CN107199336A - One-step method prepares the silicon dioxide microsphere of Surface coating nano-Ag particles - Google Patents
One-step method prepares the silicon dioxide microsphere of Surface coating nano-Ag particles Download PDFInfo
- Publication number
- CN107199336A CN107199336A CN201710405909.9A CN201710405909A CN107199336A CN 107199336 A CN107199336 A CN 107199336A CN 201710405909 A CN201710405909 A CN 201710405909A CN 107199336 A CN107199336 A CN 107199336A
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- CN
- China
- Prior art keywords
- silicon dioxide
- dioxide microsphere
- nano silver
- microballoon
- 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.)
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Classifications
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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
- B22F1/17—Metallic particles coated with metal
-
- 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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
Abstract
The present invention mainly introduces the preparation method that Nano Silver bare ball is supported on silicon dioxide microsphere surface, and major technique includes：The preparation of silicon dioxide microsphere, the nano silver particles bare ball for being supported on silicon dioxide microsphere surface then prepares two aspects.Method has the advantages that simple to operate, reaction requires that low, environment friendly is high.
Description
Technical field
A kind of preparation method of silicon dioxide coated by Nano silver microballoon of present specification, this method has environment friendly
And the characteristics of simple and fast.
Background technology
Dephasign composite attracts the research enthusiasm of chemistry and physicists always, especially by chemical reaction pair
Matrix of materials surface is handled, for example, carrying out the modification of functional group to silicon dioxide microsphere surface, is specifically included：Sulfydryl, ammonia
Base, vinyl etc., the silicon dioxide microsphere after modification are widely used in catalysis, fluoroscopic examination and biology sensor.Mesh
It is preceding frequently with method it is generally comparatively laborious, the microsphere surface for having prepared completion is attached to using organosilan or organic matter,
But adhesion amount is very limited.
Nano Silver is widely used in terms of sterilization, detection, catalysis, and sol-gal process is the one kind for preparing Nano Silver
Common method, the controllable Nano silver grain of size can be prepared in aqueous, high etc. excellent with simple, quick, degree of controllability
Point, is typically that silver-colored solution is reduced under conditions of existing containing protective agent or stabilizer and is obtained, therefore obtained nano grain of silver
Sublist face leads to production and is coated with stabilizer, it is to avoid nano silver particles continued growth or coagulation.Because nanometer silver surface is covered by stabilizer
Lid, needs to be handled in practical application, obtains exposed silver particles, this process has larger to the stability of Nano Silver
Influence, therefore Nano Silver bare ball is directly prepared with higher application value.
Because the recovery of nano-particle is typically relatively difficult, therefore when involving the need for recycling, it will generally receive
Rice material load is on carrier, and such as silicon dioxide microsphere improves the recovery of nano material under conditions of its performance is not influenceed
Rate.The present invention describes a kind of simple and easy method for the silicon dioxide microsphere for preparing nano-silver loaded.
The content of the invention
The present invention mainly introduces the preparation method that Nano Silver bare ball is supported on silicon dioxide microsphere surface, major technique bag
Include：The preparation of silicon dioxide microsphere, the nano silver particles bare ball for being supported on silicon dioxide microsphere surface then prepares two aspects.Side
Method has the advantages that simple to operate, reaction requires that low, environment friendly is high.
The present invention is realized by following technology path：Under agitation, 3- mercaptopropyi trimethoxy silicon is uniformly divided
It is dispersed in water, then adds appropriate ammoniacal liquor, in certain temperature condition stirring reaction certain hour, precipitation is then collected by centrifugation,
Respectively with ethanol and water washing three times, size is obtained in the other silicon dioxide microsphere of submicron order, and microsphere surface is rich in sulfydryl.
Finally microballoon point is spread in 0.1mol/L silver nitrate solution, stirring reaction centrifuge washing after 3 hours, collects precipitation vacuum and do
It is dry, obtain the silicon dioxide microsphere that surface is rich in nano silver particles.
Described in technical scheme：The ratio of 3- mercaptopropyi trimethoxy silicon and water is usually 1 ~ 20:100（Volume ratio）,
The 3- mercaptopropyi trimethoxies silicone oil drop being just added to the water under agitation, is gradually dispersed in water to form homogeneous transparent
Liquid, then adds ammoniacal liquor, and the volume ratio of ammoniacal liquor and water is 0.5 ~ 1.5:100, mixing speed is 400 ~ 1000rpm, reaction temperature
Spend for 20 ~ 60 DEG C, the reaction time is 12 ~ 72h.Centrifuged after reaction completely, precipitation is washed successively with ethanol, water, then will precipitation
It is added in 0.01 ~ 0.1mol/L silver salt solution, usually silver nitrate solution, centrifuge washing precipitation and vacuum after room temperature reaction
It is dried to obtain the silicon dioxide microsphere of Surface coating nano silver particles.
The advantage of the invention is that：1st, preparation method is simple, reaction requires low；2nd, compared with conventional method, of the invention
The Nano Silver beaten does not have protectant bare ball for surface, it is not necessary to which carrying out subsequent treatment both can directly apply；3rd, the silver obtained
The particle diameter begged is coated in sub-micron rank, is separated relatively simple, it is only necessary to simple filtration or centrifugation.
Embodiment one：1st, it is 400rpm to control mixing speed, and 200 μ L MPTMS is added in 10ml water, and stirring is extremely
MPTMS droplet distributions obtain transparency liquid in water.2nd, 100 μ L ammoniacal liquor is added in above-mentioned solution, continues stirring reaction
24h.3rd, precipitation is collected by centrifugation, and uses ethanol, water washing successively, is dispersed in 2ml water and preserves.4th, microballoon suspension is added
Into 10ml silver nitrate aqueous solutions, silver nitrate concentration is 0.1mol/L, reacts 3h.5th, precipitation is collected by centrifugation, and is washed with water three
Secondary, then vacuum drying obtains the silicon dioxide microsphere of Nano Silver cladding under the conditions of 40 DEG C, and this microballoon is characterized.
Embodiment two：1st, it is 500rpm to control mixing speed, and controlling reaction temperature is 40 DEG C, and 300 μ L MPTMS is added
Into 10ml water, stirring to MPTMS droplet distributions obtains transparency liquid in water.2nd, 150 μ L ammoniacal liquor is added to above-mentioned molten
In liquid, continue stirring reaction 48h.3rd, precipitation is collected by centrifugation, and uses ethanol, water washing successively, is dispersed in 2ml water and preserves.4、
Microballoon suspension is added in 10ml silver nitrate aqueous solutions, silver nitrate concentration is 0.1mol/L, reacts 3h.5th, it is heavy to be collected by centrifugation
Form sediment, and be washed with water three times, then vacuum drying obtains the silicon dioxide microsphere of Nano Silver cladding under the conditions of 40 DEG C, micro- to this
Ball is characterized.
Change reaction condition, main to influence the size of silicon dioxide microsphere, in general MPTMS consumption is higher, dioxy
The volume of SiClx microballoon is bigger；Mixing speed increase, microballoon increase, ammonia volume increase, microsphere volume diminishes；Reaction temperature
Higher, the size of microballoon is more uniform, but temperature is too high to have a negative impact to the content of microsphere surface sulfydryl, causes surface silver
Population is reduced.Concentration of silver ions mainly influences the formation speed of nano silver particles.According to above-mentioned reactions steps, change reaction
Condition can obtain the silicon dioxide microsphere of different size of cladding Nano silver grain, therefore repeat no more.
Brief description of the drawings
Accompanying drawing 1 is the scanning electron microscope (SEM) photograph of silicon dioxide microsphere.
Accompanying drawing 2 is the transmission electron microscope picture of Surface coating Nano silver grain silicon dioxide microsphere.
Claims (3)
1. a kind of simple method for preparing of silicon dioxide coated by Nano silver microballoon of present specification, its step is followed successively by：Prepare
The silicon dioxide microsphere of sub-micron or micron grain size size and its be rich in sulfydryl；This microballoon is added to containing the water-soluble of silver ion
Centrifuged in liquid, after stirring a period of time and precipitate and wash, vacuum drying obtains the silicon dioxide microsphere of Nano Silver cladding.
2. by claim 1, the method is characterised by：The use of 3-mercaptopropyi trimethoxy silane is silicon source, is promoted with ammoniacal liquor
Enter hydrolysis and prepare microballoon, reacted with microballoon and silver nitrate aqueous solution and obtain the silicon dioxide microsphere that Nano Silver is coated.
3. by claim 1, the method is characterised by, it is not necessary to which extra addition reducing agent is that can obtain Nano silver grain, and
Nano silver grain prepared by this method has good stability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710405909.9A CN107199336A (en) | 2017-06-02 | 2017-06-02 | One-step method prepares the silicon dioxide microsphere of Surface coating nano-Ag particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710405909.9A CN107199336A (en) | 2017-06-02 | 2017-06-02 | One-step method prepares the silicon dioxide microsphere of Surface coating nano-Ag particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107199336A true CN107199336A (en) | 2017-09-26 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710405909.9A Pending CN107199336A (en) | 2017-06-02 | 2017-06-02 | One-step method prepares the silicon dioxide microsphere of Surface coating nano-Ag particles |
Country Status (1)
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| CN (1) | CN107199336A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003691A (en) * | 2017-11-22 | 2018-05-08 | 浙江加州国际纳米技术研究院台州分院 | Preparation method for ocean engineering anti-halobios adhersion coating |
| CN113199034A (en) * | 2021-03-05 | 2021-08-03 | 北京服装学院 | Ag-SiO2Composite microsphere and preparation method and application thereof |
| CN113398149A (en) * | 2021-04-21 | 2021-09-17 | 上海市第十人民医院 | A compound therapeutic agent with antibacterial and colon cancer treating effects, and its preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5837166A (en) * | 1981-08-27 | 1983-03-04 | Shinroku Kawakado | Production of noble metal coated powder |
| CN103223488A (en) * | 2013-05-08 | 2013-07-31 | 宁波大学 | Preparation method for silver-coated silicon dioxide composite microsphere particles |
| CN103231072A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of silicon dioxide/silver core-shell composite powder for high temperature electronic paste |
| CN103350226A (en) * | 2013-07-16 | 2013-10-16 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
-
2017
- 2017-06-02 CN CN201710405909.9A patent/CN107199336A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5837166A (en) * | 1981-08-27 | 1983-03-04 | Shinroku Kawakado | Production of noble metal coated powder |
| CN103231072A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of silicon dioxide/silver core-shell composite powder for high temperature electronic paste |
| CN103223488A (en) * | 2013-05-08 | 2013-07-31 | 宁波大学 | Preparation method for silver-coated silicon dioxide composite microsphere particles |
| CN103350226A (en) * | 2013-07-16 | 2013-10-16 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| YAN LIU等: "Silver Nanoparticle Generators: Silicon Dioxide Microspheres", 《CHEMISTRY-A EUROPEAN JOURNAL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003691A (en) * | 2017-11-22 | 2018-05-08 | 浙江加州国际纳米技术研究院台州分院 | Preparation method for ocean engineering anti-halobios adhersion coating |
| CN113199034A (en) * | 2021-03-05 | 2021-08-03 | 北京服装学院 | Ag-SiO2Composite microsphere and preparation method and application thereof |
| CN113398149A (en) * | 2021-04-21 | 2021-09-17 | 上海市第十人民医院 | A compound therapeutic agent with antibacterial and colon cancer treating effects, and its preparation method |
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Application publication date: 20170926 |
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