CN114225884A - Continuous nitration reaction device - Google Patents

Continuous nitration reaction device Download PDF

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Publication number
CN114225884A
CN114225884A CN202111681572.7A CN202111681572A CN114225884A CN 114225884 A CN114225884 A CN 114225884A CN 202111681572 A CN202111681572 A CN 202111681572A CN 114225884 A CN114225884 A CN 114225884A
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CN
China
Prior art keywords
temperature
heat exchanger
annular reactor
low
reactor
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Pending
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CN202111681572.7A
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Chinese (zh)
Inventor
张立富
张晓红
付彬
廖梦琴
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JIANGSU JIHUA CHEMICAL CO Ltd
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JIANGSU JIHUA CHEMICAL CO Ltd
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Priority to CN202111681572.7A priority Critical patent/CN114225884A/en
Publication of CN114225884A publication Critical patent/CN114225884A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2455Stationary reactors without moving elements inside provoking a loop type movement of the reactants
    • B01J19/2465Stationary reactors without moving elements inside provoking a loop type movement of the reactants externally, i.e. the mixture leaving the vessel and subsequently re-entering it
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06Preparation of nitro compounds
    • C07C201/08Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002Chemical plants
    • B01J2219/00027Process aspects
    • B01J2219/0004Processes in series
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00081Tubes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a continuous nitration reaction device, which comprises an acid inlet mechanism, a feeding mechanism, a low-temperature annular reactor and a high-temperature annular reactor, wherein the acid inlet mechanism and the feeding mechanism are both connected with a feeding hole of the low-temperature annular reactor, and an overflow port of the low-temperature annular reactor is connected with the feeding hole of the high-temperature annular reactor. The continuous nitration reaction device can realize continuous nitration reaction, reduce the volume of equipment, reduce the storage of the material for nitration preparation, improve the heat transfer efficiency and the production efficiency, and reduce the risk of over-temperature and over-pressure of the nitration reaction.

Description

Continuous nitration reaction device
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a continuous nitration reaction device.
Background
The nitration reaction belongs to a high-risk process, and the reaction risk is higher. At present, most nitration reactions are batch kettle type or continuous kettle type nitration processes, and the production equipment is complicated, the equipment volume is large, the storage amount of materials for nitration preparation is large, the heat transfer capability is poor, the production efficiency is low, and the risk of over-temperature and over-pressure is high.
Disclosure of Invention
Aiming at the defects, the invention provides the continuous nitration reaction device, which can realize continuous nitration reaction, reduce the volume of equipment, reduce the stock of the material to be nitrated, improve the heat transfer efficiency and the production efficiency and reduce the risk of over-temperature and over-pressure of the nitration reaction.
In order to solve the technical problem, the embodiment of the invention adopts the following technical scheme:
the embodiment of the invention provides a continuous nitration reaction device, which comprises an acid inlet mechanism, a feeding mechanism, a low-temperature annular reactor and a high-temperature annular reactor, wherein the acid inlet mechanism and the feeding mechanism are both connected with a feeding hole of the low-temperature annular reactor, and an overflow port of the low-temperature annular reactor is connected with the feeding hole of the high-temperature annular reactor.
As a further improvement of the embodiment of the invention, the low-temperature annular reactor comprises a first heat exchanger and a second heat exchanger, the first heat exchanger comprises a shell, a heat exchange tube bundle is arranged in the shell, and a cooling water inlet and a cooling water outlet are arranged on the side wall of the shell; the structure of the second heat exchanger is the same as that of the first heat exchanger; an outlet of the heat exchange tube bundle of the first heat exchanger is connected with an inlet of the heat exchange tube bundle of the second heat exchanger, an outlet of the heat exchange tube bundle of the second heat exchanger is connected with an inlet of the heat exchange tube bundle of the first heat exchanger, and a cooling water outlet of the first heat exchanger is connected with a cooling water inlet of the second heat exchanger; the inlet of the heat exchange tube bundle of the first heat exchanger is provided with a feed inlet, and the outlet of the heat exchange tube bundle of the second heat exchanger is provided with an overflow port.
As a further improvement of the embodiment of the invention, the structure of the high-temperature annular reactor is the same as that of the low-temperature annular reactor.
As a further improvement of the embodiment of the invention, a first axial flow pump is arranged in the low-temperature annular reactor, and a second axial flow pump is arranged in the high-temperature annular reactor.
As a further improvement of the embodiment of the invention, the overflow port of the low-temperature annular reactor is connected with the feed inlet of the high-temperature annular reactor through a homogenizer.
As a further improvement of the embodiment of the invention, the reaction temperature of the low-temperature annular reactor is 25-30 ℃.
As a further improvement of the embodiment of the invention, the reaction temperature of the high-temperature annular reactor is 32-35 ℃.
As a further improvement of the embodiment of the invention, the acid feeding mechanism comprises an acid mixing elevated tank and an acid mixing feeding pump, the acid mixing elevated tank is connected with an inlet of the acid mixing feeding pump, and an outlet of the acid mixing feeding pump is connected with a feeding hole of the low-temperature annular reactor.
As a further improvement of the embodiment of the invention, the feeding mechanism comprises a solid feeding packing auger, a Venturi and a Venturi circulating pump, the solid feeding packing auger is connected with the Venturi, the Venturi is connected with the outlet of the Venturi circulating pump, the inlet of the Venturi circulating pump is connected with the low-temperature annular reactor, and the low-temperature annular reactor is connected with the outlet of the Venturi.
As a further improvement of the embodiment of the invention, the device also comprises a flash evaporation nitric acid recovery device, and the flash evaporation nitric acid recovery device is connected with an overflow port of the high-temperature annular reactor.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: according to the continuous nitration reaction device provided by the embodiment of the invention, the low-temperature annular reactor and the high-temperature annular reactor are arranged, the low-temperature nitration reaction is carried out in the low-temperature annular reactor, and the obtained nitration material overflows into the high-temperature annular reactor to carry out the high-temperature nitration reaction, so that the continuous nitration reaction is realized. The continuous nitration reaction device provided by the embodiment of the invention has the advantages of small equipment volume, less storage of the nitration materials, high heat transfer efficiency and production efficiency, and capability of reducing the risk of over-temperature and over-pressure of the nitration reaction.
Drawings
FIG. 1 is a schematic configuration diagram of a continuous nitrification reaction apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the structure of a low temperature loop reactor in an embodiment of the present invention;
FIG. 3 is a schematic cross-sectional view of a heat exchanger in an embodiment of the invention.
The figure shows that: the system comprises an acid mixing elevated tank 1, an acid mixing feeding pump 2, a solid feeding packing auger 3, a venturi 4, a venturi circulating pump 5, a homogenizer 6, a low-temperature annular reactor 7, a high-temperature annular reactor 8, a first axial flow pump 9, a second axial flow pump 10, a tail gas absorption device 11, a flash evaporation nitric acid recovery device 12, a first heat exchanger 71, a second heat exchanger 72, a shell 711, a heat exchange tube bundle 712, a cooling water inlet 713 and a cooling water outlet 714.
Detailed Description
The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, or uses. It should be understood that throughout the drawings, corresponding reference numerals indicate like or corresponding parts and features.
The embodiment of the invention provides a continuous nitration reaction device, which comprises an acid inlet mechanism, a feeding mechanism, a low-temperature annular reactor 7 and a high-temperature annular reactor 8, wherein the acid inlet mechanism and the feeding mechanism are connected with a feeding hole of the low-temperature annular reactor 7, and an overflow port of the low-temperature annular reactor 7 is connected with a feeding hole of the high-temperature annular reactor 8, as shown in figure 1.
In the above embodiment, the acid inlet mechanism is configured to convey the mixed acid to the low-temperature annular reactor 7, the feeding mechanism is configured to convey the solid material to the low-temperature annular reactor 7, the low-temperature annular reactor 7 performs the low-temperature nitration reaction, the obtained nitrated material overflows from the overflow port of the low-temperature annular reactor 7 and enters the high-temperature annular reactor 8, the high-temperature annular reactor 8 performs the high-temperature nitration reaction, and the obtained nitrated material overflows from the overflow port of the high-temperature annular reactor 8 and enters the flash evaporation nitric acid recovery device.
The continuous nitration reaction device adopts the low-temperature annular reactor 7 and the high-temperature annular reactor 8 to cool the released heat of the nitration materials in a sectional manner, so that the temperature of the nitration reaction is more stable and softer, and the risk of over-temperature and over-pressure of the nitration reaction is reduced. According to the continuous nitration reaction device, the axial-flow pump is adopted for forced circulation in the low-temperature annular reactor and the high-temperature annular reactor, so that the defect of low stirring mass transfer efficiency of the original kettle type is overcome. The low-temperature annular reactor and the high-temperature annular reactor are both composed of two tube-in-tube heat exchangers, and are superior to the characteristics of small heat exchange area and low heat transfer efficiency of a kettle type jacket. The low-temperature annular reactor realizes the continuous feeding of solid materials through the auger and the venturi, and fundamentally solves the disadvantage of large one-time feeding amount of the original kettle type. The continuous nitration reaction device of the embodiment has small equipment volume, less material stock for nitration preparation and high heat transfer efficiency and production efficiency.
As a preferred example, as shown in fig. 2, the low-temperature loop reactor 7 includes a first heat exchanger 71 and a second heat exchanger 72. As shown in fig. 3, the first heat exchanger 71 includes a housing 711, a heat exchange tube bundle 712 is disposed in the housing 711, and a cooling water inlet 713 and a cooling water outlet 714 are disposed on a side wall of the housing. When the device is used, the reaction materials are introduced into the heat exchange tubes of the heat exchange tube bundle, and cooling water is introduced outside the heat exchange tubes. The second heat exchanger 72 has the same structure as the first heat exchanger 71. The outlet of the heat exchange tube bundle of the first heat exchanger 71 is connected with the inlet of the heat exchange tube bundle of the second heat exchanger 72, the outlet of the heat exchange tube bundle of the second heat exchanger 72 is connected with the inlet of the heat exchange tube bundle of the first heat exchanger 71, and the first heat exchanger 71 and the second heat exchanger 72 are connected to form a ring. The cooling water outlet 714 of the first heat exchanger is connected to the cooling water inlet of the second heat exchanger. The inlet of the heat exchange tube bundle of the first heat exchanger 71 is provided with a feed inlet, and the outlet of the heat exchange tube bundle of the second heat exchanger 72 is provided with an overflow outlet.
In the above embodiment, the reaction material is introduced into the heat exchange tube bundle of the first heat exchanger 71 from the feed inlet to react and exchange heat with the cooling water in the shell of the first heat exchanger 71, and the reaction material continues to flow into the heat exchange tube bundle of the second heat exchanger 72 to react and exchange heat with the cooling chamber in the shell of the second heat exchanger 72. The reaction material continues to enter the heat exchange tube bundle of the first heat exchanger 71, so that the reaction material circularly flows between the first heat exchanger 71 and the second heat exchanger 72, and the temperature is reduced in the reaction process. The annular reactor is integrated, the two heat exchangers increase the heat exchange area, and the forced circulation of the axial flow pump enables materials to complete large-flow circulation in the reactor, so that the mass transfer efficiency and the heat transfer efficiency are improved. Meanwhile, cooling water is introduced into the shell of the first heat exchanger from the cooling water inlet 713 of the first heat exchanger 71, the cooling water exchanges heat with materials in the heat exchange tube bundles of the first heat exchanger in the shell of the first heat exchanger, then the cooling water is discharged from the cooling water outlet 714 of the first heat exchanger and enters the shell of the second heat exchanger from the cooling water inlet 72 of the second heat exchanger, the cooling water exchanges heat with the materials in the heat exchange tube bundles of the second heat exchanger in the shell of the second heat exchanger, the cooling water and the materials flow in a counter-flow manner, and the heat exchange and heat transfer efficiency is high.
Preferably, the high temperature loop reactor 8 has the same structure as the low temperature loop reactor 7. The reaction temperature of the low-temperature annular reactor 7 is 25-30 ℃, and 25 ℃ is preferred. The reaction temperature of the high-temperature annular reactor 8 is 32-35 ℃, and preferably 32 ℃. The nitration temperature range of most products is in a safe range at 25-40 ℃, and a violent reaction phenomenon can occur when the nitration temperature exceeds 40 ℃. In order to ensure the reaction safety, the temperature of the low-temperature annular reactor and the temperature of the high-temperature annular reactor are controlled to be at the bottom limit value, a regulating space is reserved for automatic interlocking, and 25 ℃ and 32 ℃ are respectively selected as the optimal reaction temperature.
Preferably, the low-temperature loop reactor 7 is provided with a first axial flow pump 9, and the high-temperature loop reactor 8 is provided with a second axial flow pump 10. Forced reflux circulation is formed in the low-temperature annular reactor through the first axial flow pump 9, forced reflux circulation is formed in the high-temperature annular reactor through the second axial flow pump 10, and the heat exchange efficiency of the two annular reactors is improved.
Preferably, the overflow port of the low-temperature annular reactor 7 is connected with the feed port of the high-temperature annular reactor 8 through the homogenizer 6. The nitrified materials are better mixed and dispersed by utilizing the high-speed shearing of the homogenizer, and the mass transfer efficiency is improved.
As a preferable example, as shown in FIG. 1, the acid feeding mechanism comprises a mixed acid head tank 1 and a mixed acid feeding pump 2, wherein the inlet of the mixed acid head tank 1 is connected with the inlet of the mixed acid feeding pump 2, and the outlet of the mixed acid feeding pump 2 is connected with the feeding hole of the low-temperature annular reactor 7. When in use, the mixed acid in the mixed acid head tank 1 is conveyed to the low-temperature annular reactor 7 through the mixed acid feeding pump 2.
As a preferable example, as shown in FIG. 1, the feeding mechanism comprises a solid feeding packing auger 3, a Venturi 4 and a Venturi circulating pump 5, the solid feeding packing auger 3 is connected with the Venturi 4, the Venturi 4 is connected with an outlet of the Venturi circulating pump 5, an inlet of the Venturi circulating pump 5 is connected with a low-temperature annular reactor 7, and the low-temperature annular reactor 7 is connected with an outlet of the Venturi 4. The Venturi 4, the Venturi circulating pump 5 and the low-temperature annular reactor 7 form circulation, and solid materials in the solid feeding auger 3 are continuously sucked into the low-temperature annular reactor 7 to carry out low-temperature nitration reaction.
As a preferable example, the continuous nitration reaction apparatus of the embodiment of the present invention further includes a flash evaporation nitric acid recovery apparatus 12, and the flash evaporation nitric acid recovery apparatus 12 is connected to an overflow port of the high temperature annular reactor 8. The flash evaporation nitric acid recovery device is used for recovering excessive nitric acid in the nitration reaction, and the cost of raw materials is reduced. The continuous nitration reaction device of the embodiment of the invention further comprises a tail gas absorption device 11, wherein the tail gas absorption device 11 is respectively connected with the low-temperature annular reactor 7 and the high-temperature annular reactor 8 and is used for absorbing gas generated in the low-temperature annular reactor 7 and the high-temperature annular reactor 8.
The operation of the continuous nitrification reactor of the above embodiment is as follows:
adding the prepared mixed acid into a mixed acid overhead tank 1, and continuously adding the mixed acid into a low-temperature annular reactor 7 through a mixed acid feeding pump 2. The solid material is continuously fed into the Venturi 4 through the solid feeding auger 3, the Venturi circulating pump 5, the Venturi 4 and the low-temperature annular reactor 7 form circulation, and the solid material is continuously sucked into the low-temperature annular reactor 7 for low-temperature nitration reaction. The nitrified material obtained in the low-temperature annular reactor 7 overflows into an inlet of the homogenizer 6, is continuously transferred into the high-temperature annular reactor 8 through the homogenizer 6 to carry out high-temperature nitration reaction, and the obtained nitrified material overflows into a flash evaporation nitric acid recovery device 12.
A specific example is provided below.
The continuous nitration reaction device provided by the embodiment of the invention is used for nitration production of 1, 5-dinitroanthraquinone and 1, 8-dinitroanthraquinone, and anthraquinone reacts with mixed acid of nitric acid and nicotinic acid to obtain 1, 5-dinitroanthraquinone and 1, 8-dinitroanthraquinone. The volume of the continuous nitration reaction device of the embodiment of the invention is 5000L, and the volume of the original nitration reaction kettle is 15000L. The continuous nitration reactor of the embodiment of the invention has a stock of nitration material in process of 4000L, and the stock of nitration material in process of the original nitration reactor is 12000L.
The continuous nitration reaction device provided by the embodiment of the invention solves the problems of complex production equipment, large equipment volume, large storage amount of the material to be nitrated, poor heat transfer capability, low production efficiency and high risk of over-temperature and over-pressure of the traditional reaction equipment.
The embodiments of the present invention are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. That is, all equivalent changes and modifications made according to the content of the claims of the present invention should be regarded as the technical scope of the present invention.

Claims (10)

1. The continuous nitration reaction device is characterized by comprising an acid inlet mechanism, a feeding mechanism, a low-temperature annular reactor (7) and a high-temperature annular reactor (8), wherein the acid inlet mechanism and the feeding mechanism are both connected with a feeding hole of the low-temperature annular reactor (7), and an overflow port of the low-temperature annular reactor (7) is connected with a feeding hole of the high-temperature annular reactor (8).
2. The continuous nitrification reaction apparatus according to claim 1, wherein the low-temperature annular reactor (7) comprises a first heat exchanger (71) and a second heat exchanger (72), the first heat exchanger (71) comprises a shell (711), a heat exchange tube bundle (712) is arranged in the shell (711), and the side wall of the shell is provided with a cooling water inlet (713) and a cooling water outlet (714); the structure of the second heat exchanger is the same as that of the first heat exchanger; an outlet of the heat exchange tube bundle of the first heat exchanger is connected with an inlet of the heat exchange tube bundle of the second heat exchanger, an outlet of the heat exchange tube bundle of the second heat exchanger is connected with an inlet of the heat exchange tube bundle of the first heat exchanger, and a cooling water outlet (714) of the first heat exchanger is connected with a cooling water inlet of the second heat exchanger; the inlet of the heat exchange tube bundle of the first heat exchanger is provided with a feed inlet, and the outlet of the heat exchange tube bundle of the second heat exchanger is provided with an overflow port.
3. The continuous nitrification reactor according to claim 2, wherein the high temperature loop reactor (8) has the same structure as the low temperature loop reactor (7).
4. The continuous nitrification reaction apparatus according to claim 2, wherein the low-temperature annular reactor (7) is provided with a first axial flow pump (9), and the high-temperature annular reactor (8) is provided with a second axial flow pump (10).
5. The continuous nitrification reactor according to claim 1, wherein the overflow port of the low temperature annular reactor (7) and the feed port of the high temperature annular reactor (8) are connected by the homogenizer (6).
6. The continuous nitrification reactor according to claim 1, wherein the reaction temperature of the low-temperature annular reactor (7) is 25 to 30 ℃.
7. The continuous nitrification reactor according to claim 1, wherein the reaction temperature of the high-temperature annular reactor (8) is 32 to 35 ℃.
8. The continuous nitration reaction device according to claim 1, wherein the acid feeding mechanism comprises a mixed acid head tank (1) and a mixed acid feeding pump (2), the inlet of the mixed acid head tank (1) is connected with the inlet of the mixed acid feeding pump (2), and the outlet of the mixed acid feeding pump (2) is connected with the feeding port of the low temperature annular reactor (7).
9. The continuous nitration reaction device according to claim 1, wherein the feeding mechanism comprises a solid feeding screw conveyor (3), a venturi (4) and a venturi circulating pump (5), the solid feeding screw conveyor (3) is connected with the venturi (4), the venturi (4) is connected with an outlet of the venturi circulating pump (5), an inlet of the venturi circulating pump (5) is connected with the low-temperature annular reactor (7), and the low-temperature annular reactor (7) is connected with an outlet of the venturi (4).
10. The continuous nitration reaction apparatus according to claim 1, further comprising a flash nitric acid recovery apparatus (12), wherein the flash nitric acid recovery apparatus (12) is connected to an overflow port of the high temperature annular reactor (8).
CN202111681572.7A 2021-12-29 2021-12-29 Continuous nitration reaction device Pending CN114225884A (en)

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