CN109332720A - High dispersancy nano silver anti-biotic material and preparation method thereof - Google Patents
High dispersancy nano silver anti-biotic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to chemical material technical field, a kind of high dispersancy nano silver anti-biotic material and preparation method thereof is provided.A kind of preparation method of high dispersancy nano silver anti-biotic material, sulfur-bearing coal is pyrolyzed to obtain the carbon material with surface functional group, the sum of the iron sulfide sulphur of the sulfur-bearing coal and the content of organic sulfur are greater than 2.5%, and the temperature of the pyrolysis is 600-1000 DEG C, and the surface functional group includes thiophene;The carbon material and silver ion solution are handled using infusion process to obtain silver ion/carbon material;Silver ion/the carbon material is obtained into required high dispersancy nano silver anti-biotic material after RF plasma processing.High dispersancy nano silver anti-biotic material can be obtained using the preparation method of the high dispersancy nano silver anti-biotic material.The present invention also provides a kind of high dispersancy nano silver anti-biotic material, the dispersed nano-silver particles loaded thereon are high, have the advantages that strong antibacterial.
Description
Technical field
The present invention relates to chemical material technical field more particularly to a kind of high dispersancy nano silver anti-biotic material and its preparations
Method.
Background technique
Globalization and urbanization bring the increase of movement of population, and various forms of bacterium infections is made to become increasingly severe,
The increase and breeding for how inhibiting bacterium also become more and more important.In numerous anti-biotic materials, silver system anti-biotic material has wide
The performance for composing antibacterial and long-acting bacteriostatic, high-efficiency antimicrobial is especially still able to maintain under low concentration, is considered as all the time
The first choice of green phosphor antibacterial agent.And mutually silver, nanoscale Argent grain can and be reacted due to its higher surface compared to body
Activities present has gone out excellent antibacterial ability, is widely used for the fields such as medical treatment & health.For nano silver, dispersion degree pair
Its antibacterial ability has a great impact, therefore the nano silver material for how obtaining polymolecularity becomes as popular R&D target.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of high dispersancy nano silver anti-biotic material is provided
And preparation method thereof.
In order to solve the above technical problems, invention uses technical solution as described below.A kind of high dispersancy nano silver antibacterial
Sulfur-bearing coal is pyrolyzed to obtain the carbon material with surface functional group, the iron sulfide of the sulfur-bearing coal by the preparation method of material
The sum of content of sulphur and organic sulfur is greater than 2.5%, and the temperature of the pyrolysis is 600-1000 DEG C, and the surface functional group includes thiophene
Pheno;The carbon material and silver ion solution are handled using infusion process to obtain silver ion/carbon material;By the silver ion/carbon materials
Material obtains required high dispersancy nano silver anti-biotic material after RF plasma processing.
Preferably, the content that the index of basicity of the sulfur-bearing coal is greater than the organic sulfur of 0.5 or the sulfur-bearing coal is greater than
2.5%.
It preferably, further include being pre-processed to sulfur-bearing coal before being pyrolyzed sulfur-bearing coal, the pretreatment includes
Sulfur-bearing coal is ground and sieved.
Preferably, when carrying out the grinding and screening, the grain diameter of control sulfur-bearing coal is 150-250 μm.
Preferably, the pyrolysis uses heating-isothermal pyrolysis, rises to target temperature constant temperature 30- again with 5-20 DEG C/min
60min。
Preferably, the concentration of the silver ion solution is 0.2-1.5g/L.
Preferably, the infusion process is equi-volume impregnating or multiple maceration.
Preferably, the frequency of the radio frequency plasma is 200-500kHz, output power 100-400W, handling duration
For 1-5min.
A kind of high dispersancy nano silver anti-biotic material, using the preparation method of above-mentioned high dispersancy nano silver anti-biotic material
It is prepared.
Preferably, the partial size of the nano-Ag particles loaded on the high dispersancy nano silver anti-biotic material is 1-5nm.
The beneficial effects of the present invention are:
The present invention provides a kind of preparation methods of high dispersancy nano silver anti-biotic material, using sulfur-bearing coal as raw material, pyrolysis
The carbon material with surface functional group is obtained afterwards, and the surface functional group includes thiophene, have between thiophene and silver ion relatively strong
Suction-operated, then through radio frequency plasma by silver ion reduction formed nano silver to get arrive required high dispersancy nano
Silver-colored anti-biotic material realizes that nano silver is immobilized in the polymolecularity of carbon material surface.Also, it can retain by radio frequency plasma
The functional group of carbon material surface realizes the green reduction of high dispersancy nano Argent grain.In addition, sulfur-bearing coal requires to be taken off greatly
It is utilized after sulphur, and the present invention is then exactly using the sulphur contained by it, to open up the Land use systems and exploitation value of sulfur-bearing coal
Value.
The present invention also provides a kind of high dispersancy nano silver anti-biotic material, the dispersed nano-silver particles loaded thereon are high,
Has the advantages that strong antibacterial.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of high dispersancy nano silver anti-biotic material in the present invention.
Fig. 2 is Fourier infrared spectrograph (FT-IR) figure of high dispersancy nano silver anti-biotic material in the present invention.
Specific embodiment
To make those skilled in the art that the purposes, technical schemes and advantages of invention be more clearly understood, below
Invention is further elaborated in conjunction with the accompanying drawings and embodiments.
Embodiment one
As shown in Figure 1, a kind of preparation method of catalyst, comprising:
Step S1: sulfur-bearing coal is pyrolyzed to obtain the carbon material with surface functional group, the iron sulfide of the sulfur-bearing coal
The sum of content of sulphur and organic sulfur is greater than 2.5%, and the temperature of the pyrolysis is 600-1000 DEG C, and the surface functional group includes thiophene
Pheno;
Step S2: the carbon material and silver ion solution are handled using infusion process to obtain silver ion/carbon material;
Step S3: the silver ion/carbon material is obtained into required polymolecularity after RF plasma processing and is received
The silver-colored anti-biotic material of rice.
Coal can be divided into low-sulfur coal (< 1%), medium sulphur coal (between 1%-2%) and sulphur coal (> 2%), institute in coal
The sulphur contained can be divided into inorganic sulfur and organic sulfur, and inorganic sulfur includes sulfate sulfur and iron sulfide sulphur.
In the present invention namely in step S1, by the sum of content of selection iron sulfide sulphur and organic sulfur greater than 2.5%
Sulfur-bearing coal, and determine that the temperature of pyrolysis guarantees sulfur-bearing pyrolysis of coal degree, so as to obtain the carbon material with thiophene.
In some preferred embodiments, the index of basicity R of the sulfur-bearing coal is greater than 0.5.The calculation expression of index of basicity R
Formula is as follows:
Wherein, Fe2O3For Fe in sulfur-bearing coal2O3Content, CaO be sulfur-bearing coal in CaO content, MgO be sulfur-bearing coal in
The content of MgO, Na2O is Na in sulfur-bearing coal2The content of O, K2O is K in sulfur-bearing coal2The content of O, SiO2For SiO in sulfur-bearing coal2's
Content, Al2O3For Al in sulfur-bearing coal2O3Content.As index of basicity R higher, captured sulfur result is good in pyrolytic process.
In other preferred embodiments, the content of the organic sulfur of the sulfur-bearing coal is greater than 2.5%.Organic sulfur relatively vulcanizes
Iron sulphur is stablized, and the ratio that thiophene is converted into pyrolytic process is high.
Preferably, the pyrolysis uses heating-isothermal pyrolysis, rises to target temperature constant temperature 30- again with 5-20 DEG C/min
60min.The wherein target temperature namely the pyrolysis temperature, it is more more stable to obtain by determining heating rate
Thiophene.It is preferred that rising to target temperature constant temperature 30-50min again with 5-15 DEG C/min.In some specific embodiments,
Target temperature constant temperature 40min again is risen to 10 DEG C/min.Preferably, the pyrolysis is to carry out under argon atmosphere.
It preferably, further include being pre-processed to sulfur-bearing coal before being pyrolyzed sulfur-bearing coal, the pretreatment includes
Sulfur-bearing coal is ground and sieved.By grinding and sieving, the grain diameter of sulfur-bearing coal can be preferably controlled, is guaranteed uniform
Property.Preferably, the grain diameter for controlling sulfur-bearing coal is 150-250 μm, and it is 150-250 μm that screening, which obtains grain diameter, after grinding
Sulfur-bearing coal.
In step s 2, it is preferable that the infusion process is equi-volume impregnating or multiple maceration, and dipping effect is good.
Wherein, equi-volume impregnating can determine that load capacity namely provided silver ion load on the carbon material well, and silver
Ion dispersing uniformity is good;Multiple maceration is then that can effectively improve load capacity.It is appreciated that when using incipient impregnation,
Need first to measure the saturated water adsorptive value of carrier namely the saturated water adsorptive value of carbon material.
The concentration of the silver ion solution is too high, will cause waste, and the concentration of the silver ion solution is too low, and load capacity is not
Foot influences anti-microbial property.Preferably, the concentration of the silver ion solution is 0.2-1.5g/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, 1.2g/L.
In step s3, it is preferable that the frequency of the radio frequency plasma is 200-500kHz, output power 100-
400W, handling duration 1-5min.It is preferred that the frequency of the radio frequency plasma is 250-350kHz, output power
200-300W.Handling duration can be adjusted according to concentration of silver ions, when concentration of silver ions is less than or equal to 0.6g/L, processing
Shi Changwei 1min;When concentration of silver ions, which is greater than 0.6g/L, is less than 0.9g/L, handling duration 2-4min;When concentration of silver ions is big
When being equal to 0.9g/L, handling duration 5min.
Embodiment two
A kind of high dispersancy nano silver anti-biotic material, using high dispersancy nano silver antibacterial material provided in embodiment one
The preparation method of material is prepared, and has the advantages that strong antibacterial.What is loaded on the high dispersancy nano silver anti-biotic material receives
Rice Argent grain good dispersion, and the partial size of the nano-Ag particles loaded on high dispersancy nano silver anti-biotic material is 1-5nm.
Specific experiment is provided below and corresponding result is illustrated
One, feedstock analysis (analysis of sulfur-bearing coal)
The sulfur-bearing coal (CoalA, CoalB, CoalC, CoalD) of four kinds of different matchmaker's ranks is provided, matchmaker's rank sequence is CoalA <
CoalB < CoalC < CoalD.The chemical analysis Sulfur data of four kinds of sulfur-bearing coals are shown in Table 1, four kinds of sulfur-bearing pit ash analyses
It is shown in Table 2.
The chemical analysis Sulfur data of 1 four kinds of sulfur-bearing coals of table
2 four kinds of sulfur-bearing pit ash analyses of table
The calculation expression of 2 neutral and alkali index R of table is as follows:
Wherein, Fe2O3For Fe in sulfur-bearing coal2O3Content, CaO be sulfur-bearing coal in CaO content, MgO be sulfur-bearing coal in
The content of MgO, Na2O is Na in sulfur-bearing coal2The content of O, K2O is K in sulfur-bearing coal2The content of O, SiO2For SiO in sulfur-bearing coal2's
Content, Al2O3For Al in sulfur-bearing coal2O3Content.
Two, the preparation of nano silver antibacterial material
1, the pretreatment of sulfur-bearing coal
Sulfur-bearing coal is placed in mortar and is ground, is then sieved with mesh screen, obtaining grain diameter is 150-250 μm
Sulfur-bearing coal.
2, the pyrolysis of sulfur-bearing coal
Using atmospheric fixed bed reaction unit, temperature programming-isothermal pyrolysis is carried out to the sulfur-bearing coal obtained after pretreatment
Experiment.Specific steps are as follows:
0.5 coal sample is weighed, is uniformly placed on the sintered plate at quartz reactor center.Argon gas conduct pyrolysis carrier gas (purity,
> 99.99%), it is passed through with the flow velocity of 600mL/min from reactor head, the air in metathesis reactor, in reactor
After air is sufficiently displaced from, setting program temperature controller is raised to target temperature with the heating rate of 10 DEG C/min, according to different realities
The constant corresponding time is tested, the i.e. required carbon material with surface functional group of thermal decomposition product is obtained.
3, infusion process carries silver-colored (incipient impregnation)
Survey the saturated water adsorptive value of carrier: weighing the carrier that a certain amount of step 2 obtains (has the carbon materials of surface functional group
Material), the deionized water for measuring volume is added, stands overnight, deionized water rubber head dropper in upper layer is sucked out, its volume is surveyed,
The reduction amount of volume is the saturated water adsorptive value of a certain amount of carbon material.
According to saturated water adsorptive value, corresponding silver nitrate solution is weighed, carbon material is added in silver nitrate solution, stood
After 12-24h or ultrasound 1-3h, it is placed in vacuum oven drying at 50 DEG C and obtains silver ion/carbon material for 24 hours.
4, radio frequency plasma restores
Silver ion/the carbon material for taking step 3 to obtain is placed in beaker, is put on the chip bench in radio frequency plasma source;According to
Secondary unlatching water pump, general supply, mechanical pump, then vacuumize, and helium switch, regulating gas stream are opened after vacuum degree is lower than 5Pa
Amount makes to react cavity pressure lower than 60Pa;It opens radio-frequency power supply and preheats regulation power after 5-10min, issue aura.Wait react
Radio-frequency power supply, gas trap, mechanical pump, general supply and water pump are successively closed after a certain period of time, obtain required nanometer silver antimicrobial material
Material.
It is more by selecting different sulfur-bearing coals, pyrolysis temperature, silver nitrate concentration, plasma parameter and handling duration to carry out
Group experiment, the concrete condition of different experiments group are shown in Table 3.
The experiment condition of 3 experimental group 1-9 of table
Three, experimental result characterization and analysis
1, it is pyrolyzed interpretation of result
Sulfur content therein is measured for the carbon material obtained after pyrolysis, and utilizes Fourier infrared spectrograph (FT-IR)
Determine its surface functional group type (Fig. 2).
Sulfur content is shown in Table 4 in carbon material obtained by each experimental group.
Table 4
As shown in Fig. 2, by FT-IR spectrum to raw coal, CO2And N2The surface function of the carbon material of formation is pyrolyzed under atmosphere
Group is analyzed.By Fig. 2 analysis it is found that No. 1 (experimental group 1) as former state in 471,537 and 1030cm-1There is infrared suction in place
Peak, caused by being respectively-S-H- ,-S-S- ,-S=O- stretching vibration, 2911cm-1For-CH2Characteristic absorption peak.It is provided by consulting
Material is it can be extrapolated that the most of presence in the form of disulfide of organic sulfur.No. 2 (experimental groups 4) and No. 3 (experimental group 7) are in CO2And N2No
With being pyrolyzed the carbon material of formation under atmosphere in 418 and 660cm-1Corresponding-C-S- stretching vibration absworption peak.Illustrate in high temperature pyrolysis mistake
The functional groups such as thiophene are mainly generated in journey.
2, the anti-microbial property of nano silver antibacterial material
For nano silver antibacterial material obtained by each group, using antibacterial its anti-microbial property of around-France measurement.The strain of selection
The respectively Escherichia coli and staphylococcus aureus of Gram-negative bacteria and positive bacteria representative.
Each experimental group inhibition zone diameter is shown in Table 5.
Table 5
Antibacterial around-France standard be inhibition zone diameter be greater than 7mm then illustrate there is antibacterial effect, the diameter the big, indicates antibacterial
Effect is more preferable.
Claims (10)
1. a kind of preparation method of high dispersancy nano silver anti-biotic material, it is characterised in that: be pyrolyzed sulfur-bearing coal and had
There is the carbon material of surface functional group, the sum of the iron sulfide sulphur of the sulfur-bearing coal and the content of organic sulfur are greater than 2.5%, the pyrolysis
Temperature be 600-1000 DEG C, the surface functional group includes thiophene;
The carbon material and silver ion solution are handled using infusion process to obtain silver ion/carbon material;
Silver ion/the carbon material is obtained into required high dispersancy nano silver antibacterial material after RF plasma processing
Material.
2. the preparation method of high dispersancy nano silver anti-biotic material as described in claim 1, it is characterised in that: the sulfur-bearing coal
Index of basicity be greater than 0.5 or the sulfur-bearing coal organic sulfur content be greater than 2.5%.
3. the preparation method of high dispersancy nano silver anti-biotic material as described in claim 1, it is characterised in that: by sulfur-bearing coal
It further include being pre-processed to sulfur-bearing coal before being pyrolyzed, the pretreatment includes that sulfur-bearing coal is ground and sieved.
4. the preparation method of high dispersancy nano silver anti-biotic material as claimed in claim 3, it is characterised in that: ground described in progress
When mill and screening, the grain diameter of control sulfur-bearing coal is 150-250 μm.
5. the preparation method of high dispersancy nano silver anti-biotic material as described in claim 1, it is characterised in that: the pyrolysis is adopted
With heating-isothermal pyrolysis, target temperature constant temperature 30-60min again is risen to 5-20 DEG C/min.
6. the preparation method of high dispersancy nano silver anti-biotic material as described in claim 1, it is characterised in that: the silver ion
The concentration of solution is 0.2-1.5g/L.
7. the preparation method of high dispersancy nano silver anti-biotic material as described in claim 1, it is characterised in that: the dipping
Method is equi-volume impregnating or multiple maceration.
8. the preparation method of high dispersancy nano silver anti-biotic material as described in claim any one of 1-7, it is characterised in that:
The frequency of the radio frequency plasma is 200-500kHz, output power 100-400W, handling duration 1-5min.
9. a kind of high dispersancy nano silver anti-biotic material, it is characterised in that: using the high dispersancy nano described in claim 1
The preparation method of silver-colored anti-biotic material is prepared.
10. high dispersancy nano silver anti-biotic material as claimed in claim 9, it is characterised in that: the nano silver loaded thereon
The partial size of grain is 1-5nm.
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