CN107375993B - Preparation method of copper-silver nano-cluster composite hydrogel - Google Patents
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Abstract
The invention provides a preparation method of copper-silver nanocluster composite hydrogel, which comprises the following steps: firstly, preparing a reagent; secondly, preparing a precursor; and thirdly, carrying out photopolymerization to prepare the copper-silver nanocluster composite hydrogel. The invention takes L-cysteine of a sulfhydryl compound as a cross-linking agent, adopts an ultraviolet light reduction method to synthesize the stable copper and silver nano-cluster composite hydrogel in one step, and provides the optimized conditions of the molar ratio and the ultraviolet light illumination for synthesizing the copper and silver nano-cluster composite hydrogel. The invention has the beneficial effects that the prepared copper-silver nano-cluster composite hydrogel containing two metals has the bactericidal effect on both silver and copper in the hydrogel, has the slow-release and moisturizing effects, and can be used as a wound dressing, so that the copper-silver nano-cluster composite hydrogel has better properties and wider application. And the novel performance is endowed to the copper nano material and the silver nano material through modification, so that the practicability and the application range of the material are widened.
Description
Technical Field
The invention relates to a preparation method of hydrogel, in particular to a preparation method of copper-silver nano-cluster composite hydrogel used in the fields of materials, medicine, bioengineering and the like.
Background
Hydrogel is a material with a network structure. It contains a large amount of water inside. Hydrogels are classified into physical hydrogels and chemical hydrogels according to chemical bonds. The physical hydrogel is formed by mainly using physical bonds such as pi-pi bonds, hydrogen bonds and the like as the bonding mode between components. Chemical hydrogels are primarily composed of chemically bonded molecules. The bonding mode of the hydrogel determines the physical properties of the hydrogel. For example, stability, physical hydrogels are stable and can be transformed between liquid and solid states under the influence of external conditions. The chemical hydrogel is relatively stable, its shape does not easily change, but its texture is very soft.
With the progress of modern science and technology, metal nano materials are produced. The antibacterial ability of heavy metals can be improved by times by nanocrystallizing the antibacterial metals. The antibacterial silver nano material and the antibacterial copper nano material are applied to food manufacturing, medical engineering, industrial production and other places. However, the storage of metal nanoparticles is unstable. Therefore, in order to maintain the stability of the metal nano material, the metal nano material is made into metal nano cluster hydrogel, so that the oxidation and agglomeration of the metal nano are prevented, and the technology becomes a technology for researching the metal nano material.
At present, although a plurality of methods for synthesizing silver nanocluster hydrogel and copper nanocluster hydrogel exist, the preparation method has the characteristics of complexity, high cost, instability of silver or copper nanoclusters and the like. The hydrogel formed by the interaction of small molecule sulfhydryl compounds, such as L-cysteine, and silver ions or copper ions not only has simple preparation process and stable finished product, but also endows the material with new performance. In addition, the metal nanocluster hydrogel prepared currently has metal nanoclusters inside which are mostly single metal, either silver, copper or gold. In order to improve the performance of the antibacterial nano material, it is imperative to study a method for synthesizing the metal nanocluster composite hydrogel having more than two metal atoms.
Therefore, it is required to develop a method for preparing copper-silver nanocluster composite hydrogel so as to facilitate the use of copper nano and silver nano materials.
Disclosure of Invention
In order to solve the problems, the technical scheme provided by the invention is that the preparation method of the copper-silver nanocluster composite hydrogel is characterized by comprising the following steps.
In the first step, reagents are prepared. Accurately weighing a certain amount of silver nitrate AgNO at room temperature3Preparing silver nitrate solution with the molar concentration of 0.05-0.5 mol/L for later use. Accurately weighing a certain amount of copper nitrate trihydrate Cu (NO)3)2·3H2And O, preparing a copper nitrate solution with the molar concentration of 0.05-0.5 mol/L for later use. Accurately weighing a certain amount of L-cysteine to prepare an L-cysteine solution with the molar concentration of 0.005 mol/L-0.05 mol/L for later use.
And step two, preparing a precursor. And calculating the standby solution strictly according to the molar mass of the silver Ag, the copper Cu and the L-cysteine, and calculating according to the molar ratio of Ag to Cu to L-cysteine = 1.6-2.2 to 1 to 2, so as to obtain the respective volume amounts of the three reagent solutions which meet the molar ratio and need to be prepared under one total volume. The molar ratio of each component is one of the important inventions of the invention, which is made by a large number of optimization experiments, and the effect of other proportions is not good. This is because if the precursor solution does not meet the requirement of the molar ratio, in the subsequent preparation process, the silver nanoclusters and the copper nanoclusters formed after the reduction by illumination may be agglomerated due to insufficient attached cysteine, without reaching the protection effect, or the formation and quality of the copper-silver nanocluster composite hydrogel may be affected by excessive cysteine. Accurately transferring the silver nitrate solution, the copper nitrate solution and the L-cysteine solution for later use respectively according to the calculated volume amount, and placing the solutions in a beaker for mixing. Stirring with a mechanical stirrer for a stirring time of 5min/10mL based on the total volume. The stirring time calculated by 5min/10mL according to the total volume is also optimized, the insufficient time can affect the protection and grafting rate of the L-cysteine to silver ions and copper ions, and the long time can easily agglomerate to affect the dispersion effect. And preparing a precursor of the uniformly mixed copper-silver nanocluster composite hydrogel. The prepared precursor was then placed in a centrifuge tube with a lid, which was closed tightly for future use. The centrifuge tube with the cover is used for ensuring that the volatilization of water is avoided in the next preparation process. In the past, in order to ensure the uniform illumination of the next step, wide-mouth vessels such as culture dishes, large beakers and the like are adopted, but the water is volatile, and the hydrogel is not easy to form.
And thirdly, carrying out photopolymerization. Putting the precursor of the prepared copper-silver nanocluster composite hydrogel into a dark chamber, and irradiating for more than or equal to 8 hours by using 365nm ultraviolet light; and (3) violently shaking and mixing for 3-5 min by using a vortex oscillator at an interval of 20-40 min in the irradiation process, and standing for gelation for more than or equal to 2h to prepare the copper-silver nanocluster composite hydrogel. The oscillation operation is needed in the irradiation process, which is also critical to the preparation of the copper-silver nano-cluster composite hydrogel and is a key point of the invention. Because the photopolymerization process is limited by the transmission depth of ultraviolet light and the influence of the uniformity of components in the precursor, repeated polymerization and oscillation dispersion are particularly emphasized in the step, and the copper-silver nano-cluster composite hydrogel with good system dispersion can be prepared. This is also a main inventive point of the present invention. The illumination time is obtained in the experimental optimization. The preparation of the copper-silver nano-cluster composite hydrogel needs the irradiation of ultraviolet light at 365nm for 8 hours to form a light blue solution, namely the solution before gelation. The preparation of the copper-silver nanocluster composite hydrogel requires such a long ultraviolet irradiation time because the activity of copper ions is low and more energy is required for the reaction with cysteine. The copper-silver nanocluster hydrogel prepared by the invention is a physical hydrogel, has thixotropy and can be easily converted between a fluid and a solid.
In the technical scheme, the L-cysteine can be replaced by other sulfhydryl compounds. For example by glutathione. The present invention is not limited to L-cysteine, a reagent.
In the technical scheme, the silver nitrate AgNO3Can be replaced by other inorganic water-soluble silver salt which does not react with copper ions or organic silver salt; the copper nitrate trihydrate Cu (NO)3)2·3H2O can be replaced by other inorganic water-soluble copper salt which does not react with silver ions or organic copper salt; the copper-silver nanocluster composite hydrogel material prepared by the invention can be applied to medical treatment and used as an antibacterial and anti-infection dressing. The invention can be popularized and applied to various similar reagents, and has wide applicability.
The invention provides the optimized technical conditions of the mole ratio and the ultraviolet illumination for synthesizing the copper-silver nano-cluster composite hydrogel. The method has stronger specialty and convenient method, and the invention has the following beneficial effects.
(1) The prepared copper-silver nanocluster composite hydrogel containing two metals has the advantages that both silver and copper in the hydrogel have the bactericidal effect, and the hydrogel has the slow-release and moisturizing effects and can be used as a wound dressing. The performance and the application range of the copper nano and silver nano materials are expanded through the modified preparation of the copper nano and silver nano materials. The copper-silver nano-cluster composite hydrogel prepared by the invention has better properties and wider application.
(2) In the aspect of the preparation method, an ultraviolet light irradiation reduction method is adopted, and the method is simple and easy to control. The method shortens the preparation time, is environment-friendly, and the formed hydrogel is stable.
(3) The prepared hydrogel is physical hydrogel which has stability and can be converted between a liquid state and a solid state under the influence of external conditions.
Drawings
FIG. 1 is a scanning electron microscope photograph of the dried copper-silver nanocluster composite hydrogel prepared by the present invention, magnified 1K times.
FIG. 2 is a scanning electron microscope photograph of the dried Cu-Ag nanocluster composite hydrogel prepared by the present invention, magnified 500 times.
FIG. 3 is a scanning electron micrograph of the energy spectrum sampling region of FIG. 2 of the present invention.
FIG. 4 is an energy spectrum of the sample region of FIG. 3 according to the present invention.
FIG. 5 is a graph of the spectral analysis of the sample region of FIG. 3 showing the component content of the sample region according to the present invention.
Detailed Description
The invention is further described with reference to the following figures and examples.
Referring to fig. 1 to 5, a method for preparing a copper-silver nanocluster composite hydrogel is characterized by comprising the following steps.
In the first step, reagents are prepared. 1.208g of Cu (NO) are accurately weighed at room temperature3)2·3H2Preparing the O into Cu (NO) with the concentration of 0.1mol/L in a volumetric flask with the constant volume of 50mL3)2And (3) solution. Accurately preparing 0.1mol/L AgNO3The solution is prepared into 0.01mol/L L-cysteine solution for later use.
And step two, preparing a precursor. The above-mentioned solution is mixed with silver ion Ag+Copper ion Cu2+Calculating the molar mass of L-cysteine according to the molar ratio Ag+∶Cu2+And calculating the ratio of L-cysteine = 2: 1: 2 to obtain the respective volume amounts of the three reagent solutions according to the molar ratio under the condition of preparing the total volume of 10 mL. Accurately transferring the silver nitrate solution, the copper nitrate solution and the L-cysteine solution for later use respectively according to the calculated volume amount, and placing the solutions in a beaker for mixing. The total volume of the mixture is 10mL, and the precursor of the uniformly mixed copper-silver nanocluster composite hydrogel is prepared after stirring for 5 min. The prepared precursor was then placed in a 20mL centrifuge tube with a lid, and the centrifuge tube lid was closed and ready for use.
And thirdly, carrying out photopolymerization. And (3) putting the precursor of the prepared copper-silver nanocluster composite hydrogel into a dark room box, irradiating by using ultraviolet light at 365nm, violently shaking and mixing for 3min by using a vortex oscillator every 20min, standing for gelation for 2h after the total photochemical time is 9 h.
And (3) carrying out casting film formation on the copper-silver nanocluster composite hydrogel prepared in the example, and then freezing and drying. The freeze-dried sample was then placed on a conductive silicon wafer and platinum sprayed for S-3700N scanning electron microscopy characterization, see FIG. 1. And observing the film forming appearance of the copper-silver nano-cluster composite hydrogel, and showing the appearance of a scanning electron microscope, wherein the prepared copper-silver nano-cluster composite hydrogel has a good film forming effect.
Dropping the copper-silver nanocluster composite hydrogel prepared in the embodiment on a conductive silicon chip, placing and drying the conductive silicon chip, spraying platinum, and performing S-3700N scanning electron microscope characterization, which is shown in figure 2. FIG. 2 shows that the dried copper-silver nanocluster composite hydrogel is naturally cracked, has a smooth surface, and has smooth faults without impurities or agglomeration. The energy spectrum analysis is shown in fig. 3 and fig. 4, and the result shows that the content of copper and silver meets the required proportion in the preparation process, and is shown in fig. 5. FIG. 4 shows the peak of Pt, which is caused by the nano-platinum powder sprayed on the surface before the scanning electron microscope.
The copper-silver nano-cluster composite hydrogel prepared in the embodiment is used as a dressing and is applied to an experimental process of the band-aid, and the fact that the copper-silver nano-cluster composite hydrogel does not affect the characteristics of softness and comfort of the band-aid is found, and the copper-silver nano-cluster composite hydrogel can be well attached to the surface of the band-aid.
Claims (3)
1. A preparation method of copper-silver nanocluster composite hydrogel is characterized by comprising the following steps:
firstly, preparing a reagent; accurately weighing a certain amount of silver nitrate AgNO at room temperature3Preparing silver nitrate solution with the molar concentration of 0.05-0.5 mol/L for later use; accurately weighing a certain amount of copper nitrate trihydrate Cu (NO)3)2·3H2O, preparing a copper nitrate solution with the molar concentration of 0.05-0.5 mol/L for later use; accurately weighing a certain amount of L-cysteine to prepare an L-cysteine solution with the molar concentration of 0.005-0.05 mol/L for later use;
secondly, preparing a precursor; the above-mentioned solution is mixed with silver ion Ag+Copper ion Cu2+Calculating the molar mass of L-cysteine according to the molar ratio Ag+∶Cu2+Calculating the ratio of L-cysteine = 1.6-2.2: 1: 2 to obtain respective volume quantities of the three reagent solutions which meet the molar ratio and are required to be prepared under a total volume, accurately transferring the silver nitrate solution, the copper nitrate solution and the L-cysteine solution for later use respectively according to the calculated volume quantities, and placing the solution in a beaker for mixing; stirring by using a mechanical stirrer for 5min/10mL of stirring time according to the total volume amount to prepare a precursor of the uniformly mixed copper-silver nanocluster composite hydrogel; then placing the prepared precursor into a centrifuge tube with a cover, and tightly covering the centrifuge tube cover for later use;
thirdly, photopolymerization is carried out; putting the precursor of the prepared copper-silver nanocluster composite hydrogel into a dark chamber, and irradiating for more than or equal to 8 hours by using 365nm ultraviolet light; and (3) violently shaking and mixing for 3-5 min by using a vortex oscillator at an interval of 20-40 min in the irradiation process, and standing for gelation for more than or equal to 2h to prepare the copper-silver nanocluster composite hydrogel.
2. The preparation method of the copper-silver nanocluster composite hydrogel according to claim 1, which is characterized by comprising the following steps of: the L-cysteine can also be replaced by other sulfhydryl compounds.
3. The preparation method of the copper-silver nanocluster composite hydrogel according to claim 1, which is characterized by comprising the following steps of: the silver nitrate AgNO3Can be replaced by other inorganic water-soluble silver salt which does not react with copper ions or organic silver salt; the copper nitrate trihydrate Cu (NO)3)2·3H2O can be replaced by other inorganic water-soluble copper salt which does not react with silver ions or organic copper salt; the copper-silver nanocluster composite hydrogel material prepared by the preparation method can be used for preparing medical antibacterial and anti-infection dressings.
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| 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 |
| CN112710223B (en) * | 2020-12-24 | 2022-11-01 | 福建师范大学 | Preparation method of flexible strain sensor based on silver-coated copper powder composite gelatin hydrogel |
| CN114533947B (en) * | 2022-02-22 | 2022-11-01 | 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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