JP5801819B2 - リン酸の生成方法 - Google Patents
リン酸の生成方法 Download PDFInfo
- Publication number
- JP5801819B2 JP5801819B2 JP2012541500A JP2012541500A JP5801819B2 JP 5801819 B2 JP5801819 B2 JP 5801819B2 JP 2012541500 A JP2012541500 A JP 2012541500A JP 2012541500 A JP2012541500 A JP 2012541500A JP 5801819 B2 JP5801819 B2 JP 5801819B2
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- Prior art keywords
- slurry
- reactor
- phosphoric acid
- hemihydrate
- sulfuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims description 76
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 65
- 239000002002 slurry Substances 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 39
- 239000013078 crystal Substances 0.000 claims description 26
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 24
- 238000000354 decomposition reaction Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 claims description 7
- 238000005336 cracking Methods 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 239000008346 aqueous phase Substances 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002367 phosphate rock Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 2
- 229940095672 calcium sulfate Drugs 0.000 claims 1
- 229940057306 hemihydrate calcium sulfate Drugs 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 239000010440 gypsum Substances 0.000 description 23
- 229910052602 gypsum Inorganic materials 0.000 description 23
- 150000004683 dihydrates Chemical class 0.000 description 18
- 229910019142 PO4 Inorganic materials 0.000 description 16
- 235000021317 phosphate Nutrition 0.000 description 16
- 239000010452 phosphate Substances 0.000 description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 13
- 238000001914 filtration Methods 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000007796 conventional method Methods 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ARLZGEXVMUDUQZ-UHFFFAOYSA-N O.O.[Ca] Chemical compound O.O.[Ca] ARLZGEXVMUDUQZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- -1 for example Chemical compound 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/228—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen one form of calcium sulfate being formed and then converted to another form
- C01B25/231—Dihydrate-hemihydrate process
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/228—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen one form of calcium sulfate being formed and then converted to another form
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Description
70から90℃の間に含まれる第1の温度において、リン鉱石を硫酸によって水性媒体中で分解するステップであって、38から50重量%の間に含まれる遊離P2O5含量と、0.5重量%未満であり且つ0.05重量%を超える遊離SO3含量とを有する酸性水相中に、懸濁した硫酸カルシウム二水和物結晶の第1のスラリーを形成するステップ、
この第1のスラリーを転換するステップであって、90℃を超える温度まで加熱して、硫酸カルシウム二水和物結晶を可溶化し、可溶化した硫酸カルシウムを再結晶させて、リン酸による水相中に懸濁した、硫酸カルシウム半水和物結晶から形成された、第2のスラリーを生じるステップ、及び
2重量%未満であり且つ0.05重量%を超える遊離SO3含量を有する生成リン酸と、硫酸カルシウム半水和物を主体としたろ過ケーキとに、第2のスラリーを分離するステップを含む方法が提供される。
温度 70〜80℃
遊離P2O5の%:38〜50重量%
遊離SO3の%:0.05重量%〜<0.5重量%
滞留時間 2〜4時間
である。
温度:90〜105℃
P2O5の%:35〜45重量%
SO3の%:0.1重量%〜<1.0重量%
滞留時間:0.5〜1.5時間
を適用する。
パイロット試験を、29.5%のP2O5、45.3%のCaO、3.2%のF、3.8%のCO2を含有した中東産のリン酸塩堆積物に対して実施した。
P2O5含量:38.2重量%
SO3過剰量:0.45重量%
温度:76℃
固形分:33重量%
硫酸カルシウムとリン酸から、P2O5が50%、SO3が0.15%の重量力価で形成されたスラリーを、北アフリカ産リン酸塩(30%のP2O5、50.1%のCaO、3.6%のF)を分解することによって得る。
硫酸カルシウムとリン酸から、P2O5が41.6%、SO3が0.4%、Al2O3が0.24%、Fが0.99%の重量力価で形成されたスラリーを、北アフリカ産リン酸塩を分解することによって得る。
Claims (10)
- 70から90℃の間に含まれる第1の温度において、リン鉱石を硫酸によって水性媒体中で分解するステップであって、38から50重量%の間に含まれる遊離P2O5含量と、0.5重量%未満であり且つ0.05重量%を超える遊離SO3含量とを有する酸性水相中に、懸濁した硫酸カルシウム二水和物結晶の第1のスラリーを形成するステップ、
前記第1のスラリーを転換するステップであって、90℃を超える温度まで加熱して、硫酸カルシウム二水和物結晶を可溶化し、可溶化した硫酸カルシウムを再結晶させて、リン酸による水相中に懸濁した、半水和物硫酸カルシウム結晶から形成された第2のスラリーを生じるステップ、及び
2重量%未満であり且つ0.05重量%を超える遊離SO3含量を有する生成リン酸と、硫酸カルシウム半水和物を主体としたろ過ケーキとに、第2のスラリーを分離するステップ
を含む、リン酸を生成するための方法。 - 得られた生成リン酸が、35から45重量%までのP2O5含量を有することを特徴とする、請求項1に記載の方法。
- 第1のスラリーを転換するステップ中に、硫酸の第1のスラリーへの導入を含むことを特徴とする、請求項1及び2のいずれか一項に記載の方法。
- 第1のスラリーを加熱するステップが、硫酸の添加を全く含まないことを特徴とする、請求項1及び2のいずれか一項に記載の方法。
- 第1の反応器内での分解ステップと、転換ステップを実施して第2のスラリーを形成することになる第2の反応器に、第1の反応器の第1のスラリーを移送するステップとを含み、分離ステップが、ろ過器上で実施されることを特徴とする、請求項1から4までのいずれか一項に記載の方法。
- 加熱ステップが、第2の反応器の加熱、第2のスラリーへの蒸気の注入、又はこれらのプロセス両方の同時実施により行われることを特徴とする、請求項5に記載の方法。
- 第1の反応器内での滞留時間が、2から4時間までであり、第2の反応器内での滞留時間が、0.5から1.5時間までであることを特徴とする、請求項5及び6のいずれか一項に記載の方法。
- ろ過ケーキを洗浄液によって洗浄し、リン酸洗浄生成物を得るための少なくとも1つのステップをさらに含むことを特徴とする、請求項1から7までのいずれか一項に記載の方法。
- 少なくとも1つの前記洗浄ステップから生じたリン酸洗浄生成物を、分解ステップに再循環するステップをさらに含むことを特徴とする、請求項8に記載の方法。
- 連続的に実施されることを特徴とする、請求項1から9までのいずれか一項に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BEBE2009/0740 | 2009-12-02 | ||
BE2009/0740A BE1019055A3 (fr) | 2009-12-02 | 2009-12-02 | Procede de production d'acide phosphorique. |
PCT/EP2010/068709 WO2011067321A1 (fr) | 2009-12-02 | 2010-12-02 | Procede de production d'acide phosphorique |
Publications (3)
Publication Number | Publication Date |
---|---|
JP2013512837A JP2013512837A (ja) | 2013-04-18 |
JP2013512837A5 JP2013512837A5 (ja) | 2015-05-14 |
JP5801819B2 true JP5801819B2 (ja) | 2015-10-28 |
Family
ID=42115503
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2012541500A Active JP5801819B2 (ja) | 2009-12-02 | 2010-12-02 | リン酸の生成方法 |
Country Status (19)
Country | Link |
---|---|
US (1) | US9255006B2 (ja) |
EP (1) | EP2507168B1 (ja) |
JP (1) | JP5801819B2 (ja) |
KR (1) | KR101700338B1 (ja) |
AP (1) | AP2012006286A0 (ja) |
AU (1) | AU2010326637B2 (ja) |
BE (1) | BE1019055A3 (ja) |
BR (1) | BR112012012994B1 (ja) |
CA (1) | CA2780078C (ja) |
EA (1) | EA020618B1 (ja) |
EG (1) | EG26913A (ja) |
ES (1) | ES2441558T3 (ja) |
IL (1) | IL220002A (ja) |
MA (1) | MA33817B1 (ja) |
MX (1) | MX2012006380A (ja) |
PE (1) | PE20130474A1 (ja) |
PL (1) | PL2507168T3 (ja) |
TN (1) | TN2012000197A1 (ja) |
WO (1) | WO2011067321A1 (ja) |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101770814B1 (ko) * | 2011-06-01 | 2017-08-23 | 프라이온 테크놀로지스 | 디하이드레이트/헤미하이드레이트 유형의 인산 제조 방법 |
PL2771280T3 (pl) | 2011-10-24 | 2018-10-31 | Hydrometal Sa | Sposób obróbki skał fosfatowych |
AU2014225473A1 (en) * | 2013-03-08 | 2015-10-01 | The Mosaic Company | Production of phosphoric acid by a two-stage crystallization process |
DE102013018650B3 (de) | 2013-11-06 | 2014-09-18 | Remondis Aqua Gmbh & Co. Kg | Verfahren zur Behandlung von phosphathaltigen Aschen aus Abfallverbrennungsanlagen durch nasschemischen Aufschluss zur Gewinnung von Aluminium-, Kalzium-, Phosphor- und Stickstoffverbindungen |
BE1025894B1 (fr) | 2017-08-11 | 2020-02-21 | Prayon Tech | Procede d’attaque acide d’une source phosphatee |
CN107840317B (zh) * | 2017-10-30 | 2019-12-03 | 安徽六国化工股份有限公司 | 一种一步法二水-半水湿法磷酸生产工艺 |
IL313842A (en) | 2021-12-27 | 2024-08-01 | Prayon | A method for purifying at least one aqueous solution of phosphoric acid |
Family Cites Families (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA915883A (en) * | 1972-12-05 | Pavonet Engelhard | Method for manufacturing phosphoric acid and hemihydrate calcium sulphate by the wet process | |
CA195883A (en) * | 1920-01-06 | B. Williamson George | Defecation of sugar solutions | |
LU49007A1 (ja) | 1965-07-07 | 1967-01-09 | ||
US3523754A (en) * | 1966-04-02 | 1970-08-11 | Central Glass Co Ltd | Process for preparing phosphoric acil |
DE1592287A1 (de) * | 1966-08-19 | 1971-04-15 | Piesteritz Stickstoff | Verfahren zur Herstellung von Phosphorsaeure |
US3984525A (en) * | 1967-02-01 | 1976-10-05 | Albright & Wilson Limited | Manufacture of phosphoric acid |
US4196172A (en) * | 1976-07-07 | 1980-04-01 | Occidental Petroleum Corporation | Hemihydrate type phosphoric acid process |
JPS57129811A (en) * | 1981-01-28 | 1982-08-12 | Toyo Soda Mfg Co Ltd | Manufacture of wet process phosphoric acid |
LU84713A1 (fr) * | 1983-03-25 | 1984-11-14 | Prayon Soc | Procede et preparation d'acide phosphorique et de sulfate de calcium hemihydrate alpha |
DE3583209D1 (de) * | 1984-11-05 | 1991-07-18 | Prayon Dev Sa | Kontinuierliches verfahren zur herstellung von phosphorsaeure und von calciumsulfat. |
US4853201A (en) * | 1988-07-11 | 1989-08-01 | Occidental Chemical Corporation | Recovery of P2 O5 values from phosphoric acid hemihydrate crystals |
US5009873A (en) * | 1990-01-29 | 1991-04-23 | Nalco Chemical Company | Crystal modification in wet process phosphoric acid production |
CN1340457A (zh) * | 2000-09-01 | 2002-03-20 | 山东鲁北企业集团总公司 | 一种磷酸生产工艺 |
JP4036426B2 (ja) * | 2001-08-23 | 2008-01-23 | 下関三井化学株式会社 | ろ過性の優れた石膏の製造方法 |
BE1016065A3 (fr) | 2004-06-01 | 2006-02-07 | Prayon Technologies | Procede de production d'acide phosphorique. |
-
2009
- 2009-12-02 BE BE2009/0740A patent/BE1019055A3/fr not_active IP Right Cessation
-
2010
- 2010-12-02 ES ES10787103.0T patent/ES2441558T3/es active Active
- 2010-12-02 AP AP2012006286A patent/AP2012006286A0/xx unknown
- 2010-12-02 US US13/513,486 patent/US9255006B2/en active Active
- 2010-12-02 BR BR112012012994A patent/BR112012012994B1/pt active IP Right Grant
- 2010-12-02 PE PE2012000749A patent/PE20130474A1/es active IP Right Grant
- 2010-12-02 KR KR1020127015594A patent/KR101700338B1/ko active IP Right Grant
- 2010-12-02 PL PL10787103T patent/PL2507168T3/pl unknown
- 2010-12-02 JP JP2012541500A patent/JP5801819B2/ja active Active
- 2010-12-02 MX MX2012006380A patent/MX2012006380A/es active IP Right Grant
- 2010-12-02 EA EA201200834A patent/EA020618B1/ru not_active IP Right Cessation
- 2010-12-02 WO PCT/EP2010/068709 patent/WO2011067321A1/fr active Application Filing
- 2010-12-02 AU AU2010326637A patent/AU2010326637B2/en active Active
- 2010-12-02 CA CA2780078A patent/CA2780078C/fr active Active
- 2010-12-02 EP EP10787103.0A patent/EP2507168B1/fr active Active
-
2012
- 2012-04-27 TN TNP2012000197A patent/TN2012000197A1/fr unknown
- 2012-05-24 IL IL220002A patent/IL220002A/en active IP Right Grant
- 2012-05-31 EG EG2012050977A patent/EG26913A/xx active
- 2012-06-13 MA MA34960A patent/MA33817B1/fr unknown
Also Published As
Publication number | Publication date |
---|---|
MA33817B1 (fr) | 2012-12-03 |
ES2441558T3 (es) | 2014-02-05 |
CA2780078C (fr) | 2017-01-17 |
AP2012006286A0 (en) | 2012-06-30 |
EP2507168A1 (fr) | 2012-10-10 |
WO2011067321A1 (fr) | 2011-06-09 |
AU2010326637A1 (en) | 2012-06-21 |
IL220002A (en) | 2016-02-29 |
EG26913A (en) | 2014-12-17 |
TN2012000197A1 (fr) | 2013-12-12 |
EA201200834A1 (ru) | 2012-11-30 |
JP2013512837A (ja) | 2013-04-18 |
MX2012006380A (es) | 2012-06-19 |
BE1019055A3 (fr) | 2012-02-07 |
KR101700338B1 (ko) | 2017-01-26 |
PE20130474A1 (es) | 2013-05-01 |
EA020618B1 (ru) | 2014-12-30 |
US20130004403A1 (en) | 2013-01-03 |
BR112012012994A2 (pt) | 2017-03-01 |
US9255006B2 (en) | 2016-02-09 |
KR20120112459A (ko) | 2012-10-11 |
EP2507168B1 (fr) | 2013-11-06 |
PL2507168T3 (pl) | 2014-03-31 |
AU2010326637B2 (en) | 2014-12-04 |
BR112012012994B1 (pt) | 2019-10-22 |
IL220002A0 (en) | 2012-07-31 |
CA2780078A1 (fr) | 2011-06-09 |
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