CN109332720B - High-dispersity nano-silver antibacterial material and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of chemical materials, and provides a high-dispersity nano-silver antibacterial material and a preparation method thereof. A preparation method of a high-dispersity nano-silver antibacterial material comprises the steps of pyrolyzing sulfur-containing coal to obtain a carbon material with surface functional groups, wherein the sum of the contents of iron sulfide and organic sulfur in the sulfur-containing coal is more than 2.5 percent, the pyrolysis temperature is 600-1000 ℃, and the surface functional groups comprise thiophene; treating the carbon material and the silver ion solution by adopting an impregnation method to obtain a silver ion/carbon material; and (3) treating the silver ion/carbon material by using radio frequency plasma to obtain the required high-dispersity nano silver antibacterial material. The high-dispersity nano-silver antibacterial material can be obtained by the preparation method of the high-dispersity nano-silver antibacterial material. The invention also provides a high-dispersity nano-silver antibacterial material, and the nano-silver particles loaded on the high-dispersity nano-silver antibacterial material have the advantages of high dispersity and strong antibacterial capability.
Description
Technical Field
The invention relates to the technical field of chemical materials, in particular to a high-dispersity nano-silver antibacterial material and a preparation method thereof.
Background
Globalization and urbanization have brought about an increase in population mobility, so that various forms of bacterial infection have become more and more serious, and it has become more and more important how to inhibit the increase and reproduction of bacteria. Among a plurality of antibacterial materials, the silver-based antibacterial material has the performances of broad-spectrum antibacterial and long-acting antibacterial, particularly can still keep high-efficiency antibacterial property at a lower concentration, and is always considered as the first choice of a green inorganic antibacterial agent. Compared with bulk silver, the nano-silver particles have excellent antibacterial ability due to higher surface energy and reactivity, and are widely used in the fields of medical health and the like. For nano silver, the dispersibility has a great influence on the antibacterial ability of the nano silver, and therefore, how to obtain a nano silver material with high dispersibility becomes a popular research and development target.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-dispersity nano-silver antibacterial material and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme. A preparation method of a high-dispersity nano-silver antibacterial material comprises the steps of pyrolyzing sulfur-containing coal to obtain a carbon material with surface functional groups, wherein the sum of the contents of iron sulfide and organic sulfur in the sulfur-containing coal is more than 2.5 percent, the pyrolysis temperature is 600-1000 ℃, and the surface functional groups comprise thiophene; treating the carbon material and the silver ion solution by adopting an impregnation method to obtain a silver ion/carbon material; and (3) treating the silver ion/carbon material by using radio frequency plasma to obtain the required high-dispersity nano silver antibacterial material.
Preferably, the basicity index of said sulfur-containing coal is greater than 0.5 or the organosulfur content of said sulfur-containing coal is greater than 2.5%.
Preferably, the method further comprises pretreating the sulfur-containing coal before pyrolyzing the sulfur-containing coal, wherein the pretreating comprises grinding and screening the sulfur-containing coal.
Preferably, the particle size of the sulfur-containing coal is controlled to be 150-250 μm when the grinding and screening are performed.
Preferably, the pyrolysis adopts temperature rise-constant temperature pyrolysis, the temperature is raised to the target temperature at the speed of 5-20 ℃/min, and then the temperature is kept for 30-60 min.
Preferably, the concentration of the silver ion solution is 0.2-1.5 g/L.
Preferably, the impregnation method is an equal-volume impregnation method or a multiple impregnation method.
Preferably, the frequency of the RF plasma is 200-500kHz, the output power is 100-400W, and the processing time is 1-5 min.
The high-dispersity nano-silver antibacterial material is prepared by the preparation method of the high-dispersity nano-silver antibacterial material.
Preferably, the particle size of the nano silver particles loaded on the high-dispersity nano silver antibacterial material is 1-5 nm.
The invention has the beneficial effects that:
the invention provides a preparation method of a high-dispersity nano-silver antibacterial material, which is characterized in that sulfur-containing coal is used as a raw material, a carbon material with surface functional groups is obtained after pyrolysis, the surface functional groups comprise thiophene, and the thiophene and silver ions have a strong adsorption effect, and then the silver ions are reduced by radio frequency plasma to form nano-silver, so that the required high-dispersity nano-silver antibacterial material is obtained, and the high-dispersity immobilization of the nano-silver on the surface of the carbon material is realized. And functional groups on the surface of the carbon material can be reserved by means of radio frequency plasma, so that green reduction of the high-dispersity nano silver particles is realized. In addition, most of the sulfur-containing coal needs to be desulfurized and then utilized, and the invention utilizes the sulfur contained in the sulfur-containing coal, thereby exploiting the utilization mode and the utilization value of the sulfur-containing coal.
The invention also provides a high-dispersity nano-silver antibacterial material, and the nano-silver particles loaded on the high-dispersity nano-silver antibacterial material have the advantages of high dispersity and strong antibacterial capability.
Drawings
Fig. 1 is a flow chart of a method for preparing a high-dispersibility nano silver antibacterial material according to the present invention.
Fig. 2 is a fourier infrared spectrometer (FT-IR) diagram of the highly dispersible nano silver antibacterial material of the present invention.
Detailed Description
For those skilled in the art to more clearly understand the objects, technical solutions and advantages of the present invention, the following description will be further provided in conjunction with the accompanying drawings and examples.
Example one
As shown in fig. 1, a method for preparing a catalyst comprises:
step S1: pyrolyzing sulfur-containing coal to obtain a carbon material with surface functional groups, wherein the sum of the contents of iron sulfide and organic sulfur in the sulfur-containing coal is more than 2.5 percent, the pyrolysis temperature is 600-1000 ℃, and the surface functional groups comprise thiophene;
step S2: treating the carbon material and the silver ion solution by adopting an impregnation method to obtain a silver ion/carbon material;
step S3: and (3) treating the silver ion/carbon material by using radio frequency plasma to obtain the required high-dispersity nano silver antibacterial material.
The coal can be divided into low-sulfur coal (less than 1%), medium-sulfur coal (between 1% and 2%) and high-sulfur coal (more than 2%), and the sulfur contained in the coal can be divided into inorganic sulfur and organic sulfur, and the inorganic sulfur comprises sulfate sulfur and iron sulfide sulfur.
In the present invention, that is, in step S1, the carbon material having thiophene can be obtained by selecting the sulfur-containing coal having a sum of the contents of iron sulfide and organic sulfur of more than 2.5%, and determining the pyrolysis temperature to ensure the pyrolysis degree of the sulfur-containing coal.
In some preferred embodiments, the sulfur-containing coal has a basicity index, R, of greater than 0.5. The calculation expression of the basicity index R is as follows:
wherein, Fe2O3For Fe in sulfur-containing coal2O3CaO is the content of CaO in the sulfur-containing coal, MgO is the content of MgO in the sulfur-containing coal, Na2O is Na in sulfur-containing coal2Content of O, K2O is K in sulfur-containing coal2Content of O, SiO2For SiO in sulfur-containing coal2Content of (C), Al2O3For Al in sulfur-containing coal2O3The content of (a). When the alkalinity index R is higher, the sulfur fixing effect in the pyrolysis process is good.
In other preferred embodiments, the sulfur-containing coal has an organic sulfur content of greater than 2.5%. The organic sulfur is more stable than the iron sulfide sulfur, and the proportion of the organic sulfur converted into thiophene in the pyrolysis process is high.
Preferably, the pyrolysis adopts temperature rise-constant temperature pyrolysis, the temperature is raised to the target temperature at the speed of 5-20 ℃/min, and then the temperature is kept for 30-60 min. Wherein the target temperature, namely the pyrolysis temperature, is used for obtaining more stable thiophene by determining the temperature rising rate. Preferably, the temperature is increased to the target temperature at the speed of 5-15 ℃/min and then is kept constant for 30-50 min. In some specific embodiments, the temperature is raised to the target temperature at 10 ℃/min and then kept constant for 40 min. Preferably, the pyrolysis is carried out under an argon atmosphere.
Preferably, the method further comprises pretreating the sulfur-containing coal before pyrolyzing the sulfur-containing coal, wherein the pretreating comprises grinding and screening the sulfur-containing coal. Through grinding and screening, the particle size of the sulfur-containing coal can be better controlled, and the uniformity is ensured. Preferably, the particle size of the sulfur-containing coal is controlled to be 150-250 μm, and the sulfur-containing coal with the particle size of 150-250 μm is obtained by screening after grinding.
In step S2, the dipping method is preferably an equal-volume dipping method or a multiple-dipping method, and the dipping effect is good. The loading capacity can be well determined by the isometric impregnation method, namely the provided silver ions are loaded on the carbon material, and the dispersion uniformity of the silver ions is good; multiple impregnations are effective in increasing the loading. It will be appreciated that when an equivalent volume impregnation is used, it is necessary to first determine the saturated water absorption capacity of the support, i.e. the carbon material.
The concentration of the silver ion solution is too high, waste is caused, the concentration of the silver ion solution is too low, and the antibacterial performance is affected due to insufficient loading capacity. Preferably, the concentration of the silver ion solution is 0.2-1.5 g/L. In some specific embodiments, the concentration of the silver ion solution is 0.6g/L, 0.8g/L, 0.9g/L, 1.0g/L, 1.2 g/L.
In step S3, preferably, the frequency of the RF plasma is 200-500kHz, the output power is 100-400W, and the processing time is 1-5 min. Preferably, the frequency of the RF plasma is 250-350kHz, and the output power is 200-300W. The treatment time can be adjusted according to the silver ion concentration, and when the silver ion concentration is less than or equal to 0.6g/L, the treatment time is 1 min; when the concentration of silver ions is more than 0.6g/L and less than 0.9g/L, the treatment time is 2-4 min; when the concentration of silver ions is more than or equal to 0.9g/L, the treatment time is 5 min.
Example two
The high-dispersity nano-silver antibacterial material is prepared by the preparation method of the high-dispersity nano-silver antibacterial material provided in the first embodiment, and has the advantage of high antibacterial capability. The nano silver particles loaded on the high-dispersity nano silver antibacterial material have good dispersity, and the particle size of the nano silver particles loaded on the high-dispersity nano silver antibacterial material is 1-5 nm.
The following provides a description of specific experiments and corresponding results
First, raw material analysis (analysis of coal containing sulfur)
Four different rank sulfur-bearing coals (CoalA, CoalB, CoalC, CoalD) are provided, with rank order of CoalA < CoalB < CoalC < CoalD. The chemical analysis morphological sulfur data of the four sulfur-containing coals are shown in table 1, and the ash analysis of the four sulfur-containing coals is shown in table 2.
TABLE 1 chemical analysis morphological Sulfur data for four sulfur-containing coals
TABLE 2 Ash analysis of four sulfur-containing coals
The calculated expression of the basicity index R in table 2 is as follows:
wherein, Fe2O3For Fe in sulfur-containing coal2O3CaO is the content of CaO in the sulfur-containing coal, MgO is the content of MgO in the sulfur-containing coal, Na2O is Na in sulfur-containing coal2Content of O, K2O is K in sulfur-containing coal2Content of O, SiO2For SiO in sulfur-containing coal2Content of (C), Al2O3For Al in sulfur-containing coal2O3The content of (a).
Preparation of nano silver antibacterial material
1. Pretreatment of sulfur-containing coal
The sulfur-containing coal was ground in a mortar and then sieved with a mesh screen to obtain sulfur-containing coal having a particle size of 150-.
2. Pyrolysis of sulfur-containing coal
And (3) carrying out a temperature programming-constant temperature pyrolysis experiment on the pretreated sulfur-containing coal by adopting a normal-pressure fixed bed reaction device. The specific operation steps are as follows:
0.5 sample of coal was weighed and placed evenly on the sinter plate in the center of the quartz reactor. Argon gas is used as pyrolysis carrier gas (purity is more than 99.99 percent) and is introduced from the top of the reactor at the flow rate of 600mL/min to replace the air in the reactor, after the air in the reactor is fully replaced, a program temperature controller is set, the temperature is raised to a target temperature at the temperature rise rate of 10 ℃/min, and corresponding time is kept according to different experiments to obtain a pyrolysis product, namely the required carbon material with surface functional groups.
3. Impregnation method silver loading (isovolumetric impregnation)
Measuring the saturated water absorption capacity of the carrier: weighing a certain amount of the carrier (namely the carbon material with the surface functional groups) obtained in the step 2, adding a metered volume of deionized water, standing overnight, sucking the upper layer of deionized water out by using a rubber head dropper, and measuring the volume, wherein the reduction of the volume is the saturated water absorption capacity of the certain amount of the carbon material.
Weighing corresponding silver nitrate solution according to the saturated water absorption capacity, adding the carbon material into the silver nitrate solution, standing for 12-24h or carrying out ultrasonic treatment for 1-3h, and drying in a vacuum drying oven at 50 ℃ for 24h to obtain the silver ion/carbon material.
4. Radio frequency plasma reduction
Putting the silver ion/carbon material obtained in the step (3) into a beaker, and putting the beaker on a substrate table of a radio frequency plasma source; sequentially starting a water pump, a main power supply and a mechanical pump, then vacuumizing, opening a helium switch after the vacuum degree is lower than 5Pa, and adjusting the gas flow to enable the pressure in the reaction cavity to be lower than 60 Pa; turning on the radio frequency power supply, preheating for 5-10min, adjusting power, and emitting glow. After reacting for a certain time, closing the radio frequency power supply, the gas valve, the mechanical pump, the main power supply and the water pump in sequence to obtain the required nano silver antibacterial material.
A plurality of groups of experiments are carried out by selecting different sulfur-containing coal, pyrolysis temperature, silver nitrate concentration, plasma parameters and treatment time, and the specific conditions of different experimental groups are shown in Table 3.
TABLE 3 Experimental conditions for Experimental groups 1-9
Third, characterization and analysis of experimental results
1. Analysis of pyrolysis results
The sulfur content of the carbon material obtained after pyrolysis was measured, and the type of the surface functional group was determined by a Fourier Infrared spectrometer (FT-IR) (FIG. 2).
The sulfur content in the carbon material obtained in each experimental group is shown in Table 4.
TABLE 4
As shown in FIG. 2, the FT-IR spectrum was used for raw coal and CO2And N2The surface functional groups of the carbon material formed by pyrolysis under an atmosphere were analyzed. As can be seen from the analysis of FIG. 2, the value of No. 1 (Experimental group 1) was 471, 537 and 1030cm as it was-1Infrared absorption peaks appeared at the positions of 2911cm and caused by-S-H-, -S-S-and-S ═ O-stretching vibration-1is-CH2-characteristic absorption peaks. By reviewing the data, it can be concluded that organic sulfur is present in large part in the form of disulfide. No. 2 (experimental group 4) and No. 3 (experimental group 7) in CO2And N2The carbon material formed by pyrolysis in different atmospheres was at 418 and 660cm-1Corresponds to the-C-S-stretching vibration absorption peak. Indicating that functional groups such as thiophene are mainly generated in the high-temperature pyrolysis process.
2. Antibacterial property of nano silver antibacterial material
Aiming at the nano-silver antibacterial materials prepared by each group, the antibacterial performance of the nano-silver antibacterial materials is measured by a bacteriostatic ring method. The selected strains are respectively escherichia coli and staphylococcus aureus represented by gram-negative bacteria and gram-positive bacteria.
The diameters of the bacteriostatic rings of each experimental group are shown in Table 5.
TABLE 5
The standard of the bacteriostatic ring method is that if the diameter of the bacteriostatic ring is more than 7mm, the antibacterial effect is shown, and if the diameter is larger, the antibacterial effect is better.
Claims (10)
1. A preparation method of a high-dispersity nano-silver antibacterial material is characterized by comprising the following steps: pyrolyzing sulfur-containing coal to obtain a carbon material with surface functional groups, wherein the sum of the contents of iron sulfide and organic sulfur in the sulfur-containing coal is more than 2.5 percent (wt%), the pyrolysis temperature is 600-1000 ℃, and the surface functional groups comprise thiophene;
treating the carbon material and the silver ion solution by adopting an impregnation method to obtain a silver ion/carbon material;
and (3) treating the silver ion/carbon material by using radio frequency plasma to obtain the required high-dispersity nano silver antibacterial material.
2. The method for preparing the high-dispersibility nano-silver antibacterial material according to claim 1, wherein the method comprises the following steps: the sulfur-containing coal has a basicity index of greater than 0.5 or the sulfur-containing coal has an organic sulfur content of greater than 2.5% (wt%).
3. The method for preparing the high-dispersibility nano-silver antibacterial material according to claim 1, wherein the method comprises the following steps: the method also comprises the step of pretreating the sulfur-containing coal before pyrolyzing the sulfur-containing coal, wherein the pretreatment comprises grinding and screening the sulfur-containing coal.
4. The method for preparing the high-dispersibility nano-silver antibacterial material according to claim 3, wherein the method comprises the following steps: during the grinding and screening, the particle size of the sulfur-containing coal is controlled to be 150-250 μm.
5. The method for preparing the high-dispersibility nano-silver antibacterial material according to claim 1, wherein the method comprises the following steps: the pyrolysis adopts temperature rise-constant temperature pyrolysis, the temperature is raised to the target temperature at the speed of 5-20 ℃/min, and then the temperature is kept for 30-60 min.
6. The method for preparing the high-dispersibility nano-silver antibacterial material according to claim 1, wherein the method comprises the following steps: the concentration of the silver ion solution is 0.2-1.5 g/L.
7. The method for preparing the high-dispersibility nano-silver antibacterial material according to claim 1, wherein the method comprises the following steps: the impregnation method is an equal-volume impregnation method or a multiple impregnation method.
8. The method for preparing a highly dispersible nano-silver antibacterial material as claimed in any one of claims 1 to 7, wherein: the frequency of the radio frequency plasma is 200-500kHz, the output power is 100-400W, and the treatment time is 1-5 min.
9. A high-dispersity nano-silver antibacterial material is characterized in that: the high-dispersity nano-silver antibacterial material is prepared by the preparation method of the high-dispersity nano-silver antibacterial material in claim 1.
10. The highly dispersible nano-silver antibacterial material according to claim 9, wherein: the particle diameter of the nano silver particles loaded on the nano silver particles is 1-5 nm.
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