CN103999873A - Nano-silver antibacterial agent and preparation method thereof - Google Patents
Nano-silver antibacterial agent and preparation method thereof Download PDFInfo
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- CN103999873A CN103999873A CN201410273548.3A CN201410273548A CN103999873A CN 103999873 A CN103999873 A CN 103999873A CN 201410273548 A CN201410273548 A CN 201410273548A CN 103999873 A CN103999873 A CN 103999873A
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Abstract
The invention provides a nano-silver antibacterial agent which includes nano-silver antibacterial stock solutions. Nano-silver is included in the nano-silver antibacterial stock solutions, and the content of the nano-silver is 0.00025 mol/kg to 0.02 mol/kg. The invention further provides a preparation method of the nano-silver antibacterial agent. The nano-silver antibacterial agent can be foam emulsion and sprays in a flow state, can be used as washing-free sprays, and is convenient for people to use when cleaning with water is inconvenient in travel.
Description
Technical field
The present invention relates to a kind of Antimicrobial sanitation articles for use, relate in particular to a kind of nano silver antimicrobials and preparation method thereof.
Background technology
In life, be flooded with various noxious bacterias.Thereby people often have clean demand in daily life.Yet existing washing agent is mainly hydrophilic, the oleophylic double-basis group that utilizes surfactant wherein, under the drive of water, will be taken away by the oiliness group at the place of washing, but it does not often possess antibiotic property.
Nano Silver is a class antibacterial agent, has the antibacterial activity of powerful antibacterial, bactericidal action and wide spectrum thereof, has the incomparable antibacterial effect of traditional inorganic antiseptic, has no drug resistance, safe.Along with antibiotic bacterial drug resistance is day by day serious, Nano Silver has more and more been subject to paying close attention to widely in research and the application in disinfection field.
Prior art, is added directly to nano silver particles in washing agent, to prepare the washing agent with antibiotic property.But this technology has following deficiency: 1. Nano Silver is stablized not, easily reunited in washing agent; 2. the dispersion of Nano Silver in washing agent is even not.Though existing, there is the silica of employing as carrier, to prepare the silica supports anti-biotic material of carrying nano silver, have not yet to see, do not adopt any Nano Silver carrier to overcome the technical scheme of preparing nano silver antibacterial material of above-mentioned technical problem.
Summary of the invention
In order to overcome above-mentioned technical problem, the invention provides a kind of nano silver antimicrobials that does not contain any Nano Silver carrier, this nano silver antimicrobials has good stability, uniformly dispersed.In addition, the present invention also provides a kind of preparation method of above-mentioned nano silver antimicrobials.
A nano silver antimicrobials, it contains nanometer silver antimicrobial stoste, in described nanometer silver antimicrobial stoste, contains Nano Silver, and wherein, the content of described Nano Silver is 0.00025-0.02mol/kg.
Preferably, the particle diameter of described Nano Silver is 1-100nm.
More preferably, described nanometer silver antimicrobial stoste also contains protectant, and described protectant is selected from least one in polyethylene glycol, polypropylene glycol, ethylene glycol, sorbierite, sodium citrate, polyvinylpyrrolidone, carboxymethyl cellulose, calgon and urea.
Preferably, described nano silver antimicrobials also contains thickener, and described thickener is selected from least one in sodium chloride, sodium citrate and carboxymethyl cellulose.
More preferably, the weight percentage of described thickener is 0-2%.
Preferably, described nano silver antimicrobials also contains chelating agent, and described chelating agent is selected from least one in disodium ethylene diamine tetraacetate or sodium citrate.
More preferably, the weight percentage of described chelating agent is 0-2%.
The preparation method of described nano silver antimicrobials, comprises the steps:
Silver nitrate is mixed with protectant;
Adopt photo-reduction, the Ag reducing in above-mentioned silver nitrate with ultraviolet excitation photoelectron
+, obtain nanometer silver antimicrobial stoste;
Nanometer silver antimicrobial stoste, surfactant, thickener, chelating agent, cosolvent, preservative, flavoring essence are mixed and stirred with pigment and water.
Preferably, the weight percentage of described nanometer silver antimicrobial stoste is 5%-20%.
More preferably, in described nano silver antimicrobials, the quality percentage composition of surfactant is 0%-30%, the quality percentage composition of thickener is 0-5%, the quality percentage composition of chelating agent is 0-2%, and the quality percentage composition of cosolvent is 0-70%, and the quality percentage composition of preservative is 0-0.002%, the quality percentage composition of flavoring essence and pigment is 0-0.03%, and surplus is water.
Compared to prior art, tool of the present invention has the following advantages:
1. the interpolation of thickener described in, can improve the viscosity of nano silver antimicrobials, makes it by liquid state, change fluidised form into, more convenient during use; Meanwhile, described thickener also has emulsification, stable or make nano silver antimicrobials be the effect of suspended state, keeps being uniformly distributed of each composition, particularly Nano Silver in nano silver antimicrobials, so can improve the antibiotic property of nano silver antimicrobials.
2. chelating agent and metal ion-chelant described in, can improve feel and the comfort level of nano silver antimicrobials; Meanwhile, described chelating agent also has non-oxidizability, can better protect skin.
3. described in, cosolvent can promote the low-temperature stability of nano silver antimicrobials, reduces congealing point and the cloud point of nano silver antimicrobials.
4. in photo catalytic reduction process, described protectant interpolation can prevent from producing and reuniting in Nano Silver reduction process, and augmenting response area, promotes reduction reaction to carry out thoroughly simultaneously.
5. described in, nano antibacterial agent can be whipped cream, the spray of fluidised form, can be used as disposable spray, is convenient for people to use when the inconvenient waters such as tourism are clean.
Embodiment
The invention provides a kind of nano silver antimicrobials, whipped cream, spray that it can be fluidised form, can be used as washing agent, hand cleanser, spray etc.; In addition, described nano silver antimicrobials also can be used as disposable spray, is convenient for people to use when the inconvenient waters such as tourism are clean.
Described nano silver antimicrobials contains nanometer silver antimicrobial stoste, surfactant, thickener, chelating agent, cosolvent, preservative, flavoring essence and pigment and water, and wherein, the percentage by weight of above-mentioned each composition is as follows:
Nanometer silver antimicrobial stoste: 5%-20%;
Surfactant: 0%-30%, preferably, 5-20%; When nano silver antimicrobials is spray, the preferred 0-2% of surfactant;
Thickener: 0-5%, preferably, 0.5-5%; When nano silver antimicrobials is that spray can not added thickener;
Chelating agent: 0-2%, preferably, 0.1-2%; When nano silver antimicrobials is spray, the preferred 0-2% of chelating agent;
Cosolvent: 0-70%, preferably, 0.5-10%; When nano silver antimicrobials is spray, cosolvent is preferably 0.5-70%;
Preservative: 0-0.002%, preferably, 0.001-0.002%; When nano silver antimicrobials is spray, preservative is preferably 0-0.001%;
Flavoring essence and pigment: 0-0.03%, preferably, 0.02-0.03%; When nano silver antimicrobials is spray, flavoring essence and pigment are preferably 0-0.02g;
Water: surplus.
In described nanometer silver antimicrobial stoste, contain Nano Silver, wherein, the content of described Nano Silver is 0.00025-0.02mol/kg, and the particle diameter of described Nano Silver is 1-100nm; Preferably, the particle diameter of Nano Silver is 3-20nm.Further; described nanometer silver antimicrobial stoste also contains protectant, and described protectant is selected from least one in polyethylene glycol, polypropylene glycol, ethylene glycol, sorbierite, sodium citrate, polyvinylpyrrolidone (PVP), carboxymethyl cellulose, calgon and urea.
Described surfactant is selected from least one in sodium n-alkylbenzenesulfonate, sodium sulfate of polyethenoxy ether of fatty alcohol, sodium alkyl sulfate, dodecyl sodium sulfate, alkyl poly glucoside, polyethylene pyrrole network alkane ketone, dodecyldimethylammonium hydroxide inner salt, glycerin monostearate and hydrolecithin.In the present embodiment, adopt the alkyl poly glucoside that quality percentage composition is 70%.
Described thickener is selected from least one in sodium chloride, sodium citrate and carboxymethyl cellulose.Described thickener, can improve the viscosity of nano silver antimicrobials, makes it by liquid state, change fluidised form into, more convenient during use; Meanwhile, described thickener also has emulsification, stable or make nano silver antimicrobials be the effect of suspended state, keeps being uniformly distributed of each composition, particularly Nano Silver in nano silver antimicrobials, so can improve the antibiotic property of nano silver antimicrobials.
Described chelating agent is selected from least one in disodium ethylene diamine tetraacetate or sodium citrate.Described chelating agent and metal ion-chelant, can improve feel and the comfort level of nano silver antimicrobials; Meanwhile, described chelating agent also has non-oxidizability, can better protect skin.
Described cosolvent is selected from least one in ethanol, polyethylene glycol, urea, isopropyl alcohol, dimethyl sulfoxide (DMSO) and glycerine.The effect of described cosolvent is the low-temperature stability that promotes nano silver antimicrobials, reduces congealing point and the cloud point of nano silver antimicrobials.
Described preservative is selected from least one in Kathon CG, Phenoxyethanol, nipagin esters.
The present invention also provides the preparation method of described nano silver antimicrobials, comprises the steps;
The first step: the silver nitrate aqueous solution that preparation 1L concentration is 0.005-0.1mol/L; According to silver nitrate and protectant, with the mol ratio of 1:20-5:1, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is selected from least one in polyethylene glycol, polypropylene glycol, ethylene glycol, sorbierite, sodium citrate, polyvinylpyrrolidone (PVP), carboxymethyl cellulose, calgon and urea.
Second step: adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag
+, ultraviolet wavelength is 200-400nm, and catalysis time is 6-72h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.Described nanometer silver antimicrobial stoste is nano silver colloidal sol.Above-mentioned protectant can prevent from producing and reuniting in Nano Silver reduction process, and augmenting response area, promotes reduction reaction to carry out thoroughly simultaneously.In photo catalytic reduction process, the prolongation of ultraviolet lighting time can improve the conversion ratio of Nano Silver.
The 3rd step: nanometer silver antimicrobial stoste, surfactant, thickener, chelating agent, cosolvent, preservative, flavoring essence are mixed and stirred according to following percentage by weight with pigment and water:
Nanometer silver antimicrobial stoste: 5%-20%;
Surfactant: 0%-30%, preferably, 5-20%; When nano silver antimicrobials is spray, the preferred 0-2% of surfactant;
Thickener: 0-5%, preferably, 0.5-5%; When nano silver antimicrobials is that spray can not added thickener;
Chelating agent: 0-2%, preferably, 0.1-2%; When nano silver antimicrobials is spray, chelating agent is preferably 0-2%;
Cosolvent: 0-70%, preferably, 0.5-10%; When nano silver antimicrobials is spray, cosolvent is preferably 0.5-70%;
Preservative: 0-0.002%, preferably, 0.001-0.002%; When nano silver antimicrobials is spray, preservative is preferably 0-0.001%;
Flavoring essence and pigment: 0-0.03%, preferably, 0.02-0.03%; When nano silver antimicrobials is spray, flavoring essence and pigment are preferably 0-0.02g;
Water: surplus.
In described nanometer silver antimicrobial stoste, contain Nano Silver, wherein, the content of described Nano Silver is 0.00025-0.02mol/kg, and the particle diameter of described Nano Silver is 1-100nm; Preferably, the particle diameter of Nano Silver is 3-20nm.Further; described nanometer silver antimicrobial stoste also contains protectant, and described protectant is selected from least one in polyethylene glycol, polypropylene glycol, ethylene glycol, sorbierite, sodium citrate, polyvinylpyrrolidone (PVP), carboxymethyl cellulose, calgon and urea.
Described surfactant is selected from least one in sodium n-alkylbenzenesulfonate, sodium sulfate of polyethenoxy ether of fatty alcohol, sodium alkyl sulfate, dodecyl sodium sulfate, alkyl poly glucoside, polyethylene pyrrole network alkane ketone, dodecyldimethylammonium hydroxide inner salt, glycerin monostearate and hydrolecithin.In the present embodiment, adopt the alkyl poly glucoside that quality percentage composition is 70%.
Described thickener is selected from least one in sodium chloride, sodium citrate and carboxymethyl cellulose.Described thickener, can improve the viscosity of nano silver antimicrobials, makes it by liquid state, change fluidised form into, more convenient during use; Meanwhile, described thickener also has emulsification, stable or make nano silver antimicrobials be the effect of suspended state, keeps being uniformly distributed of each composition, particularly Nano Silver in nano silver antimicrobials, so can improve the antibiotic property of nano silver antimicrobials.
Described chelating agent is selected from least one in disodium ethylene diamine tetraacetate or sodium citrate.Described chelating agent and metal ion-chelant, can improve feel and the comfort level of nano silver antimicrobials; Meanwhile, described chelating agent also possesses non-oxidizability, can better protect skin.
Described cosolvent is selected from least one in ethanol, polyethylene glycol, urea, isopropyl alcohol, dimethyl sulfoxide (DMSO) and glycerine.The effect of described cosolvent is the low-temperature stability that promotes nano silver antimicrobials, reduces congealing point and the cloud point of nano silver antimicrobials.
Described preservative is selected from least one in Kathon CG, Phenoxyethanol, nipagin esters.
The 4th step: the mixed liquor that emulsification treatment the 3rd step obtains, in the present embodiment, adopts ultrasonic emulsification 0-30 minute.The nano silver antimicrobials obtaining after emulsification treatment is whipped cream type.
Compared to prior art, the present invention, by ultraviolet catalytic reducing process, prepares nanometer silver antimicrobial stoste under the condition that does not add reductant.Using this nanometer silver antimicrobial stoste as Antibacterial Constituents, around it, design Nano Silver washing agent and exempt from spray.Washing agent is given the anti-microbial property of wide spectrum, makes it when removing oily matter, has antibacterial ability.Disposable spraying can be travelled outdoors and antimicrobial treatment be carried out in the position of needs cleaning while being inconvenient to use washing agent in daily life.
Embodiment 1
The silver nitrate aqueous solution that preparation 1L concentration is 0.005mol/L; According to silver nitrate and protectant, with the mol ratio of 1:20, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is urea.Adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag
+, ultraviolet wavelength is 200nm, and catalysis time is 6h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.
Sodium chloride 1g, sodium sulfate of polyethenoxy ether of fatty alcohol 5g, isopropyl alcohol 0.5ml, sodium citrate 0.1g, nanometer silver antimicrobial stoste 5ml, Kathon CG 0.001g, flavoring essence 0.01g and pigment 0.01g are mixed, add water to 100ml and stir.To the mixed liquor ultrasonic emulsification of this 100ml 5 minutes, obtain nanometer silver antimicrobial cleaning solution.Afterwards, carry out filling.
Embodiment 2
The silver nitrate aqueous solution that preparation 1L concentration is 0.1mol/L; According to silver nitrate and protectant, with the mol ratio of 5:1, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is calgon.Adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag
+, ultraviolet wavelength is 400nm, and catalysis time is 72h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.
By sodium citrate 5g, sodium sulfate of polyethenoxy ether of fatty alcohol 10g, sodium alkyl sulfate 20g,, polyethylene glycol 10ml, disodium ethylene diamine tetraacetate 2g, nanometer silver antimicrobial stoste 20ml, nipagin esters 0.001g and flavoring essence 0.03g mix, add water to 100ml and stir.To the mixed liquor ultrasonic emulsification of this 100ml 30 minutes, obtain nanometer silver antimicrobial cleaning solution.Afterwards, carry out filling.
Embodiment 3
The silver nitrate aqueous solution that preparation 1L concentration is 0.08mol/L; According to silver nitrate and protectant, with the mol ratio of 1:1, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is carboxymethyl cellulose.Adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag
+, ultraviolet wavelength is 285nm, and catalysis time is 48h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.
5ml nanometer silver antimicrobial stoste is mixed with 0.5ml dimethyl sulfoxide (DMSO), adds water to 100ml, stir the disposable spraying of nanometer silver antimicrobial.
Embodiment 4
The silver nitrate aqueous solution that preparation 1L concentration is 0.05mol/L; According to silver nitrate and protectant, with the mol ratio of 1:10, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is polyethylene pyrrole network alkane ketone.Adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag
+, ultraviolet wavelength is 365nm, and catalysis time is 36h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.
Sodium chloride 0.5g, sodium citrate 2g, sodium n-alkylbenzenesulfonate 6g, polyethylene pyrrole network alkane ketone 3g, sodium sulfate of polyethenoxy ether of fatty alcohol 6g, urea 2.5g, disodium ethylene diamine tetraacetate 1g, nanometer silver antimicrobial stoste 12ml, Kathon CG 0.001g, nipagin esters 0.001g, flavoring essence 0.01g and pigment 0.01g are mixed, add water to 100ml and stir.To the mixed liquor ultrasonic emulsification of this 100ml 15 minutes, obtain nanometer silver antimicrobial cleaning solution.Afterwards, carry out filling.
Embodiment 5
The silver nitrate aqueous solution that preparation 1L concentration is 0.01mol/L; According to silver nitrate and protectant, with the mol ratio of 1:5, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is sodium citrate.Adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag
+, ultraviolet wavelength is 254nm, and catalysis time is 48h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.
Nanometer silver antimicrobial stoste 10ml, ethanol 40ml, disodium ethylene diamine tetraacetate 1g, urea 3g and polyvinylpyrrolidone 2g are mixed, add water to 100ml, stir the disposable spraying of nanometer silver antimicrobial.
Embodiment 6
The silver nitrate aqueous solution that preparation 1L concentration is 0.1mol/L; According to silver nitrate and protectant, with the mol ratio of 5:1, in silver nitrate aqueous solution, add protectant, and stir until visually observe protectant and dissolve completely.Described protectant is calgon.Adopt photo-reduction, with ultraviolet excitation photoelectron reduction Ag+, ultraviolet wavelength is 400nm, and catalysis time is 72h, and solution colour, by the colourless dark color that transfers to, obtains nanometer silver antimicrobial stoste.
Nanometer silver antimicrobial stoste 20ml, ethanol 40ml, polyethylene glycol 8ml, sodium citrate 2g are mixed, alkyl poly glucoside 5ml, Kathon CG 0.001g, flavoring essence 0.01g and pigment 0.01g, add water to 100ml, stir add in spray bottle the disposable spraying of nanometer silver antimicrobial.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a nano silver antimicrobials, is characterized in that: this nano silver antimicrobials contains nanometer silver antimicrobial stoste, in described nanometer silver antimicrobial stoste, contains Nano Silver, and wherein, the content of described Nano Silver is 0.00025-0.02mol/kg.
2. nano silver antimicrobials as claimed in claim 1, is characterized in that: the particle diameter of described Nano Silver is 1-100nm.
3. nano silver antimicrobials as claimed in claim 1 or 2; it is characterized in that: described nanometer silver antimicrobial stoste also contains protectant, and described protectant is selected from least one in polyethylene glycol, polypropylene glycol, ethylene glycol, sorbierite, sodium citrate, polyvinylpyrrolidone, carboxymethyl cellulose, calgon and urea.
4. nano silver antimicrobials as claimed in claim 1, is characterized in that: described nano silver antimicrobials also contains thickener, and described thickener is selected from least one in sodium chloride, sodium citrate and carboxymethyl cellulose.
5. nano silver antimicrobials as claimed in claim 4, is characterized in that: the weight percentage of described thickener is 0-2%.
6. nano silver antimicrobials as claimed in claim 1, is characterized in that: described nano silver antimicrobials also contains chelating agent, and described chelating agent is selected from least one in disodium ethylene diamine tetraacetate or sodium citrate.
7. nano silver antimicrobials as claimed in claim 6, is characterized in that: the weight percentage of described chelating agent is 0-2%.
8. the preparation method of nano silver antimicrobials described in any one in claim 1-7, comprises the steps:
Silver nitrate is mixed with protectant;
Adopt photo-reduction, the Ag reducing in above-mentioned silver nitrate with ultraviolet excitation photoelectron
+, obtain nanometer silver antimicrobial stoste;
Nanometer silver antimicrobial stoste, surfactant, thickener, chelating agent, cosolvent, preservative, flavoring essence are mixed and stirred with pigment and water.
9. the preparation method of the nano silver antimicrobials of claim 8 described in, is characterized in that: the weight percentage of described nanometer silver antimicrobial stoste is 5%-20%.
10. the preparation method of the nano silver antimicrobials of claim 9 described in, it is characterized in that: in described nano silver antimicrobials, the quality percentage composition of surfactant is 0%-30%, the quality percentage composition of thickener is 0-5%, the quality percentage composition of chelating agent is 0-2%, and the quality percentage composition of cosolvent is 0-70%, and the quality percentage composition of preservative is 0-0.002%, the quality percentage composition of flavoring essence and pigment is 0-0.03%, and surplus is water.
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Application publication date: 20140827 |