2,3-dihydroxybutanedioate manganese(2+) Chemical compound C(=O)([O-])C(O)C(O)C(=O)[O-].[Mn+2].[Li+] LMDGMYBVQCPUTJ-UHFFFAOYSA-L 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical class [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000131 polyvinylidene Polymers 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/14—Dynamic membranes
- B01D69/141—Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes
- B01D69/147—Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes containing embedded adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/12—Adsorbents being present on the surface of the membranes or in the pores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/42—Ion-exchange membranes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
Claims (14)
- 스피넬 구조를 갖는 리튬 망간 산화물인 전구체 분말을 합성하는 단계;상기 전구체 분말을 중공사막 필터 내부에 충진시키는 단계; 및상기 전구체 분말이 충진된 중공사막 필터를 산처리하는 단계;를 포함하는 중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 스피넬 구조를 갖는 하기 화학식 1[화학식 1]LinMn2 - xO4(식중, 1≤n≤1.33, 0≤x≤0.33, n≤1+x 임)의 전구체 분말을 합성하는 단계;상기 전구체 분말을 중공사막 필터 내부에 충진시키는 단계; 및상기 전구체 분말이 충진된 중공사막 필터를 산처리하는 단계;를 포함하는 중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 제2항에 있어서,상기 화학식 1의 전구체 분말은 스피넬 구조를 갖는 하기 화학식 2[화학식 2]Li1 .33Mn1 .67O4의 리튬 망간 산화물인중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 제1항에 있어서,상기 전구체 분말은 스피넬 구조를 갖는 하기 화학식 3[화학식 3]Li1 .6Mn1 .6O4의 리튬 망간 산화물인중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 제1항 또는 제2항에 있어서,상기 산처리는 0.3~1.0M의 산성 용액에서 행하는 것인중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 제5항에 있어서,상기 산처리는 0.3~1.0M의 산성 용액에서 1회당 22~24시간씩 3~5회 행하는 것인중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 제6항에 있어서,`상기 산처리는 0.5M의 염산 용액에서 1회당 24시간씩 4회 행하는 것인중공사막 필터를 이용한 이온 교환형 리튬 흡착제의 제조방법.
- 중공사막 필터 내부에 스피넬 구조를 갖는 이온 교환형 망간 산화물이 충진되어 이루어진, 중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
- 중공사막 필터 내부에 스피넬 구조를 갖는 하기 화학식 1a[화학식 1a]HnMn2 - xO4(식 중, 1≤n≤1.33, 0≤x≤0.33, n≤1+x 임)의 이온 교환형 망간 산화물이 충진되어 이루어진중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
- 제9항에 있어서,상기 화학식 1a의 망간 산화물은 스피넬 구조를 갖는 하기 화학식 2a[화학식 2a]H1 .33Mn1 .67O4의 이온 교환형 망간 산화물인중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
- 제8항에 있어서,상기 망간 산화물은 스피넬 구조를 갖는 하기 화학식 3a[화학식 3a]H1 .6Mn1 .6O4의 이온 교환형 망간 산화물인중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
- 제9항에 있어서,상기 화학식 1a의 이온 교환형 망간 산화물은 하기 화학식 1[화학식 1]LinMn2 - xO4(식중, 1≤n≤1.33, 0≤x≤0.33, n≤1+x 임)의 리튬 망간 산화물 전구체를 산처리하여 얻어지는중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
- 제10항에 있어서,상기 화학식 2a의 이온 교환형 망간 산화물은 하기 화학식 2[화학식 2]Li1 .33Mn1 .67O4의 리튬 망간 산화물 전구체를 산처리하여 얻어지는중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
- 제11항에 있어서,상기 화학식 3a의 이온 교환형 망간 산화물은 하기 화학식 3[화학식 3]Li1 .6Mn1 .6O4의 리튬 망간 산화물 전구체를 산처리하여 얻어지는중공사막 필터를 이용한 이온 교환형 리튬 흡착제.
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KR102265697B1 (ko) * | 2017-12-26 | 2021-06-15 | 주식회사 포스코 | 리튬 흡착제, 및 이를 이용한 리튬 흡착 장치 |
KR102353729B1 (ko) * | 2019-12-12 | 2022-01-19 | 주식회사 포스코 | 리튬 흡착 성형체, 및 이를 이용한 리튬 흡착 모듈 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH038443A (ja) * | 1989-06-02 | 1991-01-16 | Agency Of Ind Science & Technol | リチウム吸着剤及びそれを用いたリチウム回収方法 |
US6207129B1 (en) | 1998-05-21 | 2001-03-27 | Carus Corporation | Lithiated manganese oxide |
JP2005149885A (ja) | 2003-11-14 | 2005-06-09 | Tatung Co | リチウムイオン二次電池の正極材料の製造方法 |
KR100536957B1 (ko) | 2003-11-10 | 2005-12-14 | 한국지질자원연구원 | 허니컴 형태의 이온 교환형 리튬-망간산화물 흡착제 및그의 제조 방법 |
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2007
- 2007-11-16 KR KR1020070117251A patent/KR100912095B1/ko active IP Right Grant
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JPH038443A (ja) * | 1989-06-02 | 1991-01-16 | Agency Of Ind Science & Technol | リチウム吸着剤及びそれを用いたリチウム回収方法 |
US6207129B1 (en) | 1998-05-21 | 2001-03-27 | Carus Corporation | Lithiated manganese oxide |
KR100536957B1 (ko) | 2003-11-10 | 2005-12-14 | 한국지질자원연구원 | 허니컴 형태의 이온 교환형 리튬-망간산화물 흡착제 및그의 제조 방법 |
JP2005149885A (ja) | 2003-11-14 | 2005-06-09 | Tatung Co | リチウムイオン二次電池の正極材料の製造方法 |
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