CN103042227A - Nano-silver sol antibacterial agent and preparation method thereof - Google Patents
Nano-silver sol antibacterial agent and preparation method thereof Download PDFInfo
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- CN103042227A CN103042227A CN2012105536143A CN201210553614A CN103042227A CN 103042227 A CN103042227 A CN 103042227A CN 2012105536143 A CN2012105536143 A CN 2012105536143A CN 201210553614 A CN201210553614 A CN 201210553614A CN 103042227 A CN103042227 A CN 103042227A
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Abstract
The invention discloses a nano-silver sol antibacterial agent and a preparation method thereof. The preparation method includes the steps: dissolving silver nitrate in water, adding ammonia water, adjusting pH (potential of hydrogen) to be 10+/-0.5 and adjusting the concentration of Ag+ to range from 0.006mol/l to 0.1mol/l to prepare silver ammonium solution; dissolving a reducing agent and a protective agent in the water to obtain reducing agent and protective agent solution; and slowly adding the reducing agent and protective agent solution into the silver ammonium solution according to the volume ratio of 1:1-5 of the reducing agent and protective agent solution to the silver ammonium solution when the silver ammonium solution is at 20-40 DEG C and 100-200rpm, performing ultrasonic operation for mixed solution for 5-20min under the condition of ice-bath after mixed reaction, and finally filtering the mixed solution to obtain colorless and transparent nano-silver sol antibacterial agent. In the silver ammonium solution, the quantity relative ratio of n (the reducing agent) to n (Ag+) is 1-5:1, the mass ratio of the n (the reducing agent to m (the protective agent) is 1-2:1, and output power is 150-200w. The nano-silver sol antibacterial agent can avoid agglomeration of nano-silver particles in long-term storage and use process.
Description
Technical field
The invention belongs to the antiseptic preparation field, be specifically related to a kind of efficient, environmental protection, nano silver colloidal sol antiseptic of agglomeration and preparation method thereof can not occur.
Background of invention
Along with a large amount of uses of the chemicalses such as antibiotic, disinfectant and bactericide, more and more because of the microbial variation population that drug resistance causes, the global microbial plague event that is caused by microorganism and mutation thereof occurs again and again.For the generation of the malignant event that prevents these harm humans health, in the urgent need to the research and development of novel antibacterial material.Nano Silver is owing to have good anti-microbial property, be described as the antiseptic of 21st century a new generation, its application market is wide, can be applicable to daily necessities field (various clothes, clothes and all kinds of abrasive item are such as cotton-wadded quilt, pillow, sanitary napkin, underwear pants, Children's diaper, cosmetics, shampoo, toothpaste, perfumed soap, food, tableware etc.), medicine and hygiene fields (is used for medical apparatus sterilizing, externally used antimicrobial medicine and health products, beauty treatment instrument and care product, purification of water quality, the aspects such as agricultural plant bactericide), building materials field (is used for coating, paint, timber floor, the aspects such as pottery), electronics industry (is used for computer, television set, mobile phone, the antibiotic and sterilizing of the electronic products such as automobile) etc.The good anti-microbial property of Nano Silver is mainly manifested in the following aspects: 1. Nano Silver has the anti-microbial property of wide spectrum.Nano Silver not only has antibacterial activity to bacterium, and can press down antifungal and viral, has a broad antifungal spectrum.2. Nano Silver has efficient antibacterial activity.With other Metal Phase ratio, the antibacterial activity of silver ranks first, Nano Silver is again because its atomic arrangement is " Jie's attitude " between solid and molecule, show quantum effect, small-size effect and great specific area, has the antibacterial activity that is far superior to silver ion, the antibiotic concentration of silver ion is in micromole's level, and the antibiotic concentration of Nano Silver is in the nanomole level.3. Nano Silver has the advantage of low toxicity.So-called low toxicity refers to that Nano Silver is low to mammalian toxicity, environmental friendliness, but but very large to the toxicity of microorganism.4. Nano Silver has and is difficult for making the drug-fast advantage of microorganisms.So far be separated to both at home and abroad can anti-silver microorganism very little, and according to the present Research foundation in this laboratory, even can filter out the microorganism of tolerance low-concentration metallic silver by progressively improving silver concentration, but the characteristic of this microorganism tolerance silver can not genetic stability, the phenomenon that its anti-silver-colored characteristic can suddenly disappear after going down to posterity.5. the anti-microbial property of Nano Silver is far superior to the Ag-carried antibacterial material of other form, the various forms of compounds of silver ion, silver, silver zeolite etc., and their anti-microbial property all is nothing like Nano Silver.
But Nano Silver is not adding under protectant normal condition, and nano silver particles occurs easily to reunite and loses nano-meter characteristic, affects its antibacterial effect.The agglomeration of Nano Silver has limited its research and application in some field.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have wide spectrum, efficient antibacterial activity, and nano silver colloidal sol antiseptic of nano silver particles agglomeration and preparation method thereof can not occur in long term storage and use procedure.
Nano silver colloidal sol antiseptic of the present invention prepares by the following method, and this preparation method may further comprise the steps: silver nitrate is soluble in water, and add ammoniacal liquor, regulate pH to 10 ± 0.5, Ag
+Concentration is 0.006~0.1mol/l, makes silver-colored ammonium salt solution; Reducing agent and protective agent is soluble in water, obtain reducing agent and protective agent solution; Be in 20~40 ℃ at silver-colored ammonium salt solution; under 100~200rpm condition, with reducing agent and protective agent solution by volume reducing agent and protective agent solution: silver-colored ammonium salt solution is that the ratio of 1:1 ~ 5 slowly joins in the silver-colored ammonium salt solution, and makes in the solution; press molar ratio, the n(reducing agent): n(Ag
+) be 1 ~ 5:1, in mass ratio, the m(reducing agent): the m(protective agent) be 1~2:1; after the hybrid reaction, mixed liquor is carried out ultrasonic 5 ~ 20min under condition of ice bath, power output is 150~200w; at last mixed liquor is filtered, make water white nano silver colloidal sol antiseptic.Can as the case may be solution be concentrated or dilute during use, also can be prepared into nano-silver powder through freeze drying.
Described reducing agent is preferably ascorbic acid, glucose or fructose.
Described protective agent is preferably polyvinylpyrrolidone (PVP), beta-schardinger dextrin-or gelatin.
Described with reducing agent and protective agent solution by volume reducing agent and protective agent solution: silver-colored ammonium salt solution is that the ratio of 1:1 ~ 5 slowly joins in the silver-colored ammonium salt solution and preferably slowly adds reducing agent and protective agent solution by constant pressure funnel or buret.
Principle of the present invention is: utilize the reducing agents such as ascorbic acid with silver ion reduction, the principle of this chemical reaction is exactly usually said silver mirror reaction, and chemical equation is as follows:
CH
2OH-(CHOH)
4-CHO+2Ag(NH
3)
2OH-------H
2O+2Ag!+3NH
3+CH
2OH-(CHOH)
4-COONH
4
According to above-mentioned preparation method, can prepare particle diameter less than nano silver colloidal sol or the nano-silver powder of 100nm, agglomeration can not occur in the nano silver colloidal sol of the present invention's preparation, therefore overcome Nano Silver agglomeration traits in use, the application of nano silver antimicrobials be can widen, development and the extensive use of nano silver antimicrobials promoted.
The specific embodiment:
Embodiment 1:
Take by weighing the 10.2mg silver nitrate, be dissolved in the 5ml deionized water, add ammoniacal liquor, transfer pH to 10, deionized water is settled to 10ml, and namely concentration of silver ions is 0.006mol/l, obtains silver-colored ammonium salt solution.Take by weighing the PVP of 10.6mg ascorbic acid and 10.6mg, be dissolved in the 10ml deionized water, obtain reducing agent and protective agent solution.Reducing agent and protective agent solution are added drop-wise in the silver-colored ammonium salt solution by buret in room temperature; in the process that adds; the silver ammonium salt solution is in 40 ℃; under the 100rpm condition, and the control rate of addition first quick and back slow, after the hybrid reaction; with mixed liquor ultrasonic 10min under condition of ice bath; power output is 190W, and the colloidal sol of at last reaction being finished membrane filtration one time obtains clarifying water white nano silver colloidal sol antiseptic.
After measured, the nano silver colloidal sol antiseptic of present embodiment, its silver particles particle diameter is 5~50nm, stores 12 months and opens and uses the nano silver colloidal sol antiseptic of placing 6 months present embodiments and still clarify water white transparency, agglomeration can not occur in nano silver particles.
Embodiment 2:
Take by weighing the 0.51g silver nitrate, be dissolved in the 25ml deionized water, add ammoniacal liquor, regulate pH to 10, deionized water is settled to 50ml, and making concentration of silver ions is 0.06mol/l, makes silver-colored ammonium salt solution.Take by weighing ascorbic acid 2g, PVP1g is dissolved in the 50ml deionized water, obtains reducing agent and protective agent solution.Reducing agent and protective agent solution are added drop-wise in the silver-colored ammonium salt solution by buret in room temperature, in the process that adds, silver-colored ammonium salt solution is in 20 ℃; under the 200rpm condition, and the control rate of addition first quick and back slow, after the hybrid reaction; with mixed liquor ultrasonic 10min under condition of ice bath, power output is 200W.The mixed liquor of at last reaction being finished membrane filtration one time obtains clarifying water white nano silver colloidal sol antiseptic.
After measured, the nano silver colloidal sol antiseptic of present embodiment, its silver particles particle diameter is 5~50nm, stores 12 months and opens and uses the nano silver colloidal sol antiseptic of placing 6 months present embodiments and still clarify water white transparency, agglomeration can not occur in nano silver particles.
Embodiment 3:
Take by weighing the 0.102g silver nitrate, be dissolved in the 15ml deionized water, add ammoniacal liquor, regulate pH to 10.5, deionized water is settled to 30ml, and making concentration of silver ions is 0.02mol/l, makes silver-colored ammonium salt solution.Take by weighing ascorbic acid 0.5g, PVP0.4g is dissolved in the 60ml deionized water, obtains reducing agent and protective agent solution.Reducing agent and protective agent solution are added drop-wise in the silver-colored ammonium salt solution by buret in room temperature, in the process that adds, silver-colored ammonium salt solution is in 30 ℃; under the 150rpm condition, and the control rate of addition first quick and back slow, after the hybrid reaction; with mixed liquor ultrasonic 5min under condition of ice bath, power output is 200W.The mixed liquor of at last reaction being finished membrane filtration one time obtains clarifying water white nano silver colloidal sol antiseptic.
After measured, the nano silver colloidal sol antiseptic of present embodiment, its silver particles particle diameter is 5~50nm, stores 12 months and opens and uses the nano silver colloidal sol antiseptic of placing 6 months present embodiments and still clarify water white transparency, agglomeration can not occur in nano silver particles.
Embodiment 4:
Take by weighing the 1.7g silver nitrate, be dissolved in the 50ml deionized water, add ammoniacal liquor, regulate pH to 9.5, deionized water is settled to 100ml, and making concentration of silver ions is 0.1mol/l, makes silver-colored ammonium salt solution.Take by weighing ascorbic acid 7g, PVP4g is dissolved in the 100ml deionized water, obtains reducing agent and protective agent solution.Reducing agent and protective agent solution are added drop-wise in the silver-colored ammonium salt solution by buret in room temperature, in the process that adds, silver-colored ammonium salt solution is in 30 ℃; under the 150rpm condition, and the control rate of addition first quick and back slow, after the hybrid reaction; with mixed liquor ultrasonic 8min under condition of ice bath, power output is 200W.The mixed liquor of at last reaction being finished membrane filtration one time obtains clarifying water white nano silver colloidal sol antiseptic.
After measured, the nano silver colloidal sol antiseptic of present embodiment, its silver particles particle diameter is 5~50nm, stores 12 months and opens and uses the nano silver colloidal sol antiseptic of placing 6 months present embodiments and still clarify water white transparency, agglomeration can not occur in nano silver particles.
Embodiment 5:
Take by weighing the 3.4mg silver nitrate, be dissolved in the 10ml deionized water, add ammoniacal liquor, regulate pH to 10, deionized water is settled to 20ml, and making concentration of silver ions is 0.001mol/l, makes silver-colored ammonium salt solution.Take by weighing ascorbic acid 5mg, PVP5mg is dissolved in the 20ml deionized water, obtains reducing agent and protective agent solution.Reducing agent and protective agent solution are added drop-wise in the silver-colored ammonium salt solution by buret in room temperature, in the process that adds, silver-colored ammonium salt solution is in 30 ℃; under the 150rpm condition, and the control rate of addition first quick and back slow, after the hybrid reaction; with mixed liquor ultrasonic 20min under condition of ice bath, power output is 150W.The mixed liquor of at last reaction being finished membrane filtration one time obtains clarifying water white nano silver colloidal sol antiseptic.
After measured, the nano silver colloidal sol antiseptic of present embodiment, its silver particles particle diameter is 5~50nm, stores 12 months and opens and uses the nano silver colloidal sol antiseptic of placing 6 months present embodiments and still clarify water white transparency, agglomeration can not occur in nano silver particles.
Embodiment 6:
Take by weighing the 10.2mg silver nitrate, be dissolved in the 5ml deionized water, add ammoniacal liquor, regulate pH to 10, deionized water is settled to 10ml, and making concentration of silver ions is 0.006mol/l, makes silver-colored ammonium salt solution.Take by weighing ascorbic acid 53mg, PVP53mg is dissolved in the 50ml deionized water, obtains reducing agent and protective agent solution.Reducing agent and protective agent solution are added drop-wise in the silver-colored ammonium salt solution by buret in room temperature, in the process that adds, silver-colored ammonium salt solution is in 30 ℃; under the 150rpm condition, and the control rate of addition first quick and back slow, after the hybrid reaction; with mixed liquor ultrasonic 10min under condition of ice bath, power output is 190W.The mixed liquor of at last reaction being finished membrane filtration one time obtains clarifying water white nano silver colloidal sol antiseptic.
After measured, the nano silver colloidal sol antiseptic of present embodiment, its silver particles particle diameter is 5~50nm, stores 12 months and opens and uses the nano silver colloidal sol antiseptic of placing 6 months present embodiments and still clarify water white transparency, agglomeration can not occur in nano silver particles.
Claims (5)
1. the preparation method of a nano silver colloidal sol antiseptic is characterized in that, may further comprise the steps: silver nitrate is soluble in water, and add ammoniacal liquor, regulate pH to 10 ± 0.5, Ag
+Concentration is 0.006~0.1mol/l, makes silver-colored ammonium salt solution; Reducing agent and protective agent is soluble in water, obtain reducing agent and protective agent solution; Be in 20~40 ℃ at silver-colored ammonium salt solution; under 100~200rpm condition, with reducing agent and protective agent solution by volume reducing agent and protective agent solution: silver-colored ammonium salt solution is that the ratio of 1:1 ~ 5 slowly joins in the silver-colored ammonium salt solution, and makes in the solution; press molar ratio, the n(reducing agent): n(Ag
+) be 1 ~ 5:1, in mass ratio, the m(reducing agent): the m(protective agent) be 1~2:1; after the hybrid reaction, mixed liquor is carried out ultrasonic 5 ~ 20min under condition of ice bath, power output is 150~200w; at last mixed liquor is filtered, make water white nano silver colloidal sol antiseptic.
2. preparation method according to claim 1 is characterized in that, described reducing agent is ascorbic acid, glucose or fructose.
3. preparation method according to claim 1 is characterized in that, described protective agent is polyvinylpyrrolidone, beta-schardinger dextrin-or gelatin.
4. preparation method according to claim 1; it is characterized in that described with reducing agent and protective agent solution by volume reducing agent and protective agent solution: silver-colored ammonium salt solution is that the ratio of 1:1 ~ 5 slowly joins in the silver-colored ammonium salt solution is slowly to add reducing agent and protective agent solution by constant pressure funnel or buret.
5. nano silver colloidal sol antiseptic for preparing according to claim 1,2,3 or 4 described preparation methods.
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CN103406548A (en) * | 2013-08-08 | 2013-11-27 | 广西大学 | Silver nano particle and preparation method and application thereof |
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 |
CN104308180A (en) * | 2014-10-16 | 2015-01-28 | 天津大学 | Preparation method of organic-system high-concentration nano silver sol |
CN104403448A (en) * | 2014-10-23 | 2015-03-11 | 中油新星纳米工程技术有限公司 | Nano cuprous oxide and nano silver compounded sea anti-fouling paint |
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