EP1165218B1 - Vorrichtung zum mischen und reagieren mehrphasiger gasförmiger und flüssiger gemische und verwendung dieser vorrichtung - Google Patents
Vorrichtung zum mischen und reagieren mehrphasiger gasförmiger und flüssiger gemische und verwendung dieser vorrichtung Download PDFInfo
- Publication number
- EP1165218B1 EP1165218B1 EP00902646A EP00902646A EP1165218B1 EP 1165218 B1 EP1165218 B1 EP 1165218B1 EP 00902646 A EP00902646 A EP 00902646A EP 00902646 A EP00902646 A EP 00902646A EP 1165218 B1 EP1165218 B1 EP 1165218B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- mixing
- space
- liquid
- mixer
- chamber
- 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.)
- Expired - Lifetime
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
- B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
- B01F25/31425—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction with a plurality of perforations in the axial and circumferential direction covering the whole surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
- B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S261/00—Gas and liquid contact apparatus
- Y10S261/75—Flowing liquid aspirates gas
Definitions
- the invention relates to a device for mixing and reacting multiphase gaseous and liquid mixtures, with homogeneously immiscible liquid homogeneous Solutions with homogeneous solutions in which several solid or liquid substances or several gases are dissolved in intensive contact with each other, and a use of this device and manufactured using the device Diphenyl carbonate and polycarbonate.
- stirred kettles or mixers can not be arbitrary enlarge, since often a chemical reaction takes place during mixing, so that during the mixing process in the reactor mixing and / or reaction enthalpy is released or is needed.
- the interior of the reactor is an additional heat exchanger necessary because the ratio of heat exchange area to reactor volume with increasing stirred tank radius is getting smaller.
- the stirred tank volume reduced by expanding the number of stirred tanks or the heat transfer by attaching additional heat exchangers in the secondary flow be intensified.
- the invention is therefore based on the object, the known and described in more detail above Device for mixing and reacting multiphase gaseous and to improve liquid mixtures so that with little design effort small mixer is provided, without shaft bearings and shaft bushings needs to avoid the disadvantages described above. Of further the quality of the mixture should be improved.
- the teaching of the invention provides that the transition between the cylindrical Space and the tapered cylindrical chamber has sharp edges.
- the first stream of liquid enters the nozzle mixer through the cylindrical chamber towards the conical space, the second stream perpendicular to the middle cylindrical chamber of the nozzle mixer.
- the vertical entry of the second Solution in the nozzle mixer takes place via several openings that follow one further teaching of the invention in the inner wall of the chamber evenly over the Circumference are arranged on a line.
- the openings preferably run perpendicular or at any flat angle to the longitudinal axis of the chamber. This significantly increases the mixing intensity and the reaction rate.
- Part of the homogeneous solutions from solid, liquid and / or gaseous Fabrics can be placed in one or more jacket mixers installed in front of the nozzle mixer getting produced.
- Each jacket mixer has a cylindrical one Mixing room through which the homogeneous liquid is passed and it is a large number of inlet pipes arranged symmetrically around the mixing room for introducing the second liquid or gas to be dissolved into the jacket mixer intended.
- means for pulse-like entry of the Liquid or gas in the jacket mixer can be provided to the degree of mixing continue to improve.
- Another teaching of the invention is the use of the aforementioned device for mixing aqueous alkaline phenolate, bisphenolate solutions or other polyvalent phenolate solutions with dissolved in the solvent solid, liquid and / or gaseous substances.
- Another teaching of the invention relates to diphenyl carbonate and polycarbonate, each manufactured according to the phase interface process from one by mixing heterogeneous mixture produced in the device according to the invention from a aqueous alkaline phenolate or bisphenolate solution with solution in dichloromethane gaseous or liquid phosgene, the mixture being a very small Has residual phenylpiperidyl urethane content of ⁇ 20 ppm.
- a cascade of four stirred tanks with a total volume of 23 m 3 is flowed through by an aqueous reaction mixture at 30 ° C with a throughput of 4,500 kg / h, phosgene and dichloromethane being fed continuously into the first reactor.
- the aqueous phenolate solution is also continuously produced in a mixing vessel connected upstream of the first stirred tank in the cascade.
- reaction mixture is after the fourth stirred tank in a cascade Separation container separated into two phases, the organic phase cleaned, then the solvent and finally the diphenyl carbonate distilled.
- reaction mixture is now through the invention with the same throughput Device has been promoted, the solution in the jacket mixer was continuously produced by phosgene in dichloromethane.
- the watery Phenolate solution was continuously produced in a mixing kettle.
- reaction to the diphenyl carbonate was carried out in a nozzle mixer according to the invention from, the processing and recovery of the diphenyl carbonate exactly as with The process was carried out using the cascade of stirred tanks.
- the proportion of Phenylpiperidyl urethane can be safely reduced to values below 20 ppm, thereby better quality of the diphenyl carbonate could be achieved.
- nozzle mixer In Fig. 1 the nozzle mixer is shown, the cylindrical central space for Mixing two solutions serves.
- the four-part nozzle mixer D preferred in the exemplary embodiment shown contains a cylindrical space 1 into which a first solution F 1 enters.
- a second solution F 2 flows through the cylindrical space 2 into a central cylindrical chamber 3.
- a conical space 4 serves as an outlet.
- the central chamber 3 has a smaller diameter than the cylindrical space 1 and the transition between room 1 and chamber 3 is provided with sharp edges. With the help of the conically widening space 4 of the nozzle mixer D, it is possible to keep the pressure loss in the system low.
- the liquid for example the solution of phosgene in dichloromethane F 1
- the second solution for example the phenolate solution F 2
- the second solution is introduced into the cylindrical chamber 3 via openings 5 and mixed with the solution flowing perpendicularly therefrom from the room 1 and subjected to the reaction.
- the openings 5 are in a line on the cylindrical casing of the central chamber.
- the cylindrical mixing chamber 2 shows a cylindrical jacket mixer M to be connected upstream of the nozzle mixer D.
- the cylindrical mixing chamber has an outer annular space and inlet pipes are designed as bores in the reactor wall.
- the bores in the reactor wall preferably run at a flat angle to the flow direction of the reactor. An angle of 45 ° has proven to be particularly advantageous.
- the jacket mixer has a cylindrical mixing space 6, the wall of which is provided with a plurality of bores 7, of which only the ring-shaped bores 7 near the entry E 1 are provided with reference numerals for the sake of clarity.
- the holes in the mixer wall are arranged in a ring, whereby expediently the holes evenly over the circumference of each ring are distributed.
- a particularly good mixture results when eight holes are arranged on each ring and the holes each adjacent rings in the direction of flow at an angle of 45 ° to each other are staggered.
- the length of the jacket mixer M evenly distributed rows of holes, rings 7A, 7B and 7C, arranged, of which for the sake of clarity only the left three rings closer are designated.
- Each ring 7A, 7B, 7C preferably has eight bores 7 and they are the openings of two adjacent rings 7A, 7B and 7B, 7C, respectively arranged at 45 ° to each other. In this way, an optimal Mixing in the interior of the mixing chamber 6 of the jacket mixer M is achieved.
- a first homogeneous liquid such as dichloromethane
- a first homogeneous liquid is fed into the reactor space 6 of the jacket mixer M by the entry E 1 .
- the second component to be mixed such as gaseous or liquid phosgene
- the second component to be mixed is passed into an annular space 8 surrounding the mixing space 6 and introduced into the liquid, preferably in pulsed fashion, through the bores 7.
- the bores 7 are arranged at an angle of 45 ° to the direction of flow of the liquid. In this way, an optimal mixing of liquid with gas or another liquid can be achieved.
- FIG. 3 shows a preferred arrangement of the mixers of the device according to the invention, the jacket mixer M being followed by a first heat exchanger WT 1 and the nozzle mixer D being followed by a second heat exchanger WT 2 . In this way, the maintenance of the required mixing and reaction temperature is reliably ensured.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Polyesters Or Polycarbonates (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Accessories For Mixers (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
Description
Phenylpiperidylurethan | 13 bis 30 ppm |
Niedrigsieder | 15 bis 25 ppm |
Hochsieder | 0 bis 90 ppm |
Phenylpiperidylurethan | 11 bis 16 ppm |
Niedrigsieder | 10 bis 25 ppm |
Hochsieder | 0 bis 90 ppm |
- Fig. 1
- einen erfindungsgemäßen Düsenmischer, geschnitten,
- Fig. 2
- einen Mantelmischer, teilgeschnitten, und
- Fig. 3
- eine bevorzugte Anordnung der Mischer aus Fig. 1 und 2 in schematischer Darstellung.
Claims (21)
- Vorrichtung zum Mischen und Reagieren mehrphasiger gasförmiger und flüssiger Gemische, wobei homogen nicht mischbare flüssige homogene Lösungen mit homogenen Lösungen, in denen mehrere feste oder flüssige Stoffe bzw. mehrere Gase gelöst sind in intensiven Kontakt miteinander gebracht werden, gekennzeichnet durch einen Düsenmischer (D) als Mischer und Reaktor mit einem zylindrischen Raum (1) für den Eintritt der ersten Lösung, wenigstens einer gegenüber dem Raum (1) verjüngten zylindrischen Kammer (3), in der das Mischen und Reagieren von mindestens zwei Lösungen erfolgt, wobei der Übergang zwischen dem zylindrischen Raum (1) und der verjüngten zylindrischen Kammer (3) scharfe Kanten aufweist, einem zum Raum (1) senkrecht angeordneten zylindrischen Raum (2) für den Zulauf der zweiten Lösung, einem Raum (4) für den Austritt der gemischten und reagierten Lösungen aus dem Düsenmischer (D).
- Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass sich der Querschnitt des Raums (4) in Strömungsrichtung konisch erweitert.
- Vorrichtung nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, dass für den Eintritt der zweiten Lösung in die Kammer (3) eine Mehrzahl von im wesentlichen senkrecht zur Strömungsrichtung der ersten Lösung angeordnete Öffnungen (5) in der Wandung der Kammer (3) vorgesehen ist.
- Vorrichtung nach Anspruch 3, dadurch gekennzeichnet, dass die Öffnungen (5) in der Innenwand der Kammer (3) gleichmäßig über den Umfang verteilt auf einer Linie angeordnet sind.
- Vorrichtung nach Anspruch 4, dadurch gekennzeichnet, dass die Öffnungen (5) senkrecht zur Längsachse der Kammer (3) verlaufen.
- Vorrichtung nach Anspruch 4, dadurch gekennzeichnet, dass die Öffnungen (5) unter einem beliebigen Winkel zur Längsachse der Kammer (3) verlaufen.
- Vorrichtung nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, dass dem Düsenmischer (D) wenigstens ein Mantelmischer (M) vorgeschaltet ist, in dem gasförmige oder flüssige Stoffe mit flüssigen Stoffen gemischt werden können.
- Vorrichtung nach Anspruch 7, dadurch gekennzeichnet, dass der Mantelmischer (M) einen zylinderförmigen Mischraum (6) aufweist, durch den die homogene Flüssigkeit geleitet wird und dass eine Vielzahl von symmetrisch um den Mischraum angeordneten Einlaufrohren zum Eintragen der zu lösenden zweiten Flüssigkeit oder des Gases in den Mantelmischer (M) vorgesehen ist.
- Vorrichtung nach Anspruch 8, dadurch gekennzeichnet, dass die Vorrichtung Mittel zum pulsartigen Eintragen der zu mischenden Komponenten aufweist.
- Vorrichtung nach einem der Ansprüche 7 bis 9, dadurch gekennzeichnet, dass der zylindrische Mischraum (6) einen äußeren Ringraum (8) aufweist und dass die Einlaufrohre als Bohrungen (7) in der Reaktorwandung ausgeführt sind.
- Vorrichtung nach Anspruch 10, dadurch gekennzeichnet, dass die Bohrungen (7) in der Wandung des Mischraums (6) ringförmig angeordnet sind.
- Vorrichtung nach Anspruch 11, dadurch gekennzeichnet, dass die Bohrungen (7) gleichmäßig über den Umfang eines jeden Rings (7A, 7B, 7C) verteilt angeordnet sind.
- Vorrichtung nach Anspruch 12, dadurch gekennzeichnet, dass die Bohrungen (7) jeweils benachbarter Ringe (7A, 7B bzw. 7B, 7C) in Strömungsrichtung gegeneinander versetzt angeordnet sind.
- Vorrichtung nach Anspruch 13, dadurch gekennzeichnet, dass jeder Ring (7A, 7B, 7C) acht Bohrungen (7) aufweist und dass die Bohrungen (7) jeweils benachbarter Ringe (7A, 7B bzw. 7B, 7C) um 45° gegeneinander versetzt angeordnet sind.
- Vorrichtung nach einem der Ansprüche 8 bis 14, dadurch gekennzeichnet, dass die Bohrungen (7) unter einem flachen Winkel zur Strömungsrichtung verlaufen.
- Vorrichtung nach Anspruch 15, dadurch gekennzeichnet, dass der Winkel zwischen 30 und 60° beträgt.
- Vorrichtung nach Anspruch 16, dadurch gekennzeichnet, dass der Winkel 45° beträgt.
- Vorrichtung nach einem der Ansprüche 1 bis 17, dadurch gekennzeichnet, dass dem Düsenmischer (D) und ggf. dem Mantelmischer (M) Wärmetauscher (WT) vorund/oder nachgeschaltet sind.
- Verwendung der Vorrichtung nach einem der Ansprüche 1 bis 18 zum Mischen von wässrigen alkalischen Phenolat-, Bisphenolat-Lösungen bzw. anderen mehrwertigen Phenolat-Lösungen mit im Lösungsmittel gelösten festen, flüssigen und/oder gasförmigen Stoffen.
- Diphenylcarbonat, herstellbar nach dem Phasengrenzflächenverfahren aus einem durch Mischen in einer Vorrichtung nach einem der Ansprüche 1 bis 18 hergestellten heterogenen Gemisch aus einer wässrigen Phenolatlösung mit in Dichlormethan gelöstem gasförmigen oder flüssigen Phosgen, gekennzeichnet durch einen sehr kleinen Restgehalt an Phenylpiperidylurethan von kleiner 20 ppm.
- Polycarbonat, herstellbar nach dem Phasengrenzflächenverfahren aus einem durch Mischen in einer Vorrichtung nach einem der Ansprüche 1 bis 18 hergestellten heterogenen Gemisch aus einer wässrigen alkalischen Bisphenolatlösung mit in Dichlormethan gelöstem gasförmigen oder flüssigen Phosgen, gekennzeichnet durch einen sehr kleinen Restgehalt an Phenylpiperidylurethan von kleiner 20 ppm.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19905572A DE19905572A1 (de) | 1999-02-11 | 1999-02-11 | Vorrichtung zum Mischen und Reagieren mehrphasiger gasförmiger und flüssiger Gemische und Verwendung dieser Vorrichtung |
DE19905572 | 1999-02-11 | ||
PCT/EP2000/000788 WO2000047314A1 (de) | 1999-02-11 | 2000-02-07 | Vorrichtung zum mischen und reagieren mehrphasiger gasförmiger und flüssiger gemische und verwendung dieser vorrichtung |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1165218A1 EP1165218A1 (de) | 2002-01-02 |
EP1165218B1 true EP1165218B1 (de) | 2003-05-21 |
Family
ID=7897081
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00902646A Expired - Lifetime EP1165218B1 (de) | 1999-02-11 | 2000-02-07 | Vorrichtung zum mischen und reagieren mehrphasiger gasförmiger und flüssiger gemische und verwendung dieser vorrichtung |
Country Status (10)
Country | Link |
---|---|
US (1) | US6726354B1 (de) |
EP (1) | EP1165218B1 (de) |
JP (1) | JP4818512B2 (de) |
CN (1) | CN1222351C (de) |
AT (1) | ATE240776T1 (de) |
AU (1) | AU2440800A (de) |
DE (2) | DE19905572A1 (de) |
ES (1) | ES2199766T3 (de) |
HK (1) | HK1044729B (de) |
WO (1) | WO2000047314A1 (de) |
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US20060087910A1 (en) * | 2003-02-15 | 2006-04-27 | Darrell Knepp | Water injection method and apparatus for concrete mixer |
US6921047B2 (en) * | 2003-09-22 | 2005-07-26 | Hamilton Sundstrand | Aircraft air conditioning system mixer |
US6971607B2 (en) * | 2003-09-22 | 2005-12-06 | Hamilton Sundstrand | Aircraft air conditioning system mixer with corrugations |
JP4936433B2 (ja) * | 2006-06-29 | 2012-05-23 | 株式会社Kri | アクリル粒子ならびにその製造方法およびマイクロリアクター |
SE530767C2 (sv) * | 2006-10-03 | 2008-09-09 | Alfa Laval Corp Ab | Värmeväxlarreaktor med blandningszoner och användning av värmeväxlarreaktorn |
EP2136908B1 (de) | 2007-03-15 | 2011-12-07 | Dow Global Technologies LLC | Mischer für einen durchlaufreaktor |
US7779864B2 (en) * | 2007-08-27 | 2010-08-24 | Mazzei Angelo L | Infusion/mass transfer of treatment substances into substantial liquid flows |
EP2078898A1 (de) * | 2008-01-11 | 2009-07-15 | Siemens Aktiengesellschaft | Brenner und Verfahren zur Verringerung von selbstinduzierten Flammenschwingungen |
US20090314702A1 (en) * | 2008-06-19 | 2009-12-24 | Mazzei Angelo L | Rapid transfer and mixing of treatment fluid into a large confined flow of water |
US20100101673A1 (en) * | 2008-10-24 | 2010-04-29 | Walter Cornwall | Aerator fitting having curved baffle |
WO2012050858A1 (en) | 2010-09-28 | 2012-04-19 | Dow Global Technologies Llc | Reactive flow static mixer with cross-flow obstructions |
DE102012214519A1 (de) * | 2012-08-15 | 2014-02-20 | Putzmeister Engineering Gmbh | Vorrichtung zum Ausbringen von Dickstoffen |
JP2014117635A (ja) * | 2012-12-13 | 2014-06-30 | Asahi Organic Chemicals Industry Co Ltd | 流体混合器および流体混合器を用いた装置 |
CN103449393B (zh) * | 2013-08-21 | 2014-12-17 | 瓮福(集团)有限责任公司 | 一种饲料级磷酸氢钙生产装置 |
US10058828B2 (en) | 2015-06-01 | 2018-08-28 | Cameron International Corporation | Apparatus for mixing of fluids flowing through a conduit |
US10023317B2 (en) * | 2015-06-23 | 2018-07-17 | The Boeing Company | Flight deck takeoff duct and trim air mix muff |
US9931602B1 (en) | 2017-06-23 | 2018-04-03 | Mazzei Injector Company, Llc | Apparatus and method of increasing the mass transfer of a treatment substance into a liquid |
CN109908712B (zh) * | 2019-04-24 | 2024-04-02 | 攀钢集团钛业有限责任公司 | 用于四氯化钛吸收的气液混合器 |
CN110423149A (zh) * | 2019-07-31 | 2019-11-08 | 海南省海洋与渔业科学院 | 海草营养盐配方及其反应装置 |
CN115463566B (zh) * | 2022-09-29 | 2023-09-26 | 上海蕙黔新材料科技有限公司 | 一种用于气相法羰基合成碳酸二甲酯的氧气混合器 |
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-
1999
- 1999-02-11 DE DE19905572A patent/DE19905572A1/de not_active Withdrawn
-
2000
- 2000-02-07 DE DE50002263T patent/DE50002263D1/de not_active Expired - Lifetime
- 2000-02-07 CN CNB008037094A patent/CN1222351C/zh not_active Expired - Fee Related
- 2000-02-07 WO PCT/EP2000/000788 patent/WO2000047314A1/de active IP Right Grant
- 2000-02-07 JP JP2000598261A patent/JP4818512B2/ja not_active Expired - Fee Related
- 2000-02-07 ES ES00902646T patent/ES2199766T3/es not_active Expired - Lifetime
- 2000-02-07 EP EP00902646A patent/EP1165218B1/de not_active Expired - Lifetime
- 2000-02-07 AU AU24408/00A patent/AU2440800A/en not_active Abandoned
- 2000-02-07 AT AT00902646T patent/ATE240776T1/de not_active IP Right Cessation
- 2000-02-07 US US09/913,061 patent/US6726354B1/en not_active Expired - Fee Related
-
2002
- 2002-08-27 HK HK02106327.9A patent/HK1044729B/zh not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
HK1044729A1 (en) | 2002-11-01 |
US6726354B1 (en) | 2004-04-27 |
JP4818512B2 (ja) | 2011-11-16 |
AU2440800A (en) | 2000-08-29 |
CN1222351C (zh) | 2005-10-12 |
DE19905572A1 (de) | 2000-08-31 |
ES2199766T3 (es) | 2004-03-01 |
CN1339982A (zh) | 2002-03-13 |
EP1165218A1 (de) | 2002-01-02 |
DE50002263D1 (de) | 2003-06-26 |
HK1044729B (zh) | 2006-07-14 |
JP2002536163A (ja) | 2002-10-29 |
ATE240776T1 (de) | 2003-06-15 |
WO2000047314A1 (de) | 2000-08-17 |
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