CN105903485A - Synthesis method of porous carbon nitride/hydroxy iron nanorod composite photo-Fenton material with visible light response - Google Patents
Synthesis method of porous carbon nitride/hydroxy iron nanorod composite photo-Fenton material with visible light response Download PDFInfo
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- 239000002073 nanorod Substances 0.000 title abstract 4
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 16
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- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
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- 230000015572 biosynthetic process Effects 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000003786 synthesis reaction Methods 0.000 abstract description 11
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 9
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- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001448 ferrous ion Inorganic materials 0.000 abstract description 2
- 229920000877 Melamine resin Polymers 0.000 abstract 1
- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 abstract 1
- 230000031700 light absorption Effects 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 abstract 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
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- 229910021642 ultra pure water Inorganic materials 0.000 description 6
- 239000012498 ultrapure water Substances 0.000 description 6
- 229910052724 xenon Inorganic materials 0.000 description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
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- 238000002474 experimental method Methods 0.000 description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 229910016874 Fe(NO3) Inorganic materials 0.000 description 2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
The invention discloses a synthesis method of a porous carbon nitride/hydroxy iron nanorod composite photo-Fenton material with visible light response. The method solves the problems of low photocatalytic activity caused by low specific surface area, easy oxidation of ferrous ions, low persulfate activation rate and other reasons of present carbonitride. Carbon nitride macromolecules undergo ultrasonic treatment to form quantum dots, so the light absorptivity of the material is greatly improved; a nano-rod composite material with visible light response is obtained on carbon nitride through in situ synthesis using iron nitrate nonahydrate, hydroxy iron and carbon nitride form heterojunctions to reduce the photoelectron recombination-hole recombination rate, and the composite material improves the light absorption range of carbon nitride to the visible light region from the ultraviolet light region, so the photocatalytic activity of the material is substantially improved. A raw material melamine used in the invention has a low price, and undergoes a simple in situ synthesis reaction and a hydrothermal reaction to prepare a carbon nitride/hydroxy iron nanorod composite; and persulfate with good stability and low price is directly introduced, and cooperates with the formed heterostructure, so the photoelectron-hole recombination rate is obviously reduced, and the photocatalysis ability of the material is effectively improved.
Description
Technical field
The present invention relates to a kind of composite technology of preparing, the synthetic method of a kind of nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material.
Background technology
Incretion interferent is a kind of exogenous substances, and it can interfere with the synthesis of organism natural hormone, secretes, combines, acts on and remove, thus affects the dynamic equilibrium of organism, breeds, grows and behavior.This kind of material has that concentration is low, hazardness greatly, the feature such as more difficult removal, sewage disposal receives increasing concern.Bisphenol-A is a kind of typical incretion interferent, and it is used to polycarbonate synthesis, epoxy resin, fire retardant and other chemical products, has wide range of applications.So that the catalyst that research is gentle, cheap, physical and chemical performance is stable, photo-catalysis capability is strong carrys out the persistent pollutant in degradation water, to ensure that commercial production is lived with people, reduce its destruction to environment, and then realize sustainable economic development.
Owing to there is environment and energy problem, the light fenton catalyst that searching can convert solar energy into chemical energy and catalytic activation persulfate is extremely urgent, and synthesis has response, simple, stable, efficient photocatalyst remain a huge challenge in visible region.Titanium dioxide is nontoxic due to it, and stable, good photocatalytic activity becomes present stage the most widely used semiconductor light-catalyst.But.The absorption region of titanium dioxide is at ultraviolet region, and ultraviolet light only accounts for and enters about the 5% of atmospheric solar energy, and the utilization rate for solar energy is too low, although the many modified composite titania materials crossed of nowadays appearance, but design synthesizesNovelLight Fenton catalysis material the most particularly significant.This project is to researchNovelLight Fenton catalysis material is significant.
Carbonitride/metal-oxide is a kind of by supermolecular mechanism and metal ion and the formation of g-C3N4 coordinationNovelComposite.Its precursor polymer quasiconductor graphite phase carbon nitride has stable physical and chemical performance, good medium electron energy band (2.7eV), become the most attracting photocatalysis of one and light Fenton material, it is nontoxic, inexpensive, and stable characteristic can be applied at numerous areas, such as photolysis water hydrogen, photocatalytic degradation of dye, light Fenton degradation of contaminant, ultracapacitor etc..But g-C3N4 there is also shortcomings, such as light induced electron recombination rate is high, and solar energy utilization ratio is relatively low, and specific surface area is little.In order to solve these problems, need g-C3N4 is modified.So far, yet there are no and utilize supermolecular mechanism and coordination, the related process technologies using fabricated in situ and hydro-thermal reaction to prepare carbonitride/iron carbonyl nano composite material occurs.
Summary of the invention
For solving the deficiencies in the prior art, object of the present invention is to provide the synthetic method of the light Fenton agent of a kind of visible light-responded carbonitride/iron carbonyl nano composite material, it is low that the method solves existing carbonitride specific surface area, ferrous ion easily aoxidizes, and persulfate activation rate is relatively low etc. former thus results in the problem that photocatalytic activity is low.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that:
A kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, comprises the steps:
Step one, loads tripolycyanamide in porcelain boat, temperature reaction 4 hours in argon atmosphere, then cools down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder；
Step 2, product step one prepared loads beaker, adds isopropanol solvent, puts into ultrasonic machine continual ultrasonic 4h, ultrasonic for carbonitride macromole stripping is become carbonitride quantum dot；
Step 3, carbonitride step 2 peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is 10,30 DEG C of temperature constant magnetic stirring half an hour with PH regulator by pH regulator, mixed liquor is transferred in reactor, after 100 DEG C of reaction 10h, by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
Aforesaid a kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, the argon atmosphere in step one be argon flow velocity be 50cc/min.
Aforesaid a kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, the condition of the temperature reaction in step one includes: start to warm up to 540 degrees Celsius to 600 degrees Celsius from room temperature；Liter per minute 2.3 DEG C.
Aforesaid a kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, the carbonitride quantum dot in step 2 is single-layer silicon nitride carbon.
Aforesaid a kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, the power bracket of the ultrasonic machine in step 2 is arranged between 700 watts.
Aforesaid a kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, the PH regulator in step 3 is sodium hydroxide.
The invention have benefit that: the present invention becomes quantum dot by ultrasonic for carbonitride macromole, be greatly improved the material absorbance to light；The present invention uses Fe(NO3)39H2O fabricated in situ to obtain visible light-responded nanometer rod composite material on carbonitride, hetero-junctions is formed by iron carbonyl and carbonitride, reduce light induced electron and be combined-hole-recombination rate, the light abstraction width of carbonitride is brought up to visible region from ultraviolet region by composite simultaneously, significantly improves the photocatalytic activity of material；Raw material tripolycyanamide cheap that the present invention uses, is just prepared for carbonitride/iron carbonyl nano composite material through simple in-situ synthesized reaction and hydro-thermal reaction method；Process is simple, and preparation is convenient, and at a low price, the heterojunction structure of formation significantly reduces photo-generate electron-hole recombination rate to raw material, is effectively increased the photo-catalysis capability of material.
Accompanying drawing explanation
Figure 1It it is the scanning electron microscope of carbonitride/iron carbonyl nano composite material that test two obtainsFigure；
Figure 2UV-vis DRS for carbonitride/iron carbonyl nano composite material that test one obtainsFigure；
Figure 3The different proportion composition carbonitride/iron carbonyl nano composite material catalyst light Fenton degrading activity obtained for test fourFigure；
Figure 4Catalyst for test five acquisition recyclesFigure；
Figure 5Carbonitride/iron carbonyl nano composite material catalyst light degradation at different conditions activity for test six acquisitionFigure。
Detailed description of the invention
Below in conjunction withAccompanying drawingWith specific embodiment, the present invention made concrete introduction.
A kind of synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, comprises the steps:
Step one, loads tripolycyanamide in porcelain boat, temperature reaction 4 hours in argon atmosphere, then cools down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder；
Step 2, product step one prepared loads beaker, adds isopropanol solvent, puts into ultrasonic machine continual ultrasonic 4h, ultrasonic for carbonitride macromole stripping is become carbonitride quantum dot；
Step 3, carbonitride step 2 peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is 10,30 DEG C of temperature constant magnetic stirring half an hour with PH regulator by pH regulator, mixed liquor is transferred in reactor, after 100 DEG C of reaction 10h, by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
It should be understood that the above-mentioned argon atmosphere in step one is argon flow velocity is 50cc/min.The condition of the above-mentioned temperature reaction in step one includes: start to warm up to 540 degrees Celsius to 600 degrees Celsius from room temperature；Liter per minute 2.3 DEG C.In order to maximum increases its surface area, being beneficial to follow-up synthesis, the carbonitride quantum dot in step 2 is single-layer silicon nitride carbon.The power bracket of the ultrasonic machine in step 2 is arranged on 700 watts.Preferred as one, the PH regulator in step 3 is sodium hydroxide.
The preparation of embodiment 1 carbonitride/iron carbonyl nano composite material
1) 3g tripolycyanamide is loaded in porcelain boat, in argon atmosphere 540 DEG C with 2.3 DEG C of speed temperature reactions per minute 4 hours, then cool down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder.Argon flow velocity is 50cc/min.
2) product appropriate step 1) prepared loads 500ml beaker, adds isopropanol solvent, 700w power continual ultrasonic 4h, makes carbonitride stripping as far as possible become monolayer, and maximum increases its surface area, is beneficial to follow-up synthesis.
3) by 2) carbonitride peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is about 10 with sodium hydroxide by pH regulator, 30 DEG C of temperature constant magnetic stirring half an hour, being transferred in reactor by mixed liquor, 100 DEG C of reaction 10h, afterwards by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
The preparation of embodiment 2 carbonitrides/iron carbonyl nano composite material
1) 3g tripolycyanamide is loaded in porcelain boat, in argon atmosphere 560 DEG C with 5 DEG C of speed temperature reactions per minute 4 hours, then cool down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder.Argon flow velocity is 50cc/min.
2) product appropriate step 1) prepared loads 500ml beaker, adds isopropanol solvent, 800w power continual ultrasonic 4h, makes carbonitride stripping as far as possible become monolayer, and maximum increases its surface area, is beneficial to follow-up synthesis.
3) by 2) carbonitride peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is about 10 with sodium hydroxide by pH regulator, 30 DEG C of temperature constant magnetic stirring half an hour, being transferred in reactor by mixed liquor, 100 DEG C of reaction 10h, afterwards by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
The preparation of embodiment 3 carbonitrides/iron carbonyl nano composite material
1) 3g tripolycyanamide is loaded in porcelain boat, in argon atmosphere 580 DEG C with 7 DEG C of speed temperature reactions per minute 4 hours, then cool down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder.Argon flow velocity is 50cc/min.
2) product appropriate step 1) prepared loads 500ml beaker, adds isopropanol solvent, 750w power continual ultrasonic 4h, makes carbonitride stripping as far as possible become monolayer, and maximum increases its surface area, is beneficial to follow-up synthesis.
3) by 2) carbonitride peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is about 10 with sodium hydroxide by pH regulator, 30 DEG C of temperature constant magnetic stirring half an hour, being transferred in reactor by mixed liquor, 100 DEG C of reaction 10h, afterwards by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
The preparation of embodiment 4 carbonitrides/iron carbonyl nano composite material
1) 3g tripolycyanamide is loaded in porcelain boat, in argon atmosphere 600 DEG C with 2.3 DEG C of speed temperature reactions per minute 4 hours, then cool down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder.Argon flow velocity is 50cc/min.
2) product appropriate step 1) prepared loads 500ml beaker, adds isopropanol solvent, 650w power continual ultrasonic 4h, makes carbonitride stripping as far as possible become monolayer, and maximum increases its surface area, is beneficial to follow-up synthesis.
3) by 2) carbonitride peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is about 10 with sodium hydroxide by pH regulator, 30 DEG C of temperature constant magnetic stirring half an hour, being transferred in reactor by mixed liquor, 100 DEG C of reaction 10h, afterwards by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
Beneficial effects of the present invention is proved by tests below.
Test one:
1) 3g tripolycyanamide is loaded in porcelain boat, in argon atmosphere 540 DEG C with 2.3 DEG C of speed temperature reactions per minute 4 hours, then cool down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder.Argon flow velocity is 50cc/min.
2) product appropriate step 1) prepared loads 500ml beaker, adds isopropanol solvent, 700w power continual ultrasonic 4h, makes carbonitride stripping as far as possible become monolayer, and maximum increases its surface area, is beneficial to follow-up synthesis.
3) by 2) carbonitride peeled off adds the ferric nitrate of different quality, magnetic agitation is uniform, then it is about 10 with sodium hydroxide by pH regulator, 30 DEG C of temperature constant magnetic stirring half an hour, being transferred in reactor by mixed liquor, 100 DEG C of reaction 10h, afterwards by product centrifugation, 60 DEG C of dry 24h in an oven, obtain the carbonitride/iron carbonyl nano composite material of different proportion.
Test two: use scanning electron microscope that carbonitride/iron carbonyl nano composite material that experiment one prepares is carried out electron-microscope scanning and obtainSuch as figure 1Shown carbonitride/iron carbonyl nano composite material SEMFigure, fromFigure 1Can be seen that carbonitride/iron carbonyl nano composite material SEM that test one preparesFigure, fromFigure 1Can be seen that carbonitride/iron carbonyl nano composite material that test one prepares is nanometer rods, there is iron carbonyl on surface.
Test three: use UV-vis DRS spectrogrph that carbonitride/iron carbonyl nano composite material that experiment one prepares is carried out electron-microscope scanning and obtainSuch as figure 2Shown carbonitride/iron carbonyl nano composite material DRSFigure, fromFigure 2Can be seen that carbonitride/iron carbonyl nano composite material DRS that test one preparesFigure, fromFigure 2Can be seen that absorption to light is remarkably reinforced carbonitride/iron carbonyl nano composite material that experiment one prepares in visible region relative to pure graphite phase carbon nitride, therefore produces more photoelectron and separates with hole, contributes to the degraded for pollutant.
Test four: utilize the carbonitride/iron carbonyl nano composite material degraded bisphenol-A of test one preparation, with graphite phase carbon nitride, iron carbonyl, load different proportion iron carbonyl carbonitride/iron carbonyl nano composite material as matched group and experimental group, detailed process is as follows:
Weigh 20mg test one and prepare carbonitride/iron carbonyl nano composite material, ultrasonic 2h is scattered in 41ml ultra-pure water, add 5ml 100mg/L bisphenol-A, put into lucifuge magnetic agitation half an hour in photoreaction instrument, ensure absorption-resolving balance,, with the xenon lamp of 300w as light source, before timing, add 4ml 100mmol/L persulfate carry out the degraded bisphenol-A test reaction of light Fenton.
Weigh 20mg graphite phase carbon nitride, ultrasonic 2h is scattered in 41ml ultra-pure water, add 5ml 100mg/L bisphenol-A, put into lucifuge magnetic agitation half an hour in photoreaction instrument, ensure absorption-resolving balance, with the xenon lamp of 300w as light source, before timing, add 4ml 100mmol/L persulfate carry out the test reaction of light degradation bisphenol-A.
Weigh 20mg iron carbonyl, ultrasonic 2h is scattered in 41ml ultra-pure water, add 5ml 100mg/L bisphenol-A, put into lucifuge magnetic agitation half an hour in photoreaction instrument, ensure absorption-resolving balance, with the xenon lamp of 300w as light source, before timing, add 4ml 100mmol/L persulfate carry out the test reaction of light degradation bisphenol-A.
Take 1.5ml reactant liquor every reasonable time, measure its absorbance by liquid phase after being centrifuged, obtainSuch as figure 3Shown light degradation curveFigure.nullThe effect of the light Fenton degradation of contaminant of the carbonitride/iron carbonyl nano composite material of doping 15% is best，Reason is as follows: carbonitride is limited to the activation of persulfate，The carbonitride of doping 20%/iron carbonyl nano composite material doping excess，Carbonitride photocatalysis is caused substantially to weaken，Two kinds of effects combine，Cause adulterating 15% the effect of activation degraded bisphenol-A of carbonitride/iron carbonyl nano composite material best，Light region can had more preferable absorbance by the carbonitride/iron carbonyl nano composite material relatively carbonitride of doping 15%，Tested as shown in three，The most under visible light，Light induced electron is passed to iron carbonyl and is produced the iron carbonyl of bivalence by carbonitride，Light induced electron is occurred to separate with hole，Oxygen reduction is super oxygen root free radical by light induced electron，Super oxygen root free radical produces hydrogen peroxide，Hydrogen peroxide and the persulfate being directly added into produce hydroxyl radical free radical and potentiometric titrations respectively via the catalysis of the iron carbonyl of bivalence，Two kinds of free radicals all can be with mineralising pollutant；While photoelectron is passed to the iron carbonyl of iron carbonyl generation bivalence of trivalent by carbonitride, consume photoelectron, greatly reduce photoelectron hole and separate, hole direct mineralising pollutant bisphenol-A, thus reach the purpose of environmental conservation.
Test five: by the carbonitride/iron carbonyl nano composite material centrifugal drying in test four, it is scattered in the bisphenol-A that 50ml concentration is 10mg/L, put into lucifuge stirring half an hour in photoreaction instrument, reach catalyst and bisphenol-A absorption-parsing balance, with the xenon lamp of 300w as light source, carry out light Fenton degradation experiment, be so repeated twice and obtainSuch as figure 4Shown light Fenton catalytic degradation repeatability curveFigure.Light Fenton catalysis activity keeps constant.
Test six: utilize the 15% carbonitride/iron carbonyl nano composite material degraded bisphenol-A of test one preparation, with light Fenton, only illumination, only Fenton condition as experimental group or matched group, detailed process is as follows:
Weigh 20mg 15% carbonitride/iron carbonyl nano composite material, ultrasonic 2h is scattered in 41ml ultra-pure water, add 5ml 100mg/L bisphenol-A, put into lucifuge magnetic agitation half an hour in photoreaction instrument, ensure absorption-resolving balance, with the xenon lamp of 300w as light source, before timing, add 4ml 100mmol/L persulfate carry out the test reaction of light degradation bisphenol-A.
Weigh 20mg 15% carbonitride/iron carbonyl nano composite material, ultrasonic 2h is scattered in 41ml ultra-pure water, add 5ml 100mg/L bisphenol-A, put into lucifuge magnetic agitation half an hour in photoreaction instrument, ensure absorption-resolving balance, with the xenon lamp of 300w as light source, directly carry out the test reaction of light degradation bisphenol-A.
Weigh 20mg 15% carbonitride/iron carbonyl nano composite material, ultrasonic 2h is scattered in 41ml ultra-pure water, add 5ml 100mg/L bisphenol-A, put into lucifuge magnetic agitation half an hour in photoreaction instrument, ensure absorption-resolving balance, under conditions of dark lucifuge, directly carry out the test reaction of light degradation bisphenol-A.
The present invention becomes quantum dot by ultrasonic for carbonitride macromole, is greatly improved the material absorbance to light；The present invention uses Fe(NO3)39H2O fabricated in situ to obtain visible light-responded nanometer rod composite material on carbonitride, hetero-junctions is formed by iron carbonyl and carbonitride, reduce light induced electron and be combined-hole-recombination rate, the light abstraction width of carbonitride is brought up to visible region from ultraviolet region by composite simultaneously, significantly improves the photocatalytic activity of material；Raw material tripolycyanamide cheap that the present invention uses, is just prepared for carbonitride/iron carbonyl nano composite material through simple in-situ synthesized reaction and hydro-thermal reaction method；Process is simple, and preparation is convenient, and at a low price, the heterojunction structure of formation significantly reduces photo-generate electron-hole recombination rate to raw material, is effectively increased the photo-catalysis capability of material.
The ultimate principle of the present invention, principal character and advantage have more than been shown and described.Skilled person will appreciate that of the industry, above-described embodiment limits the present invention, the technical scheme that the mode of all employing equivalents or equivalent transformation is obtained the most in any form, all falls within protection scope of the present invention.
Claims (6)
1. a synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, it is characterised in that comprise the steps:
Step one, loads tripolycyanamide in porcelain boat, temperature reaction 4 hours in argon atmosphere, then cools down in nitrogen atmosphere, the final carbonitride obtaining yellow shape, grind into powder；
Step 2, product step one prepared loads beaker, adds isopropanol solvent, puts into ultrasonic machine continual ultrasonic 4h, ultrasonic for carbonitride macromole stripping is become carbonitride quantum dot；
Step 3, carbonitride step 2 peeled off adds appropriate ferric nitrate, magnetic agitation is uniform, then it is 10,30 DEG C of temperature constant magnetic stirring half an hour with PH regulator by pH regulator, mixed liquor is transferred in reactor, after 100 DEG C of reaction 10h, by product centrifugation, 60 DEG C of dry 24h in an oven, obtain carbonitride/iron carbonyl nano composite material.
2. a synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, it is characterised in that the above-mentioned argon atmosphere in step one be argon flow velocity be 50cc/min.
3. a synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, it is characterised in that the condition of the above-mentioned temperature reaction in step one includes: start to warm up to 540 degrees Celsius to 600 degrees Celsius from room temperature；Liter per minute 2.3 DEG C.
4. a synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, it is characterised in that the above-mentioned carbonitride quantum dot in step 2 is single-layer silicon nitride carbon.
5. a synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, it is characterised in that the power bracket of the above-mentioned ultrasonic machine in step 2 is arranged on 700 watts.
6. a synthetic method with visible light-responded nitride porous carbon/iron carbonyl nanometer rods complex light Fenton material, it is characterised in that the above-mentioned PH regulator in step 3 is sodium hydroxide.
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