CN115255380B - Preparation method and preparation device of nano silver particles - Google Patents
Preparation method and preparation device of nano silver particles Download PDFInfo
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- CN115255380B CN115255380B CN202210890719.1A CN202210890719A CN115255380B CN 115255380 B CN115255380 B CN 115255380B CN 202210890719 A CN202210890719 A CN 202210890719A CN 115255380 B CN115255380 B CN 115255380B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
The invention belongs to the technical field of nano silver, in particular to a preparation method and a preparation device of nano silver particles; comprises a freeze dryer, a placing rack, a tray and a cover plate; the freeze dryer comprises a cavity, wherein a plurality of trays are arranged on two sides of the cavity, moist nano silver particles are filled in the trays, a cover plate is arranged on the top surface of the tray, and a plurality of air holes are formed in the cover plate; after the freeze dryer is started, the interior of the freeze dryer is vacuumized, cooled and frozen, the moisture of the wetted nano silver particles is frozen and then evaporated to be discharged out of the freeze dryer, water vapor is discharged out of the tray from the air holes, and air flow generated when the freeze dryer vacuumizes and opens and closes the door is blocked by the cover plate, so that the air flow in the tray is relatively static, and the probability of the nano silver particles flying along with the air flow is reduced.
Description
Technical Field
The invention belongs to the technical field of nano silver, and particularly relates to a preparation method and a preparation device of nano silver particles.
Background
Nano silver particles are particles composed of silver atoms; silver ions are released on the surfaces of the nano silver particles in a large quantity, the size of the nano silver particles is smaller than that of viruses, and the nano silver particles can directly damage cell membranes and enter various cells through the silver ions on the surfaces of the nano silver particles to cause apoptosis or necrosis of the cells, so that the nano silver particles have a remarkable sterilization effect.
One chinese patent with publication No. CN110026569B discloses a method for preparing nano silver particles, which comprises the following steps: mixing a dispersing agent solution containing ethylcellulose as a dispersing agent and a solution containing silver ions, adjusting the pH value of the solution, controlling the reaction temperature under the condition of ultrasonic stirring, dripping a reducing agent to reduce and precipitate nano silver particles, and then subjecting the nano silver to solid-liquid separation, washing and freeze drying. According to the method, a small amount of ethyl cellulose is used as a dispersing agent to coat the surfaces of silver particles, and the ethyl cellulose is used as an adhesive and a film forming agent in the application of electronic paste and conductive ink, so that the dispersion and stability of nano silver are ensured, the problems of demulsification and separation difficulty of a solvent and silver powder in the prior art (such as a microemulsion method) are solved, the process is simplified, the cost is reduced, and the performance of the silver powder is improved. The obtained nano silver has average granularity of 60-300nm, can be redispersed in various oily solvents, and has solid content of 40%.
After the nano silver particles are prepared, the nano silver particles are required to be sent into a freeze dryer for drying treatment, and the freeze dryer can generate air flow when vacuuming and opening and closing a door.
Therefore, the invention provides a preparation method and a preparation device of nano silver particles.
Disclosure of Invention
In order to overcome the deficiencies of the prior art, at least one technical problem presented in the background art is solved.
The technical scheme adopted for solving the technical problems is as follows: the invention relates to a preparation method of nano silver particles, which comprises the following steps:
s1: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, regulating the pH value to be neutral or alkaline, and heating to 80 ℃ for constant-temperature stirring;
s2: adding crown ether under the state of constant temperature stirring, and then adding sodium borohydride under the state of constant temperature stirring to obtain a nano silver particle mixed solution;
s3: carrying out solid-liquid separation and washing on the nano silver particle mixed solution to obtain wet nano silver particles;
s4: and drying the wet nano silver particles by using a freeze dryer to obtain the dried nano silver particles.
Preferably, the drying treatment method includes the steps of:
s1: placing the wet nano silver particles into the tray, and covering the tray with a cover plate;
s2: uniformly discharging the trays to two sides of the placing frame, pushing the placing frame into the freeze dryer, and closing a sealing door of the freeze dryer;
s3: and starting the freeze dryer to carry out vacuumizing, cooling and freezing, and evaporating and discharging the frozen moisture of the wetted nano silver particles out of the freeze dryer to finish the drying treatment of the nano silver particles.
The preparation device of the nano silver particles is suitable for the preparation method of the nano silver particles, and comprises a freeze dryer, a placing rack, a tray and a cover plate; the freeze dryer comprises a cavity, wherein a plurality of trays are arranged on two sides of the cavity, moist nano silver particles are filled in the trays, a cover plate is arranged on the top surface of the tray, and a plurality of air holes are formed in the cover plate; during operation, put into the inside of tray with moist nano silver particle, cover the apron again, evenly put the both sides of rack with the tray, push the inside of freeze-dryer into the rack, and close the sealing door of freeze-dryer, after the freeze-dryer starts, to the inside evacuation and the cooling freezing of freeze-dryer, evaporation discharge freeze-dryer behind the frozen moisture of moist nano silver particle, steam is discharged the tray from the gas pocket, the air current that produces when the freeze-dryer carries out evacuation and switch door is stopped by the apron, make the air current in the tray static relatively, thereby reduced nano silver particle along with the probability that the air current flies upward.
Preferably, a frame plate is placed in the tray, a baffle is fixedly connected to the bottom surface of the frame plate, and the baffle stretches into nano silver particles in the tray; the frame plate in the embodiment is flat and provided with a plurality of square holes; the shape of the partition plate in the embodiment is the same as that of the frame plate, and the thickness of the partition plate is larger than that of the frame plate; when the device works, after the moist nano silver particles are placed in the tray, the frame plate is placed in the tray, so that the partition plates divide the nano silver particles into a plurality of small blocks, the flying probability of the nano silver particles is further reduced, and meanwhile, the hardening probability of the nano silver particles is reduced; the top surface of the outer ring of the tray is provided with a ring groove, the outer ring of the bottom surface of the cover plate is fixedly connected with a ring plate, the outer wall of the ring plate is in sliding fit with the inner wall of the ring groove, the bottom surface of the ring groove and the bottom surface of the ring plate are fixedly connected with a plurality of magnets, and the magnets on the two surfaces are attracted mutually; when the top surface of tray is placed to the during operation with the apron, the inside of annular is slided to the annular for the mutual actuation of magnet on two sides is fixed the top surface of tray with the apron, through the mutual appeal of magnet, has improved the fixed strength between apron and the tray, is convenient for the staff to take off the apron simultaneously.
Preferably, a cylinder is arranged on the inner thread of the air hole, a plurality of sliding grooves are formed in the inner wall of the cylinder in a surrounding mode, an inner cavity is formed in the bottom of the sliding groove, a bag body is fixedly connected to the inner bottom surface of the inner cavity, clear water is filled in the bag body, a double-head sliding rod is slidably arranged at the top of the inner cavity, the double-head sliding rod penetrates through the bottom wall of the sliding groove in a sliding mode, an arc-shaped connecting plate is slidably arranged in the sliding groove, top covers are fixedly connected to the top ends of the arc-shaped connecting plates, and the bottom surface of the top cover is in sliding fit with the top surface of the cylinder; in the embodiment, the two ends of the double-end sliding rod are round baffle plates, and the middle part is rod-shaped; when the freezing dryer is in operation, when the inside of the freezing dryer is cooled and frozen, clear water in the inner part of the bag body is gradually frozen, the volume of the frozen clear water is increased, the volume of the bag body is increased, the bag body is expanded upwards due to the blocking of the side wall of the inner cavity, the double-headed slide rod is pushed to slide into the inside of the slide groove, the arc-shaped connecting plate is pushed to slide upwards along the slide groove, the top cover is pushed to be separated from the top surface of the barrel body, and water vapor in the tray is discharged out of the tray; when the inside of the freeze dryer is not cooled and frozen and the tray is positioned outside the freeze dryer, the clear water in the bag body is in a liquid state, at the moment, the top cover is attached to the top surface of the barrel body, external dust and the like are prevented from entering the inside of the tray, and the purity degree of the nano silver particles is improved.
Preferably, a hollow sealing ring is inlaid on the outer ring of the bottom surface of the top cover, the outer wall of the hollow sealing ring is in sliding fit with the top surface of the cylinder body, and a plurality of through holes are formed in the inner ring of the hollow sealing ring; when the device is in operation, after the inside cooling and freeze drying of the freeze dryer are completed, the inside temperature of the freeze dryer is gradually increased and restored, so that ice in the bag body is gradually thawed, the top cover slides downwards, the hollow sealing ring extrudes the top surface of the barrel, gas in the hollow sealing ring is discharged from the through hole, slight air flow downwards passes through the barrel, and nano silver particles adhered to the inner wall of the barrel are brought back to the inside of the tray, so that the loss of the nano silver particles is further reduced.
Preferably, a plurality of grooves are formed in the top surfaces of the flat plates on the two sides of the placing frame, a plurality of inlaid strips are fixedly connected to the bottom surface of the tray, a plurality of ball grooves are formed in the bottom surface of each groove, balls are arranged in the ball grooves in a rolling mode, and the outer walls of the balls are in sliding fit with the bottom surfaces of the inlaid strips; during operation, when putting the tray to the both sides of rack evenly, the panel card is gone into the inside of recess for the top surface of ball is contacted to the bottom surface of panel, pushes the tray into the both sides of rack, has reduced the frictional force between bottom surface and the rack of tray through the ball, through the cooperation of panel and recess, has reduced the tray and has taken place the probability of rocking, has improved the stability when the tray removes.
Preferably, the outer wall of the ball is provided with dents, the inner wall of the ball groove is embedded with a plurality of graphite blocks, and the outer wall of the graphite blocks is in sliding fit with the outer wall of the ball; during operation, when the ball rolls in the ball groove, the dent on the outer wall of the ball scratches the graphite block, so that graphite powder of the graphite block is stained on the surface of the ball, the lubrication degree of the surface of the ball is improved, and the stability of the tray during movement is further improved.
Preferably, both sides of the middle vertical plate of the placing rack are provided with fixing holes, the side surface of the tray is fixedly connected with a fixing rod, the outer wall of the fixing rod is in sliding fit with the inner wall of the fixing hole, and the outer ring of the fixing rod is sleeved with an elastic ring; when the tray pushes into the both sides of rack during operation, promote the inside of dead lever slip fixed orifices, through the slip of elastic ring and fixed orifices inner wall for the dead lever is fixed in the inside of fixed orifices, has improved the fixed firm degree of tray.
The beneficial effects of the invention are as follows:
1. according to the preparation method and the preparation device of the nano silver particles, a freeze dryer, a placing rack, a tray and a cover plate are arranged; after the freeze dryer is started, the interior of the freeze dryer is vacuumized, cooled and frozen, the moisture of the wetted nano silver particles is frozen and then evaporated to be discharged out of the freeze dryer, water vapor is discharged out of the tray from the air holes, and air flow generated when the freeze dryer vacuumizes and opens and closes the door is blocked by the cover plate, so that the air flow in the tray is relatively static, and the probability of the nano silver particles flying along with the air flow is reduced.
2. The invention relates to a preparation method and a preparation device of nano silver particles, wherein a cylinder body, a bag body, a double-head slide bar, an arc-shaped connecting plate and a top cover are arranged; when the inside of the freeze dryer is cooled and frozen, the clear water in the bag body is gradually frozen, the volume of the frozen clear water is increased, the volume of the bag body is increased, the bag body is expanded upwards due to the blocking of the side wall of the inner cavity, the double-head slide rod is pushed to slide into the chute, the arc-shaped connecting plate is pushed to slide upwards along the chute, the top cover is pushed to be separated from the top surface of the barrel, and water vapor in the tray is discharged out of the tray; when the inside of the freeze dryer is not cooled and frozen and the tray is positioned outside the freeze dryer, the clear water in the bag body is in a liquid state, at the moment, the top cover is attached to the top surface of the barrel body, external dust and the like are prevented from entering the inside of the tray, and the purity degree of the nano silver particles is improved.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a perspective view of a first embodiment of the present invention;
FIG. 2 is a front view of a first embodiment of the invention;
FIG. 3 is an enlarged view of a portion of FIG. 2 at A;
FIG. 4 is an enlarged view of a portion of FIG. 3 at B;
FIG. 5 is an enlarged view of a portion of FIG. 3 at C;
FIG. 6 is a cross-sectional view of a second elastomeric ring in accordance with an embodiment of the invention;
FIG. 7 is a flow chart of a method of making the present invention;
FIG. 8 is a flow chart of a drying process of the present invention;
in the figure: 1. a freeze dryer; 2. a placing rack; 3. a tray; 4. a cover plate; 5. air holes; 6. a frame plate; 7. a partition plate; 8. a ring groove; 9. a ring plate; 10. a magnet; 11. a cylinder; 12. a chute; 13. an inner cavity; 14. a bladder; 15. a double-headed slide bar; 16. an arc-shaped connecting plate; 17. a top cover; 18. a hollow seal ring; 19. a through hole; 20. a groove; 21. a panel; 22. a ball groove; 23. a ball; 24. a dent; 25. a graphite block; 26. a fixing hole; 27. a fixed rod; 28. an elastic ring; 29. a water cavity.
Detailed Description
The invention is further described in connection with the following detailed description in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
As shown in fig. 7, the preparation method of the nano silver particles according to the embodiment of the invention comprises the following steps:
s1: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, regulating the pH value to be neutral or alkaline, and heating to 80 ℃ for constant-temperature stirring;
s2: adding crown ether under the state of constant temperature stirring, and then adding sodium borohydride under the state of constant temperature stirring to obtain a nano silver particle mixed solution;
s3: carrying out solid-liquid separation and washing on the nano silver particle mixed solution to obtain wet nano silver particles;
s4: the wet nano silver particles were dried by a freeze dryer 1 to obtain dried nano silver particles.
As shown in fig. 8, the drying treatment method includes the steps of:
s1: placing the wetted nano silver particles into the tray 3 and covering the cover plate 4;
s2: uniformly discharging the trays 3 to both sides of the rack 2, pushing the rack 2 into the interior of the freeze dryer 1, and closing the sealing door of the freeze dryer 1;
s3: and starting the freeze dryer 1 to carry out vacuumizing, cooling and freezing, and evaporating and discharging the moisture of the wetted nano silver particles out of the freeze dryer 1 after freezing, so as to finish the drying treatment of the nano silver particles.
As shown in fig. 1 to 3, a nano-silver particle preparing apparatus, which is suitable for the above-mentioned one nano-silver particle preparing method, comprises a freeze dryer 1, a rack 2, a tray 3 and a cover plate 4; a placing frame 2 is slidably arranged in the cavity of the freeze dryer 1, a plurality of trays 3 are placed on two sides of the placing frame 2, moist nano silver particles are filled in the trays 3, a cover plate 4 is arranged on the top surface of the trays 3, and a plurality of air holes 5 are formed in the cover plate 4; during operation, placing moist nano silver particles into the tray 3, covering the cover plate 4 again, evenly placing the tray 3 on two sides of the placing frame 2, pushing the placing frame 2 into the interior of the freeze dryer 1, closing the sealing door of the freeze dryer 1, vacuumizing and cooling the interior of the freeze dryer 1 after the freeze dryer 1 is started, evaporating moisture of the moist nano silver particles and discharging the moisture out of the freeze dryer 1 after freezing, discharging water vapor out of the tray 3 from the air hole 5, and blocking air flow generated when the freeze dryer 1 performs vacuumizing and opening and closing the door by the cover plate 4, so that the air flow in the tray 3 is relatively static, and the probability of flying nano silver particles along with the air flow is reduced.
As shown in fig. 3, a frame plate 6 is placed in the tray 3, a partition plate 7 is fixedly connected to the bottom surface of the frame plate 6, and the partition plate 7 extends into nano silver particles in the tray 3; the frame plate 6 in the embodiment is flat plate-shaped and is provided with a plurality of square holes; the shape of the partition 7 in the present embodiment is the same as that of the frame plate 6, and the thickness of the partition 7 is larger than that of the frame plate 6; when the device works, after the moist nano silver particles are placed in the tray 3, the frame plate 6 is placed in the tray 3, so that the partition plate 7 divides the nano silver particles into a plurality of small blocks, the flying probability of the nano silver particles is further reduced, and meanwhile, the hardening probability among the nano silver particles is reduced.
As shown in fig. 3, the top surface of the outer ring of the tray 3 is provided with a ring groove 8, the outer ring of the bottom surface of the cover plate 4 is fixedly connected with a ring plate 9, the outer wall of the ring plate 9 is in sliding fit with the inner wall of the ring groove 8, the bottom surface of the ring groove 8 and the bottom surface of the ring plate 9 are fixedly connected with a plurality of magnets 10, and the magnets 10 on the two sides are attracted mutually; when the work, place the apron 4 to the top surface of tray 3, annular plate 9 slides into the inside of annular 8 for magnet 10 on both sides is mutually attracted, is fixed the apron 4 to the top surface of tray 3, through the mutual appeal of magnet 10, has improved the fixed strength between apron 4 and the tray 3, is convenient for the staff to take off apron 4 simultaneously.
As shown in fig. 4, the air hole 5 is internally threaded with a cylinder 11, the inner wall of the cylinder 11 is circumferentially provided with a plurality of sliding grooves 12, the bottom of the sliding groove 12 is provided with an inner cavity 13, the inner bottom surface of the inner cavity 13 is fixedly connected with a bag body 14, clear water is filled in the bag body 14, the top of the inner cavity 13 is slidably provided with a double-headed slide bar 15, the double-headed slide bar 15 slidably penetrates through the bottom wall of the sliding groove 12, the inside of the sliding groove 12 is slidably provided with an arc-shaped connecting plate 16, the top ends of the arc-shaped connecting plates 16 are fixedly connected with a top cover 17, and the bottom surface of the top cover 17 is slidably matched with the top surface of the cylinder 11; the two ends of the double-end slide bar 15 in the embodiment are circular baffles, and the middle part is rod-shaped; when the freezing dryer is in operation, when the inside of the freeze dryer 1 is cooled and frozen, clear water in the bag body 14 is gradually frozen, the volume of the frozen clear water is increased, the volume of the bag body 14 is increased, the bag body 14 is expanded upwards due to the blocking of the side wall of the inner cavity 13, the double-headed slide rod 15 is pushed to slide into the chute 12, the arc-shaped connecting plate 16 is pushed to slide upwards along the chute 12, the top cover 17 is pushed to be separated from the top surface of the barrel 11, and water vapor in the tray 3 is discharged out of the tray 3; when the inside of the freeze dryer 1 is not cooled and frozen and the tray 3 is positioned outside the freeze dryer 1, clear water in the bag body 14 is in a liquid state, at the moment, the top cover 17 is attached to the top surface of the cylinder 11, and external dust and the like are prevented from entering the inside of the tray 3, so that the purity degree of the nano silver particles is improved.
As shown in fig. 4, a hollow sealing ring 18 is inlaid on the outer ring of the bottom surface of the top cover 17, the outer wall of the hollow sealing ring 18 is in sliding fit with the top surface of the cylinder 11, and a plurality of through holes 19 are formed in the inner ring of the hollow sealing ring 18; when the freezing dryer is in operation, after the inside of the freezing dryer 1 is cooled and frozen and dried, the inside temperature of the freezing dryer 1 is gradually increased and restored, so that ice in the bag body 14 is gradually thawed, the top cover 17 slides downwards, the hollow sealing ring 18 presses the top surface of the cylinder body 11, gas in the hollow sealing ring 18 is discharged from the through hole 19, slight air flow downwards passes through the cylinder body 11, and nano silver particles adhered to the inner wall of the cylinder body 11 are brought back into the tray 3, so that the loss of the nano silver particles is further reduced.
As shown in fig. 3 and 5, the top surfaces of the flat plates on both sides of the placement frame 2 are provided with a plurality of grooves 20, the bottom surface of the tray 3 is fixedly connected with a plurality of inlaid strips 21, the bottom surface of the groove 20 is provided with a plurality of ball grooves 22, balls 23 are arranged in the ball grooves 22 in a rolling manner, and the outer walls of the balls 23 are in sliding fit with the bottom surfaces of the inlaid strips 21; when the tray 3 is uniformly placed on two sides of the placing frame 2 in operation, the inlaid strip 21 is clamped into the groove 20, so that the bottom surface of the inlaid strip 21 contacts the top surface of the ball 23, the tray 3 is pushed into two sides of the placing frame 2, friction between the bottom surface of the tray 3 and the placing frame 2 is reduced through the ball 23, the shaking probability of the tray 3 is reduced through the cooperation of the inlaid strip 21 and the groove 20, and the stability of the tray 3 in moving is improved; an indent 24 is formed on the outer wall of the ball 23, a plurality of graphite blocks 25 are inlaid on the inner wall of the ball groove 22, and the outer wall of the graphite blocks 25 is in sliding fit with the outer wall of the ball 23; during operation, when the ball 23 rolls in the ball groove 22, the dent 24 on the outer wall of the ball 23 scratches the graphite block 25, so that graphite powder of the graphite block 25 is adhered to the surface of the ball 23, the lubrication degree of the surface of the ball 23 is improved, and the stability of the tray 3 during movement is further improved.
As shown in fig. 3, both sides of the middle vertical plate of the placement frame 2 are provided with fixing holes 26, the side surface of the tray 3 is fixedly connected with a fixing rod 27, the outer wall of the fixing rod 27 is in sliding fit with the inner wall of the fixing hole 26, and an elastic ring 28 is sleeved on the outer ring of the fixing rod 27; when the tray 3 is pushed into the two sides of the rack 2 during operation, the fixing rod 27 is pushed to slide into the fixing hole 26, and the fixing rod 27 is fixed in the fixing hole 26 through the sliding of the elastic ring 28 and the inner wall of the fixing hole 26, so that the fixing firmness of the tray 3 is improved.
Example two
As shown in fig. 6, in comparative example one, another embodiment of the present invention is: a plurality of water cavities 29 are formed in the elastic ring 28, clear water is filled in the water cavities 29, and the outer wall of the elastic ring 28 is in sliding fit with the inner wall of the fixing hole 26; when the fixing rod 27 slides into the fixing hole 26 during operation, fresh water in the water cavity 29 is frozen and expanded during cooling and freeze drying of the inside of the freeze dryer 1, the volume of the elastic ring 28 is increased, the fastening degree of the fixing rod 27 and the fixing hole 26 is improved, and the fixing firmness degree of the tray 3 is further improved.
When in operation, the device comprises: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, regulating the pH value to be neutral or alkaline, and heating to 80 ℃ for constant-temperature stirring; adding crown ether under the state of constant temperature stirring, and then adding sodium borohydride under the state of constant temperature stirring to obtain a nano silver particle mixed solution; carrying out solid-liquid separation and washing on the nano silver particle mixed solution to obtain wet nano silver particles;
placing the moist nano silver particles into the tray 3, placing the frame plate 6 into the tray 3, dividing the nano silver particles into a plurality of small blocks by the partition plate 7, sliding the ring plate 9 into the ring groove 8 when the cover plate 4 is placed on the top surface of the tray 3, enabling the magnets 10 on the two sides to attract each other, fixing the cover plate 4 on the top surface of the tray 3, and improving the fixing strength between the cover plate 4 and the tray 3 through the attraction of the magnets 10; at this time, the clean water in the bag body 14 is in a liquid state, the top cover 17 is attached to the top surface of the cylinder 11 under the action of the gravity of the top cover and the gravity of the arc-shaped connecting plate 16, the cylinder 11 is sealed, external dust and the like are prevented from entering the tray 3, and the purity degree of the nano silver particles is improved;
when the tray 3 is uniformly placed on two sides of the placing frame 2, the inlaid strip 21 is clamped into the groove 20, so that the bottom surface of the inlaid strip 21 contacts the top surface of the ball 23, the tray 3 is pushed into two sides of the placing frame 2, friction force between the bottom surface of the tray 3 and the placing frame 2 is reduced through the ball 23, when the ball 23 rolls in the ball groove 22, the dent 24 on the outer wall of the ball 23 scratches the graphite block 25, graphite powder of the graphite block 25 is adhered to the surface of the ball 23, and the lubrication degree of the surface of the ball 23 is improved; by matching the inlaid strip 21 with the groove 20, the probability of shaking the tray 3 is reduced; when the tray 3 is pushed into the two sides of the placing frame 2, the fixing rod 27 is pushed to slide into the fixing hole 26, and the fixing rod 27 is fixed in the fixing hole 26 through the sliding of the elastic ring 28 and the inner wall of the fixing hole 26, so that the fixing firmness of the tray 3 is improved;
after the tray 3 is placed and fixed, the placing rack 2 is pushed into the interior of the freeze dryer 1, the sealing door of the freeze dryer 1 is closed, after the freeze dryer 1 is started, the interior of the freeze dryer 1 is vacuumized, cooled and frozen, so that clear water in the bag body 14 is gradually frozen, the volume of the bag body 14 is increased after the clear water is frozen, the bag body 14 is expanded upwards due to the blocking of the side wall of the inner cavity 13, the double-headed slide bar 15 is pushed to slide into the chute 12, the arc-shaped connecting plate 16 is pushed to slide upwards along the chute 12, the top cover 17 is pushed to be separated from the top surface of the barrel 11, and water vapor in the tray 3 is discharged out of the tray 3; the air flow generated when the freeze dryer 1 vacuumizes and opens and closes the door is blocked by the cover plate 4, so that the air flow in the tray 3 is relatively static, and the probability of the nano silver particles flying along with the air flow is reduced.
The front, rear, left, right, up and down are all based on fig. 1 in the drawings of the specification, the face of the device facing the observer is defined as front, the left side of the observer is defined as left, and so on, according to the viewing angle of the person.
In the description of the present invention, it should be understood that the terms "center," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the present invention and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the scope of the present invention.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation method of nano silver particles is characterized in that: the preparation method comprises the following steps:
s1: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, regulating the pH value to be neutral or alkaline, and heating to 80 ℃ for constant-temperature stirring;
s2: adding crown ether under the state of constant temperature stirring, and then adding sodium borohydride under the state of constant temperature stirring to obtain a nano silver particle mixed solution;
s3: carrying out solid-liquid separation and washing on the nano silver particle mixed solution to obtain wet nano silver particles;
s4: drying the wet nano silver particles by using a freeze dryer (1) to obtain dried nano silver particles;
the freeze dryer is characterized in that a placing rack (2) is slidably arranged in a cavity of the freeze dryer (1), a plurality of trays (3) are placed on two sides of the placing rack (2), moist nano silver particles are filled in the trays (3), a cover plate (4) is arranged on the top surface of the trays (3), and a plurality of air holes (5) are formed in the cover plate (4);
the top surface of the outer ring of the tray (3) is provided with a ring groove (8), the outer ring of the bottom surface of the cover plate (4) is fixedly connected with a ring plate (9), the outer wall of the ring plate (9) is in sliding fit with the inner wall of the ring groove (8), the bottom surface of the ring groove (8) and the bottom surface of the ring plate (9) are fixedly connected with a plurality of magnets (10), and the magnets (10) on the two sides are attracted mutually;
the novel air conditioner is characterized in that a cylinder body (11) is arranged on the inner thread of the air hole (5), a plurality of sliding grooves (12) are formed in the inner wall of the cylinder body (11) in a surrounding mode, an inner cavity (13) is formed in the bottom of the sliding groove (12), a bag body (14) is fixedly connected to the inner bottom surface of the inner cavity (13), clear water is filled in the inner portion of the bag body (14), a double-head sliding rod (15) is slidably arranged at the top of the inner cavity (13), the double-head sliding rod (15) slidably penetrates through the bottom wall of the sliding groove (12), an arc-shaped connecting plate (16) is slidably arranged in the sliding groove (12), a top cover (17) is fixedly connected to the top ends of the arc-shaped connecting plates (16), and the bottom surface of the top cover (17) is slidably matched with the top surface of the cylinder body (11).
The novel sealing device is characterized in that a hollow sealing ring (18) is inlaid on the outer ring of the bottom surface of the top cover (17), the outer wall of the hollow sealing ring (18) is in sliding fit with the top surface of the cylinder body (11), and a plurality of through holes (19) are formed in the inner ring of the hollow sealing ring (18).
2. The method for preparing nano silver particles according to claim 1, wherein: the drying treatment method comprises the following steps:
s1: placing the wet nano silver particles into the tray (3) and covering the cover plate (4);
s2: uniformly discharging the trays (3) to two sides of the placing frame (2), pushing the placing frame (2) into the freeze dryer (1), and closing a sealing door of the freeze dryer (1);
s3: and starting the freeze dryer (1) to carry out vacuumizing, cooling and freezing, and evaporating and discharging the moisture of the wetted nano silver particles out of the freeze dryer (1) after freezing, so as to finish the drying treatment of the nano silver particles.
3. The method for preparing nano silver particles according to claim 1, wherein: the tray is characterized in that a frame plate (6) is placed in the tray (3), a partition plate (7) is fixedly connected to the bottom surface of the frame plate (6), and the partition plate (7) stretches into nano silver particles in the tray (3).
4. The method for preparing nano silver particles according to claim 1, wherein: the utility model discloses a rack, including rack (2), recess (20) have been seted up to dull and stereotyped top surface in both sides of rack (2), the bottom surface rigid coupling of tray (3) has a plurality of panel (21), a plurality of ball grooves (22) have been seted up to the bottom surface of recess (20), ball (23) are installed in the inside roll of ball groove (22), the outer wall of ball (23) and the bottom surface sliding fit of panel (21), dent (24) have been seted up to the outer wall of ball (23), a plurality of graphite blocks (25) have been inlayed to the inner wall of ball groove (22), the outer wall of graphite block (25) and the outer wall sliding fit of ball (23).
5. The method for preparing nano silver particles according to claim 1, wherein: fixing holes (26) are formed in two sides of the middle vertical plate of the placement frame (2), fixing rods (27) are fixedly connected to the side faces of the tray (3), the outer walls of the fixing rods (27) are in sliding fit with the inner walls of the fixing holes (26), and elastic rings (28) are sleeved on the outer rings of the fixing rods (27).
6. The method for preparing nano silver particles according to claim 5, wherein: a plurality of water cavities (29) are formed in the elastic ring (28), clear water is filled in the water cavities (29), and the outer wall of the elastic ring (28) is in sliding fit with the inner wall of the fixing hole (26).
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| CN202210890719.1A CN115255380B (en) | 2022-07-28 | 2022-07-28 | Preparation method and preparation device of nano silver particles |
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| CN202210890719.1A CN115255380B (en) | 2022-07-28 | 2022-07-28 | Preparation method and preparation device of nano silver particles |
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| WO2005092286A2 (en) * | 2004-03-29 | 2005-10-06 | The University Of Houston System | Metallic nano-particles and discrete polymer-coated nano-particles |
| JP4679284B2 (en) * | 2005-07-25 | 2011-04-27 | 独立行政法人理化学研究所 | Method for producing support-metal nanoparticle composite, method for producing metal nanoparticle fusion, and method for adjusting the surface area of metal nanoparticle fusion |
| DE102006010953A1 (en) * | 2006-03-03 | 2007-09-06 | Takata-Petri Ag | Airbag module for a motor vehicle |
| DE102007034084B3 (en) * | 2007-07-21 | 2008-09-04 | Motus Engineering Gmbh & Co. Kg | Device for charging and discharging an adjusting plate of a freeze drying installation comprises a sliding element having a loading element and a removal slide |
| CN102489717B (en) * | 2011-12-22 | 2013-09-04 | 云南云天化股份有限公司 | Preparation method of nanometer silver particles |
| JP6303710B2 (en) * | 2014-03-28 | 2018-04-04 | 三菱マテリアル株式会社 | Method for producing negative electrode active material for lithium ion secondary battery |
| CN206131702U (en) * | 2016-08-31 | 2017-04-26 | 大连豪翔生物酶工程有限公司 | Anti -pollution device of freeze drying dish |
| CN207634511U (en) * | 2017-12-08 | 2018-07-20 | 江苏光扬轴承有限公司 | A kind of thrust ball bearing of enhancing lubrication |
| CN209840538U (en) * | 2019-04-12 | 2019-12-24 | 上海康亨园蜂业有限公司 | Freeze dryer based on two racks |
| CN110026569B (en) * | 2019-04-30 | 2022-04-15 | 长沙新材料产业研究院有限公司 | Preparation method of nano-silver |
| CN211625874U (en) * | 2019-12-20 | 2020-10-02 | 武汉迈特维尔医学科技有限公司 | Vacuum freeze dryer |
| CN211859455U (en) * | 2020-02-07 | 2020-11-03 | 陈萍萍 | Cable testing bridge that facilitates use |
| CN112414045A (en) * | 2020-11-26 | 2021-02-26 | 李前华 | Drying device is used in intelligent tea processing |
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| CN215490624U (en) * | 2021-02-05 | 2022-01-11 | 青岛富勒姆科技有限公司 | Vacuum freeze drier |
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| CN114082443A (en) * | 2021-11-10 | 2022-02-25 | 浙江理工大学 | Preparation method and application of magnetic nano short fiber loaded with silver nanoparticles |
| CN114632340B (en) * | 2022-04-22 | 2024-03-26 | 河北维果生物科技有限公司 | Spray type lactic acid bacteria solution drying device |
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