CN101337276A - Preparation method of silver particulate solution of high dispersion and antioxidation - Google Patents
Preparation method of silver particulate solution of high dispersion and antioxidation Download PDFInfo
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- CN101337276A CN101337276A CNA2008100209223A CN200810020922A CN101337276A CN 101337276 A CN101337276 A CN 101337276A CN A2008100209223 A CNA2008100209223 A CN A2008100209223A CN 200810020922 A CN200810020922 A CN 200810020922A CN 101337276 A CN101337276 A CN 101337276A
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Abstract
The invention discloses a method for preparing an antioxidant silver microparticle solution with high-dispersity, which comprises the following steps: 1, preparing a silver solution : the concentration of silver in the silver solution is 50-2,000ppm; dissolving a water-soluble high polymer in deionized water to form a water-soluble high polymer solution; dissolving a water-soluble antioxidant in deionized water to form a water-soluble antioxidant solution; dissolving a water-soluble reducer in deionized water to form a water-soluble reducer solution; performing major granule removing treatment to the four solutions; 2, adding the silver solution in step 1 into an ultrasonic container for heating up; slowly adding the water-soluble high polymer solution into the ultrasonic container; after a while, adding the water-soluble antioxidant solution into the ultrasonic container; still after a while, adding the water-soluble reducer solution into the ultrasonic container for ultrasonic blending reaction for a certain period of time to form initial product liquid; and 3, cooling the initial product liquid in step 2 and performing major granule removing treatment to the initial product liquid to form the antioxidant silver microparticle solution with high-dispersity.
Description
Technical field
The present invention relates to the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution.
Background technology
Development along with nanometer technology, the atomic particle diameter of Nano Silver more is tending towards small, the antibiotic mechanism of silver ion has following two kinds of viewpoints: Ag+ haptoreaction theory and catalysis hypothesis theory, no matter based on which kind of theory, there is proportional relation in silver-colored particle number in the germicidal efficiency of fine silver particle and the solution, and this makes the atomic anti-microbial property of antimicrobial silver also must be in continuous raising.A kind of nano silver colloid is disclosed such as Korean Patent PCT/KR2003/002855, its nano particle size is the 1-20 nanometer, the silver content of described nano silver colloid can reach 1000-50000PPm, the anti-microbial property of this nano silver colloid is better, fine silver particle is evenly distributed solution, but when on medical dressing, using, there is difficulty.Among the Chinese invention patent application CN01110767.7, disclose a kind of antimicrobial nano silver powder, its particle diameter is the 1-100 nanometer, but can't directly apply in the production technology of dressing.
In present Nano silver solution preparation, the particle size of fine silver particle differs, and the uniformity that particle distributes in liquid can't obtain good control, and the silver particles in the Nano silver solution is subject to the influence of gravity, forms subsiding belt in various degree; Nano silver solution is easily oxidated in postpone for a long time, forms precipitation, and this not only influences the concentration of Nano Silver, more influences the antibacterial ability of subsequent product.
Summary of the invention
The invention provides the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution; it is on the basis of original Nano silver solution; by adding the decentralization of the silver particles in the high molecular polymer increase solution, reduce, prevent that by adding protective agent silver particles is subjected to the oxidation of oxygen in the air.
The present invention has adopted following technical scheme: the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution, it may further comprise the steps: step 1, prepare silver-colored solution, silver concentration is 50-2000ppm in the silver solution, the water intaking soluble high polymer is dissolved in and forms water soluble polymer solution in the deionized water, the water intaking soluble antioxidant is dissolved in and forms water soluble antioxidant solution in the deionized water, water intaking dissolubility reducing agent is dissolved in and forms water-soluble reductant solution in the deionized water, goes bulky grain to handle above-mentioned four kinds of liquid; Step 2, silver-colored solution in the step 1 added in the ultrasonic container heat up, gently water soluble polymer solution is added in the ultrasonic container then, after a while water soluble antioxidant solution is added in the ultrasonic container, water-soluble reducing agent is added that ultrasonic mixing forms finished product liquid just in the ultrasonic container after reaction a period of time after a period of time; Step 3 is cooled to room temperature after form high dispersive, oxidation resistant silver particulate solution after bulky grain is handled in the past with the first finished product liquid in the step 2.
The present invention has following beneficial effect: do not use any organic solvent in the present invention, agents useful for same all meets the related request in the NF.The present invention is by adding the decentralization of the silver particles in the high molecular polymer increase solution, reduce, prevent that by adding water soluble antioxidant and water-soluble reducing agent silver particles is subjected to the oxidation of oxygen in the air, silver particulate solution stable in properties not only like this, good dispersion degree, antibacterial ability is strong, non-oxidation precipitation in 3 months, no obvious oxidation precipitation in 1 year, has stability preferably, and silver particulate solution has has a broad antifungal spectrum, can adopt spraying process or infusion process to be applied in the fabric, reach antibiotic purpose.Silver particulate solution of the present invention also can share with some film, makes the film material, is coated on the equipment and material surface, and silver particles is passed in time and will be discharged lentamente from film, plays long-term bacteriostasis.Silver particulate solution of the present invention can be handled the development of prevention and control infectious disease and generation to the shared device and the ground of public place.Silver particulate solution of the present invention can combine or directly apply in the cosmetics of everyday use with other additive or excipient; Nano silver solution of the present invention also can be used for the washing agent of clinical some open wound, inflammatory wound, chronic infection wound, but is not useable for the above burn wound of III degree.
Description of drawings
Fig. 1 is preparation technology's flow chart of the present invention
Fig. 2 is the broken line graph of the present invention's silver solution and general silver-colored solution precipitation result
The specific embodiment
Embodiment 1: according to Fig. 1 and Fig. 2, present embodiment is the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution, and it may further comprise the steps: one, prepare silver-colored solution 500ml, silver concentration is 100ppm; Get in the deionization pure water that 20ml polyethylene glycol-400 is dissolved in 280ml, the molecular weight of polyethylene glycol is the liquid polyethylene glycol below 700; Get 1g 2,6-BHT (BHT) is dissolved in the 100ml deionization pure water; Getting the 1g Vitamin C is dissolved in the 100ml deionization pure water.More than four kinds of liquid all go bulky grain to handle through 200nm, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm; Two, silver-colored solution 500ml is joined in the ultrasonic container, solution temperature is risen to 90 ℃, heating or outer heating in the mode of control temperature adopts, ultrasonic power output is 800w, slowly polyethylene glycol-400 solution is joined in the ultrasonic container then; After spending 30 minutes, with 2,6-BHT (BHT) solution joins in the ultrasonic container; After spending 30 minutes, Vitamin C solution is joined in the ultrasonic container, ultrasonic again mixing reaction 30 minutes, three, with the aforesaid liquid cool to room temperature, after 200nm removes bulky grain concentration be the high dispersive of 50ppm, oxidation resistant silver particulate solution, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm, the particle diameter of silver particles is 5-200nm.
Embodiment 2: according to Fig. 1 and Fig. 2, present embodiment is the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution, and it may further comprise the steps: one, prepare silver-colored solution 500ml, silver concentration is 200ppm; Get in the deionization pure water that the 2g shitosan is dissolved in 300ml; Get 1g 2,6-BHT (BHT) is dissolved in the 100ml deionization pure water; Get the 2g Vitamin C and be dissolved in the 100ml deionization pure water water, more than four kinds of liquid all remove bulky grain through 200nm, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm; Two, silver-colored solution 500ml is joined in the ultrasonic container, solution temperature is risen to 90 ℃, heating or outer heating in the mode of control temperature adopts, ultrasonic power output is 800w, slowly chitosan solution is joined in the ultrasonic container; After spending 30 minutes, with 2,6-BHT (BHT) solution joins in the ultrasonic container; After spending 30 minutes, Vitamin C solution is joined in the ultrasonic container ultrasonic again mixing reaction 30 minutes; Three, with the aforesaid liquid cool to room temperature, after 200nm removes bulky grain concentration be the high dispersive of 100ppm, oxidation resistant silver particulate solution, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm, the particle diameter of silver particles is 5-200nm.
Embodiment 3: according to Fig. 1 and Fig. 2, the invention provides the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution, it may further comprise the steps: one, prepare silver-colored solution 500ml, silver concentration is 100ppm; Get the 10ml PEG400, the 1g shitosan is dissolved in the deionization pure water of 290ml; Get 1g 2,6-BHT (BHT) is dissolved in the 100ml deionization pure water; Get the 2g Vitamin C and be dissolved in the 100ml deionization pure water, more than four kinds of liquid all remove bulky grain through 200nm, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm; Two, silver-colored solution 500ml is joined in the ultrasonic container, solution temperature is risen to 90 ℃, heating or outer heating in the mode of control temperature adopts, ultrasonic power output is 900w, slowly polyethylene glycol-chitosan solution is joined in the ultrasonic container; After spending 30 minutes, with 2,6-BHT (BHT) solution joins in the ultrasonic container; After spending 30 minutes, Vitamin C solution is joined in the ultrasonic container, ultrasonic again mixing reaction 30 minutes, three, with the aforesaid liquid cool to room temperature, after 200nm removes bulky grain concentration be the high dispersive of 50ppm, oxidation resistant silver particulate solution, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm, the particle diameter of silver particles is 5-200nm.
Embodiment 4: according to Fig. 1 and Fig. 2, the invention provides the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution, it may further comprise the steps: one, prepare silver-colored solution 500ml, silver concentration is 100ppm; Get in the deionization that the 10ml PEG400 is dissolved in 290ml, the molecular weight of polyethylene glycol is the liquid polyethylene glycol below 700; Getting the 2g Vitamin C is dissolved in the 200ml deionized water.More than three kinds of liquid all remove bulky grain through 200nm, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm; Two, silver-colored solution 500ml is joined in the ultrasonic container, solution temperature is risen to 90 ℃, heating or outer heating in the mode of control temperature adopts, ultrasonic power output is 800w, slowly polyethylene glycol-chitosan solution is joined in the ultrasonic container; After spending 30 minutes, Vitamin C solution is joined in the ultrasonic container, ultrasonic again mixing reaction 30 minutes, three, with the aforesaid liquid cool to room temperature, after 200nm removes bulky grain concentration be the high dispersive of 50ppm, oxidation resistant silver particulate solution, go bulky grain to handle to be to remove treating method greater than the particle of 200nm through the filter membrane of 200nm, the particle diameter of silver particles is 5-200nm.
Claims (10)
1, the preparation method of a kind of decentralization height, oxidation resistant silver particulate solution, it may further comprise the steps:
Step 1, prepare silver-colored solution, silver concentration is 50-2000ppm in the silver solution, the water intaking soluble high polymer is dissolved in and forms water soluble polymer solution in the deionized water, the water intaking soluble antioxidant is dissolved in and forms water soluble antioxidant solution in the deionized water, water intaking dissolubility reducing agent is dissolved in and forms water-soluble reductant solution in the deionized water, goes bulky grain to handle above-mentioned four kinds of liquid;
Step 2, silver-colored solution in the step 1 added in the ultrasonic container heat up, gently water soluble polymer solution is added in the ultrasonic container then, after a while water soluble antioxidant solution is added in the ultrasonic container, water-soluble reducing agent is added that ultrasonic mixing forms finished product liquid just in the ultrasonic container after reaction a period of time after a period of time;
Step 3 is cooled to room temperature after form high dispersive, oxidation resistant silver particulate solution after bulky grain is handled in the past with the first finished product liquid in the step 2.
2, the preparation method of decentralization height according to claim 1, oxidation resistant silver particulate solution, it is characterized in that step 1 silver solution is 500ml, the concentration of water soluble polymer solution is 0.5-20%, the water soluble antioxidant solution concentration is 0.01-0.02%, the concentration of water-soluble reductant solution is 0.01-0.2%, and deionized water is for adopting deionization pure water or water for injection.
3, the preparation method of decentralization height according to claim 1, oxidation resistant silver particulate solution is characterized in that bulky grain in step 1 and the step 3 is handled to be meant through the filter membrane of 200nm and to remove treating method greater than the particle of 200nm.
4, decentralization height according to claim 1, the preparation method of oxidation resistant silver particulate solution, the ultrasonic power that it is characterized in that ultrasonic container in the step 2 is being 100-1500W, silver solution adds in the ultrasonic container and heats up, temperature is controlled between 60-95 ℃, the mode of control temperature is interior heating or outer heating, spend 30 minutes water soluble antioxidant solution is added in the ultrasonic container gently water soluble polymer solution being added in the ultrasonic container back, water-soluble reducing agent added in 30 minutes again and proceed ultrasonic mixing reaction 30 minutes in the ultrasonic container.
5,, it is characterized in that described water soluble polymer is one or more in polyethylene glycol, shitosan, cellulose derivative, the CMS according to the preparation method of claim 1,2 or 4 described decentralization height, oxidation resistant silver particulate solution.
6, the preparation method of decentralization height according to claim 5, oxidation resistant silver particulate solution, the molecular weight that it is characterized in that polyethylene glycol is the liquid polyethylene glycol below 700.
7, the preparation method of decentralization height according to claim 5, oxidation resistant silver particulate solution is characterized in that described cellulose derivative is methylcellulose or ethyl cellulose.
8, according to the preparation method of claim 1,2 or 4 described decentralization height, oxidation resistant silver particulate solution, it is characterized in that described water soluble antioxidant is 2,6-BHT, the tert-butyl group are in hydroxyl fennel ether, the n-propyl gallate one or more.
9, according to the preparation method of claim 1,2 or 4 described decentralization height, oxidation resistant silver particulate solution, it is characterized in that described water-soluble reducing agent is one or more in glucose Portugal derivative, the Vitamin C, glucose Portugal derivative is glucuronic acid or gluconic acid.
10, the preparation method of decentralization height according to claim 1, oxidation resistant silver particulate solution, the particle diameter that it is characterized in that fine silver particle in the step 3 silver particulate solution is 5-200nm, concentration is 50-100ppm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505461A (en) * | 2011-10-28 | 2012-06-20 | 褚省吾 | Preparation method for silver-loaded calcium alginate fiber or silver-loaded medical non-woven fabric |
| CN104815990A (en) * | 2015-04-20 | 2015-08-05 | 西安理工大学 | Method for preparing nanometer sliver colloid with liquid phase reduction method |
| CN105436517A (en) * | 2015-12-24 | 2016-03-30 | 苏州思美特表面材料科技有限公司 | Method for preparing metal powder by utilizing nano crystal seed induction |
| CN110041765A (en) * | 2019-03-27 | 2019-07-23 | 河北晨阳工贸集团有限公司 | Antibacterial aqueous paint of one kind and preparation method thereof |
-
2008
- 2008-08-07 CN CNA2008100209223A patent/CN101337276A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505461A (en) * | 2011-10-28 | 2012-06-20 | 褚省吾 | Preparation method for silver-loaded calcium alginate fiber or silver-loaded medical non-woven fabric |
| CN104815990A (en) * | 2015-04-20 | 2015-08-05 | 西安理工大学 | Method for preparing nanometer sliver colloid with liquid phase reduction method |
| CN104815990B (en) * | 2015-04-20 | 2017-05-03 | 西安理工大学 | Method for preparing nanometer sliver colloid with liquid phase reduction method |
| CN105436517A (en) * | 2015-12-24 | 2016-03-30 | 苏州思美特表面材料科技有限公司 | Method for preparing metal powder by utilizing nano crystal seed induction |
| CN110041765A (en) * | 2019-03-27 | 2019-07-23 | 河北晨阳工贸集团有限公司 | Antibacterial aqueous paint of one kind and preparation method thereof |
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Open date: 20090107 |