CN108007976A - MoS2The preparation of/graphene composite material and structure elemental mercury from vapor sensor - Google Patents
MoS2The preparation of/graphene composite material and structure elemental mercury from vapor sensor Download PDFInfo
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Abstract
A kind of MoS2The preparation of/graphene composite material and structure elemental mercury from vapor sensor, belong to monitoring technical field.The purpose of the present invention is discharge the MoS that gaseous elemental mercury can monitor real-time online in flue gas mainly for coal-burning power plant2The preparation of/graphene composite material and structure elemental mercury from vapor sensor.The composite material of elder generation's formation determination mercury sensor of the invention, then prepare MoS with this composite material2/ graphene composite material, finally prepares MoS2The elemental mercury from vapor sensor of/graphene composite material structure.The structure and morphology of the present invention is good, and the repeatability and stability of sensor are very excellent, have good selectivity.
Description
Technical field
The invention belongs to monitoring technical field.
Background technology
The close attention for causing people to air pollution that increasingly sharpens of haze weather.Coal produces in combustion
Various pollutants be one of important sources of air pollution.The research that trace metal discharges in coal combustion process becomes burning
A Disciplinary Frontiers in pollution.Particularly mercury vapour, the amplification due to its toxicity and in biological chain are serious to endanger people
Body health, makes the research of mercury become the hot spot studied in recent years.Mercury is liquid at normal temperatures, highly volatile, the mercury vapour of generation
There is huge damaging effect to human body, liver and cerebral function are seriously affected after human body suction, a large amount of suctions can disable or even cause
Life.In daily industry, the industry such as electric power, smelting, cement, mining can all discharge a certain amount of mercury into air, wherein electricity
Lixing industry is current maximum mercury pollution source with the coal-burning power plant of thermal power generation.At present, mercury pollution is all caused by fire coal for various countries
Attach great importance to, consider from ecological environment, human health, sustainable development, it is that environment is protected to develop effective gas mercury monitoring device
Protect essential condition.
After coal combustion, mainly there are three kinds in the existence form of mercury in flue gas：Hg0（Element state）, Hg2+（Oxidation state）, Hgp
（Particulate form）.Hg0It is not soluble in water, it is more difficult to remove, mean residence time was up to half a year to 2 years in an atmosphere, containing in flue gas
Amount reaches more than 70%, can be stable in the presence of in air and with air and diffuse to form global mercury pollution.Gaseous state divalence
Mercury Hg2+It is very unstable, and the mercury of many divalent states is very soluble in water, so the easy-to-use absorption method of gaseous state bivalent mercury, washing
Method removes, and coal-burning power plant's wet desulphurization equipment can be removed 80% ~ 95% gaseous state bivalent mercury.Particle mercury HgPIt is in flue gas
Gaseous elemental mercury and bivalent mercury adsorbed grit form is in contact with flying dust during flow of flue gas.Generally recognize
The ratio that total mercury emission after coal combustion is accounted for for, particle mercury is less than 5%, and the mercury of this portion forms is easily by sack cleaner
Or electrostatic precipitator removes.
The mercury of different shape, not only their physics, chemistry, biological nature and environmental transport and transfer ability are otherwise varied, and
And the harm produced to human health and environment also differs greatly, but the harm of the mercury emissions of coal-burning power plant is huge, so combustion
Coal-fired plant effectively will control and administer the discharge of gas mercury, it is necessary first to can measure the content of mercury, it is therefore desirable to realize online
Monitoring real-time, provides information accurately and timely for mercury emission, otherwise would become hard to the mesh for reaching effectively preventing mercury pollution
's.
The content of the invention
The purpose of the present invention is discharge gaseous elemental mercury in flue gas mainly for coal-burning power plant to supervise real-time online
The MoS of survey2The preparation of/graphene composite material and structure elemental mercury from vapor sensor.
The preparation method of composite material of present invention measure mercury sensor is：
The preparation of graphite oxide powder：
（1）Measure the dense H of 23ml2SO4As in three-necked flask, 0.3g graphite powders and 0.3g NaNO are weighed respectively3, it is uniformly mixed
Afterwards, add into three-necked flask；After stirring 3min, 1.5g potassium permanganate is added, ice-water bath, ensures whole system temperature at 10 DEG C
Left and right, stirs 2h；
（2）Three-necked flask is transferred in 35 DEG C of oil baths, continues to stir 30min；
（3）The deionized water of 23ml is measured, is slowly added dropwise, while is warming up to 98 DEG C, after continuous heating stirring 20min,
Stop heating；
（4）The hydrogen peroxide that 5g concentration is 30% is weighed, after being added dropwise in three-necked flask, is placed into room temperature；
（5）Products therefrom is washed to upper strata liquid-transparent using 5% HCl, repeatedly washed using deionized water afterwards to
Supernatant liquid is neutrality, finally by product freeze-drying process, that is, obtains graphite oxide powder；
MoS2The preparation of/graphene composite material：
（1）The GO samples of 10mg dryings are weighed, add 100ml ethylene glycol, after high density ultrasound 2h, prepare the graphite of 0.1mg/ml
Alkene dispersion liquid, saves backup；
（2）Measure the above-mentioned GO dispersion liquids of 1.5ml and be diluted with water to 30ml, add 0.38g thiocarbamides, after high density ultrasound 5min, to
0.45g ammonium molybdates, high density ultrasound 30min are added in solution；
（3）Above-mentioned solution is moved in 50ml autoclaves, under conditions of 200 DEG C, reacts 24h, question response kettle is cooled to
Room temperature, product are cleaned with deionized water and ethanol respectively, 60 DEG C of drying.
The MoS of the present invention2/ graphene composite material forms substantial amounts of spherical knot by the stratiform gusset much interconnected
Structure is formed, and has the surface area of super large.
MoS of the present invention2/ graphene composite material builds elemental mercury from vapor sensor：Take the sulfur doping graphene prepared
Composite sample is dissolved in deionized water, and ultrasonic vibration 5 minutes, makes sample be fully dispersed in deionized water, Ran Houqu
It is convex in the ceramic pipe surface for being covered with gold electrode to mix drop, deionized water volatilization finishes.
It is an advantage of the invention that：
（1）The good graphene oxide of pattern is prepared using Hummers methods are improved, and is prepared as raw material using hydro-thermal method
MoS2/ graphene composite material, scanning electron microscope characterization has been carried out to it（SEM）, X-ray diffraction characterization（XRD）And Raman spectrum
Characterization, it is found that the structure and morphology of the material is good.
（2）Based on MoS2The sensor of/graphene composite material is at room temperature to 2.18mg/m3To 452.51mg/m3Mercury
Steam has carried out sensing testing, and discovery sensor shows quickly response and recovery capability, response time and recovery time
Respectively 500s and recovery time are respectively 1 000s-1 500s；By cycle sensor as 126.18mg/m3Mercury steam
10 days in compression ring border, it is found that sensor does not occur the sign of deterioration, illustrates the repeatability of sensor over time
It is very excellent with stability；Coal-burning power plant common contaminant gas H of the sensor in high concentration at the same time2S、NH3、NO2In not
Show significantly to respond, illustrate that sensor has good selectivity.
（3）Change the addition of graphite oxide, prepare the different composite material of graphene mass fraction, and to it into promoting the circulation of qi
Quick property test, the results showed that, when the mass fraction of graphene is 0.5%, susceptibility highest of the composite material to mercury vapour.
Brief description of the drawings
Fig. 1 is the SEM figures of GO；
Fig. 2 is the XRD spectra of GO；
Fig. 3 is MoS2The SEM figures of/graphene composite material；
Fig. 4 is MoS2The XRD diagram of/graphene composite material；
Fig. 5 is Raman spectrogram；Wherein a) graphite oxide； b) MoS2/ graphene composite material；
Fig. 6 is the air-sensitive testing element schematic diagram of composite material；Wherein a) section plan；B) three-dimensional cutaway view；1 is gold in figure
Electrode, 2 be platinum filament, and 3 be ceramic tube, and 4 be resistance wire, and 5 be MoS2/ graphene composite material；
Fig. 7 is MoS2/ graphene composite material response and response time relation curve；
Fig. 8 is MoS2The relation of/graphene composite material responsiveness and mercury vapour concentration；
Fig. 9 is 126.18 mg/m3Responsiveness change curve in mercury vapour atmosphere；
Figure 10 is 126.18 mg/m3Mercury vapour susceptibility stability compares figure；
Figure 11 is MoS2/ graphene composite material is to SO2、NH3、NO2Selectivity curve；
Figure 12 is influence of the mass fraction to responsiveness of graphene；
Device resistance variation diagram when Figure 13 is N-type semiconductor adsorbed gas.
Embodiment
The preparation method of composite material of present invention measure mercury sensor is：
Graphite oxide powder（GO）Preparation：
（1）Measure the dense H of 23ml2SO4As in three-necked flask, 0.3g graphite powders and 0.3g NaNO are weighed respectively3, it is uniformly mixed
Afterwards, add into three-necked flask；After stirring 3min, 1.5g potassium permanganate is added, ice-water bath, ensures whole system temperature at 10 DEG C
Left and right, stirs 2h；
（2）Three-necked flask is transferred in 35 DEG C of oil baths, continues to stir 30min；
（3）The deionized water of 23ml is measured, is slowly added dropwise, while is warming up to 98 DEG C, after continuous heating stirring 20min,
Stop heating；
（4）The hydrogen peroxide that 5g concentration is 30% is weighed, after being added dropwise in three-necked flask, is placed into room temperature；
（5）Products therefrom is washed to upper strata liquid-transparent using 5% HCl, repeatedly washed using deionized water afterwards to
Supernatant liquid is neutrality, finally by product freeze-drying process, that is, obtains graphite oxide powder；
MoS2The preparation of/graphene composite material：
（1）The GO samples of 10mg dryings are weighed, add 100ml ethylene glycol, after high density ultrasound 2h, prepare the graphite of 0.1mg/ml
Alkene dispersion liquid, saves backup；
（2）Measure the above-mentioned GO dispersion liquids of 1.5ml and be diluted with water to 30ml, add 0.38g thiocarbamides, after high density ultrasound 5min, to
0.45g ammonium molybdates, high density ultrasound 30min are added in solution；
（3）Above-mentioned solution is moved in 50ml autoclaves, under conditions of 200 DEG C, reacts 24h, question response kettle is cooled to
Room temperature, product are cleaned with deionized water and ethanol respectively, 60 DEG C of drying.
The MoS of the present invention2/ graphene composite material forms substantial amounts of spherical knot by the stratiform gusset much interconnected
Structure is formed, and has the surface area of super large.
MoS of the present invention2/ graphene composite material builds elemental mercury from vapor sensor：Take the sulfur doping graphene prepared
Composite sample is dissolved in deionized water, and ultrasonic vibration 5 minutes, makes sample be fully dispersed in deionized water, Ran Houqu
It is convex in the ceramic pipe surface for being covered with gold electrode to mix drop, deionized water volatilization finishes.
Following additional copy invention is described in further detail and verifies：
The scanning electron microscope (SEM) photograph of GO as shown in Figure 1, it is in lamelliform solid state to show GO in figure, shows that GO has in preparation process
Delamination to a certain extent, does not reunite, and property is stablized.And due to the introducing of a large amount of oxygen-containing functional groups, GO lamellas go out
Now obvious fold, is the pattern of typical GO.
The XRD spectra of GO as shown in Figure 2,001 peak in spectrogram at 2 θ=10.8 ° and 2 θ=44 ° for GO feature diffraction
Peak, 002 peak at 2 θ=26.5 ° are the characteristic diffraction peak of native graphite.It can be seen from the figure that the feature of GO is spread out in product
Penetrate that peak intensity is very big, and the characteristic diffraction peak intensity of native graphite is then very weak, further illustrates native graphite in oxidizing process
Due to the introducing of oxygen-containing functional group so that graphite layers distance is significantly lifted, and the degree of oxidation of product is very high, GO limellar strippings
Degree is higher.
MoS2The SEM characterizations of/graphene composite material are as shown in Figure 3.Left figure is MoS in Fig. 32/ graphene composite material
Low amplification factor SEM figure, it can be seen from the figure that MoS2/ graphene composite material is made of substantial amounts of chondritic.Figure
3 right figures are MoS2The high magnification numbe SEM figures of/graphene composite material, by that can be more clearly seen in figure, MoS2/ graphene
Composite material is layered self-packaging nanometer spherical structure, and this chondritic is made of the stratiform gusset much interconnected.
MoS2The crystal structure and thing phase purity of/graphene composite material are obtained by X-ray diffraction analysis.From Fig. 4
As can be seen that MoS2Diffraction maximum it is corresponding with standard card JPCDS NO.37-1492, be hexagonal phase MoS2.Diffraction maximum
Widthization is very serious, this is because MoS2Caused by ultra-thin lamella fold.MoS2C layers about 12 ° of diffraction maximum position, this is just
It is S-Mo-S layers.Result above shows, MoS2The layer structure of nanosphere only may include several pleats, and the spacing of layer and layer
It is wider.
To GO and MoS2/ graphene composite material has carried out Raman Characterization.Due to the C=C double bonds being conjugated in carbon material
Raman enhancing effect can be produced, therefore, Raman spectrum is a kind of common tool for the crystal structure for differentiating carbon material.G peaks generation
Table C sp2The E of atom2gQuantum is shaken, by C sp2The extensional motion of atom produces, and D peaks represent C sp2The A1g vibrations of atom
Quantum, by C sp2Atom breathing vibrating mode produces.GO and MoS2Raman characterization result such as Fig. 5 institutes of/graphene composite material
Show, the D bands and G bands of GO are located at 1331cm respectively-1And 1585cm-1Place, for MoS2/ graphene composite material, its D band and G bands
Positioned at 1334cm-1And 1584cm-1Place, compared with graphite oxide, the D peaks of graphene and the intensity at G peaks（D/G）Enhancing, this
Show during graphite oxide reduces, sp2Atomic volume diminishes.This phenomenon can be construed to, and be reduced in graphite oxide
During, a large amount of new graphite mass are generated, the volume of these materials will be much smaller than to be present in graphite oxide before
Material.In addition, the D band strengths of GO are more than G band strengths, this is because GO in freezing dry process, has sub-fraction oxygen-containing group
Caused by group is reduced.
The making of gas sensor
The present invention is based on MoS2The organigram of the air-sensitive testing element of/graphene composite material is as shown in fig. 6, take a small amount of system
The MoS got ready2/ graphene composite material sample is dissolved in a small amount of deionized water, and ultrasonic vibration 5 minutes, makes sample complete
It is scattered in deionized water, then takes mixing drop convex in the ceramic pipe surface for being covered with gold electrode, treat that deionized water is waved
Tested after hair for air-sensitive.
The sensitive test selection static system test platform of mercury vapour, the sensor component prepared is put into by when test to be filled
In the wide-mouth bottle of some liquid mercuries.Resistance measurement uses digital table（Multimeter-Fluke 8846A）With 1 point each second
Speed obtain resistance value, universal meter is connected with computer carries out data processing.Under the atmospheric environment that system is maintained to room temperature, survey
The concentration of mercury vapour is by the temperature control of panel heater in test system, and the corresponding saturation mercury vapour concentration of different temperatures is by the U.S.
Department of Labor website checks in, and the saturation mercury vapour concentration value that this experiment is chosen at corresponding 5 temperature is tested, such as table 3-1 institutes
Show.
The relation of table 3-1 different temperatures and mercury vapour concentration
。
To test MoS2/ graphene composite material compares the material under different condition to the air-sensitive property of elemental mercury
To the sensitive response curve of elemental mercury（Adsorption time and desorption time）.Response be defined as S=（Rg-R0）/R0, R here0
Represent the resistance value and R of device in Atmosphere System airgRepresent the resistance value of device in mercury vapour system.
Fig. 7 is to be based on MoS at room temperature2Response of the sensor of/graphene composite material to various concentrations mercury vapour recovers
Curve, the excursion of mercury vapour concentration is 2.18mg/m3To 452.51mg/m3, can clearly be found from figure, composite wood
Material be to elemental mercury it is very sensitive, its linear variability law and without mutation occur.At the same time, in wider mercury vapour
In concentration range, its linear variability law and without mutation occur, sensor show quickly response and recovery capability, and
It is responded and recovery time does not change and significant changes with mercury vapour concentration.According to determining for sensor response time and recovery time
Justice, in terms of the result shown from Fig. 7, its response time is 500s or so and recovery time is respectively 1 000s-1 500s.
Fig. 8 is variation relation of the susceptibility with mercury vapour concentration of sensor.It can be seen from the figure that susceptibility is proportional to
The concentration of mercury vapour, and linear trend is excellent, when under higher mercury vapour concentration, the susceptibility of sensor is got over
It is high.At the same time it can also be seen that when the concentration of mercury vapour reaches 452.51mg/m3When, sensitivity is up to -0.7, and it is sensitive
Degree does not occur the phenomenon of saturation.This illustrates based on MoS2The sensor of/graphene composite material has mercury vapour
Good adsorption capacity.
The reappearance and long-time stability of sensor are considered as the key character index in practice, especially in height
In the elemental mercury of concentration.Fig. 9 is that sensor is exposed to 126.18mg/m3Responsiveness change in concentration mercury vapour environment is bent
Line.For reappearance of the detection sensor in whole process, make its periodic exposure in 126.18mg/m3The mercury vapour of concentration
In environment.It can be clearly seen that from figure, sensor responsiveness does not have the sign that any deterioration occurs, and the sensor sheet
Excellent response and recovery capability are revealed.In mercury vapour environment, the corresponding susceptibility of sensor reduces, and in a short time
Reach balance.When sensor is moved in atmospheric environment, the susceptibility of sensor has just been promptly restored to its original baseline.
These phenomenons are all indicated based on MoS2The sensor of/graphene composite material has the reappearance of height.
Figure 10 is stability test of the sensor at room temperature in 10 days.The stability of sensor represents the length in its service life
It is short.Sensor is exposed to 126.18mg/m3In concentration mercury vapour environment, from figure it can be found that the responsiveness of sensor with
The passage of time, too big change does not occur, Whole Response value is hovered between -0.55 to -0.60.This explanation is whole
During a sensing, the stability of composite material is very excellent.
For sensor, high applicability is the guarantee that its performance is stablized.To test the selectivity of sensor, by it
In coal-burning power plant's common contaminant gas of some high concentrations, it is set to show specific otherness.Figure 11 gives
At room temperature, based on MoS2The sensor of/graphene composite material is to SO2、NH3、NO2Three kinds of coal-burning power plant's common contaminant gas
The disturbance response test of body.It can be seen from the figure that with 126.18 mg/m3Mercury vapour compare, in the H of 1ppm2S、NH3、NO2
The not obvious response of sensor in three kinds of gases.This demonstrate that it is based on MoS2The sensor of/graphene composite material is in room
The lower anti-interference with height of temperature.
Influence of the content of graphene to sensor air-sensitive property in composite material
According to above-mentioned preparation process, a certain amount of 0.1mg/ml graphene oxide dispersions are prepared, are saved backup.Measure respectively
0ml, 0.3ml, 1.5ml, 3ml, 15ml and 30ml（The mass fraction of graphene is followed successively by 0%, 0.1%, 0.5%, 1%, 5%, 10%）,
Above-mentioned GO dispersion liquids are diluted with water to 30ml, add 0.38g thiocarbamides, and after 5 min of high density ultrasound, 0.45g is added into solution
Ammonium molybdate, high density ultrasound 30min；Above-mentioned solution is moved in 50 ml autoclaves, under conditions of 200 DEG C, reaction
24h.Question response kettle is cooled to room temperature, and product is cleaned with deionized water and ethanol respectively, 60 DEG C of drying.Take 6 prepared on a small quantity
A MoS2/ graphene composite material sample is dissolved separately in a small amount of deionized water, and ultrasonic vibration 5 minutes, makes sample complete
It is scattered in deionized water, then takes mixed liquor to drip respectively convex in the ceramic pipe surface for being covered with gold electrode, treat deionization
Water volatilization, which finishes, is placed on 126.18mg/m3In mercury vapour concentration, its responsiveness is measured, as a result as shown in figure 12.Can from figure
To find out, with the increase of the mass fraction of graphene in composite material, responsiveness raises after falling before.To find out its cause, may
It is that graphene is more dispersed, is unfavorable for the movement of carrier, therefore resistance variations because when the mass fraction of graphene is too low
It is smaller；When its mass fraction is higher, causes the superposition or reunion of graphene sheet layer, reduce the adsorption potential of gas molecule, make spirit
Sensitivity reduces.In conclusion when the mass fraction of graphene is 0.5%, composite material is minimum to the responsiveness of mercury vapour, rings
Answer best results.
From Fig. 7 MoS2/ graphene composite material response can be seen that with response time relation curve works as MoS2/ graphene
When composite material contacts mercury vapour, the resistance value of material is that downward trend is presented, and finally drops to a stationary value, and contact
The mercury vapour of various concentrations, the value that resistance value declines is also different, and aggregate performance is bigger for mercury vapour concentration, and electric conductivity is stronger, electricity
Resistance value is smaller.Mercury manifests themselves as easy betatopic, therefore mercury vapour is reducibility gas.Mercury atom touches MoS2/ graphene
During the surface of composite material, electronics more flows into the surface of composite material, so that the electric conductivity enhancing of composite material, resistance value
Decline, from the point of view of this performance, which should belong to N-type semiconductor sensor, its sensor mechanism such as Figure 13
It is shown.Because for the free electron in N-type semiconductor far more than hole concentration, it is to be used as current-carrying subconductivity using free electron.
When the free electron of semiconductor material surface increases, the electric conductivity of material just strengthens.So touch material table
The mercury atom in face is more, and the free electron of mercury atom itself is captured by composite material.The concentration of free electron is bigger, and material is led
It is electrically bigger, and into certain linear relationship.So, MoS bigger from the concentration for macroscopically showing as mercury vapour2/ graphite
The electric conductivity of alkene composite material is stronger, and resistance value is lower.And MoS2/ graphene composite material is stratiform stratiform gusset composition
, surface area is very big, farthest ensure that the contact with mercury vapour, is advantageous to contact of the material to mercury vapour and inhales
It is attached, the optimum efficiency of mercury sensing is ensure that from principle.
Claims (3)
- A kind of 1. MoS2The preparation of/graphene composite material, it is characterised in that：The preparation of graphite oxide powder：（1）Measure the dense H of 23ml2SO4As in three-necked flask, 0.3g graphite powders and 0.3g NaNO are weighed respectively3, it is uniformly mixed Afterwards, add into three-necked flask；After stirring 3min, 1.5g potassium permanganate is added, ice-water bath, ensures whole system temperature at 10 DEG C Left and right, stirs 2h；（2）Three-necked flask is transferred in 35 DEG C of oil baths, continues to stir 30min；（3）The deionized water of 23ml is measured, is slowly added dropwise, while is warming up to 98 DEG C, after continuous heating stirring 20min, Stop heating；（4）The hydrogen peroxide that 5g concentration is 30% is weighed, after being added dropwise in three-necked flask, is placed into room temperature；（5）Products therefrom is washed to upper strata liquid-transparent using 5% HCl, repeatedly washed using deionized water afterwards to Supernatant liquid is neutrality, finally by product freeze-drying process, that is, obtains graphite oxide powder；MoS2The preparation of/graphene composite material：（1）The GO samples of 10mg dryings are weighed, add 100ml ethylene glycol, after high density ultrasound 2h, prepare the graphite of 0.1mg/ml Alkene dispersion liquid, saves backup；（2）Measure the above-mentioned GO dispersion liquids of 1.5ml and be diluted with water to 30ml, add 0.38g thiocarbamides, after high density ultrasound 5min, to 0.45g ammonium molybdates, high density ultrasound 30min are added in solution；（3）Above-mentioned solution is moved in 50ml autoclaves, under conditions of 200 DEG C, reacts 24h, question response kettle is cooled to Room temperature, product are cleaned with deionized water and ethanol respectively, 60 DEG C of drying.
- 2. MoS according to claim 12The preparation of/graphene composite material, it is characterised in that：MoS2/ graphene is compound Material forms substantial amounts of chondritic by the stratiform gusset much interconnected and forms, and has the surface area of super large.
- 3. the MoS described in claim 12/ graphene composite material builds elemental mercury from vapor sensor, it is characterised in that：Take preparation Good sulfur doping graphene composite material sample is dissolved in deionized water, and ultrasonic vibration 5 minutes, is fully dispersed in sample In ionized water, then take mixing drop convex in the ceramic pipe surface for being covered with gold electrode, deionized water volatilization finishes.
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