CN102240815A - Method for preparing nano silver particles by using plant extract for reduction, and application of method - Google Patents
Method for preparing nano silver particles by using plant extract for reduction, and application of method Download PDFInfo
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- CN102240815A CN102240815A CN2011101617240A CN201110161724A CN102240815A CN 102240815 A CN102240815 A CN 102240815A CN 2011101617240 A CN2011101617240 A CN 2011101617240A CN 201110161724 A CN201110161724 A CN 201110161724A CN 102240815 A CN102240815 A CN 102240815A
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Abstract
The invention discloses a method for preparing nano silver particles by using plant extract for reduction, and application of the method. In the method, the extract of natural plants such as chrysanthemum, honeysuckle flower, or bud of Japanese pagoda tree which serves as a reducing agent reacts with Ag<+> in aqueous solution of silver nitrate to ensure that Ag<+> is reduced into elementary substance silver nano particles. The method is simple, reaction conditions are mild, additives except for silver nitrate are not needed, the plant extract which is low in cost and can be easily obtained is used as the reducing agent, and the method is environment-friendly; the nano silver particles obtained by the method have smaller diameters, and high dispersibility and stability in aqueous solution; and Chinese herbal medicine components which have the effects of antibiosis and antiphlogosis are added, and the method has the characteristics of disinfection and sterilization, bacteriostasis, safety, no toxicity or irritation and the like and can be directly applied to multiple kinds of dermatological and surgical bacterial infection or medical equipment and cosmetics.
Description
Technical field
The present invention relates to a kind of nano-Ag particles, especially relate to method and application thereof that a kind of reducing plant extract prepares nano-Ag particles.
Background technology
The bactericidal properties of silver just has been found that as far back as 1938 people at that time puts into milk with silver coin, so Ke Yan Long milk Cun Fang Time Inter in air.United states drug Food and Drug Administration (FDA) employed common silver-colored particle before pointing out the Nano Silver ratio on the file of delivering on September 13rd, 1991 has stronger biocidal efficacies.Argent itself has bactericidal, the prevention wound festers and the effect of accelerating wound healing, sharply increase through its specific area after the nanometer technology, sterilizing ability can improve about 300 times, and antibacterial activity is difficult for consuming with reaction simultaneously, can keep original bactericidal ability for a long time.Nano Silver Related product Application and Development is quite extensive on the market at present, comprises products such as medical nano silver gel, bandage, socks, water fountain, air-conditioning, refrigerator and washing machine, has extensive market prospects.
The antibacterial mechanisms of Nano Silver mainly is that the silver-colored particle of nanometer can discharge positively charged silver ion, behind the bacterial cell of silver ion contact zones negative electrical charge, can be because silver ion and protein (specificity combination SH), pierce through cell membrane and cell membrane appearance, combine with protease, make bacterial cell can't metabolism, schizogamy, until death.
The preparation method of Nano Silver is always based on physics method and chemical method, but they exist higher, the easy contaminated environment of production cost, and the while is more residual harmful compositions in product easily.In recent years, there is the researcher to report abroad successively and can utilizes the plant extracts synthesizing nano-silver.As utilize the reduction of manioca emulsion to prepare nano-Ag particles (Colloids and Surfaces A:Physicochemical andEngineering Aspects, 2009 (339) 134-139.), utilize fish pelargonium to boil liquid reduction preparation Nano Silver (Biotechnology ProgressVolume 19, Issue 6, pages 1627-1631,2003.) utilize pepper extract synthesizing nano-silver (Green Chemistry, 2007,9,852-858.).
At normal temperatures, utilize plant biomass or extract Ag+ reduction can be become nano-Ag particles, its reduction rate and and prepared nano-Ag particles can compare favourably with the traditional preparation process method, can effectively develop the natural plant resource of China's abundant.
Because a lot of natural Chinese medicinal herb of China itself have very good bactericidal ability (as mother chrysanthemum, buds of japanese pagoda tree etc.), by Chinese medical extract and Nano Silver synergy, it is stronger to obtain sterilizing ability, nontoxic to human body, use Nano Silver product more widely.
Summary of the invention
The present invention is intended at the deficiencies in the prior art, provides that a kind of the preparation method is simple under temperate condition, utilizes plant extraction liquid Ag+ to be reduced into the method for Nano Silver.
Another object of the present invention is to provide the bactericidal of above-mentioned nano-Ag particles in various dept. of dermatology, surgery bacterial infection or medicine equipment and cosmetics to use.
Above-mentioned purpose of the present invention is achieved by following scheme:
Get raw material chrysanthemum, honeysuckle or bud of japanese pagoda tree or three and make up arbitrarily, add the water or the ethanol water of certain mass, it is plant extraction liquid that gained filtrate is filtered in the heating back, and plant extraction liquid and liquor argenti nitratis ophthalmicus than mixing, promptly make nano-Ag particles with certain mass.
The raw material of above-mentioned preparation plant extraction liquid and water or ethanol water mass ratio are 0.01～2: 1; Plant extraction liquid and liquor argenti nitratis ophthalmicus mass ratio are 0.5～11: 1.
The whole molar concentration of the silver ion of above-mentioned liquor argenti nitratis ophthalmicus is 0.02mM～10M.
The reaction time that above-mentioned plant extraction liquid mixes with liquor argenti nitratis ophthalmicus is 2～120h.
Reducing plant extract provided by the invention prepares nano-Ag particles and uses at preparation dept. of dermatology, surgery bacterial-infection resisting medicine and the bactericidal in medicine equipment or cosmetics.
Compared with prior art, the present invention has following beneficial effect:
1. chrysanthemum of the present invention, honeysuckle, bud of japanese pagoda tree medicinal history are long, have the effect clearing heat and detoxicating, that sterilization is antibiotic, have safe, nontoxic, non-stimulated characteristics, and the scope of application is extensive;
2. preparation method of the present invention is simple, environmentally friendly, needn't control reaction condition and temperature, and cost of material is cheap;
3. by using plant extracts to make reducing agent innovatively, make the bactericidal property of product be enhanced, security gets a promotion, therefore add in various gels, coating, commodity, the textile, and be applied in the various inflammation of treatment, dept. of dermatology, surgical infection or medicine equipment and the cosmetics.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) figure of the nano-Ag particles of reducing plant extract preparation of the present invention.Fig. 1 as can be seen, the particle diameter of the nano-Ag particles that reducing plant extract prepares is little, good uniformity, good dispersion.
Fig. 2 is high-resolution-ration transmission electric-lens (TEM) figure of the nano-Ag particles of reducing plant extract preparation of the present invention.Fig. 2 as can be seen, high-resolution-ration transmission electric-lens shows that nano-Ag particles forms nanostructure thickness and only is
Crystalline thin layer, between the crystal layer nano-Ag particles distance be
Fig. 3 is the antibacterial experiment design sketch of the nano-Ag particles of reducing plant extract preparation of the present invention.Micro-Organism Culture Dish is the Nano Silver that has added the reducing plant extract preparation of 8ppm concentration among Fig. 3.The nano-Ag particles that can be seen the reducing plant extract preparation by Fig. 3 has the good sterilization effect to staphylococcus aureus, and fungistatic effect reaches 99.99%.
Fig. 4 is the antibacterial experiment blank sheet of the nano-Ag particles of invention reducing plant extract preparation.Micro-Organism Culture Dish is the normal growth staphylococcus aureus that does not add the Nano Silver of reducing plant extract preparation among Fig. 4.
The specific embodiment
Below in conjunction with concrete case study on implementation the present invention is described further, but specific embodiment is not done any qualification to the present invention.
Embodiment 1
Take by weighing 0.5g chrysanthemum dry powder after dry chrysanthemum is pulverized, add 50mL distilled water, filter the heating back in the 1000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 100mL
3React in the solution, the silver nitrate final concentration is 0.1mM, obtain nano-Ag particles behind the reaction 5h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 30.8nm.
Embodiment 2
Take by weighing 100g chrysanthemum dry powder after dry chrysanthemum is pulverized, add 900mL distilled water and 100mL ethanol, filter the heating back in the 2000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 200mL
3React in the solution, the silver nitrate final concentration is 10mM, obtain nano-Ag particles behind the reaction 120h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 25.8nm.
Embodiment 3
Take by weighing 50g chrysanthemum dry powder after dry chrysanthemum is pulverized, add 250mL distilled water, filter the heating back in the 1000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 300mL
3React in the solution, the silver nitrate final concentration is 10mM, obtain nano-Ag particles behind the reaction 2h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 32.8nm.
Embodiment 4
Take by weighing 100g after dry bud of japanese pagoda tree is pulverized, add 50mL distilled water, filter the heating back in the 1000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 150mL
3React in the solution, the silver nitrate final concentration is 0.5mM, obtain nano-Ag particles behind the reaction 24h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 24.8nm.
Embodiment 5
Respectively take by weighing 40g after dry chrysanthemum and bud of japanese pagoda tree are pulverized, both mix the back and add 800mL distilled water, and filter the heating back in the 2000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 200mL
3React in the solution, the silver nitrate final concentration is 10M, obtain nano-Ag particles behind the reaction 96h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 27.1nm.
Embodiment 6
Dry chrysanthemum, bud of japanese pagoda tree and honeysuckle respectively take by weighing 30g after pulverizing, and the three mixes the back and adds 300mL distilled water and 200mL ethanol, and filter the heating back in the 2000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 100mL
3React in the solution, the silver nitrate final concentration is 1M, obtains nano-Ag particles behind the reaction 48h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, and the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 30.0nm.
Embodiment 7
Dry chrysanthemum, bud of japanese pagoda tree and honeysuckle respectively take by weighing 25g after pulverizing, and the three mixes the back and adds 500mL distilled water and 100mL ethanol, and filter the heating back in the 2000mL beaker.The gained plant extraction liquid is added drop-wise to the AgNO of 100mL
3React in the solution, the silver nitrate final concentration is 5M, obtains nano-Ag particles behind the reaction 72h, get Nano silver solution with ZETA current potential particle diameter instrument and transmission electron microscope (TEM) observation post, wherein the pattern of nano-Ag particles is subsphaeroidal, and the particle diameter overwhelming majority is distributed in 20～80nm, and average grain diameter is 29.0nm.
Embodiment 8
The present embodiment reducing plant extract prepares nano-Ag particles and is applied in the medical ultrasonic coupling agent, and its raw material is made up of each component of following parts by weight:
It is as follows that present embodiment prepares the medical ultrasonic coupling agent step:
In the enamel agitated kettle, in carbomer, glycerine, add the part deionized water, stirring and dissolving, the Nano Silver concentration that adds 100mL then is the Nano silver solution of the reducing plant extract preparation of 500 μ g/mL, stir, supply the surplus deionized water, add small amount of N aOH solution and regulate pH value and viscosity, control about whole system pH=6.
Embodiment 9
The present embodiment reducing plant extract prepares nano-Ag particles and is applied in cosmetics antibiotic anticorrosion, and its raw material is made up of each component of following parts by weight:
The present embodiment reducing plant extract prepares nano-Ag particles, and to be applied in the cosmetics step as follows:
Add stearic acid, monoglyceride, glycerine at the single neck round-bottomed flask of 250mL, 70 ℃ of water-bath heating fully mix, and mixing speed is controlled at about 4000r/min, after the lotion exquisiteness is even, add the Nano silver solution of reducing plant extract preparation, stop reaction after stirring.
Embodiment 10
The present embodiment reducing plant extract prepares nano-Ag particles and is applied in the antibacterial gel, and its raw material is made up of each component of following parts by weight:
The present embodiment reducing plant extract prepares nano-Ag particles, and to be applied in the antibacterial gel step as follows:
Carboxymethyl cellulose is added in the deionized water, add the Nano silver solution of glycerine, dodecyl sodium sulfate, reducing plant extract preparation after heating for dissolving stirs, obtain the nano silver antimicrobial gel of reducing plant extract preparation behind the stirring 15min.
Embodiment 11
Present embodiment test plants extract reduction preparation nano-Ag particles particle diameter distribution situation, the average grain diameter that is obtained the nano-Ag particles of reducing plant extract preparation by Zeta potential particle diameter distribution instrument examining report is 27.1nm, particle size distribution data shows that Nano Silver size major part is at 12.99～34.37nm, particle diameter distributes more concentrated, particle size distribution data such as following table:
Claims (5)
1. a reducing plant extract prepares the method for nano-Ag particles, it is characterized in that this method has following steps: get raw material chrysanthemum, honeysuckle or bud of japanese pagoda tree or three and make up arbitrarily, the water or the ethanol water that add certain mass, it is plant extraction liquid that gained filtrate is filtered in the heating back, plant extraction liquid and liquor argenti nitratis ophthalmicus than mixing, promptly make nano-Ag particles with certain mass.
2. reducing plant extract as claimed in claim 1 prepares the method for nano-Ag particles, it is characterized in that: the raw material of above-mentioned preparation plant extraction liquid and water or ethanol water mass ratio are 0.01 ~ 2:1; Plant extraction liquid and liquor argenti nitratis ophthalmicus mass ratio are 0.5 ~ 11:1.
3. reducing plant extract as claimed in claim 1 prepares the method for nano-Ag particles, it is characterized in that: the whole molar concentration of the silver ion of above-mentioned liquor argenti nitratis ophthalmicus is 0.02mM ~ 10M.
4. reducing plant extract as claimed in claim 1 prepares the method for nano-Ag particles, it is characterized in that: the reaction time that above-mentioned plant extraction liquid mixes with liquor argenti nitratis ophthalmicus is 2 ~ 120h.
5. the described reducing plant extract of claim 1 prepares nano-Ag particles in preparation dept. of dermatology, surgery bacterial-infection resisting medicine and the application of the bactericidal in medicine equipment or cosmetics.
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