CN106044852A - Preparation method of nano tin antimony oxide powder - Google Patents

Preparation method of nano tin antimony oxide powder Download PDF

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Publication number
CN106044852A
CN106044852A CN201610677327.1A CN201610677327A CN106044852A CN 106044852 A CN106044852 A CN 106044852A CN 201610677327 A CN201610677327 A CN 201610677327A CN 106044852 A CN106044852 A CN 106044852A
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frame
fixed
push
cylinder
rod
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CN106044852B (en
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林晓丽
陈晔
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Guangdong Defusheng New Material Technology Co ltd
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Haining Yongxin Technology Consulting Co Ltd
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Priority to CN201710321489.6A priority Critical patent/CN106986382B/en
Priority to CN201610677327.1A priority patent/CN106044852B/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00Compounds of antimony
    • C01G30/004Oxides; Hydroxides; Oxyacids
    • C01G30/005Oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/0012Devices for disintegrating materials by collision of these materials against a breaking surface or breaking body and/or by friction between the material particles (also for grain)
    • B02C19/0043Devices for disintegrating materials by collision of these materials against a breaking surface or breaking body and/or by friction between the material particles (also for grain) the materials to be pulverised being projected against a breaking surface or breaking body by a pressurised fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Food Science & Technology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Accessories For Mixers (AREA)

Abstract

The invention provides a preparation method of nano tin antimony oxide powder and solves the technical problem that a preparation method in the prior art has complex steps, requires manual operations and is low in production speed. The preparation method includes the following steps: A) dissolving tin tetrachloride and antimony nitrate in dilute hydrochloric acid, stirring the solution and gradually adding an alkali solution until the pH value is 7-9, continuously stirring the solution until tin ions and antimony ions are completely precipitated to prepare a tin hydroxide and antimony hydroxide precursor; B) filtering and separating the tin hydroxide and antimony hydroxide precursor and washing the tin hydroxide and antimony hydroxide precursor with deionized water; C) adding water and polyethylene glycol to the washed precursor, stirring the mixture uniformly, moving the mixture to a reaction kettle to prepare nano slurry; and D) separating and drying the nano slurry, and calcining the nano slurry at 400-700 DEG C for 2-6 h, and crushing the calcined substance through an air-flow crusher to prepare the nano tin antimony oxide powder. The method is high in production efficiency.

Description

A kind of preparation method of nano antimony tin oxide powder
Technical field
The present invention relates to a kind of preparation method, the preparation method of a kind of nano antimony tin oxide powder.
Background technology
Nano antimony tin oxide is the Multifunction transparent material in nonferrous metal property chain with high-performance and high added value Material, because of its have good electric conductivity, light-coloured transparent, intercept infrared ray and ultraviolet, good weatherability and stability with And catalytic etc., it is widely used in the fields such as transparent heat-insulated insulation film, anti-static coating and anti-fouling and self-cleaning film.
Through retrieval, as Chinese patent literature discloses the low temperature ball-milling preparation method [Shen of a kind of tin antimony oxide nano-powder Please number: 201210582264.3;Publication number: CN 103041896A].The preparation method of this tin antimony oxide nano-powder, it is special Levy and be, the low temperature ball-milling preparation method of a kind of tin antimony oxide nano-powder, the method that the method employing comprises the following steps: (1) Being that 10:1~100:1 joins in ball grinder by zirconium oxide balls and raw material powder according to ball material weight ratio, raw material powder is stannum oxide Powder, oxidation antimony powder;(2) in ball grinder, it is passed through liquid nitrogen, makes raw material powder and zirconium oxide balls be fully immersed in liquid nitrogen, temperature For≤-180 DEG C, and keep the volatile quantity of liquid nitrogen with intake balance so that liquid level stabilizing;(3) constant temperature starts ball after 30 minutes Mill, ball milling 1~48 hours;(4) powder body after ball milling is placed in the environment of 50~200 DEG C and carries out nitrogen desorption and process 0.5~3 little Time;Through above-mentioned steps, obtain described tin antimony oxide nano-powder.
Although the preparation method disclosed in this patent is with low cost, but, the complex steps of this preparation method, and need people Work operates, and speed of production is slow, and therefore, the preparation method designing a kind of nano antimony tin oxide powder is necessary.
Summary of the invention
It is an object of the invention to there are the problems referred to above for existing technology, it is proposed that a kind of nano antimony tin oxide powder Preparation method, this preparation method has the advantages that production efficiency is high.
The purpose of the present invention can be realized by following technical proposal: the preparation method of a kind of nano antimony tin oxide powder, It is characterized in that, comprise the steps of:
A, butter of tin, nitric acid antimony are dissolved in dilute hydrochloric acid, during stirring, are gradually added aqueous slkali until pH Value reaches 7-9, continues stirring, until tin ion and antimony ion precipitation are completely, obtains stannic hydroxide and antimony hydroxide predecessor;
B, filtration separate and utilize deionized water wash stannic hydroxide and antimony hydroxide predecessor, are removed by solable matter Go, wash 2-5 time;
C, predecessor after step b is washed add water and Polyethylene Glycol, is transferred to after stirring in reactor, control The temperature of reactor processed is 180-280 DEG C, successive reaction 2-4h under conditions of stirring, prepares nano pulp;
D, separation after drying, prepare tin-antiomony oxide powders mixture, calcine 2-6h, then lead under conditions of 400-700 DEG C Cross jet mill to pulverize, prepare nano antimony tin oxide powder.
Using above method, can realize it by various plant equipment and prepare, replace manual operation, production efficiency is high.
Jet mill in described step d includes frame, and described frame is disposed with feeding device, mixing dress Put, reducing mechanism and packing apparatus, described feeding device includes feeding tube, storage tank and props up for positioning the location of raw material bag Frame, locating support and storage tank are arranged in frame, and storage tank lower end has the first delivery outlet, is provided with in the first delivery outlet First electromagnetic valve, storage tank upper end has the first charging aperture, and the first charging aperture is connected with feeding tube one end, the feeding tube other end It is positioned at above locating support, and this end has guide portion, frame is provided with a moving machine that guide portion can be driven to move up and down Structure, is additionally provided with the first delivery pump in feeding tube;Described travel mechanism includes cylinder and mounting ring, and the cylinder body of cylinder is fixed on machine On frame, straight down, the piston rod end of cylinder is connected with mounting ring the piston rod of cylinder by connecting rod, and guide portion is fixed on In mounting ring, frame is additionally provided with the controlling organization that can control cylinder action;Described mixing arrangement includes blending bin, fog-spray nozzle With reserving liquid tank, blending bin and reserving liquid tank are each attached in frame, blending bin top has powder body input port, and powder body input port is passed through First connecting tube is connected with the first delivery outlet, and blending bin bottom has powder body delivery outlet, is provided with second in powder body delivery outlet Electromagnetic valve, fog-spray nozzle is arranged in blending bin, and the liquid outlet of fog-spray nozzle down, managed by conveying and liquid storage by the inlet of fog-spray nozzle Case is connected, and is provided with the second delivery pump in conveying pipe, and blending bin top is additionally provided with shaft, shaft upper end and stirring electricity Machine is connected, and shaft lower end penetrates and is connected with stirring vane in blending bin, frame is provided with and can draw material in blending bin Draw frame machine, draw frame machine includes suction pipe, the second push-rod electric machine, asepwirator pump, mounting blocks and case, and the second push-rod electric machine leads to Crossing one can drive its moving structure moved horizontally to be arranged in blending bin, the push rod of the second push-rod electric machine straight down, second The push rod end of push-rod electric machine and mounting blocks fix, and the feed end of suction pipe is fixed on mounting blocks, and this feed end is down, The discharge end of suction pipe passes blending bin and is positioned at case, and asepwirator pump is arranged in suction pipe;Described packing apparatus includes depositing Batch can, material stock tank is fixed in frame, and material stock tank top has the second input port, and the second connecting tube and powder are passed through in the second input port Body delivery outlet is connected, and material stock tank bottom has the second delivery outlet, is provided with the 3rd electromagnetic valve, frame sets in the second delivery outlet Being equipped with the detent mechanism that can be positioned at finished bag edge, frame is additionally provided with shock structure, shock structure includes the second shake Dynamic plate, the second vibration motor and the second installing plate, the second installing plate can drive its first elevating mechanism moved up and down by one Being arranged in frame, the second jolting plate is arranged on the second installing plate, and the second jolting plate is in immediately below the second delivery outlet, the There is between two jolting plates and the second installing plate the 3rd spring, the 3rd spring one end and the second jolting plate lower surface be connected, the 3rd The spring other end and the second installing plate upper surface are connected, and the second vibration motor is fixed on the second jolting plate lower surface.
The operation principle of jet mill is as follows: the raw material bag being used for depositing raw material is positioned at locating support, opens First delivery pump, the first delivery pump by feeding tube by the feedstock transportation in raw material bag to storage tank, along with in raw material bag Raw material gradually decreases, and the piston rod controlling cylinder drives mounting ring to move down, and mounting ring drives guide portion to move down, and makes to lead Material portion contacts with the raw material in raw material bag all the time;Raw material in storage tank was transported in blending bin by the first communicating pipe, controlled The output shaft of stirring motor drives shaft to rotate, and shaft drives stirring vane to rotate, and meanwhile, opens the second delivery pump, the Modifying agent in reserving liquid tank is transported in fog-spray nozzle by two delivery pumps by conveying pipe, makes modifying agent and raw material uniformly mix;Mixed Raw material in mould assembling through pulverizing after by being transported to the second communicating pipe in material stock tank, by detent mechanism by the edge of finished bag It is fixed on the second delivery outlet, controls the 3rd electromagnetic valve and make the second equipped at outlet port in open mode;By the first elevating mechanism band Dynamic second installing plate moves up and down, and the second installing plate drives the second jolting plate to move up and down, and makes the second jolting plate and finished bag Bottom contact, drives the second jolting plate to shake by the second vibration motor, and the second jolting plate drives finished bag to produce vibrations and makes into Product are packed full, thus complete its processing operation, and production efficiency is high.
Described controlling organization includes that displacement transducer, mounting rod and controller, mounting rod one end are connected with mounting ring, peace The dress bar other end is connected with displacement transducer, and the induction part of displacement transducer is fixed on machine towards locating support, controller On frame, cylinder is connected with this controller with displacement transducer.
Use above structure, by the distance of raw material in displacement transducer detection guide portion and material bag, signal is transmitted To controller, controller controls the piston rod of cylinder and moves down, and controls precisely.
Described locating support upper end has the locating dowel that can position raw material bag, and locating support lower end has can be entered raw material bag The percussion mechanism of row vibrations, described percussion mechanism includes the first jolting plate and the first vibration motor, and the first jolting plate is arranged on fixed On the base plate of position support, there is between the first jolting plate and the base plate of locating support the first spring, one end of the first spring and the One jolting plate fixes, and the other end of the first spring and the base plate of locating support fix, and the first vibration motor is fixed on first Jolting plate lower surface.
When raw material bag is shaken by needs, the edge of raw material bag is penetrated in locating dowel, by the first vibration motor Making the first jolting plate produce vibrations, the first jolting plate drives raw material bag vibrations, makes the material in raw material bag move down, vibrations side Just.
Being additionally provided with anti-slipping mechanism on described locating support, anti-slipping mechanism includes claw and the second spring, claw lower end and Locating support is hinged, and one end of the second spring is connected with in the middle part of claw, and the other end of the second spring is connected with locating support Connecing, claw upper end can be resisted against on locating support.
Use above structure, make claw and locating support lean by the second spring, thus raw material bag can be avoided from fixed Position post slides out, good antiskid effect.
Described locating dowel upper end has introduction part.
Using above structure, can be facilitated by introduction part and penetrate in locating dowel by raw material bag edge, guide effect is good.
Described locating dowel lower end is arranged with rubber ring.
Use above structure, its frictional force can be increased by rubber ring, rational in infrastructure.
Being additionally provided with some rollers on described locating support, roller and can drive the second elevating mechanism of its oscilaltion It is connected.
Use above structure, roller can be packed up or put down by the second elevating mechanism, practical.
Described second elevating mechanism includes the first installing plate, the first push-rod electric machine, guide rail and slide block, and guide rail is vertically fixed on On locating support, slide block is arranged in guide rail, and the first push-rod electric machine is fixed on the base plate of locating support, the first push-rod electric machine Straight down, the push rod end of the first push-rod electric machine is connected push rod with slide block, and the first installing plate upper surface is connected with slide block, First installing plate lower surface is connected with roller.
When roller is packed up or put down by needs, the push rod band movable slider controlling the first push-rod electric machine moves up and down, slide block Driving the first installing plate to move up and down, the first installing plate drives roller to move up and down, thus can be packed up by roller or put down.
It is additionally provided with in described frame and the material of blending bin side-walls can be pushed to the delivery device at shaft, push Mechanism includes that some propelling movement is managed and air compressor machine, and some propelling movement pipes are vertically located on blending bin sidewall, and pushing pipe lower end is blind end, Pushing pipe upper end is inlet end, pushes pipe and is connected with air compressor machine by communicating pipe, pushes tube side part and offers some ventholes, Venthole is towards shaft.
Using above structure, deliver air to push in pipe by air compressor machine, air exports from venthole, at air-flow Effect under, the material of blending bin side-walls is pushed at shaft, can time of the most less stirring, push effective.
Described moving structure includes driving cylinder, movable plate, slide block and guide rail, and guide rail is horizontally fixed in blending bin, sliding Block is arranged in guide rail, drives the cylinder body of cylinder to be fixed in blending bin, drives the piston rod end of cylinder to be connected with slide block, moves Dynamic plate is fixed on slide block, and the second push-rod electric machine is fixed on movable plate.
When needs make the second push-rod electric machine move back and forth, control to drive the piston rod band movable slider of cylinder along guide rail Return is dynamic, and slide block drives movable plate to move back and forth, and movable plate drives the second push-rod electric machine to move back and forth, thus can make the second push rod Motor moves back and forth.
Described conveying pipe is additionally provided with flow control valve.
Use above structure, by the uninterrupted of liquid in flow control valve scalable conveying pipe, easy to adjust.
It is provided with observation port in described blending bin, at observation port, is provided with transparent access panel.
Use above structure, by access panel can rapid examination to the working condition in blending bin, it is directly perceived, convenient to observe.
Being additionally provided with passage on described suction pipe, passage upper end is connected with the feed end of suction pipe, under passage End can be resisted against bottom blending bin.
Using above structure, can conveniently transport material in suction pipe by passage, guide effect be good.
Described first elevating mechanism includes the 3rd push-rod electric machine, slide block and guide rail, and guide rail is vertically fixed in frame, slide block Being arranged in guide rail, the 3rd push-rod electric machine is fixed in frame, the push rod of the 3rd push-rod electric machine straight up, the 3rd push-rod electric machine Push rod end be connected with slide block, the second installing plate is fixed on slide block.
When needs make the second installing plate move up and down, control the push rod band movable slider of the 3rd push-rod electric machine along on guide rail Lower movement, slide block drives the second installing plate to move up and down, thus the second installing plate can be made to move up and down.
Described detent mechanism includes locating ring, locating piece and positioning cylinder, and locating ring is sheathed and is fixed on the second delivery outlet On, positioning cylinder is fixed in frame by support, and the piston rod of positioning cylinder is towards the second delivery outlet, the piston of positioning cylinder Boom end and locating piece fix, and locating piece offers the locating slot matched with locating ring.
When needing to be fixed on the second delivery outlet the edge of finished bag, the edge of finished bag is enclosed within locating ring, The piston rod controlling positioning cylinder drives locating piece to move, and locating piece and locating ring lean, thus can be by the edge of finished bag Being fixed on the second delivery outlet, location is quickly.
Described locating slot is provided with rubber strip, rubber strip has the protuberance of some protrusions.
Use above structure, its frictional force can be increased by rubber strip, it is to avoid the phenomenon slided, job stability occur Good.
Being additionally provided with prompting mechanism in described frame, prompting mechanism includes that travel switch, detection bar, alarm bell and PLC can compile Range controller, alarm bell is fixed in frame, and travel switch is fixed on the second installing plate lower surface, and detection bar is fixed in frame, Detection bar can contact with travel switch, and travel switch is all connected with this PLC with alarm bell.
After in finished bag, material is filled, the push rod of the 3rd push-rod electric machine drives the second installing plate to move down, the second peace Loading belt moves travel switch and moves down, and travel switch contacts with detection bar, and signal is passed to PLC programmable control by travel switch Device processed, PLC makes alarm bell send alarm sound, and prompting is directly perceived, convenient.
Described 3rd electromagnetic valve is connected with above-mentioned PLC.
Use above structure, the 3rd electromagnetic valve can be controlled by PLC and obtain electric or dead electricity.
Being fixed with some limited posts on described second jolting plate, a high position for limited post is 30 50mm.
Use above structure, can the bottom of finished bag be carried out spacing by limited post, it is to avoid finished bag is from the second vibrations Departing from plate, position-limiting action is good.
Compared with prior art, the preparation method of this nano antimony tin oxide powder has the advantage that
1, can realize it by various plant equipment in this preparation method to prepare, replace manual operation, production efficiency is high.
2, making the first jolting plate produce vibrations by the first vibration motor, the first jolting plate drives raw material bag vibrations, makes former Material in pocket moves down, and vibrations are convenient.
3, make claw and locating support lean by the second spring, raw material bag can be avoided to slide out from locating dowel, Good antiskid effect.
4, by suction pipe up and down and is moved horizontally, asepwirator pump by suction pipe by defeated for mixture everywhere in blending bin Go out in case, can realize comprehensive to sampling in blending bin, check precisely.
5, delivering air to push in pipe by air compressor machine, air exports from venthole, by blending bin side-walls Material is pushed at shaft, can time of the most less stirring, push effective.
Accompanying drawing explanation
Fig. 1 is the planar structure schematic diagram of feeding device.
Fig. 2 is the close-up schematic view in Fig. 1 at A.
Fig. 3 is the close-up schematic view in Fig. 1 at B.
Fig. 4 is the sectional view of mixing arrangement.
Fig. 5 is the close-up schematic view in Fig. 4 at C.
Fig. 6 is the sectional view of delivery device in mixing arrangement.
Fig. 7 is the planar structure schematic diagram of packing apparatus.
Fig. 8 is the close-up schematic view in Fig. 7 at D.
Fig. 9 is the perspective view that packing apparatus removes part.
In figure, 1, frame;2, the first electromagnetic valve;3, storage tank;3a, the first delivery outlet;3b, the first charging aperture;4, first Delivery pump;5, feeding tube;5a, guide portion;6, link;7, locating support;7a, base plate;8, connecting rod;9, mounting ring;10, displacement Sensor;10a, induction part;11, mounting rod;12, cylinder;13, locating dowel;13a, introduction part;14, claw;15, the second spring; 16, the first installing plate;17, the first vibration motor;18, the first jolting plate;19, the first spring;20, the first push-rod electric machine;21, lead Rail;22, slide block;23, roller;24, controller;25, blending bin;25a, powder body delivery outlet;25b, observation port;25c, powder body input Mouthful;26, stirring vane;27, the second electromagnetic valve;28, case;29, suction pipe;30, asepwirator pump;31, access panel;32, stirring Axle;33, stirring motor;34, guide rail;35, fog-spray nozzle;36, conveying pipe;37, flow control valve;38, the second delivery pump;39, storage Liquid case;40, cylinder is driven;41, slide block;42, movable plate;43, the second push-rod electric machine;44, mounting blocks;45, passage;46, even Siphunculus;47, air compressor machine;48, pipe is pushed;48a, venthole;49, PLC;50, alarm bell;51, support;52, fixed Position cylinder;53, locating piece;53a, locating slot;54, locating ring;55, the 3rd electromagnetic valve;56, material stock tank;56a, the second delivery outlet; 56b, the second input port;57, detection bar;58, the 3rd push-rod electric machine;59, guide rail;60, slide block;61, limited post;62, the second shake Dynamic plate;63, the second vibration motor;64, the second installing plate;65, the 3rd spring;66, travel switch;67, rubber strip.
Detailed description of the invention
The following is the specific embodiment of the present invention and combine accompanying drawing, technical scheme is further described, But the present invention is not limited to these embodiments.
The preparation method of this nano antimony tin oxide powder, comprises the steps of:
A, butter of tin, nitric acid antimony are dissolved in dilute hydrochloric acid, during stirring, are gradually added aqueous slkali until pH Value reaches 7-9, continues stirring, until tin ion and antimony ion precipitation are completely, obtains stannic hydroxide and antimony hydroxide predecessor;? In the present embodiment, during stirring, it is gradually added aqueous slkali until pH value reaches 8;
B, filtration separate and utilize deionized water wash stannic hydroxide and antimony hydroxide predecessor, are removed by solable matter Go, wash 2-5 time, in the present embodiment, wash 3 times;
C, predecessor after step b is washed add water and Polyethylene Glycol, is transferred to after stirring in reactor, control The temperature of reactor processed is 180-280 DEG C, successive reaction 2-4h under conditions of stirring, prepares nano pulp, at the present embodiment In, the temperature controlling reactor is 240 DEG C, successive reaction 3h under conditions of stirring;The addition of water is stannic hydroxide and hydrogen 3-6 times of stibium oxide predecessor weight;The addition of Polyethylene Glycol is the gross weight of stannic hydroxide and antimony hydroxide predecessor with water The 2-7% of amount;
D, separation after drying, prepare tin-antiomony oxide powders mixture, calcine 2-6h, then lead under conditions of 400-700 DEG C Cross jet mill to pulverize, prepare nano antimony tin oxide powder;In the present embodiment, under conditions of 550 DEG C, 4h is calcined.
Using the method, can realize it by various plant equipment and prepare, replace manual operation, production efficiency is high.
As shown in Figure 1, Figure 2, shown in Fig. 4, Fig. 5, Fig. 7, Fig. 8, the jet mill in step d includes frame 1, and frame 1 depends on Secondary being provided with feeding device, mixing arrangement, reducing mechanism and packing apparatus, reducing mechanism uses air-flow of the prior art Grinding mode;Feeding device includes feeding tube 5, storage tank 3 and for positioning the locating support 7 of raw material bag, locating support 7 and storage Batch can 3 is arranged in frame 1, and storage tank 3 lower end has the first delivery outlet 3a, is provided with the first electromagnetism in the first delivery outlet 3a Valve 2, storage tank 3 upper end has the first charging aperture 3b, the first charging aperture 3b and is connected with feeding tube 5 one end, feeding tube 5 other end It is positioned at above locating support 7, and this end has guide portion 5a, frame 1 is provided with one guide portion 5a can be driven to move up and down Travel mechanism, is additionally provided with the first delivery pump 4 in feeding tube 5;Travel mechanism includes cylinder 12 and mounting ring 9, the cylinder of cylinder 12 Body is fixed in frame 1, and the cylinder body of cylinder 12 is fixed in frame 1 by link 6;The piston rod of cylinder 12 straight down, The piston rod end of cylinder 12 is connected with mounting ring 9 by connecting rod 8, and guide portion 5a is fixed in mounting ring 9, and guide portion 5a leads to Cross bolted mode to be fixed in mounting ring 9;The controlling organization that can control cylinder 12 action it is additionally provided with in frame 1;Mixed Locking device includes that blending bin 25, fog-spray nozzle 35 and reserving liquid tank 39, blending bin 25 and reserving liquid tank 39 are each attached in frame 1, mixing Case 25 and reserving liquid tank 39 are all fixed in frame 1 by the way of welding;Blending bin 25 top has powder body input port 25c, powder Body input port 25c is connected with the first delivery outlet 3a by the first connecting tube, and blending bin 25 bottom has powder body delivery outlet 25a, Being provided with the second electromagnetic valve 27 in powder body delivery outlet 25a, fog-spray nozzle 35 is arranged in blending bin 25, the liquid outlet court of fog-spray nozzle 35 Under, the inlet of fog-spray nozzle 35 is connected with reserving liquid tank 39 by conveying pipe 36, is provided with the second delivery pump 38 in conveying pipe 36, Blending bin 25 top is additionally provided with shaft 32, and shaft 32 upper end is connected with stirring motor 33, and the upper end of shaft 32 is passed through Bonded mode is connected with the output shaft of stirring motor 33, and stirring motor 33 is fixed in blending bin 25;Shaft 32 lower end Being connected with stirring vane 26 in penetrating blending bin 25, the lower end of shaft 32 is by the way of bonded and stirring vane 26 phase Even;Being provided with in frame 1 and can draw the draw frame machine of material in blending bin 25, draw frame machine includes suction pipe the 29, second push rod Motor 43, asepwirator pump 30, mounting blocks 44 and case 28, the second push-rod electric machine 43 can drive its movement moved horizontally by one Structure is arranged in blending bin 25, the push rod of the second push-rod electric machine 43 straight down, the push rod end of the second push-rod electric machine 43 and Mounting blocks 44 fixes, and mode and mounting blocks 44 that the push rod end of the second push-rod electric machine 43 is bolted fix;Inhale The feed end taking pipe 29 is fixed on mounting blocks 44, and this feed end is down, and the discharge end of suction pipe 29 passes blending bin 25 In case 28, asepwirator pump 30 is arranged in suction pipe 29;Packing apparatus includes that material stock tank 56, material stock tank 56 are fixed on frame On 1, material stock tank 56 is fixed in frame 1 by the way of welding;Material stock tank 56 top has the second input port 56b, and second is defeated Entrance 56b is connected with powder body delivery outlet 25a by the second connecting tube, and material stock tank 56 bottom has the second delivery outlet 56a, and second Delivery outlet 56a is provided with the 3rd electromagnetic valve 55, frame 1 is provided with the detent mechanism that can be positioned at finished bag edge, machine Being additionally provided with shock structure on frame 1, shock structure includes the second jolting plate the 62, second vibration motor 63 and the second installing plate 64, Second installing plate 64 can drive its first elevating mechanism moved up and down to be arranged in frame 1 by one, and the second jolting plate 62 sets Put on the second installing plate 64, and the second jolting plate 62 is in immediately below the second delivery outlet 56a, the second jolting plate 62 and the second peace Having the 3rd spring 65 between dress plate 64, in the present embodiment, the quantity of the 3rd spring 65 is four;3rd spring 65 one end and Second jolting plate 62 lower surface is connected, and the 3rd spring 65 other end and the second installing plate 64 upper surface are connected, the second vibration motor 63 are fixed on the second jolting plate 62 lower surface, and the mode that the second vibration motor 63 is bolted is fixed on the second jolting plate 62 Lower surface.
As shown in Figure 1 and Figure 2, controlling organization includes displacement transducer 10, mounting rod 11 and controller 24, mounting rod 11 1 End is connected with mounting ring 9, and the mode that one end of mounting rod 11 is bolted is connected with mounting ring 9;Mounting rod 11 is another One end is connected with displacement transducer 10, and the mode that the other end of mounting rod 11 is bolted is connected with displacement transducer 10 Connect;And the induction part 10a of displacement transducer 10 is towards locating support 7, controller 24 is fixed in frame 1, and controller 24 passes through The mode of bolted mode is fixed in frame 1, and controller 24 uses the single-chip microcomputer can bought on market, single-chip microcomputer control The program of cylinder processed and sensor is existing, and its program need not update;Cylinder 12 and displacement transducer 10 and this control Device 24 processed is connected.
As shown in Figure 1, Figure 2, Figure 3 shows, locating support 7 upper end has the locating dowel 13 that can position raw material bag, at the present embodiment In, the quantity of locating dowel 13 is four;Locating dowel 13 upper end has introduction part 13a, uses this structure, can by introduction part 13a Conveniently penetrating in locating dowel 13 by raw material bag edge, guide effect is good;Locating dowel 13 lower end is arranged with rubber ring, uses this knot Structure, can increase its frictional force by rubber ring;Locating support 7 lower end has the percussion mechanism that can shake raw material bag, shake Motivation structure includes the first jolting plate 18 and the first vibration motor 17, and the first jolting plate 18 is arranged on the base plate 7a of locating support 7, There are between first jolting plate 18 and the base plate 7a of locating support 7 first spring 19, one end of the first spring 19 and the first vibrations Plate 18 fixes, and the other end of the first spring 19 and the base plate 7a of locating support 7 fix, and the first vibration motor 17 is fixed on One jolting plate 18 lower surface, the mode that the first vibration motor 17 is bolted is fixed on the lower surface of the first jolting plate 18.
As shown in Figure 1 and Figure 2, locating support 7 being additionally provided with anti-slipping mechanism, anti-slipping mechanism includes claw 14 and the second bullet Spring 15, claw 14 lower end and locating support 7 are hinged, and one end of the second spring 15 is connected in the middle part of claw 14, the second spring The other end of 15 is connected with locating support 7, and claw 14 upper end can be resisted against on locating support 7.
As shown in Figure 1, Figure 3, locating support 7 is additionally provided with some rollers 23, in the present embodiment, the quantity of roller 23 It it is four;Roller 23 can drive the second elevating mechanism of its oscilaltion to be connected with one, uses this structure, by the second elevator Roller 23 can be packed up or put down by structure.
As shown in Figure 1, Figure 3, the second elevating mechanism includes first installing plate the 16, first push-rod electric machine 20, guide rail 21 and slides Block 22, guide rail 21 is vertically fixed on locating support 7, and the mode that guide rail 21 is bolted is fixed on locating support 7;Sliding Block 22 is arranged in guide rail 21, and slide block 22 can move up and down along guide rail 21;First push-rod electric machine 20 is fixed on locating support 7 On base plate 7a, straight down, the push rod end of the first push-rod electric machine 20 is connected the push rod of the first push-rod electric machine 20 with slide block 22, First installing plate 16 upper surface is connected with slide block 22, and the first installing plate 16 lower surface is connected with roller 23.
As shown in Figure 6, frame 1 is additionally provided with and the material of blending bin 25 side-walls can be pushed to pushing away at shaft 32 Sending mechanism, delivery device to include some propelling movement pipes 48 and air compressor machine 47, in the present embodiment, the quantity pushing pipe 48 is 12 Root;Some propelling movement pipes 48 are vertically located on blending bin 25 sidewall, and pushing pipe 48 lower end is blind end, and pushing pipe 48 upper end is air inlet End, pushes pipe 48 and passes through to be connected with air compressor machine 47 communicating pipe 46, and air compressor machine 47 is fixed in frame 1;Push pipe 48 sidepiece to open Being provided with some venthole 48a, in the present embodiment, the quantity of venthole 48a is six;Venthole 48a is towards shaft 32.
As shown in Figure 4, Figure 5, moving structure includes driving cylinder 40, movable plate 42, slide block 41 and guide rail 34, guide rail 34 water Putting down and be fixed in blending bin 25, the mode that guide rail 34 is bolted is fixed in blending bin 25;Slide block 41 is arranged on guide rail In 34, slide block 41 can move back and forth along guide rail 34;The cylinder body driving cylinder 40 is fixed in blending bin 25, drives cylinder 40 The mode that cylinder body is bolted is fixed in blending bin 25;The piston rod end driving cylinder 40 is connected with slide block 41, drives The mode that the piston rod end of dynamic air cylinder 40 is bolted is connected with slide block 41;Movable plate 42 is fixed on slide block 41, moves The mode that dynamic plate 42 is bolted is fixed on slide block 41;Second push-rod electric machine 43 is fixed on movable plate 42, and second pushes away The mode that bar motor 43 is bolted is fixed on movable plate 42.
As shown in Figure 4, conveying pipe 36 is additionally provided with flow control valve 37;It is provided with observation port 25b in blending bin 25, sees Examining and be provided with transparent access panel 31 at the 25b of hole, access panel 31 is organic plates.
As shown in Figure 4, Figure 5, suction pipe 29 is additionally provided with passage 45, passage 45 upper end and the charging of suction pipe 29 End is connected, and passage 45 lower end can be resisted against bottom blending bin 25, uses this structure, can be facilitated material by passage 45 Being transported in suction pipe 29, guide effect is good.
As shown in Figure 7, Figure 8, the first elevating mechanism includes that the 3rd push-rod electric machine 58, slide block 60 and guide rail 59, guide rail 59 erect Directly being fixed in frame 1, the mode that guide rail 59 is bolted is fixed in frame 1;Slide block 60 is arranged in guide rail 59, sliding Block 60 can move up and down along guide rail 59;3rd push-rod electric machine 58 is fixed in frame 1, and the 3rd push-rod electric machine 58 is by bolt even The mode connect is fixed in frame 1;The push rod of the 3rd push-rod electric machine 58 straight up, the push rod end of the 3rd push-rod electric machine 58 and Slide block 60 is connected, and the mode that the push rod end of the 3rd push-rod electric machine 58 is bolted is connected with slide block 60;Second installing plate 64 are fixed on slide block 60, and the mode that the second installing plate 64 is bolted is fixed on slide block 60.
As shown in Fig. 7, Fig. 9, detent mechanism includes locating ring 54, locating piece 53 and positioning cylinder 52, and locating ring 54 is sheathed And be fixed on the second delivery outlet 56a, positioning cylinder 52 is fixed in frame 1 by support 51, the piston rod of positioning cylinder 52 Towards the second delivery outlet 56a, piston rod end and the locating piece 53 of positioning cylinder 52 fix, the tailpiece of the piston rod of positioning cylinder 52 Mode and locating piece 53 that portion is bolted fix;The locating slot matched with locating ring 54 is offered on locating piece 53 53a;In the present embodiment, the quantity of locating piece 53 and positioning cylinder 52 is two.
As it is shown in figure 9, locating slot 53a is provided with rubber strip 67, use this structure, can be increased it by rubber strip 67 and rub Wiping power, it is to avoid the phenomenon slided occurs;There is on rubber strip 67 protuberance of some protrusions, in the present embodiment, protuberance Quantity is 30.
As shown in Figure 7, Figure 8, frame 1 being additionally provided with prompting mechanism, prompting mechanism includes travel switch 66, detection bar 57, alarm bell 50 and PLC 49, alarm bell 50 is fixed in frame 1, and the mode that alarm bell 50 is bolted is fixed In frame 1;Travel switch 66 is fixed on the second installing plate 64 lower surface, and the mode that travel switch 66 is bolted is fixed Lower surface at the second installing plate 64;Detection bar 57 is fixed in frame 1, and the mode that detection bar 57 is bolted is fixed on In frame 1;Detection bar 57 can and travel switch 66 contact, travel switch 66 and alarm bell 50 all with this PLC 49 are connected, and in the present embodiment, PLC 49 uses the controller can bought on market, and controller controls row The program of Cheng Kaiguan, alarm bell and the 3rd electromagnetic valve is existing, and its program need not update;3rd electromagnetic valve 55 can with PLC Programmable controller 49 is connected, and uses this structure, can control the 3rd electromagnetic valve 55 by PLC 49 and obtains electric or lose Electricity.
As shown in Figure 7, Figure 8, the second jolting plate 62 being fixed with some limited posts 61, a high position for limited post 61 is 30 50mm, in the present embodiment, the height of limited post 61 is 40mm, uses this structure, can be to the end of finished bag by limited post 61 Portion carries out spacing, it is to avoid finished bag departs from from the second jolting plate 62, and position-limiting action is good.
The operation principle of jet mill is as follows: penetrate in locating dowel 13 by the raw material bag edge being used for depositing raw material, logical Crossing the second spring 15 makes claw 14 and locating support 7 lean, and opens the first delivery pump 4, and the first delivery pump 4 is by feeding tube 5 By in the feedstock transportation in raw material bag to storage tank 3, along with the raw material in raw material bag gradually decreases, examined by displacement transducer 10 Surveying the distance of raw material in guide portion 5a and material bag, signal passes to controller 24, controller 24 controls the piston of cylinder 12 Bar drive mounting ring 9 move down, mounting ring 9 drives guide portion 5a to move down, make guide portion 5a all the time with in raw material bag Raw material contacts;Raw material in storage tank 3, by being transported to the first communicating pipe in blending bin 25, controls the output shaft of stirring motor 33 Driving shaft 32 to rotate, shaft 32 drives stirring vane 26 to rotate, and delivers air to push pipe 48 by air compressor machine 47 In, air exports from venthole 48a, under the effect of air-flow, the material of blending bin 25 side-walls is pushed to shaft 32 Place;Meanwhile, opening the second delivery pump 38, the modifying agent in reserving liquid tank 39 is transported to spray by the second delivery pump 38 by conveying pipe 36 In mist head 35, make modifying agent and raw material uniformly mix, when it is sampled by needs, control to drive the piston rod band of cylinder 40 Movable slider 41 moves back and forth, and slide block 41 drives movable plate 42 to move back and forth, and movable plate 42 drives the second push-rod electric machine 43 to move back Dynamic;The push rod controlling the second push-rod electric machine 43 drives mounting blocks 44 to move down, and mounting blocks 44 drives suction pipe 29 to move down, Mixture everywhere in blending bin 25 can be exported in case 28 by suction pipe 29 by asepwirator pump 30, and it is comprehensive right to realize Blending bin 25 samples;Raw material in blending bin 25 by being transported to the second communicating pipe in material stock tank 56, will become after pulverizing The edge of product bag is enclosed within locating ring 54, and the piston rod controlling positioning cylinder 52 drives locating piece 53 to move, and locating piece 53 is with fixed Position ring 54 leans, and is fixed at the edge of finished bag on the second delivery outlet 56a, controls the by PLC 49 Three electromagnetic valves 55 make the second delivery outlet 56a be in open mode;Control the push rod band movable slider 60 of the 3rd push-rod electric machine 58 upwards Mobile, slide block 60 drives the second installing plate 64 to move up, and the second installing plate 64 drives the second jolting plate 62 to move up, and makes the Two jolting plates 62 contact with the bottom of finished bag, drive the second jolting plate 62 to shake by the second vibration motor 63, the second vibrations Plate 62 drives finished bag to produce vibrations, and along with in finished bag, material gradually increases, the push rod controlling the 3rd push-rod electric machine 58 drives Slide block 60 moves gradually downward, and slide block 60 drives the second installing plate 64 to move gradually downward, after material is filled in finished bag, OK Cheng Kaiguan 66 contacts with detection bar 57, and signal is passed to PLC 49, PLC PLC technology by travel switch 66 Device 49 makes alarm bell 50 send alarm sound;The mixing of raw material and other auxiliary agent can select this function according to actual needs.
Specific embodiment described herein is only explanation for example to spirit.Technical field that the present invention belongs to Described specific embodiment can be made various amendment or supplements or use similar mode to substitute by technical staff, but Without departing from invention spirit or surmount scope defined in appended claims.

Claims (10)

1. the preparation method of a nano antimony tin oxide powder, it is characterised in that comprise the steps of:
A, butter of tin, nitric acid antimony are dissolved in dilute hydrochloric acid, during stirring, are gradually added aqueous slkali until pH value reaches To 7-9, continue stirring, until tin ion and antimony ion precipitation are completely, obtain stannic hydroxide and antimony hydroxide predecessor;
B, filtration separate and utilize deionized water wash stannic hydroxide and antimony hydroxide predecessor, are removed by solable matter, wash Wash 2-5 time;
C, predecessor after step b is washed add water and Polyethylene Glycol, is transferred to after stirring in reactor, controls anti- The temperature answering still is 180-280 DEG C, successive reaction 2-4h under conditions of stirring, prepares nano pulp;
D, separation after drying, prepare tin-antiomony oxide powders mixture, calcine 2-6h, then pass through gas under conditions of 400-700 DEG C Stream pulverizer is pulverized, and prepares nano antimony tin oxide powder.
The preparation method of nano antimony tin oxide powder the most according to claim 1, it is characterised in that in described step d Jet mill includes frame, and described frame is disposed with feeding device, mixing arrangement, reducing mechanism and packing apparatus, Described feeding device includes feeding tube, storage tank and is all provided with for positioning the locating support of raw material bag, locating support and storage tank Putting in frame, storage tank lower end has the first delivery outlet, is provided with the first electromagnetic valve in the first delivery outlet, and storage tank upper end has Having the first charging aperture, the first charging aperture to be connected with feeding tube one end, the feeding tube other end is positioned at above locating support, and this end There is guide portion, frame is provided with a travel mechanism that guide portion can be driven to move up and down, feeding tube is additionally provided with first Delivery pump;Described travel mechanism includes cylinder and mounting ring, and the cylinder body of cylinder is fixed in frame, the piston rod of cylinder vertically to Under, the piston rod end of cylinder is connected with mounting ring by connecting rod, and guide portion is fixed in mounting ring, and frame is additionally provided with The controlling organization of cylinder action can be controlled;Described mixing arrangement includes blending bin, fog-spray nozzle and reserving liquid tank, blending bin and reserving liquid tank Being each attached in frame, blending bin top has powder body input port, and the first connecting tube and the first delivery outlet are passed through in powder body input port Being connected, blending bin bottom has powder body delivery outlet, is provided with the second electromagnetic valve in powder body delivery outlet, and fog-spray nozzle is arranged on mixing In case, down, the inlet of fog-spray nozzle is connected with reserving liquid tank the liquid outlet of fog-spray nozzle by conveying pipe, is provided with in conveying pipe Second delivery pump, blending bin top is additionally provided with shaft, and shaft upper end is connected with stirring motor, and shaft lower end penetrates mixed Being connected with stirring vane in mould assembling, frame is provided with and can draw the draw frame machine of material in blending bin, draw frame machine includes suction Taking pipe, the second push-rod electric machine, asepwirator pump, mounting blocks and case, the second push-rod electric machine can drive it to move horizontally by one Moving structure is arranged in blending bin, the push rod of the second push-rod electric machine straight down, the push rod end of the second push-rod electric machine and peace Dress block fixes, and the feed end of suction pipe is fixed on mounting blocks, and this feed end is down, and the discharge end of suction pipe passes mixing Case is positioned at case, and asepwirator pump is arranged in suction pipe;Described packing apparatus includes that material stock tank, material stock tank are fixed on frame On, material stock tank top has the second input port, and the second input port is connected with powder body delivery outlet by the second connecting tube, material stock tank Bottom has the second delivery outlet, is provided with the 3rd electromagnetic valve in the second delivery outlet, and frame is provided with can be fixed by finished bag edge The detent mechanism that position is lived, frame is additionally provided with shock structure, and shock structure includes the second jolting plate, the second vibration motor and the Two installing plates, the second installing plate can drive its first elevating mechanism moved up and down to be arranged in frame by one, the second vibrations Plate is arranged on the second installing plate, and the second jolting plate is in immediately below the second delivery outlet, the second jolting plate and the second installing plate Between have the 3rd spring, the 3rd spring one end and the second jolting plate lower surface be connected, the 3rd spring other end and second install Plate upper surface is connected, and the second vibration motor is fixed on the second jolting plate lower surface.
The preparation method of nano antimony tin oxide powder the most according to claim 2, it is characterised in that described controlling organization bag Including displacement transducer, mounting rod and controller, mounting rod one end is connected with mounting ring, the mounting rod other end and displacement transducer Being connected, and the induction part of displacement transducer is towards locating support, controller is fixed in frame, cylinder and displacement transducer with This controller is connected.
The preparation method of nano antimony tin oxide powder the most according to claim 3, it is characterised in that on described locating support End has the locating dowel that can position raw material bag, and locating support lower end has the percussion mechanism that can shake raw material bag, described Percussion mechanism includes the first jolting plate and the first vibration motor, and the first jolting plate is arranged on the base plate of locating support, the first shake Dynamic have the first spring between plate and the base plate of locating support, one end and first jolting plate of the first spring fix, the first bullet The other end of spring and the base plate of locating support fix, and the first vibration motor is fixed on the first jolting plate lower surface.
The preparation method of nano antimony tin oxide powder the most according to claim 4, it is characterised in that on described locating support Being additionally provided with anti-slipping mechanism, anti-slipping mechanism includes claw and the second spring, and claw lower end and locating support are hinged, the second spring One end be connected with in the middle part of claw, the other end of the second spring is connected with locating support, and claw upper end can be resisted against location On support.
The preparation method of nano antimony tin oxide powder the most according to claim 5, it is characterised in that on described locating support Being additionally provided with some rollers, roller and can drive the second elevating mechanism of its oscilaltion to be connected;Described second elevating mechanism Including the first installing plate, the first push-rod electric machine, guide rail and slide block, guide rail is vertically fixed on locating support, and slide block is arranged on leads In rail, the first push-rod electric machine is fixed on the base plate of locating support, and straight down, the first push rod is electric for the push rod of the first push-rod electric machine The push rod end of machine is connected with slide block, and the first installing plate upper surface is connected with slide block, the first installing plate lower surface and roller It is connected.
The preparation method of nano antimony tin oxide powder the most according to claim 2, it is characterised in that also set in described frame Being equipped with and the material of blending bin side-walls can be pushed to the delivery device at shaft, delivery device includes that some propelling movement is managed and empty Press, some propelling movement pipes are vertically located on blending bin sidewall, and pushing pipe lower end is blind end, and pushing pipe upper end is inlet end, pushes away Sending pipe to be connected with air compressor machine by communicating pipe, push tube side part and offer some ventholes, venthole is towards shaft.
The preparation method of nano antimony tin oxide powder the most according to claim 7, it is characterised in that described moving structure bag Including driving cylinder, movable plate, slide block and guide rail, guide rail is horizontally fixed in blending bin, and slide block is arranged in guide rail, drives cylinder Cylinder body be fixed in blending bin, drive cylinder piston rod end be connected with slide block, movable plate is fixed on slide block, and second pushes away Bar motor is fixed on movable plate.
The preparation method of nano antimony tin oxide powder the most according to claim 2, it is characterised in that described first elevator Structure includes the 3rd push-rod electric machine, slide block and guide rail, and guide rail is vertically fixed in frame, and slide block is arranged in guide rail, the 3rd push rod Motor is fixed in frame, and straight up, the push rod end of the 3rd push-rod electric machine is connected the push rod of the 3rd push-rod electric machine with slide block, Second installing plate is fixed on slide block;Described detent mechanism includes locating ring, locating piece and positioning cylinder, and locating ring is sheathed and solid Being scheduled on the second delivery outlet, positioning cylinder is fixed in frame by support, the piston rod of positioning cylinder towards the second delivery outlet, Piston rod end and the locating piece of positioning cylinder fix, and locating piece offers the locating slot matched with locating ring.
The preparation method of nano antimony tin oxide powder the most according to claim 9, it is characterised in that in described frame also Being provided with prompting mechanism, prompting mechanism includes travel switch, detection bar, alarm bell and PLC, and alarm bell is fixed on machine On frame, travel switch is fixed on the second installing plate lower surface, and detection bar is fixed in frame, and detection bar can connect with travel switch Touching, travel switch is all connected with this PLC with alarm bell;Described 3rd electromagnetic valve and above-mentioned PLC PLC technology Device is connected.
CN201610677327.1A 2016-08-16 2016-08-16 A kind of preparation method of nano antimony tin oxide powder Expired - Fee Related CN106044852B (en)

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