CN110140718A - A kind of preparation method of nano silver/microporous polymer composite bactericidal liquid - Google Patents
A kind of preparation method of nano silver/microporous polymer composite bactericidal liquid Download PDFInfo
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- CN110140718A CN110140718A CN201910471505.9A CN201910471505A CN110140718A CN 110140718 A CN110140718 A CN 110140718A CN 201910471505 A CN201910471505 A CN 201910471505A CN 110140718 A CN110140718 A CN 110140718A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/38—Silver; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6921—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit the form being a particulate, a powder, an adsorbate, a bead or a sphere
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/02—Local antiseptics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
Abstract
The invention discloses the preparation methods of a kind of nano silver and microporous polymer composite bactericidal liquid, and a certain amount of nano-silver ionic solution is mixed evenly with capillary copolymer material, obtains object nano silver and the compound bactericidal liquid of microporous polymer.The nano silver obtained by the preparation method/microporous polymer composite bactericidal liquid, in the case where no stabilizer, the high feature of Argent grain good dispersion, soilless sticking phenomenon, activity.Also, since the active retentivity of nano silver is good, which has the characteristics that bactericidal effect is lasting.In addition, this preparation method is easy to operate, the short, technology controlling and process of time-consuming, it is suitble to large-scale production.
Description
Technical field
The present invention relates to a kind of nano silver/microporous polymer composite bactericidal liquid preparation methods, belong to nanotechnology and essence
Thin chemical field.
Background technique
With the development of nano material preparation technology, people gradually recognize that silver has superpower bactericidal properties under nm regime
Energy.Nano silver is nontoxic, has no drug resistance, and bactericidal effect is extensive；And nano silver has good biocompatibility, can promote to hurt
Mouth healing, cell growth and reparation, to skin also without without any stimulation.Therefore, nano silver antibacterial material is widely answered at present
For fields such as functional paint, textile fabric, food, daily use chemicals, medical treatment, market prospects are boundless, have been increasingly becoming industry
The hot spot of research.
The bactericidal effect of nano silver is mainly realized by following two approach:
(1) contact sterilization is reacted.The cell membrane of bacterium has negative electrical charge, and silver ion can be adsorbed on carefully by the effect of Coulomb force
Bacterium cell membrane surface makes its structure change in conjunction with memebrane protein, generates damage.Also, silver ion can also further be worn
Saturating cell wall enters in bacterium, destroys the activity of cell synzyme, makes cell loss division growth ability and dead.In addition, silver-colored
Ion can also destroy the electronics and substance delivery system of bacterium and microorganism.After completing bactericidal effect, silver ion again can be from thallus
Middle separate out repeats above-mentioned fungicidal property, thus the killing bacterium moved in circles, therefore it can keep lasting and resist
Bacterium effect.
(2) catalytically bactericidal process acts on.Under the action of light, the electronics of nano silver is excited by light, so in catalyzing activation water or
Oxygen in air makes it generate hydroxyl radical free radical and negative oxygen ion.Hydroxyl radical free radical and negative oxygen ion are made with very strong sterilization
With can destroy the proliferative capacity of bacterium in a short time, accelerate the speed of Apoptosis, to achieve the purpose that antibacterial.
Usually, silver ion for sterilization is carried out by the first sterilization mechanism, and photocatalytic process also functions to
Certain effect.It is learnt from above-mentioned, silver-colored simple substance itself does not simultaneously have sterilizing ability, after contacting with bacterium, what elemental silver was discharged
Silver ion could generate bactericidal effect.Since specific surface area is smaller under the size of macroscopic view for silver metal, reaction interface is few, release
Silver ion is few, causes its activity weaker, fungistatic effect is poor.Although and active higher, the group of being easy to happen of common nano silver
Poly- phenomenon causes particle size to become larger, and reduces activity in turn, stablizes so general nano-silver sterilization liquid requires to be added
The chemical stabilizer of nano silver, these chemical stabilizers have damaging effect to human body and environment.
Summary of the invention
In the deficiencies in the prior art, it is an object of that present invention to provide a kind of nano silver/microporous polymer composite bactericidal liquid
Preparation method.
The object of the invention is achieved through the following technical solutions, a kind of preparation of nano silver/microporous polymer composite bactericidal liquid
Method, it is characterised in that the nano silver/raw material proportioning of microporous polymer composite bactericidal liquid, preparation method, product property are as follows:
(1) raw material proportioning: in terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, raw material proportioning is as follows:
1 0.5 gram of microporous polymer ~ 1 gram
2 0.02 gram ~ 1 gram of silver medal sources (in terms of silver)
31 gram of reducing agents ~ 10 grams
4 purified waters add to 500 milliliters
(2) preparation method: the microporous polymer fine powder after reducing agent and grinding is added in purified water, is added after stirring and dissolving
Silver-colored source, and add purified water to the 60% ~ 80% of target volume；Temperature is increased, the closed standing reaction 0.5 ~ 60 under 10 ~ 60 degrees Celsius
Hour；It is slowly stirred after the reaction was completed uniformly and adds purified water to target volume, it is multiple to obtain object nano silver/microporous polymer
Close bactericidal liquid；
(3) product property: the size of nano-Ag particles is between 1 ~ 5nm in nano silver/microporous polymer composite bactericidal liquid, and single point
Dissipate that property is good and soilless sticking；And have stability strong, the features such as bactericidal effect is lasting.Further, since using capillary copolymer material
Stabilized scattering nano Argent grain does not need that stabilizer additionally is added, and avoids and excessive chemical reagent is added to human skin
Stimulation.
The nanometer silver reductor be polyalcohols, as mannitol, xylitol, glucitol, fructose alcohol, lactitol,
Glycerine is one such or the combination of above-mentioned substance.
The silver-colored source is that silver nitrate, silver acetate, silver citrate, silver tartrate be one such or the group of above-mentioned substance
It closes.
The microporous polymer is the microporous polymer not soluble in water and organic solvent of high crosslinking, the aperture model of micropore
It encloses for 1-5nm, it is one such or above-mentioned to be such as conjugated microporous polymer, covalent organic polymer, metal organic framework polymer
The combination of substance.
In terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, 0.5 gram ~ 1 gram of microporous polymer additive amount, silver
0.02 gram ~ 1 gram of source additive amount, 1 gram ~ 10 grams of reducing agent additive amount, microporous polymer, Yin Yuan, reducing agent type be mention above
The substance arrived；The preparation method is as follows: the microporous polymer fine powder after reducing agent and grinding is added in purified water, stirring and dissolving
Silver-colored source is added afterwards, and adds purified water to the 60% ~ 80% of target volume；Temperature is increased, the closed standing reaction under 10 ~ 60 degrees Celsius
0.5 ~ 60 hour；It stirs evenly after the reaction was completed and adds purified water to target volume, obtain object nano silver/microporous polymer
Composite bactericidal liquid.
Charge ratio: in terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, 0.5 gram of microporous polymer additive amount
~ 1 gram, 0.02 gram ~ 1 gram of silver-colored source additive amount, 1 gram ~ 10 grams of reducing agent additive amount；
It is provided by the present invention the preparation method is as follows: by reducing agent and grinding after microporous polymer fine powder be added purified water
In, silver-colored source is added after stirring and dissolving, and add purified water to the 60% ~ 80% of target volume；Temperature is increased, under 10 ~ 60 degrees Celsius
Closed standing is reacted 0.5 ~ 60 hour；It is slowly stirred after the reaction was completed uniformly and adds purified water to target volume, obtain object
Nano silver/microporous polymer composite bactericidal liquid；
The nanometer silver reductor is polyalcohols, such as mannitol, xylitol, glucitol, fructose alcohol, lactitol, the third three
Alcohol etc. is one such, is also possible to the combination of above-mentioned substance；
It is one such that the silver-colored source can be silver nitrate, silver acetate, silver citrate, silver tartrate etc., is also possible to above-mentioned
The combination of substance；
The microporous polymer is the microporous polymer not soluble in water and organic solvent of high crosslinking, and the pore diameter range of micropore is
1-5nm, such as conjugation microporous polymer, covalent organic polymer, metal organic framework polymer are one such, are also possible to
The combination of above-mentioned substance；
In the present invention, nano silver dispersion have stronger sterilizing ability and lasting antibacterial action, microporous polymer due to
Containing microcellular structure, the pore diameter range of micropore is 1-5nm, and the crosslinking of such high polymer is insoluble in any water and organic molten
Agent, therefore can be limited silver nano-grain using microcellular structure as carrier material absorption carriage silver nano-grain,
Its agglomeration is prevented, it is made to keep the bactericidal activity of lasting height.
In the present invention, used preparation method is not necessarily to through violent reduction reaction, but is used more mild
Polyalcohols weak reductant, reaction condition is mild, easy to operate, consumes energy low.
By nano silver prepared by the preparation method/microporous polymer composite bactericidal liquid, nano silver/microporous polymer is multiple
The size of nano-Ag particles in bactericidal liquid is closed between 1 ~ 5nm, monodispersity is good and soilless sticking；And have stability strong, sterilization
The features such as effect is lasting.Further, since not needing additionally to be added steady using capillary copolymer material stabilized scattering nano Argent grain
Determine agent, avoids the stimulation that excessive chemical reagent is added to human skin.
The purpose of the present invention is prepare a kind of nano silver that long stable effect bactericidal effect can be kept without chemical stabilizer
Ion sterilizing liquid.In order to achieve the goal above, this patent proposes that, using capillary copolymer material as absorption carrier, absorption is stablized
Nano-Ag particles make to have the function that avoid nano-Ag particles aggregation to reunite in the case where stabilizer is not added, make nano silver
Grain keeps the bactericidal effect of persistent high efficiency.Nanometer not only can be improved as the carrier for stablizing nano-silver ionic in microporous polymer
The stability of Argent grain prevents its aggregation from reuniting, moreover it is possible to avoid the use of chemical stabilizer, reduce chemical reagent to human body and ring
The harm in border.The method that this patent proposes, cost input is small, low energy consumption, easy to operate, reaction is mild, non-hazardous to environment.
Detailed description of the invention
Fig. 1: by the high-resolution of nano-Ag particles in 1 gained nano silver of embodiment/microporous polymer composite bactericidal liquid sample
Transmission electron microscope photo.
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
A kind of nano silver/microporous polymer composite bactericidal liquid, in terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid,
The size of nano-Ag particles is prepared between 1 ~ 5nm by following preparation steps in nano silver/microporous polymer composite bactericidal liquid:
Raw material and proportion see the table below:
Preparation method: 0.5 gram of three alkynyl phenyl conjugation microporous polymer fine powder after 2.0nl mannitol and grinding is added
In the purified water of 300ml, 0.5 gram of silver nitrate (in terms of silver) is added after stirring and dissolving, and add purified water to 400 ml；Heating,
Closed standing is reacted 5 hours at 50 DEG C；It is slowly stirred after the reaction was completed uniformly and adds purified water to 500 ml, obtain object and receive
Meter Yin/microporous polymer composite bactericidal liquid.Fig. 1 is in 1 gained nano silver of the present embodiment/microporous polymer composite bactericidal liquid sample
The high-resolution-ration transmission electric-lens photo of nano-Ag particles.
Product property: monodispersity is good and soilless sticking；And have stability strong, the features such as bactericidal effect is lasting.In addition, by
It in using capillary copolymer material stabilized scattering nano Argent grain, does not need that stabilizer additionally is added, avoids and be added excessively
Stimulation of the chemical reagent to human skin.
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/peroxide composite bactericidal liquid is greater than 90% to the killing rate of Escherichia coli (8099 type), to golden yellow Portugal
The killing rate of grape coccus (6538 type of ATCC) is greater than 90%.
Embodiment 2
In terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, raw material and proportion be see the table below:
Preparation method: 0.8 gram of diynyl phenyl conjugation microporous polymer fine powder after 3.0 milliliters of glucitols and grinding is added
Enter in the purified water of 300ml, 0.5 gram of silver acetate (in terms of silver) is added after stirring and dissolving, and add purified water to 400 ml；Increase temperature
Degree, closed standing is reacted 6 hours at 60 DEG C；It is slowly stirred after the reaction was completed uniformly and adds purified water to 500 ml, obtain mesh
Mark object nano silver/microporous polymer 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/peroxide composite bactericidal liquid is greater than 90% to the killing rate of Escherichia coli (8099 type), to golden yellow Portugal
The killing rate of grape coccus (6538 type of ATCC) is greater than 90%.
Embodiment 3
In terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, raw material and proportion be see the table below:
Preparation method: 0.6 gram of diynyl phenyl conjugation microporous polymer fine powder after the glucitol of 2.0ml and grinding is added
Enter in the purified water of 300ml, 0.4g silver acetate (in terms of silver) is added after stirring and dissolving, and adds purified water to 400 ml；Increase temperature
Degree, closed standing is reacted 5 hours at 60 DEG C；It is slowly stirred after the reaction was completed uniformly and adds purified water to 500 ml, obtain mesh
Mark object nano silver/microporous polymer 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/peroxide composite bactericidal liquid is greater than 90% to the killing rate of Escherichia coli (8099 type), to golden yellow Portugal
The killing rate of grape coccus (6538 type of ATCC) is greater than 90%.
Embodiment 4
In terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, raw material and proportion be see the table below:
Preparation method: 0.5 gram of three alkynyl phenyl conjugation microporous polymer fine powder after 3.0nl xylitol and grinding is added
In the purified water of 300ml, 0.5 gram of silver nitrate (in terms of silver) is added after stirring and dissolving, and add purified water to 400 ml；Increase temperature
Degree, closed standing is reacted 8 hours at 60 DEG C；It is slowly stirred after the reaction was completed uniformly and adds purified water to 500 ml, obtain mesh
Mark object nano silver/microporous polymer 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/peroxide composite bactericidal liquid is greater than 90% to the killing rate of Escherichia coli (8099 type), to golden yellow Portugal
The killing rate of grape coccus (6538 type of ATCC) is greater than 90%.
Claims (4)
1. a kind of nano silver/microporous polymer composite bactericidal liquid preparation method, which is characterized in that nano silver/microporous polymer
The size of nano-Ag particles is between 1 ~ 5nm in composite bactericidal liquid, including following preparation steps:
(1) raw material proportioning: in terms of 500 milliliters of nano silvers/microporous polymer composite bactericidal liquid, raw material proportioning is as follows:
0.5 gram ~ 1 gram of microporous polymer
0.02 gram ~ 1 gram of silver-colored source (in terms of silver)
1 gram ~ 10 grams of reducing agent
Purified water adds to 500 milliliters,
Wherein the pore diameter range of the micropore of microporous polymer is 1-5nm；
(2) preparation method: the microporous polymer fine powder after reducing agent and grinding is added in purified water, is added after stirring and dissolving
Silver-colored source, and add purified water to the 60% ~ 80% of target volume；Temperature is increased, closed standing reaction 0.5 ~ 60 is small at 10 ~ 60 DEG C
When；It is slowly stirred after the reaction was completed uniformly and adds purified water to target volume, it is compound to obtain object nano silver/microporous polymer
Bactericidal liquid.
2. nano silver/microporous polymer composite bactericidal liquid preparation method according to claim 1, which is characterized in that described
Nanometer silver reductor be polyalcohols, as mannitol, xylitol, glucitol, fructose alcohol, lactitol, glycerine are therein
The combination of one kind or above-mentioned substance.
3. nano silver/microporous polymer object composite bactericidal liquid preparation method according to claim 1, which is characterized in that institute
The silver-colored source stated is that silver nitrate, silver acetate, silver citrate, silver tartrate be one such or the combination of above-mentioned substance.
4. nano silver/microporous polymer composite bactericidal liquid preparation method according to claim 1, which is characterized in that described
Microporous polymer be high crosslinking microporous polymer not soluble in water and organic solvent, including conjugation microporous polymer, covalently
Organic polymer, metal organic framework polymer be one such or the combination of above-mentioned substance.
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Cited By (3)
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| CN111296480A (en) * | 2020-02-21 | 2020-06-19 | 衢州学院 | Iron-based metal-organic framework material loaded with silver nanoparticles and preparation method and application thereof |
| CN112056328A (en) * | 2020-08-13 | 2020-12-11 | 江苏卓高环保科技有限公司 | Furniture surface Korean pine fruit nano microsphere sterilization liquid and preparation method thereof |
| CN114129594A (en) * | 2021-12-06 | 2022-03-04 | 中国人民解放军东部战区总医院 | Nano-silver loaded porous organic polymer and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111296480A (en) * | 2020-02-21 | 2020-06-19 | 衢州学院 | Iron-based metal-organic framework material loaded with silver nanoparticles and preparation method and application thereof |
| CN112056328A (en) * | 2020-08-13 | 2020-12-11 | 江苏卓高环保科技有限公司 | Furniture surface Korean pine fruit nano microsphere sterilization liquid and preparation method thereof |
| CN114129594A (en) * | 2021-12-06 | 2022-03-04 | 中国人民解放军东部战区总医院 | Nano-silver loaded porous organic polymer and preparation method and application thereof |
| CN114129594B (en) * | 2021-12-06 | 2023-09-12 | 中国人民解放军东部战区总医院 | Porous organic polymer loaded with nano silver and preparation method and application thereof |
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