CN105561988A - Synthesizing method for silicon dioxide-silver nano-composite microspheres - Google Patents
Synthesizing method for silicon dioxide-silver nano-composite microspheres Download PDFInfo
- Publication number
- CN105561988A CN105561988A CN201410550257.4A CN201410550257A CN105561988A CN 105561988 A CN105561988 A CN 105561988A CN 201410550257 A CN201410550257 A CN 201410550257A CN 105561988 A CN105561988 A CN 105561988A
- Authority
- CN
- China
- Prior art keywords
- solution
- silver
- silica
- ultra
- pure water
- 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.)
- Pending
Links
Abstract
The invention discloses a synthesizing method for silicon dioxide-silver nano-composite microspheres. The method particularly comprises the steps of preparing a Ag(NH3)2OH solution and preparing the silicon dioxide-silver nano-composite microspheres. According to the method, uniform SiO2 particles are synthesized by adopting a solution-gel method, a silver-ammonia solution and polyvinyl pyrrolidone are added, the silver-ammonia solution is reduced by ascorbic acid, and then the uniformly-dispersed dioxide-silver nano-composite microspheres are successfully prepared; by taking polyvinyl pyrrolidone as a surfactant and a dispersing agent, particle agglomeration in the silver nanoparticle synthesizing process is prevented; by loading silver nanoparticles on the surfaces of SiO2 nanoparticles, the silver using amount in the sterilizing process is decreased, and meanwhile the silver nanoparticles are prevented from being agglomerated in the catalytic process.
Description
Technical field
The invention belongs to noble metal nanometer material preparing technical field, relate to the synthetic method of a kind of silica/silver nanoparticle complex microsphere.
Background technology
Noble metal nano particles has novel physics, chemistry and biological property, is widely used in the fields such as catalysis, sterilization, battery, biological medicine and SERS (SERS) detection.Wherein, silver nano material has unique optical, electrical, magnetic property, is widely used in fields such as electronic sensor, anti-biotic material, catalyst, SERS substrates.
Silver nano-grain particle diameter is less, and antibacterial effect is better.But the specific surface that silver nano-grain is higher and free energy, cause it to reunite, and affects its performance.In catalytic reaction process, because metal nanoparticle is not protected, the specific surface energy that particle is higher and Van der Waals force easily cause metal nanoparticle to reunite, thus cause the reduction of its catalytic performance even to disappear.In addition, single silver nano-grain bactericidal effect is good, but higher silver content easily causes the problems such as environmental pollution.
Found by research, silver nano-grain is loaded into SiO
2the composite formed, not only can improve its performance, reduces the use amount of silver in sterilization process, and prevents in silver nano-grain catalytic process and reunite.
Summary of the invention
The object of this invention is to provide the synthetic method of a kind of silica/silver nanoparticle complex microsphere, solve existing single silver nano-grain and easily reunite, cause its performance to reduce, cut the problem easily causing environmental pollution.
The technical solution adopted in the present invention is, the synthetic method of a kind of silica/silver nanoparticle complex microsphere, specifically implements according to the following steps:
Step 1, preparation Ag (NH
3)
2oH solution
3 ~ 5:1000 takes AgNH in mass ratio
3and ultra-pure water, ultrasonicly make its rapid solution, make AgNH
3solution; 10% weak aqua ammonia is slowly added dropwise to AgNH
3in solution, reaction 3 ~ 5min; Ultra-pure water is added in reaction solution, namely prepare Ag (NH
3)
2oH solution;
Step 2, prepares silica/silver nanoparticle complex microsphere
2.1) 1 ~ 2:1 ~ 2:1000 takes SiO in mass ratio
2powder, polyvinylpyrrolidone and ultra-pure water, by SiO
2powder adds in ultra-pure water, ultrasonic 10 ~ 15min, then adds polyvinylpyrrolidone, ultrasonic 10 ~ 15min, obtained SiO
2-polyvinylpyrrolidone mixed liquor;
2.2) Ag (NH will be prepared in step 1
3)
2oH solution adds SiO
2in-polyvinylpyrrolidone mixed liquor, 65 DEG C ~ 75 DEG C stirring in water bath 10 ~ 15min;
2.3) ascorbic acid of 1g/L is added 2.2) in mixed liquor, reaction 25 ~ 35min, centrifugation, by the product ultra-pure water that obtains and absolute ethanol washing, then 45 DEG C ~ 55 DEG C vacuum constant temperature drying 20 ~ 26h, namely obtain silica/silver nanoparticle complex microsphere.
Feature of the present invention is also,
Wherein 10% weak aqua ammonia and AgNH in step 1
3the volume ratio of solution is 3 ~ 5:100.
Wherein in step 1, the volume ratio of ultra-pure water and reaction solution is 1.0 ~ 2.0:1.0.
Wherein Ag (NH in step 2
3)
2oH solution and SiO
2the volume ratio of-polyvinylpyrrolidone mixed liquor is 1 ~ 1.5:3.
The wherein ascorbic acid and 2.2 of 1g/L in step 2) volume ratio of mixed liquor is 1.0 ~ 1.5:4.
The invention has the beneficial effects as follows, the synthetic method of a kind of silica/silver nanoparticle complex microsphere, adopt sol-gel process to synthesize uniform SiO
2particle, adds silver ammino solution and polyvinylpyrrolidone, reduces silver ammino solution, successfully prepare homodisperse silica/silver nanoparticle complex microsphere by ascorbic acid.Think polyvinylpyrrolidone surfactant and dispersant, prevent the reunion of particle in silver nanoparticle building-up process; Silver nano-grain loads to SiO
2nano grain surface, reduces the use amount of silver in sterilization process, meanwhile, prevents silver nano-grain to reunite in catalytic process.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
A synthetic method for silica/silver nanoparticle complex microsphere, specifically implement according to the following steps:
Step 1, preparation Ag (NH
3)
2oH solution
1.1) 3 ~ 5:1000 takes AgNH in mass ratio
3and ultra-pure water, ultrasonicly make its rapid solution, make AgNH
3solution;
1.2) by 10% weak aqua ammonia and AgNH
310% weak aqua ammonia, than 3 ~ 5:100, is slowly added dropwise to AgNH by liquor capacity
3in solution, reaction 3 ~ 5min;
1.3) by ultra-pure water and 1.2) reaction solution volume ratio 1.0 ~ 2.0:1.0, ultra-pure water is added 1.2) reaction solution in, namely prepare Ag (NH
3)
2oH solution.
Step 2, prepares silica/silver nanoparticle complex microsphere
2.1) 1 ~ 2:1 ~ 2:1000 takes SiO in mass ratio
2powder, polyvinylpyrrolidone and ultra-pure water, by SiO
2powder adds in ultra-pure water, ultrasonic 10 ~ 15min, then adds polyvinylpyrrolidone, ultrasonic 10 ~ 15min, obtained SiO
2-polyvinylpyrrolidone mixed liquor;
2.2) Ag (NH will be prepared in step 1
3)
2oH solution is pressed and SiO
2-polyvinylpyrrolidone mixeding liquid volume adds SiO than 1 ~ 1.5:3
2in-polyvinylpyrrolidone mixed liquor, 65 DEG C ~ 75 DEG C stirring in water bath 10 ~ 15min;
2.3) by the ascorbic acid and 2.2 of 1g/L) mixeding liquid volume is than 1.0 ~ 1.5:4, the ascorbic acid of 1g/L is added in above-mentioned mixed liquor, reaction 25 ~ 35min, centrifugation, by the product ultra-pure water that obtains and absolute ethanol washing, then 45 DEG C ~ 55 DEG C vacuum constant temperature drying 20 ~ 26h, namely obtain silica/silver nanoparticle complex microsphere.
The synthetic method of the present invention's a kind of silica/silver nanoparticle complex microsphere, adopts sol-gel process to synthesize uniform SiO
2particle, adds silver ammino solution and polyvinylpyrrolidone, reduces silver ammino solution, successfully prepare homodisperse silica/silver nanoparticle complex microsphere by ascorbic acid.Think polyvinylpyrrolidone surfactant and dispersant, prevent the reunion of particle in silver nanoparticle building-up process; Silver nano-grain loads to SiO
2nano grain surface, reduces the use amount of silver in sterilization process, meanwhile, prevents silver nano-grain to reunite in catalytic process.
Embodiment 1
A synthetic method for silica/silver nanoparticle complex microsphere, specifically implement according to the following steps:
Step 1, preparation Ag (NH
3)
2oH solution
1.1) AgNH is taken
330mg, ultra-pure water 10g, ultrasonicly make its rapid solution, makes AgNH
3solution;
1.2) 0.3mL10% weak aqua ammonia is slowly added dropwise to AgNH
3in solution, reaction 3min;
1.3) 10mL ultra-pure water is added in reaction solution, namely prepare Ag (NH
3)
2oH solution.
Step 2, prepares silica/silver nanoparticle complex microsphere
2.1) 30mgSiO is taken
2powder adds in 30mL ultra-pure water, ultrasonic 10min, then adds 30mg polyvinylpyrrolidone, ultrasonic 10min, obtained SiO
2-polyvinylpyrrolidone mixed liquor;
2.2) Ag (NH be prepared in 10mL step 1 is measured
3)
2oH solution adds SiO
2in-polyvinylpyrrolidone mixed liquor, 65 DEG C of stirring in water bath 10min;
2.3) add in above-mentioned mixed liquor by the ascorbic acid of 10mL1g/L, reaction 25min, centrifugation, by the product ultra-pure water that obtains and absolute ethanol washing, then 45 DEG C of dry 20h of vacuum constant temperature, namely obtain silica/silver nanoparticle complex microsphere.
Embodiment 2
A synthetic method for silica/silver nanoparticle complex microsphere, specifically implement according to the following steps:
Step 1, preparation Ag (NH
3)
2oH solution
1.1) AgNH is taken
340mg, ultra-pure water 10g, ultrasonicly make its rapid solution, makes AgNH
3solution;
1.2) 0.4mL10% weak aqua ammonia is slowly added dropwise to AgNH
3in solution, reaction 4min;
1.3) 15mL ultra-pure water is added in reaction solution, namely prepare Ag (NH
3)
2oH solution.
Step 2, prepares silica/silver nanoparticle complex microsphere
2.1) 45mgSiO is taken
2powder adds in 30mL ultra-pure water, ultrasonic 12min, then adds 45mg polyvinylpyrrolidone, ultrasonic 12min, obtained SiO
2-polyvinylpyrrolidone mixed liquor;
2.2) Ag (NH be prepared in 12mL step 1 is measured
3)
2oH solution adds SiO
2in-polyvinylpyrrolidone mixed liquor, 70 DEG C of stirring in water bath 12min;
2.3) add in above-mentioned mixed liquor by the ascorbic acid of 12mL1g/L, reaction 30min, centrifugation, by the product ultra-pure water that obtains and absolute ethanol washing, then 50 DEG C of dry 22h of vacuum constant temperature, namely obtain silica/silver nanoparticle complex microsphere.
Embodiment 3
A synthetic method for silica/silver nanoparticle complex microsphere, specifically implement according to the following steps:
Step 1, preparation Ag (NH
3)
2oH solution
1.1) AgNH is taken
350mg, ultra-pure water 10g, ultrasonicly make its rapid solution, makes AgNH
3solution;
1.2) 0.5mL10% weak aqua ammonia is slowly added dropwise to AgNH
3in solution, reaction 5min;
1.3) 20mL ultra-pure water is added in reaction solution, namely prepare Ag (NH
3)
2oH solution.
Step 2, prepares silica/silver nanoparticle complex microsphere
2.1) 60mgSiO is taken
2powder adds in 30mL ultra-pure water, ultrasonic 15min, then adds 60mg polyvinylpyrrolidone, ultrasonic 15min, obtained SiO
2-polyvinylpyrrolidone mixed liquor;
2.2) Ag (NH be prepared in 15mL step 1 is measured
3)
2oH solution adds SiO
2in-polyvinylpyrrolidone mixed liquor, 75 DEG C of stirring in water bath 15min;
2.3) add in above-mentioned mixed liquor by the ascorbic acid of 15mL1g/L, reaction 35min, centrifugation, by the product ultra-pure water that obtains and absolute ethanol washing, then 55 DEG C of dry 26h of vacuum constant temperature, namely obtain silica/silver nanoparticle complex microsphere.
Claims (5)
1. a synthetic method for silica/silver nanoparticle complex microsphere, is characterized in that, specifically implements according to the following steps:
Step 1, preparation Ag (NH
3)
2oH solution
3 ~ 5:1000 takes AgNH in mass ratio
3and ultra-pure water, ultrasonicly make its rapid solution, make AgNH
3solution; 10% weak aqua ammonia is slowly added dropwise to AgNH
3in solution, reaction 3 ~ 5min; Ultra-pure water is added in reaction solution, namely prepare Ag (NH
3)
2oH solution;
Step 2, prepares silica/silver nanoparticle complex microsphere
2.1) 1 ~ 2:1 ~ 2:1000 takes SiO in mass ratio
2powder, polyvinylpyrrolidone and ultra-pure water, by SiO
2powder adds in ultra-pure water, ultrasonic 10 ~ 15min, then adds polyvinylpyrrolidone, ultrasonic 10 ~ 15min, obtained SiO
2-polyvinylpyrrolidone mixed liquor;
2.2) Ag (NH will be prepared in step 1
3)
2oH solution adds SiO
2in-polyvinylpyrrolidone mixed liquor, 65 DEG C ~ 75 DEG C stirring in water bath 10 ~ 15min;
2.3) ascorbic acid of 1g/L is added 2.2) in mixed liquor, reaction 25 ~ 35min, centrifugation, by the product ultra-pure water that obtains and absolute ethanol washing, then 45 DEG C ~ 55 DEG C vacuum constant temperature drying 20 ~ 26h, namely obtain silica/silver nanoparticle complex microsphere.
2. the synthetic method of a kind of silica/silver nanoparticle complex microsphere according to claim 1, is characterized in that, 10% weak aqua ammonia and AgNH described in step 1
3the volume ratio of solution is 3 ~ 5:100.
3. the synthetic method of a kind of silica/silver nanoparticle complex microsphere according to claim 1, is characterized in that, in step 1, the volume ratio of ultra-pure water and reaction solution is 1.0 ~ 2.0:1.0.
4. the synthetic method of a kind of silica/silver nanoparticle complex microsphere according to claim 1, is characterized in that, (the NH of Ag described in step 2
3)
2oH solution and SiO
2the volume ratio of-polyvinylpyrrolidone mixed liquor is 1 ~ 1.5:3.
5. the synthetic method of a kind of silica/silver nanoparticle complex microsphere according to claim 1, is characterized in that, the ascorbic acid of 1g/L described in step 2 and 2.2) volume ratio of mixed liquor is 1.0 ~ 1.5:4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410550257.4A CN105561988A (en) | 2014-10-16 | 2014-10-16 | Synthesizing method for silicon dioxide-silver nano-composite microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410550257.4A CN105561988A (en) | 2014-10-16 | 2014-10-16 | Synthesizing method for silicon dioxide-silver nano-composite microspheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105561988A true CN105561988A (en) | 2016-05-11 |
Family
ID=55872943
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410550257.4A Pending CN105561988A (en) | 2014-10-16 | 2014-10-16 | Synthesizing method for silicon dioxide-silver nano-composite microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105561988A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450345A (en) * | 2016-09-12 | 2017-02-22 | 华南理工大学 | Silver nanoparticle-SiO<2> porous composite material and preparation method and application |
| CN106853367A (en) * | 2016-11-18 | 2017-06-16 | 江苏大学 | A kind of preparation method of the spherical xerogel catalyst of silver/silicon dioxide |
| CN107598184A (en) * | 2017-08-18 | 2018-01-19 | 江西师范大学 | A kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder |
| CN107930544A (en) * | 2017-11-27 | 2018-04-20 | 陕西师范大学 | Magnetic responsiveness support type Janus multi-stage porous SiO2Complex microsphere and preparation method thereof |
| CN107970925A (en) * | 2017-12-18 | 2018-05-01 | 苏州铜宝锐新材料有限公司 | The preparation method of spherical silver-SiO 2 catalyst |
| CN110354849A (en) * | 2018-03-26 | 2019-10-22 | 中国石油化工股份有限公司 | Loading type silver catalyst and its preparation method and application |
| CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
| CN112778892A (en) * | 2020-12-31 | 2021-05-11 | 重庆文理学院 | Method for preparing rod-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint |
| CN113199034A (en) * | 2021-03-05 | 2021-08-03 | 北京服装学院 | Ag-SiO2Composite microsphere and preparation method and application thereof |
| CN114716235A (en) * | 2022-06-07 | 2022-07-08 | 佛山市陶莹新型材料有限公司 | Super-heat-conduction rare earth nano ceramic material and preparation method thereof |
-
2014
- 2014-10-16 CN CN201410550257.4A patent/CN105561988A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450345A (en) * | 2016-09-12 | 2017-02-22 | 华南理工大学 | Silver nanoparticle-SiO<2> porous composite material and preparation method and application |
| CN106450345B (en) * | 2016-09-12 | 2019-12-10 | 华南理工大学 | Silver nanoparticle-SiO 2 porous composite material and preparation method and application thereof |
| CN106853367A (en) * | 2016-11-18 | 2017-06-16 | 江苏大学 | A kind of preparation method of the spherical xerogel catalyst of silver/silicon dioxide |
| CN107598184A (en) * | 2017-08-18 | 2018-01-19 | 江西师范大学 | A kind of preparation method of silver nano-grain parcel silicon dioxide microsphere powder |
| CN107930544A (en) * | 2017-11-27 | 2018-04-20 | 陕西师范大学 | Magnetic responsiveness support type Janus multi-stage porous SiO2Complex microsphere and preparation method thereof |
| CN107970925A (en) * | 2017-12-18 | 2018-05-01 | 苏州铜宝锐新材料有限公司 | The preparation method of spherical silver-SiO 2 catalyst |
| CN110354849A (en) * | 2018-03-26 | 2019-10-22 | 中国石油化工股份有限公司 | Loading type silver catalyst and its preparation method and application |
| CN110354849B (en) * | 2018-03-26 | 2022-03-29 | 中国石油化工股份有限公司 | Supported silver catalyst and preparation method and application thereof |
| CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
| CN112778892A (en) * | 2020-12-31 | 2021-05-11 | 重庆文理学院 | Method for preparing rod-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint |
| CN113199034A (en) * | 2021-03-05 | 2021-08-03 | 北京服装学院 | Ag-SiO2Composite microsphere and preparation method and application thereof |
| CN114716235A (en) * | 2022-06-07 | 2022-07-08 | 佛山市陶莹新型材料有限公司 | Super-heat-conduction rare earth nano ceramic material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105561988A (en) | Synthesizing method for silicon dioxide-silver nano-composite microspheres | |
| Liao et al. | Facile preparation of uniform nanocomposite spheres with loading silver nanoparticles on polystyrene-methyl acrylic acid spheres for catalytic reduction of 4-nitrophenol | |
| Esumi et al. | Role of poly (amidoamine) dendrimers for preparing nanoparticles of gold, platinum, and silver | |
| CN102632247B (en) | Preparation method of load-type silver nano-composite material | |
| Zhang et al. | Permeable silica shell through surface-protected etching | |
| Xia et al. | Preparation of bismuth nanoparticles in aqueous solution and its catalytic performance for the reduction of 4-nitrophenol | |
| Seh et al. | Synthesis and multiple reuse of eccentric Au@ TiO 2 nanostructures as catalysts | |
| CN103100725B (en) | Preparation method of silver/carbon quantum dot composite nanometer materials | |
| CN101161336B (en) | Oxidized graphite of loading nanometer metallic silver particle and its preparing method | |
| CN101787502B (en) | Method for preparing metal, metallic oxide or metallic hydroxide and carbon nano tube composite | |
| CN105126715A (en) | Magnetic mesoporous silica microsphere material with yolk structure and preparing method thereof | |
| CN103990814B (en) | A kind of preparation method of gold nano grain | |
| CN103042227A (en) | Nano-silver sol antibacterial agent and preparation method thereof | |
| CN104550941B (en) | Preparation method of silica @ noble metal nano-composite microspheres | |
| CN105149612A (en) | Method for preparing SiO2-coated Au@Ag core-shell nanorod | |
| CN105618038A (en) | Supported gold catalyst, preparation method thereof, and p-aminophenol preparation method | |
| CN103357360A (en) | Method for preparing controllable-shell-layer-thickness high-magnetic-response core-shell nano microspheres Fe3O4@TiO2 | |
| CN103194030A (en) | Preparation method for temperature-sensitive hydrogel/silver nanocomposite | |
| CN102366838A (en) | Preparation method of silver nano-particle with uniformity in particle size and favorable monodisperse stability | |
| CN107522169A (en) | A kind of normal temperature prepares pure organic homogeneous precipitation method of nano-oxide | |
| CN104193862A (en) | Preparation method of polystyrene/silver/titanium dioxide composite material | |
| CN106040307B (en) | One step hydro thermal method synthesizes Fe3O4(PAA) preparation method of@C-Au core-shell structure microballoon | |
| CN106311275A (en) | Preparation method of magnetic core-shell type Fe3O4@SiO2-Ag nanoparticles | |
| CN105056850B (en) | Method for preparing nanometer precious metal shell and magnetic core composite particle through self-assembling | |
| CN103920537A (en) | Method for preparing magnetic polyaniline noble metal nanometer catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160511 |