CN103143724A - Preparation method of nanometer silver colloid in different shapes - Google Patents
Preparation method of nanometer silver colloid in different shapes Download PDFInfo
- Publication number
- CN103143724A CN103143724A CN2013101044375A CN201310104437A CN103143724A CN 103143724 A CN103143724 A CN 103143724A CN 2013101044375 A CN2013101044375 A CN 2013101044375A CN 201310104437 A CN201310104437 A CN 201310104437A CN 103143724 A CN103143724 A CN 103143724A
- Authority
- CN
- China
- Prior art keywords
- preparation
- different
- nano silver
- solution
- surfactant
- 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
Links
Images
Abstract
The invention discloses a preparation method of nanometer silver colloid in different shapes, which is low in cost, simple and easy to operate and capable of preparing different nanometer silver colloid of different morphologies under a water solution system and normal temperature and pressure, and belongs to the technical field for preparing nanometer material in liquid-phase chemical reduction method. The preparation method is characterized in that reducing agent solution under an alkali condition is placed into silver nitrate water solution containing surface active agent under normal temperature and pressure, nanometer silver colloid in different shapes such as a spherical shape, a hexagonal shape and a disc shape can be prepared by controlling technological conditions and the type and consumption of the surface active agent, the colloid particles fall in the range of 10nm to 90nm, and the dispersion stability of the prepared nanometer silver colloid is good. The preparation method is simple in process, low in cost of reducing agent, moderate in reaction, short in time, high in efficiency, free from needing external energy and large-sized special device and applicable to the mass production.
Description
Technical field:
The invention belongs to the nano material preparing technical field, be specifically related to a kind of preparation method of different-shape nano silver sol.
Background technology:
Silver ion antimicrobial agent occupies leading position in inorganic antiseptic, on market, most commercial inorganic antibacterial bactericide are all to carry silver.Nano silver colloidal sol is widely used as the antiseptic of health care, coating, fibre, sports goods, plastic products etc., and the technology of preparing of the extensive use of nano silver colloidal sol and nano silver colloidal sol maturation is closely-related.
Chemical reduction method is to prepare at present nano silver colloidal sol preparation method the most widely, this method mainly utilizes one or several in glucose, ascorbic acid, boron hydride, sodium metaphosphate, sodium hypophosphite, trisodium citrate, hydrogen peroxide, hydrazine hydrate, ethylene glycol, polyethylene glycol or glycerine as reducing agent, is the nanometer elargol with silver nitrate reduction.This method production equipment is simple, technological process is simple and easy to control, especially for the preparation of nanometer elargol, can realize at present spherical, cube, the synthetic (Y.G.Sun of control of the different-shapes such as hexagon, pentagon, triangle, Y.N.Xia.Science, 2002,298 (13): 2176-2179; Y.N.Xia, Y.J.Xiong, B.Lim, S.E.Skrabalak.Angew.Chem.Int.Ed., 2008,47,2-46; A.R.Siekkinen, J.M.McLellan, J.Chen, Y.N.Xia.Chem.Phys.Lett., 2006,432,491-496.).But the nano silver colloidal sol existence and stability of most methods preparation is poor, reaction is difficult to control and can't mass industrialized production etc. shortcoming.
Chinese patent CN1557588A discloses a kind of manufacture method of Nano Silver: main source take silver nitrate as silver particles, take isopropyl alcohol as the aqueous solution in the free scavenger of oxidisability; And the speed of growth of controlling nucleus by hydrophilic surface active agent polyvinyl alcohol is to control particle size, the electron beam that utilizes electron accelerator to produce carries out radiation treatment, with the solution after irradiation through wash, centrifugation, oven dry is although get final product to get the method Nano Silver powder of black.Thisly can obtain Nano Silver, but adopt electron beam irradiation, need the expensive equipment of cover, increase production cost.
Summary of the invention:
In order to overcome the deficiency of existing technology, the object of the present invention is to provide a kind of with low cost, easy, preparation method mass production different-shape nano silver sol under water solution system and normal temperature and pressure simple to operate.
2AgNO
3+Na
2S
2O
4+4NaOH＝2Ag+2Na
2SO
3+2NaNO
3+2H
2O
According to above-mentioned reaction, the present invention adopts sodium dithionite (sodium hydrosulfite) to prepare the reducing agent of nanometer elargol for liquid-phase reduction, adopting different surfactants is dispersant, and the reduction silver nitrate obtains making the fulmargin of different-shape, stably dispersing under alkali condition.
The invention provides a kind of preparation method of different-shape nano elargol, it is characterized in that: described method is carried out successively as follows:
(1) silver nitrate that takes certain mass is dissolved in deionized water, makes certain density liquor argenti nitratis ophthalmicus, and the water soluble surfactant active is dissolved in mentioned solution, mixes, and wherein, the mass ratio of silver nitrate and surfactant is 1: 0.5-1: 12.
(2) produce the solution that finite concentration contains the dithionite reducing agent, high-concentration sodium hydroxide solution is added in mentioned solution, adjust pH=11, mix.
(3) reductant solution with step (2) adds in the liquor argenti nitratis ophthalmicus that contains surfactant, dripping speed is the 0.5-20 ml/min, use simultaneously magnetic stirrer, drip rear continuation stirring reaction 0.5-1h, namely make nano silver colloidal sol, wherein the reducing agent molal weight be silver nitrate 1-3 doubly.
Preferably, the concentration of described liquor argenti nitratis ophthalmicus is 0.005mol/L-0.05mol/L.
Preferably, the concentration of described reductant solution is 0.005mol/L-0.05mol/L.
Described reducing agent is sodium dithionite (sodium hydrosulfite).
Described surfactant is selected from one or more in laruyl alcohol PEO ether sulfuric acid, polyvinylpyrrolidone, alkyl phosphate diethanolamine salt antistatic additive P, imidazoline, ester quat type cationic surfactant 1227, AEO silane WA, softex kw, antistatic additive PK.
The color of the nanometer elargol that the present invention is prepared can be bronzing, dark brown, light yellow, yellow, buff, pink, dirty-green, blueness etc.
Preparation method's beneficial effect provided by the present invention is: not only have reaction condition gentleness (normal temperature and pressure), the characteristics such as with low cost, easy and simple to handle, with short production cycle, and prepared nano silver colloidal sol diameter of particle in the 10-90nm scope and dispersion stabilization good, can stablize and preserve more than 1 year.
Description of drawings:
Fig. 1 is the process chart of the embodiment of the present invention, and wherein, 1 fully mixes for silver nitrate and surfactant; 2 regulate pH for sodium hydroxide solution adds in reductant solution; 3 fully react for reductant solution is added drop-wise in liquor argenti nitratis ophthalmicus; 4 is the target product Performance Detection.
Fig. 2 is the XRD picture of the nanometer elargol that makes of embodiment 1.
Fig. 3 is the transmission electron microscope photo of the nanometer elargol that makes of embodiment 1.
Fig. 4 is the transmission electron microscope photo of the nanometer elargol that makes of embodiment 2.
Fig. 5 is the transmission electron microscope photo of the nanometer elargol that makes of embodiment 3.
Fig. 6 is the transmission electron microscope photo of the nanometer elargol that makes of embodiment 4.
The specific embodiment:
The present invention will be further described below in conjunction with accompanying drawing 1 and embodiment.
Embodiment 1
Take the 0.34g silver nitrate and be mixed with deionized water the liquor argenti nitratis ophthalmicus that 400ml concentration is 0.05mol/L, then take 0.68g surfactant laruyl alcohol PEO ether sulfuric ester and be dissolved in (mass ratio of laruyl alcohol PEO ether sulfuric ester and silver nitrate is 2: 1) in above-mentioned silver nitrate aqueous solution, stir; Take the 0.522g sodium dithionite and be mixed with the hydrosulfurous acid sodium solution that 600ml concentration is 0.05mol/L (mol ratio of silver nitrate and sodium hydrosulfite is 1: 1.5) with deionized water, add high concentration NaOH solution to adjust pH=11; Then the hydrosulfurous acid sodium solution is added drop-wise in liquor argenti nitratis ophthalmicus with the speed of 20 ml/min at normal temperatures and pressures, uses simultaneously magnetic stirrer, stir 30min wait dripping rear continuation, finally can get jonquilleous nano silver colloidal sol.
Prepared sample is carried out the properties test, and test case and result thereof are as follows:
With X-ray diffraction analysis (XRD), can determine that by accompanying drawing 2 prepared colloidal sol is nano silver colloidal sol; Utilize transmission electron microscope to observe, by accompanying drawing 3 as can be known, micelle is the spherical nano-silver of average grain diameter 10nm left and right.
Embodiment 2
Take the 0.17g silver nitrate and be mixed with deionized water the liquor argenti nitratis ophthalmicus that 500ml concentration is 0.002mol/L, then take 1.7g surfactant imidazoles woods and be dissolved in (mass ratio of imidazoles woods and silver nitrate is 10: 1) in above-mentioned silver nitrate aqueous solution, stir; Take the 0.522g sodium dithionite and be mixed with the hydrosulfurous acid sodium solution that 600ml concentration is 0.005mol/L (mol ratio of silver nitrate and sodium hydrosulfite is 1: 3) with deionized water, add high concentration NaOH solution to adjust pH=11; Then the hydrosulfurous acid sodium solution is added drop-wise in liquor argenti nitratis ophthalmicus with the speed of 15 ml/min at normal temperatures and pressures, uses simultaneously magnetic stirrer, stir 30min wait dripping rear continuation, finally can get nano silver colloidal sol russet.By accompanying drawing 4 as can be known, micelle is the spherical nano-silver of average grain diameter 16nm left and right.
Embodiment 3
Take the 0.26g silver nitrate and be mixed with deionized water the liquor argenti nitratis ophthalmicus that 500ml concentration is 0.003mol/L, then take 0.78g quaternary ammonium salt cationic surfactant 1227 and be dissolved in (quaternary ammonium salt cationic surfactant 1227 is 3: 1 with the mass ratio of silver nitrate) in above-mentioned silver nitrate aqueous solution, stir; Take the 0.522g sodium dithionite and be mixed with the hydrosulfurous acid sodium solution that 500ml concentration is 0.06mol/L (mol ratio of silver nitrate and sodium hydrosulfite is 1: 2) with deionized water, add high concentration NaOH solution to adjust pH=11; Then the hydrosulfurous acid sodium solution is added drop-wise in liquor argenti nitratis ophthalmicus with the speed of 0.5 ml/min at normal temperatures and pressures, uses simultaneously magnetic stirrer, stir 30min wait dripping rear continuation, finally can get pink nano silver colloidal sol.By accompanying drawing 5 as can be known, micelle is the irregular hexagon Nano Silver in average grain diameter 45nm left and right.
Embodiment 4
Take the 0.51g silver nitrate and be mixed with deionized water the liquor argenti nitratis ophthalmicus that 100ml concentration is 0.03mol/L, then take 0.26g polyvinylpyrrolidone surfactant and be dissolved in (mass ratio of polyvinylpyrrolidone and silver nitrate is 0.5: 1) in above-mentioned silver nitrate aqueous solution, stir; Take the 1.04g sodium dithionite and be mixed with the hydrosulfurous acid sodium solution that 100ml concentration is 0.06mol/L (mol ratio of silver nitrate and sodium hydrosulfite is 1: 2) with deionized water, add high concentration NaOH solution to adjust pH=11; Then the hydrosulfurous acid sodium solution is added drop-wise in liquor argenti nitratis ophthalmicus with the speed of 1 ml/min at normal temperatures and pressures, uses simultaneously magnetic stirrer, stir 1h wait dripping rear continuation, finally can get blue nano silver colloidal sol.By accompanying drawing 6 as can be known, micelle is the discoid Nano Silver of average grain diameter 90nm left and right.
Claims (5)
1. the preparation method of a different-shape nano silver sol, it is characterized in that: described method is carried out successively as follows:
(1) silver nitrate that takes certain mass is dissolved in deionized water, makes certain density liquor argenti nitratis ophthalmicus, and the water soluble surfactant active is dissolved in mentioned solution, mixes, and wherein, the mass ratio of silver nitrate and surfactant is 1: 0.5-1: 12.
(2) produce the solution that finite concentration contains reducing agent, high-concentration sodium hydroxide solution is added in mentioned solution, adjust pH=11, mix.
(3) reductant solution with step (2) is added drop-wise in the liquor argenti nitratis ophthalmicus that contains surfactant, dripping speed is the 0.5-20 ml/min, use simultaneously magnetic stirrer, drip rear continuation stirring reaction 0.5-1h, namely make the different-shape nano silver sol, wherein the reducing agent molal weight be silver nitrate 1-3 doubly.
2. the preparation method of a kind of different-shape nano silver sol according to claim 1, it is characterized in that: the concentration of described liquor argenti nitratis ophthalmicus is 0.005mol/L-0.05mol/L.
3. the preparation method of a kind of different-shape nano silver sol according to claim 1, it is characterized in that: the concentration of described reductant solution is 0.005mol/L-0.05mol/L.
4. the preparation method of a kind of different-shape nano silver sol according to claim 1, it is characterized in that: described reducing agent is sodium dithionite.
5. the preparation method of a kind of different-shape nano silver sol according to claim 1, it is characterized in that: described surfactant is selected from one or more in laruyl alcohol PEO ether sulfuric acid, polyvinylpyrrolidone, alkyl phosphate diethanolamine salt antistatic additive P, imidazoline, ester quat type cationic surfactant 1227, AEO silane WA, softex kw, antistatic additive PK.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310104437.5A CN103143724B (en) | 2013-03-16 | 2013-03-16 | Preparation method of nanometer silver colloid in different shapes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310104437.5A CN103143724B (en) | 2013-03-16 | 2013-03-16 | Preparation method of nanometer silver colloid in different shapes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103143724A true CN103143724A (en) | 2013-06-12 |
| CN103143724B CN103143724B (en) | 2015-04-22 |
Family
ID=48542194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310104437.5A Active CN103143724B (en) | 2013-03-16 | 2013-03-16 | Preparation method of nanometer silver colloid in different shapes |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103143724B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014804A (en) * | 2014-05-20 | 2014-09-03 | 苏州明动新材料科技有限公司 | Preparation method of nanometer silver powder with particles controllable |
| CN104148664A (en) * | 2014-07-18 | 2014-11-19 | 广西科技大学 | nano silver collosol preparing method |
| CN104259472A (en) * | 2014-09-03 | 2015-01-07 | 江苏科技大学 | Organic composition of ultrafine sheet copper powder and preparation method of organic composition |
| CN104338936A (en) * | 2014-10-29 | 2015-02-11 | 西南大学 | Synthetic method of stable silver nanoparticles |
| CN105345027A (en) * | 2015-11-30 | 2016-02-24 | 成都市天甫金属粉体有限责任公司 | Production method of high-dispersion submicron silver powder |
| CN109201114A (en) * | 2018-10-19 | 2019-01-15 | 清华大学深圳研究生院 | A kind of aqueous catalysis material colloidal sol and its preparation method and application |
| CN110340367A (en) * | 2019-08-02 | 2019-10-18 | 中国恩菲工程技术有限公司 | The solid sintering preparation method of magnesium scandium alloy |
| CN112142098A (en) * | 2019-06-28 | 2020-12-29 | 东北大学 | Ag coated SnO2Preparation of SO2Method for sensing material |
| CN113275586A (en) * | 2021-05-31 | 2021-08-20 | 广东省江门市质量计量监督检测所 | Method for preparing nano silver with different particle sizes by using surfactant |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| WO2006126771A1 (en) * | 2005-05-23 | 2006-11-30 | Korea Research Institute Of Bioscience And Biotechnology | Multicolor-encoded colloidal particles coated with metal nanoparticles mixture having colors in the visible region and method for preparing the same |
| CN101554664A (en) * | 2009-05-20 | 2009-10-14 | 广东风华高新科技股份有限公司 | Method for preparing nano-scale silver powder |
| CN101733410A (en) * | 2009-12-31 | 2010-06-16 | 广东风华高新科技股份有限公司 | Preparation method of high dispersibility superfine silver powder with adjustable grain diameter |
| CN101990475A (en) * | 2008-04-28 | 2011-03-23 | 塔塔化学有限公司 | A process for the preparation of silver nano particles |
| CN102837003A (en) * | 2012-09-07 | 2012-12-26 | 中国科学院深圳先进技术研究院 | Nano silver particles with multilevel structure and preparation method thereof |
-
2013
- 2013-03-16 CN CN201310104437.5A patent/CN103143724B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006126771A1 (en) * | 2005-05-23 | 2006-11-30 | Korea Research Institute Of Bioscience And Biotechnology | Multicolor-encoded colloidal particles coated with metal nanoparticles mixture having colors in the visible region and method for preparing the same |
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| CN101990475A (en) * | 2008-04-28 | 2011-03-23 | 塔塔化学有限公司 | A process for the preparation of silver nano particles |
| CN101554664A (en) * | 2009-05-20 | 2009-10-14 | 广东风华高新科技股份有限公司 | Method for preparing nano-scale silver powder |
| CN101733410A (en) * | 2009-12-31 | 2010-06-16 | 广东风华高新科技股份有限公司 | Preparation method of high dispersibility superfine silver powder with adjustable grain diameter |
| CN102837003A (en) * | 2012-09-07 | 2012-12-26 | 中国科学院深圳先进技术研究院 | Nano silver particles with multilevel structure and preparation method thereof |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014804A (en) * | 2014-05-20 | 2014-09-03 | 苏州明动新材料科技有限公司 | Preparation method of nanometer silver powder with particles controllable |
| CN104014804B (en) * | 2014-05-20 | 2016-01-20 | 苏州明动新材料科技有限公司 | A kind of preparation method of nano-silver powder of size tunable |
| CN104148664B (en) * | 2014-07-18 | 2016-08-24 | 广西科技大学 | A kind of preparation method of nano silver colloidal sol |
| CN104148664A (en) * | 2014-07-18 | 2014-11-19 | 广西科技大学 | nano silver collosol preparing method |
| CN104259472A (en) * | 2014-09-03 | 2015-01-07 | 江苏科技大学 | Organic composition of ultrafine sheet copper powder and preparation method of organic composition |
| CN104259472B (en) * | 2014-09-03 | 2016-09-28 | 江苏科技大学 | A kind of organic composite of superfine sheet copper powder and preparation method thereof |
| CN104338936A (en) * | 2014-10-29 | 2015-02-11 | 西南大学 | Synthetic method of stable silver nanoparticles |
| CN105345027A (en) * | 2015-11-30 | 2016-02-24 | 成都市天甫金属粉体有限责任公司 | Production method of high-dispersion submicron silver powder |
| CN109201114A (en) * | 2018-10-19 | 2019-01-15 | 清华大学深圳研究生院 | A kind of aqueous catalysis material colloidal sol and its preparation method and application |
| CN112142098A (en) * | 2019-06-28 | 2020-12-29 | 东北大学 | Ag coated SnO2Preparation of SO2Method for sensing material |
| CN110340367A (en) * | 2019-08-02 | 2019-10-18 | 中国恩菲工程技术有限公司 | The solid sintering preparation method of magnesium scandium alloy |
| CN110340367B (en) * | 2019-08-02 | 2021-05-07 | 中国恩菲工程技术有限公司 | Solid sintering preparation method of magnesium-scandium alloy |
| CN113275586A (en) * | 2021-05-31 | 2021-08-20 | 广东省江门市质量计量监督检测所 | Method for preparing nano silver with different particle sizes by using surfactant |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103143724B (en) | 2015-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103143724B (en) | Preparation method of nanometer silver colloid in different shapes | |
| Gontijo et al. | pH effect on the synthesis of different size silver nanoparticles evaluated by DLS and their size-dependent antimicrobial activity | |
| Valodkar et al. | Morphology and antibacterial activity of carbohydrate-stabilized silver nanoparticles | |
| Mavani et al. | Synthesis of silver nanoparticles by using sodium borohydride as a reducing agent | |
| CN106106522B (en) | A kind of nano zine oxide-load silver chitosan compound anti-bacteria agent and preparation method thereof | |
| CN104194004B (en) | A kind of green synthesis method of Nano Silver sodium alginate compound | |
| CN103071808B (en) | Environmentally-friendly synthetic method for metal nanoparticle | |
| CN106563814B (en) | A kind of controllable method for preparing of light inducible to silver nanoparticle triangular plate | |
| CN101731272A (en) | Method for preparing antibacterial nanometer silver colloid | |
| CN103506631B (en) | Method for preparing small-size nano-silver with chitosan as reducing agent | |
| CN102090395A (en) | Abscisic acid-embedded chitosan nanoparticles and preparation method thereof | |
| CN103600088B (en) | A kind of preparation method of the controlled silver nano-grain of size | |
| Wan et al. | Bioreduction and stabilization of nanosilver using Chrysanthemum phytochemicals for antibacterial and wastewater treatment | |
| CN105945302A (en) | Preparation method for antioxidant copper nanopowder | |
| CN103611944A (en) | Preparation method of ClO3- ionic liquid dispersed iron nanoparticles | |
| CN111992738B (en) | Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method | |
| CN109485084A (en) | A kind of method and application of form controlledly synthesis cuprous oxide powder | |
| CN105127448A (en) | Room-temperature preparation method for nano silver sheet with ultra-large area | |
| CN105522162A (en) | Method for preparing silver nanoparticles by step-by-step growth method | |
| CN105081340A (en) | Dispersed nano iron particle and preparation method thereof | |
| CN104148664B (en) | A kind of preparation method of nano silver colloidal sol | |
| CN103737011B (en) | The preparation method of high compaction spherical silver powder | |
| CN111347060A (en) | Preparation method of nano-silver colloid with controllable particle size | |
| CN104073462A (en) | Method for preparing antibacterial plant tissue culture medium | |
| CN104551009A (en) | Preparation method of two-dimensional fractal silver nanoparticles in alcohol-water system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210526 Address after: No.33, Lane 159, Taiye Road, Fengxian District, Shanghai, 201400 Patentee after: Shanghai Yuanbao Industrial Design Co.,Ltd. Address before: Anhui University of technology, 59 Hudong Road, Huashan District, Ma'anshan City, Anhui Province 243002 Patentee before: ANHUI University OF TECHNOLOGY |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221216 Address after: 710000 Room 1501, Unit 1, Building 3, Capital Shangyuan, Yuancheng Road, Xi'an Economic and Technological Development Zone, Shaanxi Province Patentee after: Shaanxi Hengfang Technology Co.,Ltd. Address before: No.33, Lane 159, Taiye Road, Fengxian District, Shanghai, 201400 Patentee before: Shanghai Yuanbao Industrial Design Co.,Ltd. |
|
| TR01 | Transfer of patent right |