CN115255380A - Preparation method and preparation device of nano-silver particles - Google Patents

Preparation method and preparation device of nano-silver particles Download PDF

Info

Publication number
CN115255380A
CN115255380A CN202210890719.1A CN202210890719A CN115255380A CN 115255380 A CN115255380 A CN 115255380A CN 202210890719 A CN202210890719 A CN 202210890719A CN 115255380 A CN115255380 A CN 115255380A
Authority
CN
China
Prior art keywords
tray
silver particles
nano
wall
nano silver
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202210890719.1A
Other languages
Chinese (zh)
Other versions
CN115255380B (en
Inventor
周江聪
朱茂兰
应宗波
张恒星
丘寿达
游俊雄
陈芬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujian Zijin Precious Metal Material Co ltd
Xiamen University of Technology
Longyan University
Original Assignee
Fujian Zijin Precious Metal Material Co ltd
Xiamen University of Technology
Longyan University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fujian Zijin Precious Metal Material Co ltd, Xiamen University of Technology, Longyan University filed Critical Fujian Zijin Precious Metal Material Co ltd
Priority to CN202210890719.1A priority Critical patent/CN115255380B/en
Publication of CN115255380A publication Critical patent/CN115255380A/en
Application granted granted Critical
Publication of CN115255380B publication Critical patent/CN115255380B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Drying Of Solid Materials (AREA)
  • Medical Preparation Storing Or Oral Administration Devices (AREA)

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; a placing frame is slidably mounted inside a cavity of the freeze dryer, a plurality of trays are placed on two sides of the placing frame, wet nano-silver particles are filled inside the trays, a cover plate is arranged on the top surface of each tray, and a plurality of air holes are formed in the cover plate; after the freeze drier starts, to the inside evacuation of freeze drier and cooling freezing, the freeze drier of evaporation discharge after the moisture of moist nano-silver granule freezes, steam is followed the gas pocket discharge tray, and the air current that produces is blockked by the apron when the freeze drier carries out evacuation and switch door for the air current in the tray is static relatively, thereby has reduced the probability that nano-silver granule flies upward along with the air current.

Description

Preparation method and preparation device of nano-silver particles
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
The nano silver particles are particles composed of silver atoms; the 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, 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, apoptosis or necrosis of the cells is caused, and the sterilizing effect is remarkable.
A chinese patent publication No. CN110026569B discloses a method for preparing nano silver particles, comprising the following steps: mixing a dispersant solution containing ethyl cellulose as a dispersant and a solution containing silver ions, adjusting the pH value of the solution, controlling the reaction temperature under the condition of ultrasonic stirring, dropping a reducing agent to reduce and precipitate nano silver particles, and then carrying out solid-liquid separation, washing and freeze drying on the nano silver. According to the method, a small amount of ethyl cellulose is used as a dispersing agent to be coated on the surface of the silver particles, and the ethyl cellulose is used as an adhesive and a film-forming agent in the application of the electronic paste and the conductive ink, so that the dispersion and the stability of the nano silver are ensured, the problem that the solvent and the silver powder are difficult to demulsify and separate in the prior art (such as a microemulsion method) is solved, the process is simplified, the cost is reduced, and the performance of the silver powder is improved. The obtained nano silver has an average particle size of 60-300nm, can be redispersed in various oily solvents, and has a solid content of 40%.
After the nano silver particles are prepared, the nano silver particles need to be sent into a freeze dryer for drying treatment, the freeze dryer can generate airflow when vacuumizing and opening and closing a door, and the nano silver particles are very small, so that the fine airflow can cause the nano silver particles to fly upwards, and the loss of the nano silver particles is caused.
Therefore, the invention provides a preparation method and a preparation device of nano silver particles.
Disclosure of Invention
To remedy the deficiencies of the prior art, at least one of the technical problems set forth in the background is addressed.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the nano-silver particles comprises the following steps:
s1: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, adjusting the pH value to be neutral or alkaline, heating to 80 ℃, and stirring at constant temperature;
s2: adding crown ether under the constant-temperature stirring state, and then adding sodium borohydride under the constant-temperature stirring state 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 dry nano silver particles.
Preferably, the drying treatment method comprises the following steps:
s1: putting the wet nano silver particles into the tray, and covering the tray with a cover plate;
s2: uniformly arranging the trays on two sides of a 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 vacuumize, cool and freeze, and evaporating and discharging the water of the wet nano silver particles out of the freeze dryer after freezing to finish the drying treatment of the nano silver particles.
A nano-silver particle preparation device is suitable for the nano-silver particle preparation method, and comprises a freeze dryer, a placing rack, a tray and a cover plate; a placing frame is slidably mounted inside a cavity of the freeze dryer, a plurality of trays are placed on two sides of the placing frame, wet nano-silver particles are filled inside the trays, a cover plate is arranged on the top surface of each tray, and a plurality of air holes are formed in the cover plate; the during operation, put into the inside of tray with moist nanometer silver granule, cover the apron again, put the both sides of rack with the tray uniformly, push into the inside of freeze drier with the rack, and close the sealing door of freeze drier, the freeze drier starts the back, to the inside evacuation of freeze drier and cooling freezing, the moisture of moist nanometer silver granule evaporates discharge freeze drier after freezing, steam is followed the gas pocket discharge tray, the air current that produces is blockked by the apron when the freeze drier carries out evacuation and switch door, make the air current in the tray static relatively, thereby the probability that the nanometer silver granule flies upward along with the air current has been reduced.
Preferably, a frame plate is placed inside the tray, a partition plate is fixedly connected to the bottom surface of the frame plate, and the partition plate extends into the nano-silver particles inside the tray; the frame plate in the embodiment is flat and is 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 tray works, after the wet nano-silver particles are placed in the tray, the frame plate is placed in the tray, so that the nano-silver particles are divided into a plurality of small blocks by the partition plate, the flying probability of the nano-silver particles is further reduced, and the hardening probability of hardening among 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 surfaces of the ring groove and the ring plate are fixedly connected with a plurality of magnets, and the magnets attract each other; during operation, when the cover plate is placed on the top surface of the tray, the ring plate slides into the annular groove, so that the magnets on the two surfaces are mutually attracted, the cover plate is fixed on the top surface of the tray, the fixing strength between the cover plate and the tray is improved through the mutual attraction of the magnets, and meanwhile, the cover plate is convenient for a worker to take down the cover plate.
Preferably, a barrel is installed on the inner portion of the air hole in a threaded manner, a plurality of sliding grooves are formed in the inner wall of the barrel in a surrounding manner, an inner cavity is formed in the bottom of each 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-end sliding rod is slidably installed at the top of the inner cavity and penetrates through the bottom wall of each sliding groove in a sliding manner, arc-shaped connecting plates are slidably installed in the sliding grooves, top ends of the arc-shaped connecting plates are fixedly connected with a top cover, and the bottom surface of the top cover is in sliding fit with the top surface of the barrel; the two ends of the double-end sliding rod in the embodiment are provided with the circular baffles, and the middle part of the double-end sliding rod is rod-shaped; when the refrigerator dryer works, when the interior of the refrigerator dryer is cooled and frozen, clear water in the bag body is gradually frozen, the clear water is frozen, the size 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 sliding groove, the arc-shaped connecting plate is pushed to slide upwards along the sliding groove, 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 freeze dryer did not cool down when freezing and the tray was located the freeze dryer outside, the clear water of utricule inside was liquid, and the top surface of top cap laminating barrel this moment blocks the inside that outside dust etc. got into the tray, has improved the pure degree of nanometer silver granule.
Preferably, a hollow sealing ring is embedded in 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 barrel, and a plurality of through holes are formed in the inner ring of the hollow sealing ring; the during operation, the inside cooling freeze drying of freeze dryer accomplishes the back, and the inside temperature of freeze dryer rises the recovery gradually for the inside ice of utricule melts gradually and freezes, makes the top cap lapse, makes the top surface of hollow sealing ring extrusion barrel, and the gaseous through-hole department of following of hollow sealing ring intra-annular discharges, and slight air current passes the barrel downwards, takes the inside of tray back to the nanometer silver granule of adhesion on the barrel inner wall, thereby has further reduced the loss of nanometer silver granule.
Preferably, a plurality of grooves are formed in the top surfaces of flat plates on two sides of the placing rack, 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 surfaces of the grooves, 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 evenly the both sides of rack, the panel card is gone into the inside of recess for the bottom surface of panel contacts the top surface of ball, pushes the both sides of rack into the tray, has reduced the frictional force between the bottom surface of tray and the rack through the ball, through the cooperation of panel and recess, has reduced the probability that the tray takes place to rock, has improved the stability when the tray removes.
Preferably, the outer wall of the ball bearing is provided with a dent, the inner wall of the ball groove is embedded with a plurality of graphite blocks, and the outer wall of each graphite block is in sliding fit with the outer wall of the ball bearing; during operation, the ball rolls in the inside of ball groove for the graphite piece is scraped to the indent of ball outer wall, makes the graphite powder of graphite piece be stained with the surface of ball, has improved the surperficial lubricated degree of ball, thereby has further improved the stability when tray removes.
Preferably, fixing holes are formed in two sides of a vertical plate in the middle of the placing rack, a fixing rod is fixedly connected to the side face of the tray, the outer wall of the fixing rod is in sliding fit with the inner wall of the fixing hole, and an elastic ring is sleeved on the outer ring of the fixing rod; during operation, when the tray pushed into the two sides of the placing rack, the fixing rods are pushed to slide into the fixing holes, and the fixing rods are fixed in the fixing holes through the elastic rings and the inner walls of the fixing holes in a sliding mode, so that the fixing firmness of the tray is improved.
The invention has the following beneficial effects:
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 drier starts, to the inside evacuation of freeze drier and cooling freezing, the freeze drier of evaporation discharge after the moisture of moist nano-silver granule freezes, steam is followed the gas pocket discharge tray, and the air current that produces is blockked by the apron when the freeze drier carries out evacuation and switch door for the air current in the tray is static relatively, thereby has reduced the probability that nano-silver granule flies upward along with the air current.
2. The invention relates to a preparation method and a preparation device of nano-silver particles, wherein a cylinder, a capsule, a double-head sliding rod, an arc-shaped connecting plate and a top cover are arranged; when the interior of the freeze dryer is cooled and frozen, clear water in the bag body is gradually frozen, the volume of the bag body is increased after the clear water is frozen, the volume of the bag body is increased, the bag body expands upwards due to the blocking of the side wall of the inner cavity, the double-head sliding rod is pushed to slide into the sliding groove, the arc-shaped connecting plate is pushed to slide upwards along the sliding groove, the top cover is pushed to be separated from the top surface of the cylinder body, and water vapor in the tray is discharged out of the tray; when the inside of freeze dryer did not cool down when freezing and the tray was located the freeze dryer outside, the clear water of utricule inside was liquid, and the top surface of top cap laminating barrel this moment blocks the inside that outside dust etc. got into the tray, has improved the pure degree of nanometer silver granule.
Drawings
The invention will be further explained with reference to the 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 present 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 present 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. placing a 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 barrel; 12. a chute; 13. an inner cavity; 14. a balloon body; 15. a double-ended 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. embedding strips; 22. a ball groove; 23. a ball bearing; 24. indenting; 25. graphite blocks; 26. a fixing hole; 27. fixing the rod; 28. an elastic ring; 29. a water chamber.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example one
As shown in fig. 7, the preparation method of the nano silver particles according to the embodiment of the present invention includes the following steps:
s1: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, adjusting the pH value to be neutral or alkaline, heating to 80 ℃, and stirring at constant temperature;
s2: adding crown ether under the constant-temperature stirring state, and then adding sodium borohydride under the constant-temperature stirring state 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 1 to obtain dry nano silver particles.
As shown in fig. 8, the drying process method includes the steps of:
s1: putting the wet nano silver particles into the tray 3, and covering the cover plate 4;
s2: the trays 3 are evenly arranged on both sides of the rack 2, the rack 2 is pushed into the freeze dryer 1, and the sealing door of the freeze dryer 1 is closed;
s3: and starting the freeze dryer 1 for vacuumizing, cooling and freezing, and evaporating and discharging moisture of the wet nano silver particles out of the freeze dryer 1 after freezing to finish the drying treatment of the nano silver particles.
As shown in fig. 1 to 3, a nano silver particle manufacturing apparatus, which is suitable for the above-mentioned one nano silver particle manufacturing method, includes a freeze dryer 1, a holder 2, a tray 3, and a cover plate 4; a placing frame 2 is slidably mounted inside a cavity of the freeze dryer 1, a plurality of trays 3 are respectively placed on two sides of the placing frame 2, wet nano-silver particles are filled inside the trays 3, a cover plate 4 is arranged on the top surface of each tray 3, and a plurality of air holes 5 are formed in the cover plate 4; the during operation, put into the inside of tray 3 with moist nano-silver granule, cover apron 4 again, put the both sides of rack 2 with tray 3 uniformly, push the inside of rack 2 into freeze drier 1, and close freeze drier 1's sealing door, after freeze drier 1 starts, to the inside evacuation and the cooling freezing of freeze drier 1, the moisture of moist nano-silver granule evaporates discharge freeze drier 1 after freezing, steam is from gas pocket 5 discharge tray 3, the air current that produces when freeze drier 1 carries out evacuation and switch door is blockked by apron 4, make the air current in the tray 3 static relatively, thereby the probability that the nano-silver granule is along with the air current that flies upward has been reduced.
As shown in fig. 3, a frame plate 6 is placed inside 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 the nano silver particles inside the tray 3; the frame plate 6 in this embodiment is a flat plate, and is provided with a plurality of square holes; the shape of the partition board 7 in the embodiment is the same as that of the frame plate 6, and the thickness of the partition board 7 is larger than that of the frame plate 6; during operation, wet nano silver particles are placed in the tray 3, and then the frame plate 6 is placed in the tray 3, so that the nano silver particles are divided into a plurality of small blocks by the partition plate 7, the flying probability of the nano silver particles is further reduced, and the hardening probability of hardening among the nano silver particles is reduced.
As shown in fig. 3, a ring groove 8 is formed in the top surface of the outer ring of the tray 3, a ring plate 9 is fixedly connected to the outer ring of the bottom surface of the cover plate 4, the outer wall of the ring plate 9 is in sliding fit with the inner wall of the ring groove 8, a plurality of magnets 10 are fixedly connected to the bottom surface of the ring groove 8 and the bottom surface of the ring plate 9, and the magnets 10 attract each other on both surfaces; when the tray fixing device works, when the cover plate 4 is placed on the top surface of the tray 3, the ring plate 9 slides into the ring groove 8, the magnets 10 on the two surfaces attract each other, the cover plate 4 is fixed on the top surface of the tray 3, the fixing strength between the cover plate 4 and the tray 3 is improved through the mutual attraction of the magnets 10, and meanwhile, the cover plate 4 is convenient for a worker to take down.
As shown in fig. 4, a cylinder 11 is installed in the air hole 5 through threads, a plurality of sliding grooves 12 are formed in the inner wall of the cylinder 11 in a surrounding manner, an inner cavity 13 is formed in the bottom of each sliding groove 12, a capsule body 14 is fixedly connected to the bottom surface of the inner cavity 13, clear water is filled in the capsule body 14, a double-headed slide rod 15 is slidably installed at the top of the inner cavity 13, the double-headed slide rod 15 slidably penetrates through the bottom wall of the sliding groove 12, an arc-shaped connecting plate 16 is slidably installed 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 in sliding fit with the top surface of the cylinder 11; the two ends of the double-end sliding rod 15 in the embodiment are round baffles, and the middle part is rod-shaped; when the freezing dryer 1 works, when the interior of the freezing dryer 1 is cooled and frozen, clear water in the capsule body 14 is gradually frozen, the volume of the clear water is increased after freezing, the volume of the capsule body 14 is increased, the capsule body 14 expands upwards due to the blocking of the side wall of the inner cavity 13, the double-head sliding 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 cylinder body 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 located outside the freeze dryer 1, the clear water inside the capsule 14 is liquid, and the top cover 17 is attached to the top surface of the cylinder 11 at the moment, so that the outside dust and the like are prevented from entering the inside of the tray 3, and the purity degree of the nano-silver particles is improved.
As shown in fig. 4, a hollow sealing ring 18 is embedded in 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; the during operation, the inside cooling freeze-drying of freeze dryer 1 accomplishes the back, the inside temperature of freeze dryer 1 rises gradually and resumes, make the inside ice of utricule 14 freeze gradually, make top cap 17 lapse, make hollow sealing ring 18 extrusion barrel 11's top surface, gas in the hollow sealing ring 18 is discharged from through-hole 19, slight air current passes barrel 11 downwards, take the inside of tray 3 back to the nanometer silver granule of adhesion on barrel 11 inner wall, thereby further reduced the loss of nanometer silver granule.
As shown in fig. 3 and 5, a plurality of grooves 20 are formed in the top surfaces of the flat plates on the two sides of the placing rack 2, a plurality of gibs 21 are fixedly connected to the bottom surface of the tray 3, a plurality of ball grooves 22 are formed in the bottom surfaces of the grooves 20, balls 23 are installed 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 gibs 21; when the tray 3 is placed on the two sides of the placing frame 2 uniformly, the inlaid strips 21 are clamped into the grooves 20, so that the bottom surfaces of the inlaid strips 21 are in contact with the top surfaces of the balls 23, the tray 3 is pushed into the two sides of the placing frame 2, the friction force between the bottom surface of the tray 3 and the placing frame 2 is reduced through the balls 23, the probability of shaking of the tray 3 is reduced through the matching of the inlaid strips 21 and the grooves 20, and the stability of the tray 3 during moving is improved; the outer wall of the ball 23 is provided with a dent 24, the inner wall of the ball groove 22 is embedded with a plurality of graphite blocks 25, and the outer wall of each graphite block 25 is in sliding fit with the outer wall of the ball 23; during operation, ball 23 is when the inside of ball groove 22 rolls for graphite block 25 is scraped to the indent 24 of ball 23 outer wall, makes graphite powder of graphite block 25 be stained with the surface of ball 23, has improved the lubricated degree on ball 23's surface, thereby has further improved the stability when tray 3 removes.
As shown in fig. 3, fixing holes 26 are formed in both sides of a middle vertical plate of the placing rack 2, a fixing rod 27 is fixedly connected to a side surface of the tray 3, an outer wall of the fixing rod 27 is in sliding fit with an inner wall of the fixing hole 26, and an elastic ring 28 is sleeved on an outer ring of the fixing rod 27; during operation, when tray 3 pushed the both sides of rack 2, promote the inside that dead lever 27 slided into fixed orifices 26, through the slip of elastic ring 28 with the fixed orifices 26 inner wall for dead lever 27 fixes in the inside of fixed orifices 26, has improved the fixed firm degree of tray 3.
Example two
As shown in fig. 6, a first comparative example, in which 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; during operation, after the fixing rod 27 slides into the fixing hole 26, when the interior of the freeze dryer 1 is cooled and freeze-dried, the clear water in the water cavity 29 is frozen and expanded, so that 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 work: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, adjusting the pH value to be neutral or alkaline, heating to 80 ℃, and stirring at constant temperature; adding crown ether under the constant-temperature stirring state, and then adding sodium borohydride under the constant-temperature stirring state 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;
the wet nano silver particles are placed in the tray 3, the frame plate 6 is placed in the tray 3, the partition plates 7 divide the nano silver particles into a plurality of small blocks, when the cover plate 4 is placed on the top surface of the tray 3, the ring plate 9 slides into the ring groove 8, the magnets 10 on the two surfaces are mutually attracted, the cover plate 4 is fixed on the top surface of the tray 3, and the fixing strength between the cover plate 4 and the tray 3 is improved through the mutual attraction of the magnets 10; at this time, the clear water inside the capsule 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 strips 21 are clamped into the grooves 20, so that the bottom surfaces of the inlaid strips 21 are in contact with the top surfaces of the balls 23, the tray 3 is pushed into the two sides of the placing frame 2, the friction force between the bottom surfaces of the tray 3 and the placing frame 2 is reduced through the balls 23, when the balls 23 roll in the ball grooves 22, the dents 24 on the outer walls of the balls 23 scrape the graphite blocks 25, the graphite powder of the graphite blocks 25 is attached to the surfaces of the balls 23, and the lubrication degree of the surfaces of the balls 23 is improved; the matching of the gib 21 and the groove 20 reduces the possibility of shaking of the tray 3; when the tray 3 is pushed into the two sides of the placing rack 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 degree of the tray 3 is improved;
after the trays 3 are placed and fixed, the placing frame 2 is pushed into the freeze dryer 1, a 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, clear water in the capsule body 14 is gradually frozen, the clear water is frozen, the size of the capsule body 14 is increased, the capsule body 14 expands upwards due to the blocking of the side wall of the inner cavity 13, the double-head 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 trays 3 is discharged out of the trays 3; the airflow generated when the freeze dryer 1 performs vacuum pumping and opens and closes the door is blocked by the cover plate 4, so that the airflow in the tray 3 is relatively static, and the probability that the nano silver particles fly along with the airflow is reduced.
The front, the back, the left, the right, the upper and the lower are all based on figure 1 in the attached drawings of the specification, according to the standard of the observation angle of a person, the side of the device facing an observer is defined as the front, the left side of the observer is defined as the left, and the like.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used merely for convenience in describing the present invention and for simplifying the description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the scope of the present invention.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A preparation method of nano-silver particles is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: adding silver nitrate, polyvinyl alcohol and ammonia water into a stirring reaction kettle, adjusting the pH value to be neutral or alkaline, heating to 80 ℃, and stirring at constant temperature;
s2: adding crown ether under the constant-temperature stirring state, and then adding sodium borohydride under the constant-temperature stirring state 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 (3) drying the wet nano silver particles by using a freeze dryer (1) to obtain dry nano silver particles.
2. The method for preparing nano silver particles according to claim 1, wherein: the drying treatment method comprises the following steps:
s1: putting the wet nano silver particles into the tray (3), and covering the cover plate (4);
s2: the trays (3) are uniformly arranged on two sides of the placing rack (2), the placing rack (2) is pushed into the freeze dryer (1), and a sealing door of the freeze dryer (1) is closed;
s3: and starting the freeze dryer (1) to vacuumize, cool and freeze, and evaporating and discharging the moisture of the wet nano silver particles out of the freeze dryer (1) after freezing to finish the drying treatment of the nano silver particles.
3. A nano-silver particle preparation facilities which characterized in that: the preparation device is suitable for the preparation method of the nano silver particles as set forth in any one of claims 1-2, and comprises a freeze dryer (1), a placing frame (2), a tray (3) and a cover plate (4); the freeze drying machine is characterized in that a placing frame (2) is slidably mounted inside a cavity of the freeze drying machine (1), a plurality of trays (3) are placed on two sides of the placing frame (2), wet nano-silver particles are filled inside the trays (3), a cover plate (4) is arranged on the top surface of each tray (3), and a plurality of air holes (5) are formed in the cover plate (4).
4. The apparatus for preparing nano silver particles according to claim 3, wherein: the tray is characterized in that a frame plate (6) is placed inside 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 the nano-silver particles inside the tray (3).
5. The apparatus for preparing nano silver particles according to claim 3, wherein: annular (8) have been seted up to the outer lane top surface of tray (3), the bottom surface outer lane rigid coupling of apron (4) has crown plate (9), the outer wall of crown plate (9) and the inner wall sliding fit of annular (8), the bottom surface of annular (8) and the equal rigid coupling in bottom surface of crown plate (9) have a plurality of magnets (10), two mutually attract between magnet (10).
6. The apparatus for preparing nano silver particles according to claim 5, wherein: barrel (11) are installed to the internal thread of gas pocket (5), the inner wall of barrel (11) is encircleed and is equipped with a plurality of spout (12), inner chamber (13) have been seted up to the bottom of spout (12), the inside bottom surface rigid coupling of inner chamber (13) has utricule (14), the inside filling of utricule (14) has the clear water, the top slidable mounting of inner chamber (13) has double-end slide bar (15), double-end slide bar (15) slide the diapire that runs through spout (12), the inside slidable mounting of spout (12) has arc connecting plate (16), and is a plurality of the top rigid coupling of arc connecting plate (16) has top cap (17), the bottom surface of top cap (17) and the top surface sliding fit of barrel (11).
7. The apparatus for preparing nano silver particles according to claim 6, wherein: the bottom surface outer lane of top cap (17) is inlayed and is had hollow sealing ring (18), the outer wall of hollow sealing ring (18) and the top surface sliding fit of barrel (11), a plurality of through-holes (19) have been seted up to the inner circle of hollow sealing ring (18).
8. The apparatus for preparing nano silver particles according to claim 3, wherein: a plurality of recesses (20) have been seted up to the dull and stereotyped top surface of both sides of rack (2), the bottom surface rigid coupling of tray (3) has a plurality of panel (21), a plurality of ball groove (22) have been seted up to the bottom surface of recess (20), the inside roll mounting of ball groove (22) has ball (23), the outer wall of ball (23) and the bottom surface sliding fit of panel (21), indent (24) have been seted up to the outer wall of ball (23), the inner wall of ball groove (22) is inlayed and is had a plurality of graphite cake (25), the outer wall of graphite cake (25) and the outer wall sliding fit of ball (23).
9. The apparatus for preparing nano silver particles according to claim 3, wherein: fixing holes (26) are formed in two sides of a middle vertical plate of the placing rack (2), a fixing rod (27) is fixedly connected to the side face of the tray (3), 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).
10. The apparatus for preparing nano silver particles according to claim 9, 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).
CN202210890719.1A 2022-07-28 2022-07-28 Preparation method and preparation device of nano silver particles Active CN115255380B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210890719.1A CN115255380B (en) 2022-07-28 2022-07-28 Preparation method and preparation device of nano silver particles

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210890719.1A CN115255380B (en) 2022-07-28 2022-07-28 Preparation method and preparation device of nano silver particles

Publications (2)

Publication Number Publication Date
CN115255380A true CN115255380A (en) 2022-11-01
CN115255380B CN115255380B (en) 2023-06-02

Family

ID=83768489

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210890719.1A Active CN115255380B (en) 2022-07-28 2022-07-28 Preparation method and preparation device of nano silver particles

Country Status (1)

Country Link
CN (1) CN115255380B (en)

Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007031753A (en) * 2005-07-25 2007-02-08 Institute Of Physical & Chemical Research Method for producing support-metal nanoparticle composite, method for producing metal nanoparticle fused body, and metal nanoparticle fused body
US20080241262A1 (en) * 2004-03-29 2008-10-02 The University Of Houston System Nanoshells and Discrete Polymer-Coated Nanoshells, Methods For Making and Using Same
US20090019724A1 (en) * 2007-07-21 2009-01-22 Accurro Gmbh Apparatus for loading and unloading a tray of a freeze drying plant and method thereof
US20090066067A1 (en) * 2006-03-03 2009-03-12 Takata-Petri Ag Airbag module
CN102489717A (en) * 2011-12-22 2012-06-13 云南云天化股份有限公司 Preparation method of nanometer silver particles
JP2015191824A (en) * 2014-03-28 2015-11-02 三菱マテリアル株式会社 Negative electrode active material for lithium ion secondary battery and method for producing the negative electrode active material
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
CN110026569A (en) * 2019-04-30 2019-07-19 长沙新材料产业研究院有限公司 A kind of preparation method of nano silver
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
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
CN113206570A (en) * 2021-06-11 2021-08-03 卢成君 Cooling device for servo motor
CN214086130U (en) * 2020-12-25 2021-08-31 大洲新燕(厦门)生物科技有限公司 Cubilose freeze-dried powder generating equipment
CN215490624U (en) * 2021-02-05 2022-01-11 青岛富勒姆科技有限公司 Vacuum freeze drier
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
CN114632340A (en) * 2022-04-22 2022-06-17 河北维果生物科技有限公司 Spray type lactein solution drying device

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080241262A1 (en) * 2004-03-29 2008-10-02 The University Of Houston System Nanoshells and Discrete Polymer-Coated Nanoshells, Methods For Making and Using Same
JP2007031753A (en) * 2005-07-25 2007-02-08 Institute Of Physical & Chemical Research Method for producing support-metal nanoparticle composite, method for producing metal nanoparticle fused body, and metal nanoparticle fused body
US20090066067A1 (en) * 2006-03-03 2009-03-12 Takata-Petri Ag Airbag module
US20090019724A1 (en) * 2007-07-21 2009-01-22 Accurro Gmbh Apparatus for loading and unloading a tray of a freeze drying plant and method thereof
CN102489717A (en) * 2011-12-22 2012-06-13 云南云天化股份有限公司 Preparation method of nanometer silver particles
JP2015191824A (en) * 2014-03-28 2015-11-02 三菱マテリアル株式会社 Negative electrode active material for lithium ion secondary battery and method for producing the negative electrode active material
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
CN110026569A (en) * 2019-04-30 2019-07-19 长沙新材料产业研究院有限公司 A kind of 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
CN214086130U (en) * 2020-12-25 2021-08-31 大洲新燕(厦门)生物科技有限公司 Cubilose freeze-dried powder generating equipment
CN215490624U (en) * 2021-02-05 2022-01-11 青岛富勒姆科技有限公司 Vacuum freeze drier
CN113206570A (en) * 2021-06-11 2021-08-03 卢成君 Cooling device for servo motor
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
CN114632340A (en) * 2022-04-22 2022-06-17 河北维果生物科技有限公司 Spray type lactein solution drying device

Also Published As

Publication number Publication date
CN115255380B (en) 2023-06-02

Similar Documents

Publication Publication Date Title
CN115255380A (en) Preparation method and preparation device of nano-silver particles
SE450075B (en) PROCEDURE FOR MICROPOROS MAKING, STRUCTURED FREEZE DRIED COFFEE PRODUCT
CN207035701U (en) A kind of vacuum freeze drier
Pick et al. Temperature changes in donor blood under different storage conditions
CN111129381A (en) Self-heat-dissipation lithium battery
EP3701205B1 (en) Vacuum assisted and heated auger feeder for achieving higher packing efficiency of powder insulation materials in vacuum insulated structures and method for drying and loading an insulation material
CN109650779A (en) A kind of preparation method of graphene aerogel/polyurethane foaming conductive composites
EP2686623A1 (en) Refrigeration device having a heat store
CN214892198U (en) Freeze dryer
CN207991055U (en) A kind of list two-chamber fast-refrigerating car refrigerator
CN212274369U (en) Refrigerating chamber structure of circulating air-cooled frostless refrigerator
CN212047963U (en) Microsphere filling machine
Annear Recoveries of bacteria after drying and heating in glutamate foams
CN217154644U (en) Bioengineering's fridge
CN111602980A (en) Chemical reagent storage method for laboratory safety management
CN111603302A (en) Self-cooled subsides of bringing down a fever
CN217125555U (en) Fluoroethylene carbonate storage device with constant temperature function
CN220287939U (en) Phospholipid vacuum continuous freeze dryer
CN218600099U (en) Flat plate quick-freezing device
CN212196518U (en) Portable receiver of lithium cell
CN220577964U (en) Storage device of plateau food
CN210220404U (en) Novel external alternative trap for freeze-drying
Cheng et al. Controlling the structure of hydroxyapatite ceramics with dual pores prepared using freeze-casting
CN217636443U (en) Energy-saving drying bin for vacuum freeze drying of food
CN215324002U (en) Blood bag fridge convenient to sample

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant