CN110143648A - A kind of preparation method of pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode - Google Patents
A kind of preparation method of pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode Download PDFInfo
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- CN110143648A CN110143648A CN201910450279.6A CN201910450279A CN110143648A CN 110143648 A CN110143648 A CN 110143648A CN 201910450279 A CN201910450279 A CN 201910450279A CN 110143648 A CN110143648 A CN 110143648A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000012986 modification Methods 0.000 title claims abstract description 17
- 230000004048 modification Effects 0.000 title claims abstract description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000243 solution Substances 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 20
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical group NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 17
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 10
- 239000000428 dust Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 9
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 229920000557 Nafion® Polymers 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 claims 1
- 239000007772 electrode material Substances 0.000 abstract description 7
- 238000002604 ultrasonography Methods 0.000 abstract description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
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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
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- B01J35/33—
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- B01J35/39—
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The present invention relates to a kind of preparation method of pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode, concrete operations follow these steps to carry out: step α is with dicyandiamide position precursor preparation carbonitride；It weighs the nitridation carbon dust in 3-5g step α and is placed in ultrasound 1h in the 250mL flask equipped with certain proportion first alcohol and water, then mechanical stirring and there is reflux unit in flask upper end at 60 DEG C, obtains azotized carbon nano stick (NTs-g-C3N4) step b；The azotized carbon nano stick that step b is obtained is weighed 1-3g to be placed in 200mL aqueous solution, using photoreduction met hod in situ, it is restored to the pt atom in platinum presoma on azotized carbon nano stick, is dried in vacuo at 60 DEG C after washing, obtain pt atom modification azotized carbon nano stick powder (PtX/NTs‑g‑C3N4)；Pt atom modification azotized carbon nano stick powder and solvent prepared by step c are obtained into viscous solution A by a certain percentage again；The solution A that finally step d is obtained is coated in FTO conductive glass surface, is then dried in vacuo at 60 DEG C, obtains the anode electrode material of photoelectrocatalysis.
Description
Technical field
The invention belongs to the photoelectrocatalysis application fields of nano catalytic material, are related to a kind of pt atom modification azotized carbon nano
The preparation method of stick photoelectrocatalysielectrode electrode.
Background technique
Photoelectrocatalysis, which refers to through the surface state of selection semiconductor light photoelectrocatalysielectrode electrode or change electrode, accelerates light
Electrochemical reaction plays light absorption and light-catalysed, generally with n-type semiconductor using semiconductor material as optoelectronic pole
Oxidation reaction occurs for light anode, principle is mainly photoproduction electricity caused by semiconductor surface of the light irradiation with electrolyte contacts
Son-hole is to the redox reaction carried out by the separated rear and effects of ion of semiconductor/electrolyte knot electric field.
Traditional photoelectrocatalysielectrode electrode material is mostly noble metal decorated semiconductor material, is partly led although its performance is purer
Body photoelectrocatalysielectrode electrode material increases, but because it leads to the biggish usage amount of noble metal to be catalyzed increased costs, so will
The nano-cluster or nano particle of noble metal are reduced to atomic size very urgent.Your gold monatomic catalyst has brought forward proof when
Belong to maximum with its surface free energy in the presence of atomic state, active highest, so being reduced to atomic size that can not only propose noble metal
High catalytic activity, and catalysis cost can be greatly reduced.
Although monatomic catalyst activity is higher, its surface free energy is too high, causes stability too poor, therefore atomic state
The selection of precious metal support is also the key of photoelectrocatalysis photoelectrocatalysielectrode electrode preparation.Noble metal platinum is used for list because of high activity
Catalyst atom research, and carbonitride is the two-dimensional semiconductor material that a kind of pair of visible light has good absorption performance, because of its nothing
Malicious, harmless advantage is applied to environmental catalysis field, the carbon azo-cycle in structure can well fixed load on its surface
Precious metal atom, therefore, using atom platinum modification azotized carbon nano stick not only can increase contact of the photoelectrocatalysielectrode electrode with water
Area, the light absorpting ability for increasing photoelectrocatalysielectrode electrode, and the preparation cost of photoelectrocatalysielectrode electrode can be reduced.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode, should
The pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode of method preparation have good vis-absorbing, electric conductivity,
PhotoelectrocatalytiPerformance Performance and stability.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method preparing platinoiridita ruthenium composite nanometer particle with microemulsion method, comprising steps of
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 5-10g is put into crucible not with cover
In, in air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 3-5g step a is placed in the 250mL flask equipped with certain proportion first alcohol and water
Then middle ultrasound 1h carries out mechanical stirring at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 1-3g to be placed in 200mL aqueous solution, also using light in situ
Former method is restored to the pt atom in platinum presoma on azotized carbon nano stick, is dried in vacuo at 60 DEG C after washing, obtains pt atom
Modify azotized carbon nano stick powder (PtX/NTs-g-C3N4)；
Step d, pt atom modification azotized carbon nano stick powder and solvent prepared by step c are obtained into stickiness by a certain percentage
Solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode；
The preparation method is a kind of photoelectrocatalysielectrode electrode of pt atom modification azotized carbon nano stick.
Compared with prior art, the invention has the following beneficial technical effects:
There is good visible light using the pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode of this method preparation
Absorbability, electric conductivity, PhotoelectrocatalytiPerformance Performance and stability.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention；
Embodiment 1
A kind of preparation method of pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode, comprising steps of
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 5g is put into crucible not with cover,
In air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 3g step a is placed in the 250mL flask equipped with 30mL methanol and 70mL water
Then ultrasonic 1h carries out mechanical stirring 1h at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 1g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method loads on the platinum to azotized carbon nano stick of 0.1wt%, is dried in vacuo at 60 DEG C after washing, obtains Pt0.1/NTs-g-C3N4；
Step d, the Pt for preparing step c0.1/NTs-g-C3N4Powder and 5%Nafion solution are 1: 3 ratio in mass ratio
Example obtains viscous solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode.
Embodiment 2
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 10g is put into crucible not with cover,
In air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 5g step a is placed in the 250mL flask equipped with 60mL methanol and 40mL water
Then ultrasonic 1h carries out mechanical stirring 3h at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 3g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method loads on the platinum to azotized carbon nano stick of 0.3wt%, is dried in vacuo at 60 DEG C after washing, obtains Pt0.3/NTs-g-C3N4；
Step d, the Pt for preparing step c0.3/NTs-g-C3N4Powder and 5%Nafion solution are 1: 3 ratio in mass ratio
Example obtains viscous solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode.
Embodiment 3
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 10g is put into crucible not with cover,
In air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 5g step a is placed in the 250mL flask equipped with 50mL methanol and 50mL water
Then ultrasonic 1h carries out mechanical stirring 5h at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 3g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method loads on the platinum to azotized carbon nano stick of 0.6wt%, is dried in vacuo at 60 DEG C after washing, obtains Pt0.6/NTs-g-C3N4；
Step d, the Pt for preparing step c0.6/NTs-g-C3N4Powder and 5%Nafion solution are 1: 3 ratio in mass ratio
Example obtains viscous solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode.
Embodiment 4
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 10g is put into crucible not with cover,
In air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 5g step a is placed in the 250mL flask equipped with 70mL methanol and 30mL water
Then ultrasonic 1h carries out mechanical stirring 10h at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 3g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method loads on the platinum to azotized carbon nano stick of 1wt%, is dried in vacuo at 60 DEG C after washing, obtains Pt1/NTs-g-C3N4；
Step d, the Pt for preparing step c1/NTs-g-C3N4Powder and 5%Nafion solution are 1: 3 ratio in mass ratio
Example obtains viscous solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode.
Embodiment 5
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 10g is put into crucible not with cover,
In air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 5g step a is placed in the 250mL flask equipped with 70mL methanol and 30mL water
Then ultrasonic 1h carries out mechanical stirring 10h at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 3g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method loads on the platinum to azotized carbon nano stick of 1.5wt%, is dried in vacuo at 60 DEG C after washing, obtains Pt1.5/NTs-g-C3N4；
Step d, the Pt for preparing step c1.5/NTs-g-C3N4Powder and 5%Nafion solution are 1: 3 ratio in mass ratio
Example obtains viscous solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode.
Embodiment 6
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 10g is put into crucible not with cover,
In air with the heating rate of 2.3 DEG C/min to 550 DEG C, the product grind into powder obtained after 4h is calcined, is labeled as g-
C3N4；
Step b, the nitridation carbon dust weighed in 5g step a is placed in the 250mL flask equipped with 70mL methanol and 30mL water
Then ultrasonic 1h carries out mechanical stirring 10h at 60 DEG C and there is reflux unit in flask upper end, be cooled to room temperature solution after 12h, passes through
10h is dried at 80 DEG C after filtering, washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 3g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method loads on the platinum to azotized carbon nano stick of 2wt%, is dried in vacuo at 60 DEG C after washing, obtains Pt2/NTs-g-C3N4；
Step d, the Pt for preparing step c2/NTs-g-C3N4Powder and 5%Nafion solution are 1: 3 ratio in mass ratio
Example obtains viscous solution A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo, obtains at 60 DEG C
To photoelectrocatalysielectrode electrode.
Application example 1
Example 3 prepare photoelectrocatalysielectrode electrode as photoelectrocatalysis anode, using titanium sheet as cathode, be placed in containing
In the phenol solution of 20mg/L, the current density that degradation reaction is arranged on constant current regulated power supply is 20mA/cm, later in sun
Visible light source is added in pole electrode side, starts to carry out photoelectrocatalysis experiment.Experiment interval sampling in different times, is tested later
Phenol in aqueous solution concentration after photoelectrocatalysis, finally obtains, electrode material phenol degrading rate after photoelectrocatalysis 90min is
The removal rate of 100%, TOC are 97.5%.
Application example 2
Example 6 prepare photoelectrocatalysielectrode electrode as photoelectrocatalysis anode, using titanium sheet as cathode, be placed in containing
In the phenol solution of 20mg/L, the current density that degradation reaction is arranged on constant current regulated power supply is 20mA/cm, later in sun
Visible light source is added in pole electrode side, starts to carry out photoelectrocatalysis experiment.Experiment interval sampling in different times, is tested later
Phenol in aqueous solution concentration after photoelectrocatalysis, finally obtains, electrode material phenol degrading rate after photoelectrocatalysis 90min is
The removal rate of 40%, TOC are 32.7%.
Application example 3
Example 2 prepare photoelectrocatalysielectrode electrode as photoelectrocatalysis anode, using titanium sheet as cathode, be placed in containing
In the phenol solution of 20mg/L, the current density that degradation reaction is arranged on constant current regulated power supply is 20mA/cm, later in sun
Visible light source is added in pole electrode side, starts to carry out photoelectrocatalysis experiment.Experiment interval sampling in different times, is tested later
Phenol in aqueous solution concentration after photoelectrocatalysis, finally obtains, electrode material phenol degrading rate after photoelectrocatalysis 90min is
The removal rate of 60%, TOC are 50.8%.
A kind of photoelectrocatalysielectrode electrode material of pt atom modification azotized carbon nano stick provided by the invention, is to be with dicyandiamide
Raw material is prepared using chloroplatinic acid as platinum source using the method for high-temperature calcination, photo-reduction in situ.The characteristics of material, mainly has: (1)
Simply, to visible light have the carbonitride of good absorption ability as the carrier of pt atom using nontoxic, harmless and preparation, it is easy to operate
(2) atom platinum is loaded with the nanorod structure of carbonitride, can not only increase pt atom load capacity, can also increase in the reaction with
The contact of aqueous solution.
The above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, although referring to above-described embodiment pair
The present invention is described in detail, it should be understood by those ordinary skilled in the art that: still can be to specific reality of the invention
The mode of applying is modified or replaced equivalently, and without departing from any modification of spirit and scope of the invention or equivalent replacement,
It should all cover in present claims range.
Claims (5)
1. a kind of preparation method of pt atom modification azotized carbon nano stick photoelectrocatalysielectrode electrode, concrete operations follow these steps into
Row:
Step a, with dicyandiamide position precursor preparation carbonitride, that is, the dicyandiamide for weighing 5-10g is put into crucible not with cover,
With the heating rate of 2.3 DEG C/min to 550 DEG C in air, the product grind into powder obtained after 4h is calcined, is labeled as g-C3N4；
Step b, it weighs the nitridation carbon dust in 3-5g step a and is placed in the 250mL flask equipped with certain proportion first alcohol and water and surpass
Then sound 1h carries out mechanical stirring at 60 DEG C and there is reflux unit in flask upper end, is cooled to room temperature solution after 12h, through filtering,
10h is dried at 80 DEG C after washing, obtains azotized carbon nano stick (NTs-g-C3N4)；
Step c, the azotized carbon nano stick that step b is obtained is weighed 1-3g to be placed in 200mL aqueous solution, using photo-reduction in situ
Method is restored to the pt atom in platinum presoma on azotized carbon nano stick, is dried in vacuo at 60 DEG C after washing, obtains pt atom and repair
Adorn azotized carbon nano stick powder (PtX/NTs-g-C3N4)；
Step d, pt atom modification azotized carbon nano stick powder and solvent prepared by step c are obtained into viscous solution by a certain percentage
A；
Step e, the solution A for obtaining step d is coated in FTO conductive glass surface, is then dried in vacuo at 60 DEG C, obtains light
Electro catalytic electrode.
2. the method according to claim 1, wherein in stepb, the volume ratio of the methanol and water is methanol
: water=X: 100-X.
3. the method according to claim 1, wherein in stepb, the mechanical stirring time is 1~6h.
4. the method according to claim 1, wherein the platinum presoma is the chlorine platinum of 0.1g/L in step c
Acid solution, and load capacity is 0.1wt%~2wt%.
5. according to the method described in claim 1, it is characterized in that in step d, Nafion solution that the solvent is 5%.
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