CN106563485A - Carbon nitride/potassium calcium niobate composite material and preparing method and application thereof - Google Patents
Carbon nitride/potassium calcium niobate composite material and preparing method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 239000011575 calcium Substances 0.000 title claims abstract description 19
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 16
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 16
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 16
- 239000011591 potassium Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 12
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title abstract description 3
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 230000001699 photocatalysis Effects 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000007146 photocatalysis Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 239000004098 Tetracycline Substances 0.000 claims description 6
- 239000013590 bulk material Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229960002180 tetracycline Drugs 0.000 claims description 6
- 229930101283 tetracycline Natural products 0.000 claims description 6
- 235000019364 tetracycline Nutrition 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 230000005588 protonation Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 150000003522 tetracyclines Chemical class 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 239000008204 material by function Substances 0.000 abstract 1
- 239000010955 niobium Substances 0.000 description 47
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 239000004202 carbamide Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- OFVLGDICTFRJMM-WESIUVDSSA-N tetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O OFVLGDICTFRJMM-WESIUVDSSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- NYRAVIYBIHCEGB-UHFFFAOYSA-N [K].[Ca] Chemical compound [K].[Ca] NYRAVIYBIHCEGB-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention relates to inorganic functional materials and the field of inorganic functional material preparation, in particular to a carbon nitride/potassium calcium niobate composite material with a heterostructure and a preparing method and application thereof. A one-step hydrothermal method is adopted for preparing g-C3N4/KCa2Nb3O10 composite photocatalyst. The specific process is as follows, KCa2Nb3O10 nanometer sheets and g-C3N4 are taken and mixed in water of a certain amount, after the mixture is stirred uniformly, an obtained mixed solution is transferred to a hydrothermal reaction kettle, the mixed solution reacts for 12 h at the temperature of 140 DEG C, centrifugal washing and drying are carried out, and the g-C3N4/KCa2Nb3O10 composite material is obtained.
Description
Technical field
The present invention relates to inorganic functional material and its preparation field, specifically a kind of carbonitride/niobium for having a heterojunction structure
Sour calcium potassium composite and preparation method thereof and purposes.
Technical background
Two dimensional oxidation thing nanometer sheet semi-conducting material is because specific surface area is big, surface energy is high and quantum size effect etc. is many
Characteristic, becomes a class focus material of photolytic hydrogen production catalyst research and development in recent years；Urge in numerous nanometer sheet light of current report
In agent, from Dion-Jacobson phases (M [An-1BnO3n+1]) KCa that separates of laminated perovskite structure niobates2Nb3O10It is many
First metal oxide nano-sheet has good stability, and especially the conduction band of such nanosheet photocatalyst is by high level
Nb 4d tracks are constituted, and the light induced electron of generation has very strong reducing power；Accordingly, with respect to other types of Nano sheet material
Material, such material is more beneficial for efficiently and stably photocatalysis Decomposition aquatic products hydrogen；However, due to being restricted by energy gap, mesh
The type niobates nanometer sheet great majority of front report cannot realize the catalytic decomposition water hydrogen manufacturing under visible light conditions；So, it is high
Effect utilizes solar energy, improves the visible absorption performance of calcium niobate potassium nanometer sheet, improves visible region photo-quantum efficiency, becomes and works as
It is front to study the difficult problem for needing to solve during such nanometer sheet material.
In recent years, polymer semiconducting material graphite phase carbon nitride (graphitic carbon nitride, g-C3N4) send out
Exhibition is very fast, because of its unique semiconductor energy band structure and excellent chemical stability, causes the extensive concern of people；It is used as one
The visible-light photocatalysis material for planting not metallic components is introduced in photocatalysis field, and such as photodissociation aquatic products hydrogen produces oxygen, photocatalysis and has
The aspects such as machine selectivity synthesis, photocatalysis degradation organic contaminant；However, gradually going deep into follow-up study, researcher
It was found that by g-C3N4Some problems are yet suffered from as catalysis material, such as specific surface area is little, photo-generate electron-hole is compound seriously,
Quantum efficiency is low seriously to restrict its application in fields such as the energy, environmental photocatlytsis.In a large amount of g-C3N4Research work, will
g-C3N4Couple with wide bandgap semiconductor (such as：TiO2,ZnO,BiPO4, ZnS and SrTiO3), can effectively improve photocatalytic degradation has
Organic pollutants efficiency；So far, it is not yet found that preparing carbonitride/calcium niobate potassium composite using hydro-thermal method and its light is urged
Change the documents and materials report of application.
The content of the invention
It is an object of the invention to provide a kind of excellent carbonitride of photocatalysis performance/calcium niobate potassium composite and its system
Preparation Method and application.
The present invention is realized by following steps：
(1) by raw material K2CO3, CaCO3And Nb2O5It is 1-1.5 according to K/Ca/Nb elemental mole ratios:2:3 grind in agate
In be well mixed.Resulting mixture is calcined into 8-16h in high temperature process furnances, KCa is obtained2Nb3O10Bulk material.Then
The bulk material for obtaining is added in 5mol/L salpeter solutions carries out protonation reaction.After reaction three days, HCa has been obtained2Nb3O10
Powder.Weigh a certain amount of resulting HCa2Nb3O10Powder disperses in deionized water, and is added thereto to TBAOH solution and enters
Row is delaminated.After reaction 7 days, by solution centrifugal, take upper strata colloid and be added dropwise in KCl solution, obtain sheet KCa2Nb3O10It is cotton-shaped
Precipitation.Deionized water and absolute ethyl alcohol clean product, and centrifugation, drying has obtained KCa2Nb3O10Nanometer sheet.
(2)g-C3N4Preparation：Prepare class graphitic carbonaceous nitrogen (g-C3N4)：Urea is weighed in semi-enclosed crucible, is first dried
It is dry, in being then transferred to temperature programming tube furnace, 550 DEG C of calcining 4- are heated to by room temperature (20 DEG C) with certain heating rate
5h.After room temperature, take out, with mortar grinder to powder after, use dilute HNO3Clean to remove residual basic species
Kind, then deionized water and the clean product of absolute ethyl alcohol, centrifugation, drying.
(3)g-C3N4/KCa2Nb3O10The preparation of composite：G-C is prepared using one step hydro thermal method3N4/KCa2Nb3O10It is multiple
Closing light catalyst, detailed process is as follows, takes KCa2Nb3O10Nanometer sheet and g-C3N4Mix in a certain amount of water, stir
Afterwards, gained mixed solution is transferred in hydrothermal reaction kettle, and 140 DEG C of reaction 12h, centrifuge washing is dried.
(4) step (1) calcining heat is 800-1400 DEG C, and heating rate is 3-10 DEG C/min.
(5) step (1) the TBAOH solution concentrations are HCa to be delaminated in 10wt%, and TBAOH and (1)2Nb3O10Thing
The ratio of the amount of matter is 1-1.5:1.
(6) step (1) deionized water and the volume ratio of TBAOH solution are 100-150：1.
(7) step (1) the KCl solution concentrations are 2-3M.
(8) step (1) KCl and HCa to be delaminated in (1)2Nb3O10The ratio of the amount of material is 10-20:1.
(9) heating rate of step (2) the calcining urea is 2.3 DEG C/min.
(10) step (2) dilute HNO3Concentration be 0.01mol/L.
(11) step (3) g-C3N4/KCa2Nb3O10G-C in composite3N4With KCa2Nb3O10Mass ratio be
0.1-0.4:1；It is preferred that 0.2:1.
(12) micromorphology analysis are carried out using X-ray diffractometer (XRD), transmission electron microscope (TEM), to product,
Photocatalytic degradation experiment is carried out as target contaminant with tetracycline (TC) solution, is inhaled by ultraviolet-visible spectrophotometer measurement
Luminosity, assesses its photocatalysis performance.
Description of the drawings
Fig. 1 is prepared KCa2Nb3O10, g-C3N4, g-C3N4/KCa2Nb3O10The XRD diffraction spectrograms of composite；From figure
In it can be seen that different quality ratio g-C3N4/KCa2Nb3O10XRD spectrum mainly by KCa2Nb3O10And g-C3N4Diffraction maximum
Constitute, and with g-C3N4And KCa2Nb3O10The increase of proportioning, g-C3N4Diffraction maximum it is more and more obvious.
Fig. 2 is prepared KCa2Nb3O10, g-C3N4, g-C3N4/KCa2Nb3O10The transmission electron microscope photo of composite sample；
As can be seen from the figure KCa2Nb3O10Thin slice and g-C3N4Thin slice is combined together.
Fig. 3 is difference g-C3N4The when m- degradation rate graph of a relation of the composite photocatalytic degradation TC solution of content, from figure
In it can be seen that 20%g-C3N4/KCa2Nb3O10Composite has highest photocatalytic activity.
Specific embodiment
Embodiment 1KCa2Nb3O10The preparation of nanometer sheet
By raw material K2CO3, CaCO3And Nb2O5According to K/Ca/Nb=1.1:2:The mixing in agate grinding of 3 ratio is equal
It is even.Resulting mixture is warming up to into 1200 DEG C in high temperature process furnances with the heating rate of 5 DEG C/min, 12h is calcined, is obtained
KCa2Nb3O10Bulk material.Then the bulk material for obtaining is added in 5M salpeter solutions carries out protonation reaction.Reaction three days
Afterwards, HCa has been obtained2Nb3O10Powder.Weigh the HCa obtained by 1g2Nb3O10Powder is dispersed in 500mL water, and is added thereto to
5mL TBAOH solution is delaminated.After reaction 7 days, by solution centrifugal, take upper strata colloid and be added dropwise to 20mL 2molL-1KCl
In solution, sheet KCa is obtained2Nb3O10Flocculent deposit.Deionized water and absolute ethyl alcohol clean product, and centrifugation, drying is obtained
KCa2Nb3O10Nanometer sheet.
The class graphitic nitralloy carbon (g-C of embodiment 23N4) preparation
g-C3N4The preparation method that uses thermal polymerization urea.The urea of 10g is weighed in semi-enclosed crucible, is put
The 48h in 80 DEG C of drying boxes, is then transferred to crucible in temperature programming tube furnace.By temperature programming tube furnace with 2.3 DEG C/
The programming rate of min is incubated 4h after being heated to 550 DEG C.After room temperature, take out, with mortar grinder to powder
Afterwards, it is 0.01molL with concentration-1Dilute HNO3Cleaning 3 times, removes residual basic specie, then deionized water and absolute ethyl alcohol
It is respectively washed 3 times.Most it is dried 12h in 80 DEG C of baking ovens.
The 10%g-C of embodiment 33N4/KCa2Nb3O10The preparation of composite
G-C is prepared using one step hydro thermal method3N4/KCa2Nb3O10Composite photo-catalyst, detailed process is as follows：Take 50mg
KCa2Nb3O10Nanometer sheet and 5.0mg g-C3N4Mixing, after stirring 30min, gained mixed solution is transferred in hydrothermal reaction kettle,
140 DEG C of reaction 12h, centrifuge washing is dried.
The 20%g-C of embodiment 43N4/KCa2Nb3O10The preparation of composite
G-C is prepared using one step hydro thermal method3N4/KCa2Nb3O10Composite photo-catalyst, detailed process is as follows：Take 50mg
KCa2Nb3O10Nanometer sheet and 10.0mg g-C3N4Mixing, after stirring 30min, gained mixed solution is transferred in hydrothermal reaction kettle,
140 DEG C of reaction 12h, centrifuge washing is dried.
The 30%g-C of embodiment 53N4/KCa2Nb3O10The preparation of composite
G-C is prepared using one step hydro thermal method3N4/KCa2Nb3O10Composite photo-catalyst, detailed process is as follows：Take 50mg
KCa2Nb3O10Nanometer sheet and 15.0mg g-C3N4Compound, after stirring 30min, gained mixed solution is transferred in hydrothermal reaction kettle,
140 DEG C of reaction 12h, centrifuge washing is dried.
The 40%g-C of embodiment 63N4/KCa2Nb3O10The preparation of composite
G-C is prepared using one step hydro thermal method3N4/KCa2Nb3O10Composite photo-catalyst, detailed process is as follows：Take 50mg
KCa2Nb3O10Nanometer sheet and 20.0mg g-C3N4Compound, after stirring 30min, gained mixed solution is transferred in hydrothermal reaction kettle,
140 DEG C of reaction 12h, centrifuge washing is dried.
The different proportion g-C of embodiment 73N4/KCa2Nb3O10The photocatalytic activity experiment of composite
(1) compound concentration is the TC solution of 35mg/L, and the solution for preparing is placed in into dark place.
(2) g-C of different quality ratio is weighed3N4/KCa2Nb3O10Composite 40mg, is respectively placed in photo catalysis reactor
In, the target degradation solution for adding 40mL steps (1) to be prepared, magnetic agitation makes composite be uniformly dispersed, and 1 is drawn per 30min
Solution in secondary response device, is used for the measurement of UV-visible absorbance after centrifugation.After magnetic agitation 90min, solution and catalyst reach
To adsorption-desorption balance, water source is opened, carry out photocatalytic degradation experiment.
(3) the photocatalytic degradation liquid in reactor is drawn per 30min, the measurement of UV-visible absorbance is used for after centrifugation.
(4) 20%g-C prepared as seen from Figure 33N4/KCa2Nb3O10Composite has excellent photocatalytic activity,
The composite of ratio TC solution degradations rate after catalytic reaction 90min reaches 81%.
Claims (9)
1. the preparation method of a kind of carbonitride/calcium niobate potassium composite, in the carbonitride/calcium niobate potassium composite,
KCa2Nb3O10Thin slice and g-C3N4Thin slice is combined together, it is characterised in that：G-C is prepared using one step hydro thermal method3N4/
KCa2Nb3O10Composite, detailed process is as follows, takes KCa2Nb3O10Nanometer sheet and g-C3N4Mix in a certain amount of water, stir
After mixing uniformly, gained mixed solution is transferred in hydrothermal reaction kettle, and 140 DEG C of reaction 12h, centrifuge washing is dried, and obtains g-C3N4/
KCa2Nb3O10Composite.
2. the preparation method of a kind of carbonitride/calcium niobate potassium composite as claimed in claim 1, it is characterised in that：It is described
g-C3N4/KCa2Nb3O10G-C in composite3N4With KCa2Nb3O10Mass ratio be 0.1-0.4:1.
3. the preparation method of a kind of carbonitride/calcium niobate potassium composite as claimed in claim 2, it is characterised in that：It is described
g-C3N4/KCa2Nb3O10G-C in composite3N4With KCa2Nb3O10Mass ratio be 0.2:1.
4. the preparation method of a kind of carbonitride/calcium niobate potassium composite as claimed in claim 1, it is characterised in that described
KCa2Nb3O10The preparation process of nanometer sheet is as follows：By raw material K2CO3, CaCO3And Nb2O5It is according to K/Ca/Nb elemental mole ratios
1-1.5:2:3 are well mixed in agate grinding, and resulting mixture is calcined into 8-16h in high temperature process furnances, obtain
KCa2Nb3O10Bulk material, then the bulk material for obtaining is added in 5mol/L salpeter solutions carries out protonation reaction, reaction
After three days, HCa has been obtained2Nb3O10Powder, weighs a certain amount of resulting HCa2Nb3O10Powder disperses in deionized water, and
It is added thereto to TBAOH solution to be delaminated, after reacting 7 days, by solution centrifugal, takes upper strata colloid and be added dropwise in KCl solution,
Obtain sheet KCa2Nb3O10Flocculent deposit, deionized water and absolute ethyl alcohol clean product, centrifugation, and drying is obtained
KCa2Nb3O10Nanometer sheet.
5. a kind of preparation method of carbonitride/calcium niobate potassium composite as claimed in claim 4, it is characterised in that (4) institute
Calcining heat is stated for 800-1400 DEG C, heating rate is 3-10 DEG C/min.
6. the preparation method of a kind of carbonitride/calcium niobate potassium composite as claimed in claim 4, it is characterised in that described
TBAOH solution concentrations are 10wt%, and TBAOH and HCa to be delaminated2Nb3O10The ratio of the amount of material is 1-1.5:1.
7. the preparation method of a kind of carbonitride/calcium niobate potassium composite as claimed in claim 4, it is characterised in that described
Deionized water is 100-150 with the volume ratio of TBAOH solution：1.
8. a kind of preparation method of carbonitride/calcium niobate potassium composite as claimed in claim 4, it is characterised in that step
(1) the KCl solution concentrations are 2-3M, KCl and HCa to be delaminated2Nb3O10The ratio of the amount of material is 10-20:1.
9. carbonitride/calcium niobate potassium composite that prepared by the preparation method as described in claim 1-8 is arbitrary is for photocatalysis drop
The purposes of solution tetracycline.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107233909A (en) * | 2017-07-20 | 2017-10-10 | 江苏大学 | A kind of preparation method and its usage of SrNb2 O6/nitridation carbon composite nano-material |
| CN107262085A (en) * | 2017-07-21 | 2017-10-20 | 江苏大学 | A kind of preparation method of bismuth/calcium niobate potassium plasma nano composite |
| CN107376943A (en) * | 2017-07-20 | 2017-11-24 | 江苏大学 | A kind of preparation method and purposes of calcium niobate potassium/cadmium sulfide composite material |
| CN108187718A (en) * | 2017-12-28 | 2018-06-22 | 江苏大学 | A kind of Preparation method and use of carbonitride/tantalic acid calcium potassium nanosheet composite material |
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