CN109725104A - A kind of catalytic activity of graphite phase carbon nitride and the research method of temperature gradient relation - Google Patents
A kind of catalytic activity of graphite phase carbon nitride and the research method of temperature gradient relation Download PDFInfo
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- CN109725104A CN109725104A CN201910028138.5A CN201910028138A CN109725104A CN 109725104 A CN109725104 A CN 109725104A CN 201910028138 A CN201910028138 A CN 201910028138A CN 109725104 A CN109725104 A CN 109725104A
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 23
- 239000010439 graphite Substances 0.000 title claims abstract description 23
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000011160 research Methods 0.000 title claims abstract description 14
- 238000002474 experimental method Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 claims abstract description 24
- 238000007146 photocatalysis Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 230000015556 catabolic process Effects 0.000 claims description 12
- 238000006731 degradation reaction Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 12
- 238000006303 photolysis reaction Methods 0.000 claims description 9
- 230000015843 photosynthesis, light reaction Effects 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000010079 rubber tapping Methods 0.000 claims description 3
- 239000002966 varnish Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 238000011056 performance test Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002146 bilateral effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention discloses the research methods of a kind of catalytic activity of graphite phase carbon nitride and temperature gradient relation, belong to catalysis technical field.Pass through the control to temperature gradient, on the one hand distribution situation of the graphite phase carbon nitride catalytic activity face on direction is had studied, on the other hand the catalytic activity performance under different heating rates is had studied, preparation process and application method when used as catalyst graphite phase carbon nitride all have directive significance, and for photocatalysis technology, catalytic performance provides certain theoretical foundation and experiment basis in practical applications.Meanwhile this method is easy to operate, easy to accomplish, and environmentally friendly.
Description
Technical field
The invention belongs to catalysis technical fields, and in particular to a kind of catalytic activity of graphite phase carbon nitride and temperature gradient close
The research method of system.
Background technique
Energy shortage and environmental pollution are always to perplex two big outstanding problems of human development progress.Photocatalysis technology is to take
Sunlight nexhaustible not to the utmost be the energy, received significant attention in the fields such as photolysis water hydrogen and contaminant degradation.It utilizes
Photocatalysis technology converts solar energy into cleaning, the Hydrogen Energy of green is stored, and answers with important researching value and well
Use prospect.Graphite phase carbon nitride (g-C3N4) it is used as a kind of non-metal optical catalyst, because suitable forbidden bandwidth (2.7eV) makes it
It just can be carried out photolysis water hydrogen reaction under visible light illumination and attract attention.In addition, because of its thermal stability and chemical stability
Well, the features such as cost of material is cheap, is widely used in photocatalytic water photocatalysis field.However, passing through the direct thermal polymerization of melamine
Gained g-C3N4Since specific surface area is small, active site is few and light induced electron and the disadvantages of high hole-recombination rate, lead to g-C3N4
The problems such as photocatalytic activity is low is played catalytic performance and is determined especially in practical applications to high activity face using particularly important
Property effect.
g-C3N4Photochemical catalyst is block catalysis material made of a kind of two-dimensional layer material is piled up, due to special two
Dimension layer structure leads to that electronics is excited to transmit that resistance is small, and interlayer resistance is big in layer, so that marginal position ((100) crystal face)
Activity is significantly larger than the activity of ((002) crystal face) on two-dimensional surface.It is traditional it is powdered urge agent sufficiently with reactant (such as photocatalytic water
Hydrogen manufacturing, CO2Reduction, NOx removal etc.) it is uniformly mixed, do not have to distinguish high activity face in catalytic process and low activity face can be real
Now efficient light-catalyzed reaction.But in practical applications, in the application such as in photocatalysis wallpaper for removing indoor formaldehyde, light
Catalyst only has part of the surface to contact with room air, to realize efficient photocatalysis performance using limited exposure, it is necessary to
Make g-C3N4The high activity face of catalyst sufficiently exposes, therefore, g-C3N4The research in high activity face is of great significance.
Summary of the invention
To solve the above-mentioned problems, the invention discloses a kind of catalytic activity of graphite phase carbon nitride and temperature gradient relations
Research method.
The present invention is to be achieved through the following technical solutions:
A kind of catalytic activity of graphite phase carbon nitride and the research method of temperature gradient relation, comprising the following steps:
Step 1: melamine powder after purification is uniformly sprinkled into several heatproof containers, by room temperature, respectively by not
Same heating rate produces g-C under with the heating of the heat source of obvious directionality3N4Solid；
Step 2: by g-C obtained3N4Solid takes out, respectively along parallel temperature gradient direction and vertical temperature gradient direction
It is cut into square block, the relationship between each surface of label square block and temperature gradient；
Step 3: uniformly coating g-C with the covering material with light transmission, water proof and insulation performance3N4Then square block is distinguished
The g-C in exposure parallel temperature gradient direction and vertical temperature gradient direction3N4The surface of square block carries out photocatalysis performance test
Experiment, obtains the catalytic activity of graphite phase carbon nitride and the relationship of temperature gradient.
Preferably, in step 1, the melamine powder of purifying is obtained after washing, drying, and washing is with anhydrous
Ethyl alcohol and deionized water are washed several times respectively；Drying is dried at 50~80 DEG C.
Preferably, in step 1, before heating, melamine powder carries out tapping in heatproof container or ultrasonic vibration is handled.
Preferably, covering material is transparent paraffin, high molecular material or varnish.
Preferably, before photocatalysis performance experiment, exposed surface is subjected to grinding process.
Preferably, photocatalysis performance experiment is using photolysis water hydrogen experiment or RhB degradation experiment.
Compared with prior art, the invention has the following beneficial technical effects:
The catalytic activity of graphite phase carbon nitride disclosed by the invention and the research method of temperature gradient relation, by temperature
On the one hand the control of gradient has studied distribution situation of the graphite phase carbon nitride catalytic activity face on direction, on the other hand studies
Catalytic activity performance under different heating rates, preparation process when used as catalyst graphite phase carbon nitride and uses
Method all has directive significance, for photocatalysis technology in practical applications catalytic performance provide certain theoretical foundation and
Experiment basis.Meanwhile this method is easy to operate, easy to accomplish, and environmentally friendly.
Further, the melamine powder for preparing graphite phase carbon nitride is washed, drying, be in order to remove impurity, with
Exempt to influence experiment effect.
Further, melamine powder carries out tapping in heatproof container or ultrasonic vibration is handled, the graphite made
Phase carbon nitride density of solid is uniform, improves the accuracy of experiment conclusion.
Further, covering material is transparent paraffin, high molecular material or varnish, has light transmission, water proof and insulation performance,
The section being wrapped by is set to can produce excitation electronics, excitation electronics can participate in photocatalysis by exposed section in interior shifting
Reaction, but light-catalyzed reaction cannot be participated on the section being wrapped by.
Further, before photocatalysis performance experiment, exposed surface is subjected to grinding process, avoids remaining covering material shadow
Ring experiment effect.
Further, photocatalysis performance experiment uses photolysis water hydrogen experiment or RhB degradation experiment, easy to operate, can
Efficiently show that required experiment conclusion, the accuracy of conclusion are high.
Detailed description of the invention
Fig. 1 is flow diagram of the invention；
Temperature gradient simulation drawing when Fig. 2 is heating of the invention；
Fig. 3 is g-C3N4The AFM in square block vertical temperature gradient section schemes；
Fig. 4 is g-C3N4The AFM in the parallel temperature gradient section of square block schemes；
Fig. 5 a is g-C3N4The RhB degradation effect figure in square block vertical temperature gradient section, Fig. 5 b are g-C of the invention3N4
The RhB degradation effect figure in the parallel temperature gradient section of square block；
Fig. 6 is g-C3N4The RhB degradation curve figure of square block vertical temperature gradient section peace trip temperature gradient in cross-section；
Fig. 7 is g-C3N4The hydrogen manufacturing curve graph of square block vertical temperature gradient section peace trip temperature gradient in cross-section；
Fig. 8 is the g-C being prepared under different heating rates3N4The RhB degradation curve in square block vertical temperature gradient section
Figure；
Fig. 9 is the g-C being prepared under different heating rates3N4The hydrogen manufacturing curve graph in square block vertical temperature gradient section.
Specific embodiment
The present invention is described in further detail With reference to embodiment, it is described be explanation of the invention and
It is not to limit.
In general, use the isothermal reaction temperature of melamine powder preparation graphite phase carbon nitride for 400~700 DEG C, it is permanent
The warm reaction time is at least 30min, and through studying, different isothermal reaction temperature is little on experiment conclusion influence of the invention,
This is illustrated using 550 DEG C of isothermal reaction temperature of experiment.The heat source of obvious directionality refers to that heater strip, adding thermal resistance etc. add
Thermal is distributed in one direction in heating equipment, such as common Muffle furnace, and heater strip can be unilateral side, be also possible to
Bilateral distribution is the temperature gradient in order to make to have single direction in heating equipment in this way, and then make g-C point-blank3N4
Square block has the direction of growth of single direction, and the conclusion for obtaining experiment is more accurate.It is used in embodiment such as Fig. 2
Shown heater strip is distributed in the Muffle furnace of two sides.
Such as Fig. 1, melamine powder is divided into several groups by mono- group of 10g, be used alternatingly respectively 100ml deionized water and
100ml dehydrated alcohol is cleaned by ultrasonic 30min at 50 DEG C, and suspension is then transferred to another beaker, outwells bottom dispersion
Uneven object and sediment are dried at 60 DEG C, are smashed to pieces uniformly, be put into the crucible of 50ml, the ultrasonic vibration in supersonic cleaning machine
30min makes melamine powder be evenly distributed, wherein 4 groups are pressed 2 DEG C, 4 DEG C, 6 DEG C and 8 DEG C of heating rate respectively, at least 3 groups
By 10 DEG C of heating rate, be heated at the same position that is individually positioned in Muffle furnace 550 DEG C then heat preservation 180min produce
g-C3N4Solid, the heater strip in Muffle furnace are distributed in furnace body two sides, distance phase of the position far from both sides heater strip that crucible is placed
Deng, the temperature gradient distribution in crucible is as shown in Figure 2.
The g-C that will be prepared3N4Solid takes out, and is cut into energy along parallel temperature gradient direction and vertical temperature gradient direction
The maximum square block accessed guarantees that the amount cut off in each direction is of substantially equal as far as possible, label each surface of square block with
There are 4 parallel temperature gradient direction sections and 2 vertical temperature gradient directions to cut for relationship between temperature gradient, the square block
Face then takes out cooled to room temperature, for use with each section is uniformly coated after the submergence of the transparent paraffin of fusing.
Photocatalytic degradation RhB experiment:
Such as Fig. 3, Fig. 4, taking one piece of heating rate is 10 DEG C of g-C3N4Solid square block carries out under an atomic force microscope
Observation, on the section in vertical temperature gradient direction, this it appears that sample shows stratiform along left and right directions in 3D figure
It is distributed, clearer can find out that two-dimensional layered structure shows the distribution of rule from the lower left corner to the upper right corner in 2 d plane picture
Transition.
On the section in parallel temperature gradient direction, 3D figure is with 2 d plane picture this it appears that the two-dimensional surface of sample
Structure is two dimension g-C3N4It piles up, forms a sharp contrast with Fig. 3.2 d plane picture clearer can find out its edge
Temperature gradient show certain two-dimensional layered structure.Pass through the comparison of Fig. 3 and Fig. 4, it can be deduced that g-C3N4Two-dimensional surface
It is grown along the direction of temperature gradient, and high activity face is then perpendicular to temperature gradient.
Taking one piece of heating rate is 10 DEG C of g-C3N4Solid square block exposes 2 vertical temperature gradient directions section respectively
Temperature gradient parallel with 2 direction section, is put into and fills 100ml, and concentration is in the beaker of the RhB of 1mg/L, at normal temperatures and pressures
RhB degradation experiment is carried out by the energy of simulated solar irradiation, while being passed through air into solution, takes 3ml sample to carry out every 20min
Test obtains instantaneous concentration and initial concentration C0's by the instantaneous concentration C of RhB in ultraviolet-visible absorption spectroscopy analysis sample
It is as shown in Figure 6 to make RhB degradation curve for ratio C/C0.As can be seen that passing through the photocatalytic degradation of 80min from Fig. 5 a and 5b
RhB is almost degraded into colourless by RhB experiment, the section of vertical temperature gradient, and the section color of parallel temperature gradient is deeper, and
On same time point, the color of the RhB of the section degradation of vertical temperature gradient is shallower than the section degradation of parallel temperature gradient
The color of RhB shows that the photocatalytic activity perpendicular to temperature gradient face (g-C3N4 marginal position) is apparently higher than and is parallel to temperature
Gradient face (g-C3N4 surface location).
Photolysis water hydrogen experiment:
Taking one piece of heating rate is 10 DEG C of g-C3N4Solid square block exposes 2 vertical temperature gradient directions section respectively
Temperature gradient parallel with 2 direction section is put into the luxuriant and rich with fragrance Lay H of pool2On-line detecting system, and 100ml is added into system and contains 3%
HPtCl6With the deionized water of 7% triethanolamine, at normal temperatures and pressures using simulated solar irradiation as energy progressive photolysis water hydrogen
Experiment, using gas-chromatography every 60min to H in system2Content is analyzed.Such as Fig. 7, it can be seen from the figure that perpendicular to
The photocatalytic activity of temperature gradient active face is significantly larger than the active face for being parallel to temperature gradient.
It can be seen that either photocatalytic degradation RhB or photolysis water hydrogen experiment, Vertical Temperature from above-mentioned experiment conclusion
The photocatalytic activity of gradient in cross-section is significantly larger than parallel temperature gradient section.
Below to g-C made from different heating rates3N4The vertical temperature gradient section catalytic activity of solid square block carries out
Experimental analysis, method is identical with more than, and detailed process repeats no more, by each g-C3N42 vertical temperature gradients of solid square block
Section exposure carries out photocatalytic degradation RhB and photolysis water hydrogen experiment respectively, and as shown in Figure 8,9, heating rate is faster, and light is urged
It is higher to change activity.
In conclusion the g-C that heating is prepared3N4The catalytic activity and temperature gradient of solid have close relationship.It is right
In same g-C3N4Solid is apparently higher than perpendicular to the photocatalytic activity in temperature gradient section and is parallel to temperature gradient section；It is right
The g-C made from different heating rates3N4Solid, heating rate is faster, and photocatalytic activity is higher.
According to above-mentioned conclusion, work as g-C3N4Solid is as catalyst in use, can during the preparation process make final
It uses the face (exposure) as the section perpendicular to temperature gradient, g-C is adjusted with this standard3N4Pendulum of the solid in heating equipment
Put position and direction.In preparation process, in the range of heating equipment allows, guarantee high heating rate as far as possible.
Claims (6)
1. a kind of catalytic activity of graphite phase carbon nitride and the research method of temperature gradient relation, which is characterized in that including following
Step:
Step 1: melamine powder after purification is uniformly sprinkled into several heatproof containers, by room temperature, respectively by different
Heating rate produces g-C under with the heating of the heat source of obvious directionality3N4Solid；
Step 2: by g-C obtained3N4Solid takes out, and is cut into respectively along parallel temperature gradient direction and vertical temperature gradient direction
Square block, the relationship between each surface of label square block and temperature gradient；
Step 3: uniformly coating g-C with the covering material with light transmission, water proof and insulation performance3N4Then square block exposes respectively
The g-C in parallel temperature gradient direction and vertical temperature gradient direction3N4The surface of square block carries out photocatalysis performance test experiments,
Obtain the catalytic activity of graphite phase carbon nitride and the relationship of temperature gradient.
2. the catalytic activity of graphite phase carbon nitride as described in claim 1 and the research method of temperature gradient relation, feature
Be, in step 1, the melamine powder of purifying is obtained after washing, drying, washing be with dehydrated alcohol and go from
Sub- water washs several times respectively；Drying is dried at 50~80 DEG C.
3. the catalytic activity of graphite phase carbon nitride as described in claim 1 and the research method of temperature gradient relation, feature
It is, in step 1, before heating, melamine powder carries out tapping in heatproof container or ultrasonic vibration is handled.
4. the catalytic activity of graphite phase carbon nitride as described in claim 1 and the research method of temperature gradient relation, feature
It is, covering material is transparent paraffin, high molecular material or varnish.
5. the catalytic activity of graphite phase carbon nitride as described in claim 1 and the research method of temperature gradient relation, feature
It is, before photocatalysis performance experiment, exposed surface is subjected to grinding process.
6. the catalytic activity of graphite phase carbon nitride as described in claim 1 and the research method of temperature gradient relation, feature
It is, photocatalysis performance experiment is using photolysis water hydrogen experiment or RhB degradation experiment.
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Cited By (1)
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| CN115414956A (en) * | 2022-09-16 | 2022-12-02 | 兰州理工大学 | Cuprous ion doped g-C 3 N 4 Composite material and preparation method and application thereof |
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