CN110150316A - A kind of preparation method of nano silver/subchloride composite bactericidal liquid - Google Patents
A kind of preparation method of nano silver/subchloride composite bactericidal liquid Download PDFInfo
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- CN110150316A CN110150316A CN201910473949.6A CN201910473949A CN110150316A CN 110150316 A CN110150316 A CN 110150316A CN 201910473949 A CN201910473949 A CN 201910473949A CN 110150316 A CN110150316 A CN 110150316A
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Abstract
The invention discloses a kind of nano silver/subchloride composite bactericidal liquid preparation methods, and the nano silver stabilizer centainly matched, auxiliary agent, Yin Yuan, reducing agent and dispersion protective agent are dissolved in water according to sequencing, then still aging under certain conditions；Subchloride is added after the completion of ageing, is slowly stirred uniformly, obtains object nano silver/subchloride composite bactericidal liquid.The nano silver obtained by the preparation method/subchloride composite bactericidal liquid, the size of nano-Ag particles are in monodispersity, soilless sticking phenomenon between 1 ~ 10 nanometer；The bactericidal liquid has the characteristics that colourless, transparent, anti-discoloration, stability are strong, pH controlled range is wide.Also, under nano silver and all lower situation of subchloride concentration, which can reach higher sterilizing rate in a relatively short period of time, and bactericidal effect is lasting.Preparation method is easy to operate, Parameter adjustable range is wide, low energy consumption, the period is short, is suitble to large-scale production.
Description
Technical field
The present invention relates to a kind of nano silver/subchloride composite bactericidal liquid preparation method, belong to nanotechnology and fine
Chemical field.
Background technique
The appearance of nanotechnology makes bactericidal property of the silver under nm regime produce qualitative leap.Nano silver is in dosage
Powerful bactericidal effect can be generated in the case where seldom, permeability is strong, and bactericidal effect wide spectrum has no drug resistance；And nano silver
It can promote the healing of wound, the growth of cell and the reparation of damaged cell, and without any toxic reaction, to skin without any thorn
Swash reaction.Therefore, nano silver antibacterial material can be applied to functional plastics, functional paint, textile fabric, air cleaning, food, day
The fields such as change, medical treatment possess very vast market prospect, have been increasingly becoming research hotspot in recent years.
The bactericidal property of silver is mainly realized by following two approach:
(1) haptoreaction.The main composition of the cell membrane of bacterium is phospholipid molecule and protein, and the phosphorus in phospholipid molecule
Acid group has negative electrical charge, this makes the cell membrane of bacterium with negative electricity, and silver ion can securely be adsorbed on cell by attractive coulombic force
On film, in conjunction with memebrane protein, makes its structure change, generate damage.Also, silver ion can also penetrate further into cell wall entrance
It is strong to attract the intracorporal sulfydryl of bacterium in bacterium, and combine rapidly therewith, make the protein coagulating of bacterium, destroys cell synthesis
The activity of enzyme makes cell loss division growth ability and dead.In addition, silver ion can also destroy microorganism electron-transport system,
Respiratory system, substance delivery system.After thallus loses activity, silver ion again can from thallus separate out, repeat to kill
Bacterium, therefore its durable antibacterial effect are constantly killed in bacterium activity in cycles.
(2) catalysis reaction.Under the action of light, silver ion and nano-scale particle can play the role of catalytic active center,
The oxygen in water or in air is activated, hydroxyl radical free radical and negative oxygen ion are generated.Hydroxyl radical free radical and negative oxygen ion can be in the short time
The interior proliferative capacity for destroying bacterium, causes cell death, to achieve the purpose that antibacterial.
Usually, based on the first sterilization mechanism, photocatalytic process also functions to certain effect.It is obtained from above-mentioned
Know, silver-colored simple substance itself does not simultaneously have sterilizing ability, and after contacting with bacterium, the silver ion that elemental silver is discharged could generate sterilization effect
Fruit.Silver metal fungistatic effect under the size of macroscopic view is more faint, if obtaining nano silver material by suitable preparation method
Material, then due to quantum effect, small-size effect and great specific surface area characteristic that nano material itself has, be remarkably improved
Bactericidal effect.
Dispersion liquid containing nano silver has more extensive industry and commercial application value.Nano silver dispersion can divide
For two kinds of nano-silver ionic colloidal dispersion and nano silver simple substance colloidal dispersion.The former is the side combined by negative ions
Formula is wrapped up mutually layer by layer, the glomerate colloidal sol glue core of shape, the diffusion electric double layer with wider range, therefore has stronger point
Dissipate property and stability.The latter be by dispersion caused by the stronger high molecular polymer of stability protection and solubilization,
Nano silver simple substance particle surface forms layer protecting film, and is steadily scattered in solution.
Both either nano-silver ionic colloidal dispersion or nano silver simple substance colloidal dispersion have stronger kill
Bacterium ability and antibacterial action is lasting.But using haptoreaction as the nano silver of major antibacterial approach, sterilization rate is not
It is very ideal.In a longer period of time, the bactericidal effect of nano silver is unquestionable；But it will be within a shorter time
(in such as a few minutes even in tens seconds), the nano silver of low concentration is difficult to realize higher sterilizing rate.
And subchloride class disinfectant, such as subchloride is hypochlorous acid, sodium hypochlorite, calcium hypochlorite, has Strong oxdiative
Ability can reach high sterilizing rate in a relatively short period of time, and have broad-spectrum sterilization performance.It is secondary in sterilization process
Chloride itself, which decomposes, generates oxygen, does not generate air pollution, does not remain any harmful substance in subject after sterilization,
It is environmentally protective.
Subchloride is sterilized by autoxidation decomposition, although within a short period of time, subchloride can be shown
High sterilizing rate, but bactericidal effect is not lasting.After subchloride decomposes, that is, lose sterilizing ability.Also, it is certain
Subchloride stability itself is poor, it is difficult to store for a long time.Therefore, when using subchloride, high stability should be selected
Subchloride, guarantee the stability of subchloride.
Therefore, it is necessary to a kind of stronger bactericidal liquid of comprehensive performance, can reach in a short time higher sterilizing rate and
Guarantee the persistence of antibacterial action.Furthermore, it is desirable to the system that a kind of cost input early period is small, low energy consumption, easy to operate, reaction is mild
Preparation Method.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of that present invention to provide a kind of nano silver/subchloride composite bactericidal liquid
Preparation method.
The object of the invention is achieved through the following technical solutions: a kind of preparation side of nano silver/subchloride composite bactericidal liquid
Method, it is characterised in that the nano silver/raw material proportioning of subchloride composite bactericidal liquid, preparation method, product property are as follows:
(1) raw material proportioning: in terms of 1000 milliliters of nano silvers/subchloride composite bactericidal liquid, raw material proportioning is as follows:
11 gram of nano silver stabilizer ~ 100 grams
21 gram of auxiliary agents ~ 100 grams
3 0.02 gram of silver medal sources ~ 2 grams (in terms of silver)
40 gram of reducing agents ~ 20 grams
50 gram ~ 50 grams of protective agent of dispersions
6 0.2 gram of subchlorides ~ 100 grams
7 purified waters add to 1000 milliliters,
(2) preparation method: nano silver stabilizer, auxiliary agent are added in purified water, silver-colored source are introduced after stirring and dissolving, after dissolution
Reducing agent and dispersion protective agent are added immediately, is stirred and dissolved into homogeneous transparent solution, and add purified water to target volume 70% ~
98%；Water temperature is increased, closed still aging 0.5 ~ 96 hour under 10 ~ 60 degrees Celsius；Subchloride is added after the completion of ageing, delays
Slowly it stirs evenly and adds purified water to target volume, obtain object nano silver/subchloride composite bactericidal liquid；
(3) product property: the size of nano-Ag particles is between 1 ~ 10 nanometer in nano silver/subchloride composite bactericidal liquid
Monodispersity, soilless sticking phenomenon；The pH controlled range of the bactericidal liquid has colourless, transparent, anti-discoloration, stabilization between 4 ~ 9
The features such as property is strong；Also, under nano silver and all lower situation of subchloride concentration, bactericidal liquid sterilization effect with higher
Fruit, sterilizing rate is high, and bactericidal effect is lasting.
The nano silver stabilizer be amino acids (glutamic acid, asparatate, taurine, glycine, alanine),
Amidates (such as sodium glutamate, Asparagus cochinchinensis ammonia acid sodium, Amcide Ammate, Sodium L-alaninate), high stable complexing agent (such as ethylenediamine
Tetraacethyl disodium, calgon, water soluble Beta-cyclodextrin) in one of which or above-mentioned substance combination.
The auxiliary agent is that boric acid, borax, lactic acid, ammonium hydroxide is one such or the combination of above-mentioned substance；Also, it is described
Auxiliary agent have the function of adjust pH.
The silver-colored source is silver nitrate, silver acetate, silver citrate, silver tartrate, nano silver simple substance colloidal sol, nano-silver ionic
Colloidal sol is one such or the combination of above-mentioned substance.
The reducing agent is polyalcohols, such as mannitol, xylitol, glucitol, fructose alcohol, lactitol, glycerine
One such or above-mentioned substance combination.
The described dispersion protective agent is the water soluble polymer of high stability, as polyvinyl alcohol and its derivative,
Polyvinylpyrrolidone and its derivative, cellulose and its derivates, water soluble chitosan and its derivative, polyethylene glycols,
Carbomer is one such or the combination of above-mentioned substance.
The subchloride is that hypochlorous acid, sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite are one such or above-mentioned
The combination of substance.
The preparation method is as follows: nano silver stabilizer, auxiliary agent are added in purified water, silver-colored source, dissolution are introduced after stirring and dissolving
After reducing agent, dispersion protective agent and subchloride stabilizer are added immediately, be stirred and dissolved into homogeneous transparent solution, and add pure
Change water to the 70% ~ 98% of target volume；Water temperature is increased, closed still aging 0.5 ~ 96 hour under 10 ~ 60 degrees Celsius；It has been aged
At rear addition subchloride solution, it is slowly stirred uniformly and adds purified water to target volume, obtain object nano silver/time chlorination
Object composite bactericidal liquid.
In of the invention one preferred technical solution, with 1000 milliliters of nano silvers/subchloride composite bactericidal liquid
Meter, secondary sodium chloride are calculated by 30% secondary sodium chloride solution, and additive amount is 0.5 milliliter ~ 200 milliliters；At this time the preparation method is as follows:
Nano silver stabilizer, auxiliary agent are added in purified water, silver-colored source is introduced after stirring and dissolving, be added immediately after dissolution reducing agent,
Disperse protective agent, is stirred and dissolved into homogeneous transparent solution, and add purified water to the 70% ~ 98% of target volume；Water temperature is increased, 10
Closed still aging 0.5 ~ 96 hour under ~ 60 degrees Celsius；Time sodium chloride solution is added after the completion of ageing, be slowly stirred uniformly and adds
Purified water obtains object nano silver/time sodium chloride composite bactericidal liquid to target volume.
In the present invention, nano silver dispersion has stronger sterilizing ability and lasting antibacterial action, and subchloride
Higher sterilizing rate can be reached in a relatively short period of time.The compound deficiency that will mutually make up other side of the two obtains comprehensive
It can stronger bactericidal liquid.Also, the addition of subchloride facilitates in nano silver activation water as the initiator of catalysis reaction
Or the oxygen in air, it generates free radicals and negative oxygen ion, improves the bactericidal effect that nano silver passes through catalyzed side reaction formula.
In the present invention, used preparation method is not necessarily to through violent reduction reaction, but is used more mild
Polyalcohols weak reductant, and gone back using amino acid, amino-acid salt or high stable complex compound as the stabilizer of nano silver, control
Former reaction rate；Using the water soluble polymer of high stability as dispersion protective agent, final equalization point is reacted in control.
After reaching reaction equalization point, the size of nano silver colloidal sol particle no longer increases, the rate of dissolution of sol particle surface elemental silver
Reach dynamic balance with the crystalline rate of silver ion.
By nano silver prepared by the preparation method/subchloride composite bactericidal liquid, the sizes of nano-Ag particles 1 ~
Between 10 nanometers, the pH controlled range of bactericidal liquid has that colourless, transparent, anti-discoloration, stability be strong, sterilizing rate between 4 ~ 9
High, the features such as bactericidal effect is lasting.Also, the preparation method is easy to operate, Parameter adjustable range is wide, low energy consumption, the period is short etc.
Feature is especially suitable for enlarged experiment and industrialized production.
Specific embodiment
Below by embodiment, the present invention is further elaborated, and purpose, which is only that, is best understood from the contents of the present invention.
Therefore, the cited case is not intended to limit protection scope of the present invention.
Embodiment 1
In terms of 1000 milliliters of nano silvers/subchloride composite bactericidal liquid, raw material and proportion be see the table below:
Preparation method: before preparation, carbomer is configured to 1% solution for standby.When preparation, purifying is added in Sodium L-alaninate, boric acid
Be introduced into water, after stirring and dissolving silver-colored source silver acetate, mannitol and 2020 solution of carbomer successively stirring and dissolving in purified water, at
Homogeneous transparent solution adds water to 960 milliliters, closed still aging 30 hours at 60 DEG C；It is down to room temperature after ageing, is added
20% hypochlorite solution is slowly stirred uniformly and adds purified water to target volume, it is multiple to obtain target product nano silver/subchloride
Close bactericidal liquid.
Bactericidal property detection: according to " disinfection technology standard " version in 2002, bactericidal property detection is carried out.Test result is aobvious
Show, above-mentioned nano silver/subchloride composite bactericidal liquid is greater than 99.9999% to the killing rate of Escherichia coli (8099 type), to golden yellow
The killing rate of color staphylococcus (6538 type of ATCC) is greater than 99.9999%, the killing to pseudomonas aeruginosa (9027 type of ATCC)
Rate is greater than 99.9999%, is greater than 99.9999% to the killing rate of Candida albicans (10231 type of ATCC).
Embodiment 2
In terms of 1000 milliliters of nano silvers/subchloride composite bactericidal liquid, raw material and proportion be see the table below:
Before preparation, polyvinyl alcohol 1750 is configured to 5% solution for standby.
Preparation method: when preparation, alanine, borax being added in purified water, introduced after stirring and dissolving silver-colored source silver citrate,
1750 solution of xylitol and polyvinyl alcohol, successively stirring and dissolving is in purified water, after homogeneous transparent solution, adds water to 800 millis
It rises, closed still aging 60 hours at 20 DEG C；After ageing, sodium hypochlorite is added, is slowly stirred and is uniformly dissolved and adds pure
Change water to target volume, obtains target product nano silver/sodium hypochlorite composite bactericidal liquid.
Bactericidal property detection: according to " disinfection technology standard " version in 2002, bactericidal property detection is carried out.Test result is aobvious
Show, above-mentioned nano silver/subchloride composite bactericidal liquid is greater than 99.99% to the killing rate of Escherichia coli (8099 type), to golden yellow
The killing rate of staphylococcus (6538 type of ATCC) is big to the killing rate of pseudomonas aeruginosa (9027 type of ATCC) greater than 99.99%
In 99.99%, 99.99% is greater than to the killing rate of Candida albicans (10231 type of ATCC).
Embodiment 3
In terms of 1000 milliliters of nano silvers/subchloride composite bactericidal liquid, raw material and proportion be see the table below:
Before preparation, polyvinylpyrrolidone k-30 is configured to 5% solution for standby.
Preparation method: when preparation, sodium glutamate, lactic acid are added in purified water, silver-colored source nano silver is introduced after stirring and dissolving
Simple substance colloidal sol, glucitol and polyvinylpyrrolidone k-30 solution, successively stirring and dissolving is molten at homogeneous transparent in purified water
After liquid, 950 milliliters are added water to, closed still aging 24 hours at 50 DEG C；It is down to room temperature after ageing, hypochlorous acid is added
Calcium is slowly stirred uniformly and adds purified water to target volume, obtains object nano silver/calcium hypochlorite composite bactericidal liquid.
Bactericidal property detection: according to " disinfection technology standard " version in 2002, bactericidal property detection is carried out.Test result is aobvious
Show, above-mentioned nano silver/subchloride composite bactericidal liquid is greater than 99.99% to the killing rate of Escherichia coli (8099 type), to golden yellow
The killing rate of staphylococcus (6538 type of ATCC) is big to the killing rate of pseudomonas aeruginosa (9027 type of ATCC) greater than 99.99%
In 99.99%, 99.99% is greater than to the killing rate of Candida albicans (10231 type of ATCC).
Embodiment 4
In terms of 1000 milliliters of nano silvers/subchloride composite bactericidal liquid, raw material and proportion be see the table below:
Before preparation, water-soluble carboxymethyl chitosan is configured to 5% solution for standby.
Preparation method: when preparation, water soluble Beta-cyclodextrin, boric acid being added in purified water, and silver-colored source is introduced after stirring and dissolving and is received
Nano silver ion colloidal sol, lactitol and water-soluble carboxymethyl chitosan solution, successively stirring and dissolving is in purified water, at homogeneous transparent
After solution, 900 milliliters are added water to, closed still aging 72 hours at 10 DEG C；After ageing, magnesium hypochlorite is added, slowly
It stirs evenly and adds purified water to target volume, obtain object nano silver/magnesium hypochlorite composite bactericidal liquid.
Bactericidal property detection: according to " disinfection technology standard " version in 2002, bactericidal property detection is carried out.Test result is aobvious
Show, above-mentioned nano silver/subchloride composite bactericidal liquid is greater than 99.99% to the killing rate of Escherichia coli (8099 type), to golden yellow
The killing rate of staphylococcus (6538 type of ATCC) is big to the killing rate of pseudomonas aeruginosa (9027 type of ATCC) greater than 99.99%
In 99.99%, 99.99% is greater than to the killing rate of Candida albicans (10231 type of ATCC).
Claims (8)
1. a kind of nano silver/subchloride composite bactericidal liquid preparation method, it is characterised in that the nano silver/subchloride is compound
The raw material proportioning of bactericidal liquid, preparation method, product property are as follows:
(1) raw material proportioning: in terms of 1000 milliliters of nano silvers/subchloride composite bactericidal liquid, raw material proportioning is as follows:
11 gram of nano silver stabilizer ~ 100 grams
21 gram of auxiliary agents ~ 100 grams
3 0.02 gram of silver medal sources ~ 2 grams (in terms of silver)
40 gram of reducing agents ~ 20 grams
50 gram ~ 50 grams of protective agent of dispersions
6 0.2 gram of subchlorides ~ 100 grams
7 purified waters add to 1000 milliliters,
(2) preparation method: nano silver stabilizer, auxiliary agent are added in purified water, silver-colored source are introduced after stirring and dissolving, after dissolution
Reducing agent and dispersion protective agent are added immediately, is stirred and dissolved into homogeneous transparent solution, and add purified water to target volume 70% ~
98%；Water temperature is increased, closed still aging 0.5 ~ 96 hour at 10 ~ 60 DEG C；Subchloride is added after the completion of ageing, slowly stirs
It mixes uniformly and adds purified water to target volume, obtain target product nano silver/subchloride composite bactericidal liquid, wherein nano silver/
The size of nano-Ag particles is in monodispersity, soilless sticking phenomenon between 1 ~ 10 nanometer in subchloride composite bactericidal liquid；This is killed
The pH controlled range of bacterium solution is between 4 ~ 9.
2. a kind of nano silver according to claim 1/subchloride composite bactericidal liquid preparation method, it is characterised in that
The preparation method is as follows: nano silver stabilizer, auxiliary agent are added in purified water, silver-colored source is introduced after stirring and dissolving, is stood after dissolution
Reducing agent, dispersion protective agent and subchloride stabilizer is added, is stirred and dissolved into homogeneous transparent solution, and add purified water to mesh
The 70% ~ 98% of standard type product；Water temperature is increased, closed still aging 0.5 ~ 96 hour at 10 ~ 60 DEG C；Time chlorine is added after the completion of ageing
Compound solution is slowly stirred uniformly and adds purified water to target volume, obtains target product nano silver/subchloride composite bactericidal
Liquid.
3. a kind of nano silver according to claim 1 or 2/subchloride composite bactericidal liquid preparation method, feature exist
It is the amino acids for including glutamic acid, asparatate, taurine, glycine, alanine in the nano silver stabilizer, wraps
Include the amidates of sodium glutamate, Asparagus cochinchinensis ammonia acid sodium, Amcide Ammate, Sodium L-alaninate, including disodium ethylene diamine tetraacetate,
Calgon, water soluble Beta-cyclodextrin high stable complexing agent in one of which or above-mentioned substance combination.
4. a kind of nano silver according to claim 1 or 2/subchloride composite bactericidal liquid preparation method, feature exist
It is that boric acid, borax, lactic acid, ammonium hydroxide is one such or the combination of above-mentioned substance, and has the work for adjusting pH in the auxiliary agent
With.
5. a kind of nano silver according to claim 1 or 2/subchloride composite bactericidal liquid preparation method, feature exist
In the silver-colored source be silver nitrate, silver acetate, silver citrate, silver tartrate, nano silver simple substance colloidal sol, nano-silver ionic colloidal sol its
One of or above-mentioned substance combination.
6. a kind of nano silver according to claim 1 or 2/subchloride composite bactericidal liquid preparation method, feature exist
In the reducing agent be polyalcohols, as mannitol, xylitol, glucitol, fructose alcohol, lactitol, glycerine are therein
The combination of one kind or above-mentioned substance.
7. a kind of nano silver according to claim 1 or 2/subchloride composite bactericidal liquid preparation method, feature exist
In the water soluble polymer that the dispersion protective agent is high stability, such as polyvinyl alcohol and its derivative, polyethylene
Pyrrolidones and its derivative, cellulose and its derivates, water soluble chitosan and its derivative, polyethylene glycols, carbomer
Class is one such or the combination of above-mentioned substance.
8. a kind of nano silver according to claim 1 or 2/subchloride composite bactericidal liquid preparation method, feature exist
It is that hypochlorous acid, sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite be one such or above-mentioned substance in the subchloride
Combination.
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