CN107375993A - A kind of preparation method of copper silver nanoclusters composite aquogel - Google Patents
A kind of preparation method of copper silver nanoclusters composite aquogel Download PDFInfo
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- CN107375993A CN107375993A CN201710698842.2A CN201710698842A CN107375993A CN 107375993 A CN107375993 A CN 107375993A CN 201710698842 A CN201710698842 A CN 201710698842A CN 107375993 A CN107375993 A CN 107375993A
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- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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Abstract
The invention provides a kind of preparation method of copper silver nanoclusters composite aquogel, comprise the following steps：The first step, preparation of reagents；It is prepared by second step, presoma；3rd step, photopolymerization, copper silver nanoclusters composite aquogel is made.The present invention is using the L cysteines of sulfhydryl compound as crosslinking agent, using the stable copper of ultraviolet photoreduction met hod one-step synthesis property and the nano-cluster composite aquogel of money kind metal, there is provided the mol ratio and the optimal conditions of ultraviolet lighting that copper silver nanoclusters compound water congealing composes.Present invention has the advantages that what is prepared is the copper silver nanoclusters composite aquogel containing two kinds of metals, silver and copper in hydrogel all have bactericidal action, hydrogel has sustained release, moisture-keeping function, it may be used as wound dressing, make the copper silver nanoclusters composite aquogel that there is more excellent property, and widely application.And by the new performance of modified imparting copper nanometer and silver nano material, the practicality and application of the material are widened.
Description
Technical field
The present invention relates to a kind of preparation method of hydrogel, from using being led in material, medical science, bioengineering etc.
A kind of preparation method for copper silver nanoclusters composite aquogel that domain uses.
Background technology
Hydrogel is a kind of mesh material.Contain substantial amounts of water in its inside.Hydrogel is divided into physics according to chemical bond
Hydrogel and chemical hydrogel.Physical hydrogel be point between bonding pattern based on secondary or physical bond, such as pi-pi bond, hydrogen bond etc..
Chemical hydrogel is mainly by chemical bond connection molecule.The bonding pattern of hydrogel determines the physical property of hydrogel.It is such as stable
Property, physical hydrogel has row stability, can changed under the influence of external condition between liquid and solid-state.Chemical hydrogel is then
More stable, its profile will not change easily, but its quality is also very soft.
With the progress of modern science and technology, metal nano material arises at the historic moment.By that by antibacterial metal nanosizing, can carry at double
Rise the antibacterial ability of heavy metal.Wherein antibiotic property silver nano material, copper nano material are raw in food manufacturing, pharmaceutical engineering, industry
There is application in the place such as production.But there is the problem of unstable in the preservation of metal nano.Therefore, it is holding metal nano material
Stability, metal nanometre cluster hydrogel is made in metal nano material, the oxidation and reunion of metal nano is prevented, turns into metal
A kind of technology of nano materials research.
At present, although the method for synthesis silver nanoclusters hydrogel and copper nano-cluster hydrogel is more, complicated, cost is prepared
The features such as height, unstable silver or copper nano-cluster.Using small molecule sulfhydryl compound, such as Cys and silver ion or copper ion
Not only preparation process is simple for the hydrogel that interaction is formed, finished product is stable, but also assigns this material new performance.Separately
Outside, the metal nanometre cluster hydrogel currently prepared, its internal metal nanometer cluster is single metal mostly, otherwise be silver,
It is copper or gold.In order to increase the performance of antimicrobial nano material, research synthesis is received with metals more than two kinds of metallic atoms
The method of rice cluster composite aquogel is imperative.
Therefore, it is necessary to a kind of preparation method of copper silver nanoclusters composite aquogel be developed, in order to promote copper nanometer and silver
The use of nano material.
The content of the invention
To solve the above problems, technical scheme provided by the invention is, a kind of preparation of copper silver nanoclusters composite aquogel
Method, it is characterised in that comprise the following steps.
The first step, preparation of reagents.Under room temperature condition, a certain amount of silver nitrate AgNO is accurately weighed3, being made into molar concentration is
0.05mol/L ~ 0.5mol/L silver nitrate solution, it is standby.Accurately weigh a certain amount of nitrate trihydrate copper Cu (NO3)2·
3H2O, the copper nitrate solution that molar concentration is 0.05mol/L ~ 0.5mol/L is made into, it is standby.Accurately weigh a certain amount of L- half
Cystine L-cysteine, the Cys solution that molar concentration is 0.005mol/L ~ 0.05mol/L is made into, it is standby.
It is prepared by second step, presoma.By above-mentioned stock solution, in strict accordance with silver-colored Ag, copper Cu, Cys L-
Cysteine molal weight calculates, and is calculated according to mol ratio Ag: Cu: L-cysteine=1.6 ~ 2.2: 1: 2, drawing needs to make
Above-mentioned three kinds of reagent solutions under a standby cumulative volume meet the respective volume of mol ratio.Each component mol ratio, it is this hair
One of bright critically important invention, this is that a large amount of Optimal Experimentals are worked it out, and other ratio effects are all bad.Because such as
Fruit does not meet the precursor solution of mol ratio requirement, in subsequent preparation process, the silver nanoclusters and copper that are formed after photoreduction
Nano-cluster can not reach the effect of protection and reunite because the cysteine of attachment is insufficient, or cysteine excess shadow
Ring formation and the quality of copper silver nanoclusters composite aquogel.According to the volume of calculating, standby silver nitrate is accurately pipetted respectively
Solution, copper nitrate solution, Cys solution, it is positioned in a beaker and mixes.With mechanical agitator, by overall accumulated amount with
The mixing time that 5min/10mL is calculated, stirring.The mixing time calculated by overall accumulated amount with 5min/10mL, and optimization are come
, the time can not enough influence protection and grafting rate of the Cys to silver ion and copper ion, long easily to reunite on the contrary,
Influence dispersion effect.The presoma of well mixed copper silver nanoclusters composite aquogel is made.Then the presoma of preparation is put
In having in the centrifuge tube of lid, centrifugation lid is covered tightly, it is standby.Have in the centrifuge tube of lid is to ensure the preparation process in next step
In, avoid the volatilization of moisture.In the past in order to ensure next step uniform illumination, using the vessel of the wide-mouths such as culture dish, large beaker, but
It is that moisture is volatile, hydrogel is not easy to be formed.
3rd step, photopolymerization.It is placed in the case of darkroom, the presoma of the copper silver nanoclusters composite aquogel of preparation with purple
Outer smooth 365nm irradiations >=8h；At interval of 20 ~ 40min in irradiation process, acutely shaken using turbula shaker mixing 3min ~
5min, gelation >=2h is stood, copper silver nanoclusters composite aquogel is made.Concussion is needed to operate in irradiation process, this is to copper silver
The preparation of nano-cluster composite aquogel is also very crucial, is the key point of the present invention.Because photo-polymerization process is by ultraviolet light
The limitation of transmission depth, and the influence of presoma internal composition uniformity, especially emphasize to need repeatedly to polymerize and shake in this step
Swing scattered, the well dispersed copper silver nanoclusters composite aquogel of system can be made.This is also the main hair of the present invention
Bright point.Light application time, obtained in optimum experimental.Prepared by copper silver nanoclusters composite aquogel need ultraviolet light 365nm to irradiate
8h could form light blue solution, i.e. solution before gelation.Prepare the purple that copper silver nanoclusters composite aquogel needs so to grow
Outer light application time, it is because of the active relatively low of copper ion, needs more energy with cysteine reaction.Copper prepared by the present invention
Silver nanoclusters hydrogel is a kind of physical hydrogel, and it has thixotropy, easily can be changed between fluid and solid.
In above-mentioned technical proposal, the Cys L-cysteine can also be replaced with other sulfhydryl compounds.Example
Such as replaced with glutathione.The present invention is not limited to a kind of reagents of Cys L-cysteine.
In above-mentioned technical proposal, the silver nitrate AgNO3It can be substituted for other inorganic not water-soluble with copper ion reaction
Property silver salt, or organic silver salts；The nitrate trihydrate copper Cu (NO3)2·3H2O can be substituted for it is other not with silver ion reaction
Inorganic water-soluble mantoquita, or organic copper salt；Copper silver nanoclusters compound hydrogel material prepared by the invention can be applied to
Medical aspect, is used as antibacterial, anti-infectious dressing.The present invention can a variety of similar reagents of popularization and application, invention should
It is wide with property.
The mol ratio and the optimisation technique condition of ultraviolet lighting composed the invention provides copper silver nanoclusters compound water congealing.
Professional stronger, method is convenient, and the present invention has following beneficial effect.
（1）What is prepared is the copper silver nanoclusters composite aquogel containing two kinds of metals, and the silver and copper in hydrogel, which all have, to kill
Bacterium acts on, and hydrogel has sustained release, moisture-keeping function, may be used as wound dressing.By receiving the modification of material to copper nanometer and silver
Prepare, extend copper nanometer and silver receives the performance and use range of material.And the copper silver nanoclusters Compound Water for preparing the present invention
Gel, there is more excellent property and widely application.
（2）In terms of preparation method, using ultraviolet light reducing process, method is simple, is easily controlled.This method shortens system
The standby time, green, the hydrogel of formation is stable.
（3）Prepared hydrogel is physical hydrogel, and physical hydrogel has row stability, can be under the influence of external condition
Changed between liquid and solid-state.
Brief description of the drawings
Fig. 1 is the dried electron scanning micrograph of copper silver nanoclusters composite aquogel prepared by the present invention, is amplified
1K times.
Fig. 2 is the dried electron scanning micrograph of copper silver nanoclusters composite aquogel prepared by the present invention, is put
It is big 500 times.
Fig. 3 is that Fig. 2 of the present invention power spectrum samples the electron scanning micrograph in region.
Fig. 4 is the energy spectrum diagram that Fig. 3 of the present invention samples region.
Fig. 5 is the component content table for the energy spectrum analysis that Fig. 3 of the present invention samples region.
Embodiment
Further the present invention is illustrated with reference to the accompanying drawings and examples.
Referring to figs. 1 to Fig. 5, a kind of preparation method of copper silver nanoclusters composite aquogel, it is characterised in that including following step
Suddenly.
The first step, preparation of reagents.Under room temperature condition, 1.208g Cu (NO are accurately weighed3)2·3H2O is settled to 50mL capacity
In bottle, the Cu (NO that concentration is 0.1mol/L are made into3)2Solution.It is accurate to prepare 0.1mol/L AgNO3Solution, accurate configuration
0.01mol/L L-cysteine solution, it is standby.
It is prepared by second step, presoma.By above-mentioned stock solution, in strict accordance with silver ion Ag+, copper ion Cu2+, the Guang ammonia of L- half
Sour L-cysteine molal weight calculates, according to mol ratio Ag+∶Cu2+: L-cysteine=2: calculate at 1: 2, show that preparation is total
Above-mentioned three kinds of reagent solutions under volume 10mL meet the respective volume of mol ratio.It is accurate respectively according to the volume of calculating
Standby silver nitrate solution, copper nitrate solution, Cys solution are pipetted, is positioned in a beaker and mixes.Mixed population
Product is 10mL, and after stirring 5min, the presoma of well mixed copper silver nanoclusters composite aquogel is made.Then by before preparation
Drive body to be placed in the 20mL centrifuge tubes of lid, cover tightly centrifugation lid, it is standby.
3rd step, photopolymerization.It is placed in the case of darkroom, the presoma of the copper silver nanoclusters composite aquogel of preparation with purple
Outer smooth 365nm irradiations, after 20min acutely shakes mixing 3min, total photochemical time 9h with turbula shaker, stand gelation
2h。
Copper silver nanoclusters composite aquogel prepared by embodiment, after prolonging stream film forming, freeze-drying.Then will freeze-drying
Sample be placed in conductive silicon chip and spray platinum, S-3700N ESEM signs are carried out, referring to Fig. 1.It is compound to observe copper silver nanoclusters
The film forming pattern of hydrogel, SEM morphology characterization illustrate the copper silver nanoclusters composite aquogel film-formation result prepared
Well.
Copper silver nanoclusters composite aquogel prepared by embodiment, is dropped in conductive silicon chip, is placed after drying, is then sprayed platinum
Gold, S-3700N ESEM signs are carried out, referring to Fig. 2.Fig. 2 shows that dried copper silver nanoclusters composite aquogel is naturally dry
Split, surface is smooth, the smooth free from admixture of tomography or group of reuniting.To its energy spectrum analysis referring to Fig. 3, Fig. 4, as a result show, copper silver content
Meet in preparation process, required ratio, referring to Fig. 5.There is platinum Pt peak in Fig. 4, is to spray superincumbent receive before ESEM
Caused by Miboplatin bronze.
Copper silver nanoclusters composite aquogel prepared by embodiment, as dressing, applies the experimentation on adhesive bandage
Middle discovery, copper silver nanoclusters composite aquogel do not interfere with the soft comfortable feature of adhesive bandage, copper silver nanoclusters compound water congealing
Glue can be fitted in adhesive bandage surface well.
Claims (3)
1. a kind of preparation method of copper silver nanoclusters composite aquogel, it is characterised in that comprise the following steps：
The first step, preparation of reagents；Under room temperature condition, a certain amount of silver nitrate AgNO is accurately weighed3, being made into molar concentration is
0.05mol/L ~ 0.5mol/L silver nitrate solution, it is standby；Accurately weigh a certain amount of nitrate trihydrate copper Cu (NO3)2·
3H2O, the copper nitrate solution that molar concentration is 0.05mol/L ~ 0.5mol/L is made into, it is standby；Accurately weigh a certain amount of L- half
Cystine L-cysteine, the Cys solution that molar concentration is 0.005mol/L ~ 0.05mol/L is made into, it is standby；
It is prepared by second step, presoma；By above-mentioned stock solution, in strict accordance with silver ion Ag+, copper ion Cu2+, Cys L-
Cysteine molal weight calculates, according to mol ratio Ag+∶Cu2+: L-cysteine=1.6 ~ 2.2: calculate at 1: 2, and drawing needs
Above-mentioned three kinds of reagent solutions under the cumulative volume to be prepared meet the respective volume of mol ratio, according to the volume of calculating
Amount, accurately pipettes standby silver nitrate solution, copper nitrate solution, Cys solution respectively, is positioned in a beaker and mixes
Close；With mechanical agitator, the mixing time calculated by overall accumulated amount with 5min/10mL, stirring, the copper silver being well mixed is made and receives
The presoma of rice cluster composite aquogel；Then the presoma of preparation is placed in the centrifuge tube of lid, covers tightly centrifugation lid, it is standby
With；
3rd step, photopolymerization；By the presoma of the copper silver nanoclusters composite aquogel of preparation, it is placed in the case of darkroom, uses ultraviolet light
365nm irradiations >=8h；At interval of 20 ~ 40min in irradiation process, acutely shaken using turbula shaker mixing 3min ~
5min, gelation >=2h is stood, copper silver nanoclusters composite aquogel is made.
A kind of 2. preparation method of copper silver nanoclusters composite aquogel according to claim 1, it is characterised in that：The L-
Cysteine L-cysteine can also be replaced with other sulfhydryl compounds.
A kind of 3. preparation method of copper silver nanoclusters composite aquogel according to claim 1, it is characterised in that：The nitre
The silver-colored AgNO of acid3Other not Inorganic water-soluble silver salt with copper ion reaction, or organic silver salts can be substituted for；The three water nitre
Sour copper Cu (NO3)2·3H2O can be substituted for other not Inorganic water-soluble mantoquitas with silver ion reaction, or organic copper salt；Institute
State copper silver nanoclusters compound hydrogel material prepared by invention and can act as therapeutic medical antibacterial, anti-infective dressing.
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Cited By (4)
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| CN110591702A (en) * | 2019-09-19 | 2019-12-20 | 山西大学 | Preparation method and application of aggregation-induced luminescent silver nanocluster |
| CN111298789A (en) * | 2020-02-25 | 2020-06-19 | 福建生物工程职业技术学院 | Au/RGO composite aerogel and preparation method and application thereof |
| CN112710223A (en) * | 2020-12-24 | 2021-04-27 | 福建师范大学 | Preparation method of flexible strain sensor based on silver-coated copper powder composite gelatin hydrogel |
| CN114533947A (en) * | 2022-02-22 | 2022-05-27 | 湖南科技大学 | Preparation method and application of carbon-based bimetallic nanocluster with antibacterial activity and wound healing accelerating capacity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591702A (en) * | 2019-09-19 | 2019-12-20 | 山西大学 | Preparation method and application of aggregation-induced luminescent silver nanocluster |
| CN110591702B (en) * | 2019-09-19 | 2021-07-27 | 山西大学 | Preparation method and application of aggregation-induced luminescent silver nanocluster |
| CN111298789A (en) * | 2020-02-25 | 2020-06-19 | 福建生物工程职业技术学院 | Au/RGO composite aerogel and preparation method and application thereof |
| CN112710223A (en) * | 2020-12-24 | 2021-04-27 | 福建师范大学 | Preparation method of flexible strain sensor based on silver-coated copper powder composite gelatin hydrogel |
| CN114533947A (en) * | 2022-02-22 | 2022-05-27 | 湖南科技大学 | Preparation method and application of carbon-based bimetallic nanocluster with antibacterial activity and wound healing accelerating capacity |
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| CN107375993B (en) | 2020-04-14 |
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