CN104889383B - A kind of argentiferous anhydrous glycerol suspension and preparation method thereof - Google Patents
A kind of argentiferous anhydrous glycerol suspension and preparation method thereof Download PDFInfo
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- CN104889383B CN104889383B CN201510263442.XA CN201510263442A CN104889383B CN 104889383 B CN104889383 B CN 104889383B CN 201510263442 A CN201510263442 A CN 201510263442A CN 104889383 B CN104889383 B CN 104889383B
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- anhydrous glycerol
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Abstract
The invention discloses anhydrous glycerol suspension of a kind of argentiferous and preparation method thereof.The feature of the suspension is：Its decentralized medium is anhydrous glycerol；Dispersed phase particles are the silver-colored simple substance particle that particle size range is 50 ~ 500 nanometers, can in glycerol medium stable suspersion；Auxiliary dispersants are PVP K30.The preparation method of the suspension is：Anhydrous glycerol and PVP K30 are mixed in the reactor of polytetrafluoroethyllining lining first, it is thermally formed the glycerite of clarification, then toward addition solid nitric acid silver in this solution, after stirring, reactor is sealed, react at a certain temperature, the anhydrous glycerol suspension of the particle containing micro-nano silver is obtained after cooling.Present invention process is simple, and cost is cheap, and the suspension has good stability, can be stored for a long time in room temperature and air atmosphere, and can resist high temperature and water-reducible effect without destroyed.
Description
Technical field
The present invention relates to argentiferous anhydrous glycerol suspension of a kind of stabilization and preparation method thereof, belong to inorganic chemistry and interface
Chemical field.
Background technology
In sub-micron（100 ~ 1000 nanometers）And nanoscale（1 ~ 100 nanometer）Simple substance Argent grain have it is huge
Surface area, can uniform high-efficiency continuously discharge a large amount of active silver ion (Ag+), so as to have good and lasting antibacterial
Effect, it is the preferable antibacterial additives in various skin care item and cosmetic applications.It is current had many prepare these elemental silvers
The method report of particle, wherein being mostly chemical reduction method, in these methods, silver salt is solvent in water with appropriate reducing agent
In reacted, add appropriate surfactant when necessary, particle diameter can be obtained in the ultra-fine of sub-micron or nanoscale
Silver powder（Zhang little Min, Zhang Zhenzhong, Zhao Fangxia, Qiu Tai, orthogonal design optimization prepare the research of high dispersancy nano silver powder, material
Engineering, 2013,11,38-42；Liu Yane, Yin Lisong, Fan Hailu, Yang Suyu, Lu Yue, Guo Zhibo, Chen Qipeng,
Hydro-thermal method prepares ball shaped nano silver particles and its sign, material Leader, 2010,24,132-134）.
Glycerine is a kind of colourless, odorless, sweet viscous liquid, not only cheap, also with good moisture absorption and
Moistening effect, it is widely used in the industries such as food, medicine, daily-use chemical industry.Glycerine has reproducibility at relatively high temperatures, can reduce
Silver ion is elemental silver.Such as Wei Qunyan reported it is a kind of using glycerine be used as reducing agent, addition organic polymeric dispersants,
Under alkaline environment medium, AgNO is reduced3The method that the aqueous solution prepares nano-silver powder（Wei Qunyan, Xie Gang, Yang Xiangjun, Li Rong
It is emerging, Wang Yu, Chen Jing, the nano-silver powder of preparation of industrialization favorable dispersibility, non-ferrous metal（Smelting Part）, 2006, 6,
46-54）；Chen Jianbo etc. is reported with silver oxide (Ag2O be) presoma, glycerine be reducing agent, have polyvinylpyrrolidone and
In the aqueous solution of inorganic base, super fine silver powder is prepared using precipitation transformation method（Chen Jianbo, Li Qihou, Li Yuhu, Liu Zhiyong,
Liu Zhihong, the precipitation transformation method using glycerine as reducing agent prepare super fine silver powder, Materials Science and Engineering of Powder Metallurgy,
2013, 18, 874-881）.However, currently have glycerine participate in elemental silver particle preparation report in, glycerine as just
Reducing agent, and carry out in the basic conditions, solvent is water.At present, there is not yet in anhydrous glycerol system silver salt reduction and
The report of micro-nano elemental silver particle preparation, also have no the report using anhydrous glycerol as the stable argentiferous suspension system of decentralized medium
Road.
The content of the invention
1st, present invention aims at provide a kind of anhydrous glycerol suspension of the argentiferous of stabilization and preparation method thereof, the argentiferous
Anhydrous glycerol suspension including anhydrous glycerol be decentralized medium, silver-colored simple substance is dispersed phase particles and PVP K30
For auxiliary dispersants, the anhydrous glycerol suspension of the argentiferous is characterised by：
1. the silver-colored simple substance dispersed phase particles are in micro-nano-scale, its particle size range is 50 ~ 500 nanometers, outward appearance 90%
~ 100% is subsphaeroidal, 0 ~ 10% be it is shaft-like, can in glycerine decentralized medium stable suspersion.
The anhydrous glycerol suspension of argentiferous described in 2. can in room temperature and air atmosphere long-term stable storage, and energy
Enough high temperature of the resistance less than 250 DEG C and the water-reducible effect of 100 times of amounts are without destroyed.
Technical scheme is used by realizing the object of the invention：
Step 1：By anhydrous glycerol and PVP K30 with mass ratio 20：（0.3~1）It has been mixed in polytetrafluoroethyl-ne
In the reactor of alkene liner, after stirring, heated 20 minutes at 90 DEG C, make PVP K30 be dissolved in anhydrous
The glycerite of clarification is formed in glycerine.
Step 2：The silver nitrate added into the glycerite obtained by step 1 equivalent to qualities of glycerin number 0.1% ~ 5% is consolidated
Body, and stir.
Step 3：Reactor is sealed, is positioned in baking oven, 2-24 hours are reacted at 120 DEG C, are then cooled to room temperature,
Brown color is obtained, sticky, the anhydrous glycerol suspension containing micro-nano silver.
The inventive step is simple, and low raw-material cost, technical difficulty is low, and without any waste discharge, green, institute
Obtaining argentiferous anhydrous glycerol suspension can store and use steadily in the long term, have sub-micron and the good sterilization effect of nano-Ag particles concurrently
Fruit, and the skin-moisturizing, skin effect of glycerine, before having good application in fields such as skin care item, cosmetics, personal care and toiletries
Scape.
Brief description of the drawings
1. Fig. 1 is silver-colored simple substance particle powder diffraction pattern in suspension of the present invention；
2. Fig. 2 is silver-colored simple substance particulate scan electron microscope in example one；
3. Fig. 3 is silver-colored simple substance particulate scan electron microscope in example two；
4. Fig. 4 is silver-colored simple substance particulate scan electron microscope in example three.
Embodiment
Embodiment one：
1st, take glycerine 20g to be positioned in the reactor of polytetrafluoroethyllining lining, add PVP K30
0.3g, stir, be put into baking oven, heated 20 minutes at 90 DEG C, make PVP K30 be dissolved in anhydrous glycerol
The middle glycerite for forming clarification.
2nd, reactor is taken out, adds 0.07g silver nitrate solids into the glycerite obtained by step 1, stir, will
Reactor seals, and is put into baking oven, is reacted 2 hours at 120 DEG C.
3rd, after reaction terminates, room temperature is cooled to, obtains the sticky argentiferous anhydrous glycerol suspension of brown color.
By gained suspension with after 5 times of amount ethanol solution dilutions, supercentrifuge centrifugation is put into, gained precipitation is
Silver-colored simple substance in the suspension, gained silver simple substance is tested with X-ray powder diffraction and SEM, it was demonstrated that institute
Must be pure phase elemental silver, outward appearance 90% ~ 100% is subsphaeroidal, and 0 ~ 10% is shaft-like, and particle size range is 50 ~ 300 nanometers（See attached
Fig. 1 and accompanying drawing 2）.
Embodiment two：
1st, take glycerine 20g to be positioned in the reactor of polytetrafluoroethyllining lining, add polyvinylpyrrolidone
K300.5g, stir, be put into baking oven, heated 20 minutes at 90 DEG C, make PVP K30 be dissolved in anhydrous
The glycerite of clarification is formed in glycerine.
2nd, reactor is taken out, 0.1g silver nitrate solids is added into step 1 gained glycerite, are stirred, will be anti-
Answer kettle to seal, be put into baking oven, reacted 12 hours at 120 DEG C.
3rd, after reaction terminates, room temperature is cooled to, obtains the sticky argentiferous anhydrous glycerol suspension of brown color.
By gained suspension with after 5 times of amount ethanol solution dilutions, supercentrifuge centrifugation is put into, gained precipitation is
Silver-colored simple substance in the suspension, gained silver simple substance is tested with SEM, it was demonstrated that gained elemental silver particle appearance
90% ~ 100% is subsphaeroidal, and 0 ~ 10% is shaft-like, and particle size range is 50 ~ 400 nanometers（See accompanying drawing 3）.
Embodiment three：
1st, take glycerine 20g to be positioned in the reactor of polytetrafluoroethyllining lining, add polyvinylpyrrolidone
K300.3g, stir, be put into baking oven, heated 20 minutes at 90 DEG C, make PVP K30 be dissolved in anhydrous
The glycerite of clarification is formed in glycerine.
2nd, reactor is taken out, adds 0.1g silver nitrate solids into the glycerite obtained by step 1, stir, will
Reactor seals, and is put into baking oven, is reacted 24 hours at 120 DEG C.
3rd, after reaction terminates, room temperature is cooled to, obtains the sticky argentiferous anhydrous glycerol suspension of brown color.
By gained suspension with after 5 times of amount ethanol solution dilutions, supercentrifuge centrifugation is put into, gained precipitation is
Silver-colored simple substance in the suspension, gained silver simple substance is tested with SEM, it was demonstrated that gained elemental silver particle appearance
90% ~ 100% is subsphaeroidal, and 0 ~ 10% is shaft-like, and particle size range is 100 ~ 300 nanometers（See accompanying drawing 4）.
Claims (2)
1. a kind of anhydrous glycerol suspension of argentiferous, including anhydrous glycerol are decentralized medium, silver-colored simple substance is dispersed phase particles and gathered
Vinylpyrrolidone K30 is auxiliary dispersants, and the anhydrous glycerol suspension of the argentiferous is characterised by：
The silver-colored simple substance dispersed phase particles are in micro-nano-scale, and its particle size range is 50~500 nanometers, outward appearance to be subsphaeroidal and
It is shaft-like, can in glycerine decentralized medium stable suspersion；
The suspension can in room temperature and air atmosphere long-term stable storage, and can resist high temperature less than 250 DEG C and
The water-reducible effect of 100 times of amounts is without destroyed.
2. a kind of preparation method of the anhydrous glycerol suspension of argentiferous as claimed in claim 1, it is characterised in that according to following
Step is carried out：
(1)：By anhydrous glycerol and PVP K30 with mass ratio 20：(0.3~1) has been mixed in polytetrafluoroethylene (PTFE)
In the reactor of lining, after stirring, heated 20 minutes at 90 DEG C, make PVP K30 be dissolved in anhydrous glycerol
The middle glycerite for forming clarification；
(2)：The silver nitrate added into the glycerite obtained by step (1) equivalent to qualities of glycerin number 0.1%~5% is consolidated
Body, and stir；
(3)：Reactor is sealed, is positioned in baking oven, 2-24 hours are reacted at 120 DEG C, room temperature is then cooled to, that is, obtains
Brown color, sticky argentiferous anhydrous glycerol suspension.
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| WO2006050251A2 (en) * | 2004-10-29 | 2006-05-11 | Nanodynamics, Inc. | Polyol-based method for producing ultra-fine metal powders |
| CN101622090B (en) * | 2007-02-27 | 2013-03-13 | 三菱麻铁里亚尔株式会社 | Dispersion solution of metal nanoparticle, method for production thereof, and method for synthesis of metal nanoparticle |
| CN102000833A (en) * | 2010-12-14 | 2011-04-06 | 天津大学 | Submicron Au particles and preparation method thereof |
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