CN105665733A - Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode - Google Patents
Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode Download PDFInfo
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- CN105665733A CN105665733A CN201510827904.6A CN201510827904A CN105665733A CN 105665733 A CN105665733 A CN 105665733A CN 201510827904 A CN201510827904 A CN 201510827904A CN 105665733 A CN105665733 A CN 105665733A
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- graphite phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
Abstract
The invention discloses a method for preparing a graphite-like C3N4/nano-silver antibacterial composite in an environmental-friendly mode. The method includes the steps that (1) grape pips are washed by distilled water and dried at a low temperature; (2) 1g of the grape pips are added into 20-30 mL of ultrapure water, and the ultrapure water with the grape pips is heated at the constant temperature of 110-120 DEG C and stirred for 2-4 hours; (3) a solution is subjected to suction filtration to obtain a grape pip extracting solution; and (4) silver nitrate and a certain quantity of ultrathin graphite-like C3N4 nano-sheet dispersion liquid are mixed and then added into the grape pip extracting solution, and then the solution is heated at the temperature of 90-95 DEG C and stirred for 15-20 minutes so as to obtain the graphite-like C3N4/nano-silver antibacterial composite. According to the method, the graphite-like C3N4/nano-silver antibacterial composite is prepared through the one-step reduction method, and the green plant seeds are used as a reducing agent and are easy to collect; the method is simple, reaction conditions are mild, environmental friendliness is achieved, and production efficiency is high. In the preparation process for the graphite-like C3N4/nano-silver antibacterial composite, silver is successfully loaded on the surface of graphite-like C3N4, and thus the antibacterial performance of the composite is effectively improved.
Description
Technical field
The present invention relates to technical field of composite materials, in particular to a kind of green syt class graphite phase C3N4The preparation method of/nano silver antibacterial matrix material.
Background technology
Four nitrogenize three carbon (C3N4) it is a kind of carboritride, the people such as DavidM.Teter passed through Theoretical Calculation in 1996, it is proposed to its five kinds of structures that may exist, and were respectively α phase, β phase, cube phase (c phase), accurate cube phase (p phase) and class graphite phase (g phase). Wherein only have class graphite four nitrogenize three carbon (g-C mutually3N4) it is then unique soft matter phase, other four kinds of structures are all superhard material, at normal temperatures g-C3N4It it is most stable structure in 5 kinds of structures. g-C3N4Middle C and atom N are with sp2Hydridization, is formed the hexagon aromatic structure of similar phenyl ring, has the laminate structure being similar to graphite by σ key, and its interlamellar spacing is slightly less than the interlamellar spacing of graphite, has the physicochemical property that same graphite is similar. g-C3N4Obtained by trimeric cyanamide, Cynuric Chloride, cyanogen amine, Dicyanodiamide, urea etc., cheap and stablize, make g-C3N4Become the focus of further investigation. In existing report, g-C3N4Based composites has been widely used in catalysis, optics and electricity etc., but also rarely has report in antibacterial. Based on this, with g-C3N4For base material, silver atoms by with g-C3N4In C N, the strong interaction load of C N key is at g-C3N4Surface, formed g-C3N4/ AgNPs matrix material. On the one hand, owing to AgNPs load is at g-C3N4Surface, prevent the reunion of Nano silver grain, make silver nano-grain stable existence; Various composition in Semen Vitis viniferae and nanometer silver interact simultaneously, further increase the stability of nanometer silver; Enhance the anti-microbial property of material.
Microbiotic plays most important role in the sick microbial communicable disease for the treatment of, with the use of microbiotic, the resistance of microorganism but been significantly enhanced, and result for the treatment of is reduced, and the fast development of nanotechnology to be biological antibacterial research provide new opportunity. In existing research is reported, Nano silver grain has remarkable anti-microbial property, is a kind of nano material with broad prospect of application. Owing to Nano silver grain is very easily oxidized, with regard to giving, its application in practice brings difficulty for this. g-C3N4As a kind of stable carbon material, make Nano silver grain load on its surface, it is possible to greatly to strengthen the stability of Nano silver grain, become the focus of people's research.In the process preparing Nano silver grain, sodium borohydride, hydrazine hydrate etc. all can be used as reductive agent, but these reductive agents all health and environment to the mankind cause very big harm. And we will adopt the method reduction Silver Nitrate of green reduction, " turn waste into wealth ", utilize the active substance in Semen Vitis viniferae extracting solution to play the dual function of reductive agent and stablizer simultaneously, without the need to adding any reductive agent and stablizer, reaction conditions is gentle, environment is green friendly, and therefore, the research of this preparation method is significant.
Summary of the invention
Goal of the invention: it is desirable to provide a kind of novel class graphite phase C3N4The preparation method of/nano silver antibacterial matrix material, is specially with Semen Vitis viniferae extracting solution as reductive agent, without the need to adding any reductive agent and stablizer in preparation process, it is achieved reaction conditions is gentle, the green friendly object of environment.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is as follows:
1. a Green synthesis class graphite phase C3N4The method of/nano silver antibacterial matrix material, it comprises the following steps:
1) get the Semen Vitis viniferae of collection, clean with self-care water, be placed in baking oven, oven drying at low temperature, obtain clean Semen Vitis viniferae;
2) take 1.0000g Semen Vitis viniferae with analytical balance, add 20-30mL ultrapure water (ratio of the quality of Semen Vitis viniferae and the volume of water is 1:20-30), under 110-120 DEG C of constant temperature heated and stirred 2-4 hour;
3) undertaken taking out filter by obtained solution, obtain Semen Vitis viniferae extracting solution;
4) adding in 100g deionized water by 0.1g class graphite phase four nitrogenize three carbon, ultrasonic liquid-phase peels off 24 hours, obtains ultra-thin class graphite phase C3N4The dispersion soln of nanometer sheet;
5) the Silver Nitrate class graphite phase C ultra-thin with 3mL of different amount is got3N4The dispersion soln of nanometer sheet mixes mutually, obtains Silver Nitrate/class graphite phase C3N4Mixed solution;
6) the Semen Vitis viniferae extracting solution getting different amount adds Silver Nitrate/ultra-thin class graphite phase C3N4In mixed solution;
7) above-mentioned mixing solutions stirs at 90-95 DEG C of constant temperature lower magnetic force, reacts 15-20 minute, namely obtains class graphite phase C3N4/ nano silver antibacterial matrix material.
2. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: the class graphite phase C adopted3N4It is prepare through high-temperature calcination trimeric cyanamide according to document.
3 class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: grape used is purchased from China Zhenhua supermarket, Yantai, manually isolates Semen Vitis viniferae, and dry from pomace.
4. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: described in the final concentration of Silver Nitrate that adds be 1-3mM.
5. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: described in the volume of Semen Vitis viniferae extracting solution that adds be 1-2mL.
6. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: the volume of described final mixing solutions is 20mL.
7. one kind by the class graphite phase C described in claim 1-6 any one3N4The class graphite phase C that the preparation method of/nano silver composite material obtains3N4/ nano silver antibacterial matrix material.
The present invention has the following advantages:
(1) Semen Vitis viniferae is beneficial to collection, adopts Semen Vitis viniferae extracting solution as reductive agent and stablizer, and environmental protection, meets the theory of Green Chemistry.
(2) Silver Nitrate is reduced to Nano silver grain, and load is at g-C3N4In substrate, effectively prevent the reunion of nano-Ag particles, substantially increase the stability of Nano silver grain.
(3) this reaction carries out in aqueous phase, and reaction conditions is gentle, the g-C of preparation3N4/ AgNPs matrix material has better fungistatic effect than the AgNPs of single green syt.
Accompanying drawing explanation
Fig. 1: prepared g-C3N4/ AgNPs antibacterial composite material, g-C3N4The uv-vis spectra of nanometer sheet and Semen Vitis viniferae extracting solution;
Fig. 2: prepared g-C3N4/ AgNPs antibacterial composite material and g-C3N4The X ray diffracting spectrum of nanometer sheet;
Fig. 3: prepared g-C3N4/ AgNPs matrix material and g-C3N4The transmission electron microscope photo figure of nanometer sheet;
Fig. 4 is g-C3N4The simple AgNPs of/AgNPs antibacterial composite material and green syt is to the antibacterial circle diameter result of Gram-negative bacteria intestinal bacteria, Pseudomonas aeruginosa and gram-positive microorganism streptococcus aureus, Bacillus subtilus.
Embodiment
Below in conjunction with accompanying drawing, provide the specific embodiment of the present invention, it is used for the present invention being further described.
The laboratory apparatus that this invention uses
Ultraviolet-visible pectrophotometer (ShimadzuUV-2550), infrared spectrometer (NicoletNexus670), X ray diffracting spectrum (XRD; RigakuD/max-2500VPC), transmission electron microscope (TEM, JEM-1230).
Embodiment 1
The g-C adopted3N4550 DEG C of high-temperature calcination trimeric cyanamides obtained (Zhang, X. in retort furnace; Xie, X.; Wang, H.; Zhang, J.; Pan, B.; Xie, Y.EnhancedPhotoresponsiveUltrathinGraphitic-PhaseC3N4NanosheetsforBioimaging.J.Am.Chem.Soc. 2013,135, 18-21.).
Product after calcining takes 0.1g in beaker, adds 100mL ultrapure water, and ultrasonic liquid-phase peels off 24h, and centrifuging and taking supernatant liquid obtains ultra-thin g-C3N4Nanometer sheet dispersion soln.
Grape used is purchased from China Zhenhua supermarket, Yantai, manually isolates Semen Vitis viniferae, and dry from pomace.
Getting the Semen Vitis viniferae of collection, clean with ultrapure water, be placed in baking oven, 50 DEG C of dryings 30 minutes, obtain clean Semen Vitis viniferae. Take 1.0000g Semen Vitis viniferae with analytical balance, add 20mL ultrapure water, stir 2 hours at 120 DEG C of constant temperature lower magnetic forces. Undertaken taking out filter by obtained solution, obtain Semen Vitis viniferae extracting solution. Get the ultra-thin g-C of 3mL3N4Nanometer sheet adds in 14mL ultrapure water, then adds silver nitrate solution and the 1mL Semen Vitis viniferae extracting solution of 2mL0.01M, stirs at 95 DEG C of constant temperature lower magnetic forces, reacts 20 minutes, namely obtain g-C3N4/ AgNPs matrix material.
Do not add g-C3N4(adding isopyknic ultrapure water), the AgNPs preparing green syt under same condition carries out antibacterial contrast experiment.
To obtained g-C3N4/ AgNPs antibacterial composite material characterizes, specific as follows:
(1) uv-visible absorption spectra characterizes
As shown in Figure 1, in figure, a, b and c are respectively g-C3N4/AgNPs、g-C3N4And the uv-visible absorption spectra figure of Semen Vitis viniferae extracting solution. As can be seen from the figure, g-C3N4/ AgNPs matrix material is at the surface plasma body resonant vibration peak that wavelength is that about 440nm place nano-Ag particles occurs, and g-C3N4And Semen Vitis viniferae extracting solution is at this region Wu Feng.
(2) X ray diffracting spectrum (XRD) test
Ultra-thin g-C3N4Nanometer sheet and g-C3N4The X ray diffracting spectrum of/AgNPs matrix material, as shown in Figure 2. In figure, a is g-C3N4The X ray diffracting spectrum of/AgNPs matrix material, b is ultra-thin g-C3N4X ray diffracting spectrum. Wherein, in a figure, 2 θ angles are respectively the characteristic diffraction peak that nano-Ag particles have all occurred in 37.8 °, 43.9 °, 64.4 °, 77.4 ° places, distinguish (111), (200), (220) and (311) crystal face of correspondence silver, demonstrate nanometer silver and successfully prepared.B figure is 13.2 ° at 2 θ angles and two characteristic diffraction peaks has occurred when 27.38 °, this correspondence g-C3N4(100) and (002) crystal face. There is not g-C in a figure3N4Diffraction peak, it may be that g-C in matrix material3N4Amount cause very little.
(3) transmission electron microscope (TEM) test
g-C3N4Nanometer sheet and g-C3N4The TEM photo of/AgNPs matrix material, as shown in Figure 3. As can be seen from the figure, the successful load of nano-Ag particles is at g-C3N4In nanometer sheet, particle diameter is greatly between 20-40nm.
(4) infrared spectra (IR) test
g-C3N4The infrared spectra of/AgNPs antibacterial composite material and Semen Vitis viniferae extracting solution, g-C3N4/ AgNPs and Semen Vitis viniferae extracting solution are at 3433.34cm-1、2921.0cm-1And 1616,16cm-1There is similar absorption peak at wavelength place. At 3433.34cm-1Locate strong and wide absorption peak to cause by-OH stretching vibration, 2921.0cm-1The peak at place is CH, CH in aliphatics2And CH3Existence cause, and 1616,16cm-1The peak at place is then the result of phenyl ring stretching vibration. The functional group that these similar absorption peaks illustrate in Semen Vitis viniferae extracting solution is successfully compounded in g-C3N4In/AgNPs, enhance the stability of matrix material.
(5) bacteriostatic experiment
1) preparation of LB substratum
The preparation of LB liquid nutrient medium: get yeast extract 5g, the old 10g of albumen, sodium-chlor 5g, ultrapure water is settled to 1000mL, by the NaOH adjust ph to 7.2 of 1M; The preparation of LB solid medium is the agar adding 1.5%-2% in the nutrient solution of above-mentioned preparation again. Above two kinds of substratum are all placed in through 120 DEG C in autoclave, 0.1Mpa autoclaving 20min, and room temperature is put in the liquid nutrient medium cooling of bacterium of having gone out, and is positioned over 4 DEG C of Refrigerator stores; Solid medium is then divided equally in time not solidifying and is loaded in test tube and culture dish, and room temperature is put in cooling, is positioned over 4 DEG C of Refrigerator stores. LB substratum is for clinical pathogenic bacteria intestinal bacteria, Pseudomonas aeruginosa, gold-coloured staphylococci and Bacillus subtilus cultivation.
2) Bactericidal test
LB substratum is adopted, 37 DEG C of cultivations for the clinical pathogenic bacteria of examination; Adopt the bacteriostatic activity of agar diffusion method detection of active material: be added in 5mL liquid nutrient medium by indicator 50 μ L, 200rpm shakes 8 ~ 10h, it is cultured to the logarithm rise period, bacterium liquid normal saline dilution is to 106CFU/mL, getting 100 μ L respectively is spread evenly across on solid medium, then places Oxford cup (cup external diameter 8mm) on substratum, adds the active substance 30 μ L of synthesis in embodiment 1 in cup, do negative control with physiological saline, do three repetitions. Observe after culture dish is cultivated in constant incubator 18h, measure antibacterial circle diameter, average, judge g-C3N4The bacteriostatic activity of the AgNPs of/AgNPs and green syt.
g-C3N4/ AgNPs antibacterial composite material and nanometer silver to the antibacterial circle diameter of intestinal bacteria, Pseudomonas aeruginosa, streptococcus aureus and Bacillus subtilus, as shown in Figure 4. It may be seen that g-C in embodiment 13N4The antibacterial circle diameter of intestinal bacteria, Pseudomonas aeruginosa, streptococcus aureus and Bacillus subtilus is respectively 15.1 ± 1.2mm, 12.0 ± 1.2mm, 11.5 ± 0.5mm and 13.0 ± 0.3mm by/AgNPs antibacterial composite material, is all greater than the antibacterial circle diameter of the AgNPs of green syt. Illustrate that Nano silver grain loads to g-C3N4After improve dispersion and the stability of nanometer silver, it is to increase the bacteriostasis property of material.
Embodiment 2
The silver nitrate solution of the 2mL0.01M added changes into the silver nitrate solution of 4mL0.01M, and 14mL ultrapure water changes 12mL ultrapure water into, repeats embodiment 1 step, the g-C obtained3N4The inhibition zone of the Nano silver grain that the inhibition zone of 4 kinds of pathogenic bacterias is still greater than under now same concentrations green syt by/AgNPs antibacterial composite material.
Above embodiment is not exhaustive, and its protection domain is not limited to given embodiment, and every all technical schemes achieved by the thinking of patent of the present invention, all belong to the protection domain of patent of the present invention.
Claims (7)
1. a Green synthesis class graphite phase C3N4The method of/nano silver antibacterial matrix material, it comprises the following steps:
1) get the Semen Vitis viniferae of collection, clean with self-care water, be placed in baking oven, oven drying at low temperature, obtain clean Semen Vitis viniferae;
2) take 1.0000g Semen Vitis viniferae with analytical balance, add 20-30mL ultrapure water (ratio of the quality of Semen Vitis viniferae and the volume of water is 1:20-30), under 110-120 DEG C of constant temperature heated and stirred 2-4 hour;
3) undertaken taking out filter by obtained solution, obtain Semen Vitis viniferae extracting solution;
4) adding in 100g deionized water by 0.1g class graphite phase four nitrogenize three carbon, ultrasonic liquid-phase peels off 24 hours, obtains ultra-thin class graphite phase C3N4The dispersion soln of nanometer sheet;
5) the Silver Nitrate class graphite phase C ultra-thin with 3mL of different amount is got3N4The dispersion soln of nanometer sheet mixes mutually, obtains Silver Nitrate/class graphite phase C3N4Mixed solution;
6) the Semen Vitis viniferae extracting solution getting different amount adds Silver Nitrate/ultra-thin class graphite phase C3N4In mixed solution;
7) above-mentioned mixing solutions stirs at 90-95 DEG C of constant temperature lower magnetic force, reacts 15-20 minute, namely obtains class graphite phase C3N4/ nano silver antibacterial matrix material.
2. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: the class graphite phase C adopted3N4It is prepare through high-temperature calcination trimeric cyanamide according to document.
3. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: grape used is purchased from China Zhenhua supermarket, Yantai, manually isolates Semen Vitis viniferae, and dry from pomace.
4. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: described in the final concentration of Silver Nitrate that adds be 1-3mM.
5. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: described in the volume of Semen Vitis viniferae extracting solution that adds be 1-2mL.
6. class graphite phase C according to claim 13N4The preparation method of/nano silver antibacterial matrix material, it is characterised in that: the volume of described final mixing solutions is 20mL.
7. one kind by the class graphite phase C described in claim 1-6 any one3N4The class graphite phase C that the preparation method of/nano silver composite material obtains3N4/ nano silver antibacterial matrix material.
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CN111515384A (en) * | 2020-04-10 | 2020-08-11 | 深圳大学 | Nano-silver material mediated and synthesized by moringa seed extract |
CN113664213A (en) * | 2021-08-04 | 2021-11-19 | 湖南伟方生命科技有限公司 | Preparation method and application of nano-silver antibacterial liquid |
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