CN104772104A - Method for preparing fixed bed reactor filling material - Google Patents
Method for preparing fixed bed reactor filling material Download PDFInfo
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- CN104772104A CN104772104A CN201510120436.9A CN201510120436A CN104772104A CN 104772104 A CN104772104 A CN 104772104A CN 201510120436 A CN201510120436 A CN 201510120436A CN 104772104 A CN104772104 A CN 104772104A
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- quartz sand
- fixed bed
- powder
- bed reactors
- filler
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000011049 filling Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000006004 Quartz sand Substances 0.000 claims abstract description 53
- 239000002245 particle Substances 0.000 claims abstract description 32
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 239000000945 filler Substances 0.000 claims description 39
- 239000011230 binding agent Substances 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000008188 pellet Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000007787 solid Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 7
- 238000003756 stirring Methods 0.000 abstract description 7
- 238000005498 polishing Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 3
- 230000001070 adhesive effect Effects 0.000 abstract 3
- 239000010453 quartz Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 17
- 239000002994 raw material Substances 0.000 description 14
- 238000005469 granulation Methods 0.000 description 11
- 230000003179 granulation Effects 0.000 description 11
- 239000007789 gas Substances 0.000 description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 229960004643 cupric oxide Drugs 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Landscapes
- Glanulating (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses a method for preparing a fixed bed reactor filling material. The preparation method comprises the following steps: (1) sieving quartz sand to obtain particles with a uniform size, mixing the sieved quartz with solid filling powder, adding an adhesive, and evenly stirring to obtain a mixed material; (2) pouring the mixed material into a cylinder polishing machine; (3) setting the rotation speed and operation time of the cylinder polishing machine, and starting the machine to produce the fixed bed reactor filling material; wherein during the production process, the powder is gradually wrapped on the external surface of the quartz sand under the co-action of the wall extrusion force generated by the centrifugal rotation of the quartz sand and the adhesive force of the adhesive so as to form particles composed of a core (quartz sand) and a shell (powder). The procedure is concise, the steps are few, the cost is low, and the operation is convenient. The reaction activity of the filling material can be improved, and moreover, the bed pressure drop of the reactor can be prominently reduced, so the method is practical and is worth to promote.
Description
Technical field
The present invention relates to a kind of filler design ap-plication field of chemical reactor, what be specifically related to is a kind of method for the preparation of fixed bed reactors filler.
Background technology
Gas-solid fixed bed reactors because its structure is simple, filler is not easy to wear, the feature of Applicable temperature and operating pressure wider range and be widely used in chemical industry (as synthetic ammonia, water gas shift, methane reforming hydrogen manufacturing etc.).Owing to needing to load solid filling material in gas-solid fixed bed reactors, in general, filler granularity is thinner, reactivity is higher, its effective rate of utilization is also higher, but under actual conditions, fine filler can cause gas flow resistance to enlarge markedly, destroy normal operating, engineer applied demand cannot be met.Therefore granulation process must be carried out to filler, to reduce bed pressure drop.
At present, in fixation reaction bed, the prilling process that filler is conventional has stirring-granulating and pressure granulation, is described below respectively:
Stirring-granulating method, is certain liquid or binding agent infiltrated in solid fine powder end and suitably stir, makes liquid and solid fine powder end close contact mutually, produce cohesive force and form granule.The most frequently used stirring means be by disk, taper or the revolution of tubular rotary drum time stir, to roll and the curtain motion that hangs has come.The advantage of paddling process is that former structure is simple, single machine yield large, and the easy rapid solution of the particle formed, drenched property are strong; But it is bad that shortcoming is particle uniformity, the granule strength formed is lower.
Pressure forming comminution granulation the powder material of granulation to be limited in particular space, compresses as dense state by applying external force.Different according to the physical system of applied external force, compression moulding method can be divided into die pressing, extrusion and extrusion―spherozation again.The advantage of pressure forming comminution granulation to manufacture larger agglomerate, and made material also has suitable mechanical strength; But it is more that shortcoming is operation, equipment controls complicated, and easily occurs material mucosa events in operating process.
In sum, for the granulation of fixed bed reactors filler, traditional stirring-granulating method, in order to obtain higher granule strength, must adopt higher binder content, but this can cause binding agent to the serious covering of powder surface; Although and the particle intensity that pressure forming comminution granulation is formed is higher, the porosity between powder particles can significantly reduce.As can be seen here, the prilling process of conventional fixed bed reactor filler, can reduce the mass transfer rate between reacting gas and powder particles, thus reduces chemical reactivity and the effective rate of utilization of filler.
Therefore, design a kind of powder prilling process that can keep powder high reaction activity, effectively can reduce again reactor pressure decrease, for gas solid reactor practical application have great importance.
Summary of the invention
In order to overcome the deficiency of above-mentioned technology, the invention provides a kind of method for the preparation of fixed bed reactors filler, the particle adopting the method to prepare is suitable as the packing material of fixed bed reactors very much, and it can meet the demand of filler high reaction activity and the pressure drop of reactor low bed layer simultaneously.
To achieve these goals, the technical solution used in the present invention is as follows:
For the preparation of a method for fixed bed reactors filler, comprise the following steps:
(1) quartz sand is sieved, obtain even-grained particle, and the quartz sand after screening is mixed with solid-filling powder, then adding binding agent is stirred to evenly, obtain compound, wherein, the ratio of described quartz sand, fixing filler powder and binding agent is 5 ~ 10: 5 ~ 10: 1;
(2) compound is poured in the cylinder of ratary mixer, and by the end cap seal of ratary mixer;
(3) rotating speed and the running time of ratary mixer are set, and starting device, make powder under the acting in conjunction of the barrel extruding force produced by quartz sand particle centrifugal rotation and binding agent cohesive force, successively wrap up to quartz sand outer surface, the granulated pellet that formation is kernel with quartz sand, powder is shell, namely obtains final fixed bed reactors filler; The rotating speed of described ratary mixer and running time are respectively 40 ~ 60r/min, 8 ~ 30min.
Further, in described step (1), the quartz sand particle of same particle size range is sieved out, and mix with solid-filling powder.
Again further, the purity of described quartz sand is on 99.9%.
Or described quartz sand is technical grade quartz sand, and before sieving, prior to calcining 5h in 800 DEG C of air atmospheres, the volatile impurity component in removing quartz sand particle.
Specifically, the solid-filling powder in described step (1) is metal or metal oxide powder.
As preferably, described solid-filling powder size is 80 orders with carefully.
As preferably, the binding agent in described step (1) is Ludox.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention take quartz sand as carrier, and be equipped with solid-filling powder and the binding agent raw materials as fixed bed reactors filler, the process being mixed by raw material, stir, rotate, extrude and bond, the granulated pellet (filler) that to have prepared take quartz sand as kernel, powder is shell, and be applied in fixed bed reactors.The present invention only needs to utilize ratary mixer to process mixed raw material, the filler of excellent performance can be obtained, this has benefited from combining closely of various raw material in the present invention and configuration proportion thereof and each preparation process, the present invention produces without the need to using large industry equipment, therefore its not only cost is very cheap, and also quite convenient in operation, be suitable for very much the preparation of fixed bed reactors filler.
(2) mode owing to rolling under present invention employs free state carries out granulation, thus in the process of granulation, powder can be bonded in the surface of quartz sand in loose condition (of surface), tessellation is not extruded significantly between powder, and then after obtained filler, still have obvious duct supplied gas molecular diffusion between powder, ensure that higher chemical reaction velocity.Therefore, the present invention compares traditional stirring-granulating method, and it not only significantly can reduce the consumption of binding agent, but also maintain the original high reaction activity of powder, meanwhile, due to the supporting role of quartz sand, particle can not efflorescence in the process of chemical reaction, still remains initial particle shape; And compare traditional pressure prilling process, particle prepared by the present invention, because its inside has a large amount of holes, thus making powder is still the state of natural packing, and then also maintains the original high reaction activity of powder.Therefore, the present invention is while effectively combining two kinds of traditional prilling advantages, also solve existing prilling Problems existing well, thus significantly improve the performance of filler, and provide strong guarantee for effective application of gas-solid fixed bed reactors.
(3) the present invention also sieves quartz sand before quartz sand particle is used as carrier, obtains even-grained particle; And in order to reduce the negative effect of quartz sand carrier to chemical reaction process further, quartz sand in the present invention both can select the pure raw material of pure analysis (purity is more than 99.9%), the industrial raw material after high-temperature calcination also can be selected to remove volatile impurity composition.So, the present invention prepares obtained granulated pellet, not only epigranular, consistent, and purity is high; And relative to the reactor that non-uniform granular is filled, particle prepared by the present invention has larger voidage, the flowing of gas molecule can be made more unobstructed, can not cause remarkable bed pressure drop, thus more can meet the application demand of engineering.
(4) the present invention adopts Ludox as binding agent, and Ludox is the colloidal solution that the silicon dioxide microparticle of aquation is scattered in water, and along with the evaporation of moisture, Ludox colloid molecules can increase, and finally forms-SiO-O-SiO-film.The present invention is by rational raw material choice and ratio thereof and technological design, take full advantage of the characteristic of Ludox, in technique of the present invention, when water evaporates in Ludox, colloidal particle wherein can be attached to body surface securely, make between particle, to form silica to combine, thus just while guarantee is to powder package action effect, can not can pollute whole reaction system.
(5) present invention process flow process is succinct, operation is few, former structure is simple, simultaneously, the filler reactivity of preparation is high and significantly can reduce the pressure drop of reactor, therefore, the present invention is with a wide range of applications, and is highly suitable for the practical application aspect large-scale promotion of gas solid reactor.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and embodiments of the present invention include but not limited to the following example.
Embodiment
The invention provides a kind of method for the preparation of chemical reactor, particularly gas-solid-solid fixed bed reactor filler newly, the method is formed primarily of flow processs such as raw material mixing, stirring and rotation, extruding and bondings, as follows respectively:
One, raw material mixing, stirring
In the present invention, the raw material preparing filler is quartz sand, solid-filling powder and binding agent.First, quartz sand particle is sieved, obtain the single-size of same particle size range (such as 20 ~ 30 orders, 30 ~ 40 orders, 40 ~ 60 orders etc.).Then, mixed by quartz sand particle with solid-filling powder, then add binding agent and be stirred to evenly, obtain compound, in this compound, the mixed proportion of described quartz sand, solid-filling powder and binding agent is 5 ~ 10: 5 ~ 10: 1.Solid-filling powder used by the present invention refers to that powder body material filled by the widely used fixed bed reactors of chemical field, comprise various metals or the metal oxide of catalytic reaction and uncatalyzed reaction, in the present embodiment, this kind of solid-filling powder refers to that 80 orders are with the powder of thin Monosized powder or combination grain; Described quartz sand can be analyze pure raw material (namely purity is more than 99.9%), also can be in 800 DEG C of air atmospheres, to calcine 5h and technical grade quartz sand after removing volatile impurity component wherein, and described binding agent then preferably adopts Ludox.
Two, raw material rotates, extrudes and bonding
After obtained compound, be poured in the cylinder of ratary mixer, and by the end cap seal of ratary mixer, ratary mixer of the present invention is standard available type product, power transmission shaft is driven to rotate by variable-frequency motor, power transmission shaft drives drum rotating again, can adjust drum rotation speed and running time.
After compound puts into polishing machine, suitable rotating speed and running time are set (in the present embodiment, the rotating speed of ratary mixer and running time are set to 40 ~ 60r/min, 8 ~ 30min respectively), and opening device, make powder under the acting in conjunction of the barrel extruding force produced by quartz sand particle centrifugal rotation and binding agent cohesive force, successively wrap up to quartz sand outer surface, the granulated pellet that formation is kernel with quartz sand, powder is shell, namely obtains the final filler that can be applied in fixed bed reactors.
According to above-mentioned preparation method, with an example, implementation process of the present invention is introduced below.
Remove due to hydrogen isotope in inert atmosphere and often adopt catalytic oxidation, therefore, its corresponding fixed bed reactors often select cupric oxide as filler.And as described below for the prilling process of this kind of fixed bed reactors filler:
One, raw material:
(1) cupric oxide powder: analyze pure raw material, granularity is about 400 orders;
(2) quartz sand: 20 ~ 30 object technical grade quartz sand particles, calcines 5h in 800 DEG C of air atmospheres, removes volatile component;
(3) Ludox;
(4) ratary mixer: standard available type, roll circumference is hexagon, and volume is 1L.
Two, granulation process
Take cupric oxide powder and each 200g of quartz sand to put into and burn in ring, then add Ludox 25g, adopt glass rod to be stirred to substantially even, obtain compound.Then, compound is poured into cylinder, and end cover.Arrange that polishing machine rotating speed is 50r/min, running time is 10min, then opening device, powder is under the acting in conjunction of the barrel extruding force produced by quartz sand particle centrifugal rotation and binding agent cohesive force, successively wrap up to quartz sand outer surface, the granulated pellet that formation is kernel with quartz sand, powder is shell, now, the oxidized copper powders of outer surface of quartz sand is completely coated, and grain graininess is even.
Adopt aforesaid way or similar fashion can carry out granulation to all the other various metals or metal-oxide powder, and the granulated pellet of required different grain size and steric bulk density can be obtained by the adjustment granularity of quartz sand and the ratio of powder and quartz sand.
The present invention utilizes quartz sand as carrier, after cooperation solid-filling powder and binding agent, by rational preparation technology, obtain the preferred fixed bed reactors filler of performance, for gas-solid fixed bed reactors provide guarantee in actual applications, meet the needs of engineering.The present invention breaches the restriction of traditional handicraft, achieves innovation well, and the design of fixed bed reactors filler has been risen to a new height by it.Therefore, compared to existing technology, the technology of the present invention progress is fairly obvious, has outstanding substantive distinguishing features and significant progress.
Above-described embodiment is only the preferred embodiments of the present invention; be not construed as limiting the scope of the present invention; in every case design principle of the present invention being adopted, and the change carried out non-creativeness work on this basis and make, all should belong within protection scope of the present invention.
Claims (7)
1. for the preparation of a method for fixed bed reactors filler, it is characterized in that, comprise the following steps:
(1) quartz sand is sieved, obtain even-grained particle, and the quartz sand after screening is mixed with solid-filling powder, then adding binding agent is stirred to evenly, obtain compound, wherein, the ratio of described quartz sand, fixing filler powder and binding agent is 5 ~ 10: 5 ~ 10: 1;
(2) compound is poured in the cylinder of ratary mixer, and by the end cap seal of ratary mixer;
(3) rotating speed and the running time of ratary mixer are set, and starting device, make powder under the acting in conjunction of the barrel extruding force produced by quartz sand particle centrifugal rotation and binding agent cohesive force, successively wrap up to quartz sand outer surface, the granulated pellet that formation is kernel with quartz sand, powder is shell, namely obtains final fixed bed reactors filler; The rotating speed of described ratary mixer and running time are respectively 40 ~ 60r/min, 8 ~ 30min.
2. a kind of method for the preparation of fixed bed reactors filler according to claim 1, is characterized in that, in described step (1), sieves out by the quartz sand particle of same particle size range, and mixes with solid-filling powder.
3. a kind of method for the preparation of fixed bed reactors filler according to claim 2, is characterized in that, the purity of described quartz sand is on 99.9%.
4. a kind of method for the preparation of fixed bed reactors filler according to claim 2, it is characterized in that, described quartz sand is technical grade quartz sand, and before sieving, prior to calcining 5h in 800 DEG C of air atmospheres, the volatile impurity component in removing quartz sand particle.
5. a kind of method for the preparation of fixed bed reactors filler according to claim 2 ~ 4 any one, is characterized in that, the solid-filling powder in described step (1) is metal or metal oxide powder.
6. a kind of method for the preparation of fixed bed reactors filler according to claim 5, is characterized in that, described solid-filling powder size is 80 orders with carefully.
7. a kind of method for the preparation of fixed bed reactors filler according to claim 6, is characterized in that, the binding agent in described step (1) is Ludox.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510120436.9A CN104772104B (en) | 2015-03-19 | 2015-03-19 | A kind of method for preparing fixed bed reactors filler |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510120436.9A CN104772104B (en) | 2015-03-19 | 2015-03-19 | A kind of method for preparing fixed bed reactors filler |
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| CN104772104A true CN104772104A (en) | 2015-07-15 |
| CN104772104B CN104772104B (en) | 2017-01-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110064339A (en) * | 2019-05-07 | 2019-07-30 | 天津西敦津洋环保科技有限公司 | The preparation method of composite particles |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3690622A (en) * | 1969-02-28 | 1972-09-12 | Pia Beatrice Brunner Rohrer | Processing and mixing machine |
| CN1030026A (en) * | 1987-05-09 | 1989-01-04 | 英国石油公司 | The preparation process of spheric granules |
| CN1148352A (en) * | 1995-03-03 | 1997-04-23 | 日本化药株式会社 | Catalyst and process for producing same |
| CN1839034A (en) * | 2003-04-15 | 2006-09-27 | 氦克逊特种化学品公司 | Particulate material containing thermoplastic elastomer and methods for making and using same |
| JP5036192B2 (en) * | 2006-02-09 | 2012-09-26 | 住友化学株式会社 | Catalyst filling method |
-
2015
- 2015-03-19 CN CN201510120436.9A patent/CN104772104B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3690622A (en) * | 1969-02-28 | 1972-09-12 | Pia Beatrice Brunner Rohrer | Processing and mixing machine |
| CN1030026A (en) * | 1987-05-09 | 1989-01-04 | 英国石油公司 | The preparation process of spheric granules |
| CN1148352A (en) * | 1995-03-03 | 1997-04-23 | 日本化药株式会社 | Catalyst and process for producing same |
| CN1839034A (en) * | 2003-04-15 | 2006-09-27 | 氦克逊特种化学品公司 | Particulate material containing thermoplastic elastomer and methods for making and using same |
| JP5036192B2 (en) * | 2006-02-09 | 2012-09-26 | 住友化学株式会社 | Catalyst filling method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110064339A (en) * | 2019-05-07 | 2019-07-30 | 天津西敦津洋环保科技有限公司 | The preparation method of composite particles |
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