CN1653907A - Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer - Google Patents
Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer Download PDFInfo
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- CN1653907A CN1653907A CN 200510049258 CN200510049258A CN1653907A CN 1653907 A CN1653907 A CN 1653907A CN 200510049258 CN200510049258 CN 200510049258 CN 200510049258 A CN200510049258 A CN 200510049258A CN 1653907 A CN1653907 A CN 1653907A
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Abstract
The present invention discloses the preparation process of nanometer silver solution and nanometer silver powder with polymer as stabilizer. Water soluble polymer as stabilizer in solution of 0.001-0.05 g/ml solution and silver nitrate in solution of 0.001-0.1 mol/L are compounded and reduced with water soluble reductant in solution of 0.001-0.2 mol/L to obtain nanometer silver particle of 5-100 nm size. The nanometer silver particle in solution may be further deposited and washed with sodium hydroxide solution, dried and crushed to obtain nanometer silver particle of 5-100 nm size. The prepared solution may be used in medical article, and prepared nanometer silver powder may be used widely in household appliance, plastic product, paint, etc. The present invention is environment friendly, low in cost and simple in operation, and the prepared nanometer silver particle has extremely powerful antibiotic capacity and wide antibiotic spectrum.
Description
Technical field
The present invention relates to a kind of wide-spectrum antiseptic nanometer silver solution and nano-silver powder preparation, particularly a kind of is the preparation method of the Nano silver solution and the nano silver powder of stabilizing agent with the high polymer.
Background technology
The anti-biotic material of Ying Yonging is many with organic antibacterial agent still in the market, but the general antibacterial effect of organic antibacterial agent is relatively poor, and only mould proof effect is stronger, all has the organic antibacterial agent of good inhibition less to the two.And the warm tolerance of organic antibacterial agent, less stable, its catabolite and volatile matter may be harmful; Thereby the inorganic antiseptic stronger to bacteriostasis, special silver-series antibacterial agent is shown one's talent.Compare with organic antibacterial agent, inorganic antibacterial material has continuation, persistence, broad spectrum activity, is difficult for producing drug resistance, good heat resistance, characteristics such as safety height.
Silver has broad spectrum antibacterial.Just be used to treat knife wound, sword cut as far back as the ancient times, ancient times three, state well-known doctor Huatuo was that the pass public affairs are scraped bone and cured the wound with silver-colored cutter just, and Compendium of Material Medica is on the books to the sterilizing function of silver." infrastructure elements chemistry " described like this to silver: silver has peculiar effect as bactericide, and 1% liquor argenti nitratis ophthalmicus is the medicine commonly used of treatment eye conjunctivitis.Argent has strong bactericidal action.
Nanometer technology is that the material with 1～100nm size is the front subject of research object.Nano Silver is because its higher specific surface area has quick, the lasting characteristic that discharges.In recent years, China's Nano Silver technological progress is bigger, and the Nano Silver industry is also developed faster.Chinese invention patent 01110767 " anti-wide-spectrum antiseptic nanometer silver micro mist and the inductrial production process assembled " discloses a kind of anti-gathering wide-spectrum antiseptic nanometer silver micro mist and inductrial production process, and nano silver powder is adsorbed on some natural many spaces vegetable materials securely.Chinese invention patent 02138891 adsorbs nano silver powder with cavity or the ghost of algae.Above patent all is to be the preparing carriers nano silver powder with the porous material, and not relating to the high polymer is that stabilizing agent prepares Nano silver solution and nano-silver powder body method.
The antibiotic mechanism of silver ion has following two kinds of viewpoints:
1.Ag
+Haptoreaction is thought Ag
+Cause the microbial activity composition to destroy or the generation obstruction by haptoreaction.Work as Trace Ag
+When arriving the microbial cell film,, rely on Coulomb attraction, make the two firm absorption, Ag because of the latter has negative electrical charge
+With the mycoprotein enzyme-SH base combines, make as the enzyme loss of activity of necessity to survive, thereby realize the effect of killing pathogenic bacteria.
Its antibiotic mechanism is:
2. catalysis hypothesis is thought the Trace Ag that material surface distributes
+Can play the effect of catalytic active center, silver can activate the oxygen in the air or in the water, produces hydroxyl radical free radical machine active oxygen ion.The multiplication capacity of their energy destroy microorganisms cells suppresses or kill bacteria.
Summary of the invention
The purpose of this invention is to provide a kind of is the preparation method of the Nano silver solution and the nano silver powder of stabilizing agent with the high polymer.
With the high polymer is the Nano silver solution preparation method of stabilizing agent: concentration is that 0.001～0.05g/ml water soluble polymer stabilizing agent and concentration are that 0.001～0.1mol/L silver nitrate is compound, re-using concentration is that the water-soluble reductant of 0.001～0.2mol/L is reduced to Nano Silver with silver nitrate, and the particle diameter of Nano Silver is 5～100nm.
With the high polymer is the nano-silver powder preparation of stabilizing agent: concentration is that 0.001～0.05g/ml shitosan stabilizing agent and concentration are that 0.001～0.1mol/L silver nitrate is compound, working concentration is that the water-soluble reductant of 0.001～0.2mol/L is reduced to Nano Silver with silver nitrate, re-use sodium hydroxide solution with Nano Silver deposition, washing, dry, pulverizing, obtaining particle diameter is the Nano Silver of 5～100nm.
The present invention not only has low, the simple operation and other advantages of cost, and the nano-Ag particles of preparation has extremely strong antibacterial ability and broad spectrum antibacterial.In the present invention, do not use any organic solvent, meet requirements of green environmental protection.Nano silver solution Nano silver solution of the present invention has no side effect, and does not have precipitation in 3 months, has stability preferably.
Nano silver solution of the present invention can be handled fabrics such as socks, towel, shoe-pad, underwear, yarn, antibiotic socks and mouth masks, and the fabric after the processing has the broad-spectrum long-acting antibacterial functions.Nano silver solution of the present invention can be handled the generation that keeps off infection to family places such as public places such as market, hospital, elevator, station and kitchens.Nano silver solution of the present invention can be made facial mask, hand cleanser, face washing liquid, bath foam etc. by combining with other additive or excipient, also can be used for the prevention and the sterilization of burn and scald, operative incision trauma surface infestation.Nano silver solution of the present invention also can be used for the treatment of bacterial vaginitis, male prostatitis etc.Nano silver solution of the present invention also can be directly used in administers the water pollution.Multiple performances such as Nano silver solution of the present invention and bone growth factor carry out compoundly with the bone carrier respectively, form release membranes, and this anti-infective bone-grafting material has wide spectrum, have no drug resistance.The stable wide-spectrum antiseptic nanometer silver micro mist of high polymer of the present invention can be used to prepare antimicrobial form plastic articles, tame electrical article, coating etc.
Description of drawings
Accompanying drawing is the nanometer silver antimicrobial design sketch.
Embodiment
Embodiment 1
With the high polymer is the Nano silver solution preparation method of stabilizing agent: get the 5g shitosan and be dissolved in the 95ml water, add the 1.69g silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the 3.5g ascorbic acid.Stir and continue 5～6 hours.Promptly get stabilized nanoscale silver solution.
Transmission electron microscope results shows: the average 100nm of nano-Ag particles.
Embodiment 2
With the high polymer is the Nano silver solution preparation method of stabilizing agent: get the 0.1g methylcellulose and be dissolved in the 95ml water, add the 34mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains 9mg formaldehyde.Stir and continue 5～6 hours.Promptly get stabilized nanoscale silver solution.
Transmission electron microscope results shows: the nano-Ag particles size distribution is in 80～100nm, average 90nm.
Embodiment 3
With the high polymer is the Nano silver solution preparation method of stabilizing agent: get the 1g polyvinylpyrrolidone and be dissolved in the 95ml water, add the 16mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the 40mg sodium borohydride.Stir and continue 12～15 hours.Promptly get stabilized nanoscale silver solution.
Transmission electron microscope results shows: the nano-Ag particles size distribution is in 20～30nm, average 27nm.
Embodiment 4
With the high polymer is the Nano silver solution preparation method of stabilizing agent: get the poly-carboxylic ethamine of 0.05g and be dissolved in the 95ml water, add the 34mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the ascorbic acid of 17.6mg.Stir and continue 5～6 hours.Promptly get stabilized nanoscale silver solution.
Transmission electron microscope results shows: the nano-Ag particles size distribution is in 20～50nm, average 30nm.
Embodiment 5
With the high polymer is the Nano silver solution preparation method of stabilizing agent: get 0.18g starch and be dissolved in the 95ml water, add the 34mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the glucose of 40mg.Spend the night 37 ℃ of stirrings.Promptly get stabilized nanoscale silver solution.
Transmission electron microscope results shows: the nano-Ag particles size distribution is in 3～10hm, average 5nm.Promptly be able to the Nano silver solution that starch is stabilizing agent.The Nano silver solution of gained can kill 96% bacterium (seeing shown in the accompanying drawing)
Embodiment 6
With the high polymer is the nano-silver powder preparation of stabilizing agent: get the 5g shitosan and be dissolved in the 95ml water, add the 1.69g silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the 3.5g ascorbic acid.Stir and continue 5～6 hours.Dropping sodium solution in the Nano silver solution, and filter.To filter gained solid distilled water wash, and under about 80 ℃ of conditions, dry.Dried sample is suitably ground dispersion.Promptly get nano silver powder.Transmission electron microscope results shows: the average 100nm of nano-Ag particles.
Embodiment 7
With the high polymer is the nano-silver powder preparation of stabilizing agent: get the 0.4g shitosan and be dissolved in the 95ml water, add the 16mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the 40mg sodium borohydride.Stir and continue 5～6 hours.Dropping sodium solution in the Nano silver solution, and filter.To filter gained solid distilled water wash, and under about 80 ℃ of conditions, dry.Dried sample is suitably ground dispersion.Promptly get nano silver powder.Transmission electron microscope results shows: the average 20nm of nano-Ag particles.
Embodiment 8
With the high polymer is the nano-silver powder preparation of stabilizing agent: get the 0.1g shitosan and be dissolved in the 95ml water, add the 16mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains 3mg formaldehyde.Stir and continue 5～6 hours.Dropping sodium solution in the Nano silver solution, and filter.To filter gained solid distilled water wash, and under about 80 ℃ of conditions, dry.Dried sample is suitably ground dispersion.Promptly get nano silver powder.Transmission electron microscope results shows: the average 5nm of nano-Ag particles.
Embodiment 9
With the high polymer is the nano-silver powder preparation of stabilizing agent: get the 2g shitosan and be dissolved in the 95ml water, add the 80mg silver nitrate, under vigorous stirring, slowly add the aqueous solution that 5ml contains the glucose of 200mg.Spend the night 37 ℃ of stirrings.Dropping sodium solution in the Nano silver solution, and filter.To filter gained solid distilled water wash, and under about 80 ℃ of conditions, dry.Dried sample is suitably ground dispersion.Promptly get nano silver powder.Transmission electron microscope results shows: the average 50nm of nano-Ag particles.
Claims (5)
1. one kind is the Nano silver solution preparation method of stabilizing agent with the high polymer, it is characterized in that concentration is that 0.001～0.05g/ml water soluble polymer stabilizing agent and concentration are that 0.001～0.1mol/L silver nitrate is compound, re-using concentration is that the water-soluble reductant of 0.001～0.2mol/L is reduced to Nano Silver with silver nitrate, and the particle diameter of Nano Silver is 5～100nm.
2. according to claim 1 a kind of be the Nano silver solution preparation method of stabilizing agent with the high polymer, it is characterized in that described water soluble polymer is: starch based derivative, shitosan, cellulose derivatives, polyvinylpyrrolidone or poly-carboxylic ethamine one or more.
3. according to claim 1 a kind of be the Nano silver solution preparation method of stabilizing agent with the high polymer, it is characterized in that described water-soluble reductant is: glucose, ascorbic acid, formaldehyde or sodium borohydride.
4. one kind is the nano-silver powder preparation of stabilizing agent with the high polymer, it is characterized in that, concentration is that 0.001～0.05g/ml shitosan stabilizing agent and concentration are that 0.001～0.1mol/L silver nitrate is compound, working concentration is that the water-soluble reductant of 0.001～0.2mol/L is reduced to Nano Silver with silver nitrate, re-use sodium hydroxide solution with Nano Silver deposition, washing, dry, pulverizing, obtaining particle diameter is the Nano Silver of 5～100nm.
5. according to claim 4 a kind of be the nano-silver powder preparation of stabilizing agent with the high polymer, it is characterized in that described water-soluble reductant is glucose, ascorbic acid, formaldehyde or sodium borohydride.
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