CN109317174A - A kind of titanium wire network loads three-dimensional bismuthyl carbonate bouquet and its preparation method and application - Google Patents
A kind of titanium wire network loads three-dimensional bismuthyl carbonate bouquet and its preparation method and application Download PDFInfo
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- CN109317174A CN109317174A CN201811223009.3A CN201811223009A CN109317174A CN 109317174 A CN109317174 A CN 109317174A CN 201811223009 A CN201811223009 A CN 201811223009A CN 109317174 A CN109317174 A CN 109317174A
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- bismuthyl carbonate
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004202 carbamide Substances 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 230000015556 catabolic process Effects 0.000 abstract description 13
- 238000006731 degradation reaction Methods 0.000 abstract description 13
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 5
- 229940043267 rhodamine b Drugs 0.000 abstract description 5
- 239000010936 titanium Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 10
- 229910052719 titanium Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910001451 bismuth ion Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 235000012501 ammonium carbonate Nutrition 0.000 description 2
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- 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
-
- 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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of titanium wire networks to load three-dimensional bismuthyl carbonate bouquet and its preparation method and application.The preparation method includes the following steps: S1: bismuth citrate and urea are dissolved to obtain mixed solution；The molar ratio of the bismuth citrate and urea is 6:1 ~ 10:1；S2: titanium wire network is added in mixed solution described in S1, and 5 ~ 8h of hydro-thermal reaction is dried to obtain titanium wire network and loads three-dimensional bismuthyl carbonate bouquet by titanium wire network taking-up rinsing after cooling at 160 ~ 180 DEG C under closed environment.Preparation process of the invention is simple, can with rapid, high volume synthesize large specific surface area, and the titanium wire network of stable structure loads three-dimensional bismuthyl carbonate bouquet.The titanium wire network that the present invention synthesizes loads three-dimensional bismuthyl carbonate bouquet, and there is excellent catalytic efficiency can be widely applied to photoelectric Material Field especially to rhodamine B degradation efficiency with higher.
Description
Technical field
The present invention relates to inorganic micro Nano material preparation fields, load three-dimensional bismuthyl carbonate more particularly to a kind of titanium wire network
Bouquet and its preparation method and application.
Background technique
With the continuous social and economic development, the mankind are also increasingly severe to the destruction of natural environment.Therefore, environmental pollution
Administer and just become one of the key subjects that are facing jointly of the whole mankind, wherein the improvement of water pollution gains a special interest.In recent years
Come, is just becoming the research focus of field for the treatment of of water pollution come the method for Degradation of Organo-pollutants in Water with Photo-catalysis using photochemical catalyst
One of.
Bismuthyl carbonate is as a kind of novel semi-conductor nano material, since it is with preferable photocatalysis performance and by more
Carry out more concerns.Under certain illumination condition, nano-calcium carbonate oxygen bismuth generates electron-hole pair after being excited by light, thus
It is provided with stronger redox ability, so that the quilt after a series of redox reaction of the organic pollutant in water
It is gradually degraded as environment amenable innocuous substance.Due to anisotropic design feature, bismuthyl carbonate can grow into two dimension
The nanometer sheet of structure.
The bismuthyl carbonate being prepared at present is mostly the nanometer sheet of two-dimensional structure.When in use due to nanometer sheet at random
Accumulation easily occurs or overlapping, available specific surface area substantially reduce.It is, thus, sought for a kind of simple process, at low cost
Honest and clean preparation method prepares large specific surface area, stable structure, the three-dimensional bismuthyl carbonate bouquet of high catalytic efficiency.
Summary of the invention
It is an object of the invention to overcome, the two-dimentional bismuthyl carbonate nanometer sheet specific surface area of prior art preparation is small, structure is steady
The defect of qualitative difference provides a kind of preparation method of three-dimensional bismuthyl carbonate bouquet of titanium wire network load.Preparation side provided by the invention
Method simple process, can with rapid, high volume synthesize large specific surface area, and the titanium wire network of stable structure loads three-dimensional bismuthyl carbonate bouquet；
The titanium wire network that the present invention synthesizes, which loads three-dimensional bismuthyl carbonate bouquet, has excellent catalytic efficiency, especially has to rhodamine B
Higher degradation efficiency can be widely applied to photoelectric Material Field.
Another object of the present invention is to provide a kind of titanium wire networks that the above method is prepared to load three-dimensional bismuthyl carbonate
Bouquet.
Another object of the present invention is to provide above-mentioned titanium wire networks to load three-dimensional bismuthyl carbonate bouquet in photoelectric material
The application in material field.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of titanium wire network loads the preparation method of three-dimensional bismuthyl carbonate bouquet, includes the following steps:
S1: bismuth citrate and urea are dissolved into obtain mixed solution；The molar ratio of the bismuth citrate and urea is 6:1 ~ 10:1；
S2: titanium wire network is added in mixed solution described in S1, under closed environment at 160 ~ 180 DEG C 5 ~ 8h of hydro-thermal reaction,
Titanium wire network is taken out after cooling and is rinsed, titanium wire network is dried to obtain and loads three-dimensional bismuthyl carbonate bouquet.
It is uniform that the three-dimensional bismuthyl carbonate bouquet pattern of titanium wire network load being prepared is combined with urea using bismuth citrate.This
It is because bismuth ion is complexed by citrate in bismuth citrate, bismuth ion release is slower.Urea is heat resolve into carbon dioxide
And ammonia, soluble in water just will be slow of both gases ionize out carbonate and hydroxide ion.The slow release of bismuth ion and
The slow ionization of carbanion is so that the nucleation rate of crystal is slower in reaction system, so that the titanium wire network load eventually formed
Three-dimensional bismuthyl carbonate bouquet pattern is uniform.If sodium carbonate, ammonium carbonate etc. are carbon source reaction with bismuth chloride, bismuth nitrate etc. for bismuth source,
It was found that this may be because when the bismuth ion in the above bismuth source, the carbon in carbon source almost without bismuthyl carbonate sample on titanium wire network
Acid group release is very fast, and just there has been precipitating in when mixing, therefore bismuthyl carbonate is difficult to grow on titanium wire network.
Bismuthyl carbonate, which is supported in conductive substrates, can promote efficiently separating for light induced electron and hole, further change
It is apt to its photocatalysis performance.But it was found by the inventors of the present invention that can only obtain two when as selected carbon plate, titanium sheet substrate to be loaded
The bismuthyl carbonate nanometer sheet of laminated structure is tieed up, accumulation or overlapping easily occur when in use for two-dimensional nano piece at random, available
Specific surface area substantially reduce.And when selecting titanium wire network as substrate, three-dimensional bismuthyl carbonate bouquet can be prepared.
Preparation method provided by the invention passes through control reaction time and temperature on the basis of selecting titanium wire network as substrate
Bismuth citrate and urea mol ratio is added in degree, and three-dimensional bismuthyl carbonate bouquet is finally prepared.The bouquet not only has bigger
Specific surface area also has better structural stability, and when use is not easily to fall off, and recycling rate of waterused greatly promotes；In addition to this,
PhotoelectrocatalytiPerformance Performance also greatly promotes, especially to rhodamine B degradation efficiency with higher.If the reaction time is too long, reaction
Temperature is excessively high, and three-dimensional bismuthyl carbonate bouquet volume is excessive, is easy to fall off from titanium wire network, can be grown in originally with stylish bouquet
Bouquet on, can not contact titanium wire network carry out electronics transfer, cause catalytic performance to decline.
Preferably, bismuth concentration is 0.02 ~ 0.05mol/L in mixed solution described in S1.
The pattern that above-mentioned specific concentration range can allow titanium wire network obtained to load three-dimensional bismuthyl carbonate bouquet is more uniform.
Preferably, the molar ratio of bismuth citrate described in S1 and urea is 20:3.
The molar ratio of the above-mentioned specific bismuth citrate and urea can make the titanium wire network generated load three-dimensional bismuthyl carbonate
The structure of bouquet is more stable.
Preferably, the temperature of hydro-thermal reaction described in S2 is 160 DEG C, time 5h.
Rinse reagent, dry environment are this field conventional selection.
Preferably, the reagent that rinse cycle described in S2 is selected is deionized water and dehydrated alcohol.
Preferably, process dry described in S2 are as follows: be dried under 60 ~ 80 DEG C of vacuum environment.
A kind of three-dimensional bismuthyl carbonate bouquet of titanium wire network load, is obtained by above-mentioned preparation method.
It is uniform that a kind of titanium wire network obtained by above-mentioned preparation method loads the size of three-dimensional bismuthyl carbonate bouquet, pattern,
Large specific surface area, stable structure.
Above-mentioned titanium wire network loads application of the three-dimensional bismuthyl carbonate bouquet in photoelectric Material Field also of the invention
In protection scope.
Compared with prior art, the invention has the following beneficial effects:
Preparation process of the invention is simple, can with rapid, high volume synthesize large specific surface area, the titanium wire network load three of stable structure
Tie up bismuthyl carbonate bouquet.The titanium wire network that the present invention synthesizes, which loads three-dimensional bismuthyl carbonate bouquet, has excellent catalytic efficiency, especially
It is that photoelectric Material Field can be widely applied to rhodamine B degradation efficiency with higher.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram that the titanium wire network that embodiment 1 provides loads three-dimensional bismuthyl carbonate bouquet；
Fig. 2 is the scanning electron microscope and transmission electron microscope picture that the titanium wire network that embodiment 1 provides loads three-dimensional bismuthyl carbonate bouquet.
Specific embodiment
Below with reference to embodiment, the present invention is further explained.These embodiments are merely to illustrate the present invention rather than limitation
The scope of the present invention.Test method without specific conditions in lower example embodiment usually according to this field normal condition or is pressed
The condition suggested according to manufacturer；Used raw material, reagent etc., unless otherwise specified, being can be from the business such as conventional market
The raw materials and reagents that approach obtains.The variation for any unsubstantiality that those skilled in the art is done on the basis of the present invention
And replacement belongs to scope of the present invention.
Embodiment 1
The present embodiment provides a kind of titanium wire networks to load three-dimensional bismuthyl carbonate bouquet (Bi2O2CO3/ Ti).It is prepared via a method which
It arrives:
The urea of the bismuth citrate of 1.5mmol and 10mmol is dissolved in 60mL deionized water under stiring and forms solution, finally
This solution is transferred in the stainless steel cauldron that 100mL liner is polytetrafluoroethylene (PTFE).The titanium wire network of a piece of 4*2cm is leant against
Inner liner of reaction kettle wall surface, is placed in drying box, hydro-thermal reaction 5 hours at 160 DEG C.Then cooled to room temperature, by titanium silk
Net deionized water and dehydrated alcohol rinse three times respectively, and are dried in vacuo 12 hours in 60 DEG C and obtain product.The X-ray of product
Diffraction pattern is shown in Fig. 1, and each diffraction maximum position and intensity are consistent with standard diffraction card (JCPDS41-1488) in figure.It scans electricity
Mirror is shown in that Fig. 2, Fig. 2 (a) show that the close-up view of titanium wire network, Fig. 2 (b) are single titanium silk figure, it can be seen that one layer is deposited on titanium silk
Spherical sample；Fig. 2 (c) is it can be seen that the sample deposited on titanium silk is the relatively uniform flower-like microsphere of size and shape, averagely directly
Diameter is about 2 μm.Fig. 2 (d) shows that bouquet is wound by many laminated structures.
Photocatalysis performance test: the bismuthyl carbonate bouquet Bi for taking the titanium wire network prepared to load2O2CO3/ Ti 0.02g(is
Deduct titanium wire network quality itself) it is added in the photo catalysis reactor equipped with the rhodamine B solution that 50mL concentration is 15mg/L, it burns
As in reactor, opening is condensed back to flowing water and guarantees that the temperature of solution is constant cup, keeps solution concentration uniform with magnetic agitation.First
Being protected from light stirring makes adsorption equilibrium in 60 minutes, then (xenon lamp adds optical filter, the filters ultraviolet light) irradiation light under 500W visible light source
Degradation 2 hours, takes 5mL reaction solution, takes supernatant to carry out absorption spectrum scanning after centrifugation, obtains maximum absorption wavelength 554nm
The absorbance at place, to calculate the degradation efficiency after reaction.
Through detecting, Bi2O2CO3The degradation efficiency of/Ti sample is 93%.
Embodiment 2
The present embodiment provides a kind of titanium wire networks to load three-dimensional bismuthyl carbonate bouquet (Bi2O2CO3/ Ti).It is prepared via a method which
It arrives:
The urea of the bismuth citrate of 1.5mmol and 12mmol is dissolved in 60mL deionized water under stiring and forms solution, finally
This solution is transferred in the stainless steel cauldron that 100mL liner is polytetrafluoroethylene (PTFE).The titanium wire network of a piece of 4*2cm is leant against
Inner liner of reaction kettle wall surface, is placed in drying box, hydro-thermal reaction 8 hours at 160 DEG C.Then cooled to room temperature, by titanium silk
Net deionized water and dehydrated alcohol rinse three times respectively, and are dried in vacuo 12 hours in 60 DEG C and obtain product.
Product is the relatively uniform flower-like microsphere of size and shape, and average diameter is about 2.5 μm.Through detecting, Bi2O2CO3/
The degradation efficiency of Ti sample is 87%.
Embodiment 3
The present embodiment provides a kind of titanium wire networks to load three-dimensional bismuthyl carbonate bouquet (Bi2O2CO3/ Ti).It is prepared via a method which
It arrives:
The urea of the bismuth citrate of 2mmol and 18mmol is dissolved in 60mL deionized water under stiring and forms solution, finally will
This solution is transferred in the stainless steel cauldron that 100mL liner is polytetrafluoroethylene (PTFE).The titanium wire network of a piece of 4*2cm is leant against instead
Kettle liner wall surface is answered, is placed in drying box, hydro-thermal reaction 6 hours at 180 DEG C.Then cooled to room temperature, by titanium wire network
It is rinsed respectively three times with deionized water and dehydrated alcohol, and is dried in vacuo in 60 DEG C and obtains within 12 hours the three-dimensional carbonic acid of titanium wire network load
Oxygen bismuth bouquet.
Product is the relatively uniform flower-like microsphere of size and shape, and average diameter is about 2.8 μm.Through detecting, Bi2O2CO3/
The degradation efficiency of Ti sample is 85%.
Embodiment 4
The present embodiment provides a kind of titanium wire networks to load three-dimensional bismuthyl carbonate bouquet.In preparation method, bismuth citrate additional amount is removed
For 3mmol, urea additional amount is 18mmol, and deionized water additional amount is outside 60mL, remaining operation and condition with embodiment 1 one
It causes.
The size and shape that gained titanium wire network loads three-dimensional bismuthyl carbonate bouquet is quite uniform, through detecting, titanium wire network load
The degradation efficiency of three-dimensional bismuthyl carbonate bouquet sample is close with embodiment 1.
Embodiment 5
The present embodiment provides a kind of titanium wire networks to load three-dimensional bismuthyl carbonate bouquet.In preparation method, bismuth citrate additional amount is removed
For 1mmol, urea additional amount is 10mmol, and deionized water additional amount is outside 50mL, remaining operation and condition with embodiment 1 one
It causes.
The size and shape that gained titanium wire network loads three-dimensional bismuthyl carbonate bouquet is quite uniform, through detecting, titanium wire network load
The degradation efficiency of three-dimensional bismuthyl carbonate bouquet sample is close with embodiment 1
Comparative example 1
This comparative example provides a kind of titanium sheet load bismuthyl carbonate.In preparation method, in addition to titanium wire network changes titanium sheet into, remaining operation
It is consistent with embodiment 1 with condition.
The titanium sheet load bismuthyl carbonate of this comparative example preparation is nanometer sheet pattern.Through detecting, titanium sheet load bismuthyl carbonate is received
The degradation efficiency of rice piece sample is 71%.
Comparative example 2
This comparative example provides a kind of titanium wire network load bismuthyl carbonate.In preparation method, except bismuth citrate changes bismuth chloride, urea into
It changes into outside sodium carbonate, remaining operation and condition are consistent with embodiment 1.
This comparative example is after the reaction was completed on titanium wire network almost without required bismuthyl carbonate sample, this may be because when with
Upper bismuth source and carbon source have just had precipitating when mixing, therefore bismuthyl carbonate is difficult to grow on titanium wire network.Such as use other bismuth sources
Such as bismuth nitrate, other carbon sources such as sodium carbonate, ammonium carbonate etc. are reacted as raw material, unattached shape on the titanium wire network after reaction
The stable bismuthyl carbonate bouquet of looks.
Those of ordinary skill in the art will understand that embodiment here be to help reader understand it is of the invention
Principle, it should be understood that protection scope of the present invention is not limited to such specific embodiments and embodiments.This field it is common
Technical staff disclosed the technical disclosures can make the various various other tools for not departing from essence of the invention according to the present invention
Body variations and combinations, these variations and combinations are still within the scope of the present invention.
Claims (8)
1. the preparation method that a kind of titanium wire network loads three-dimensional bismuthyl carbonate bouquet, which comprises the steps of:
S1: bismuth citrate and urea are dissolved into obtain mixed solution；The molar ratio of the bismuth citrate and urea is 6:1 ~ 10:1；
S2: titanium wire network is added in mixed solution described in S1, under closed environment at 160 ~ 180 DEG C 5 ~ 8h of hydro-thermal reaction,
Titanium wire network is taken out after cooling and is rinsed, titanium wire network is dried to obtain and loads three-dimensional bismuthyl carbonate bouquet.
2. institute's titanium wire network loads the preparation method of three-dimensional bismuthyl carbonate bouquet according to claim 1, which is characterized in that described in S1
Bismuth concentration is 0.02 ~ 0.05mol/L in mixed solution.
3. titanium wire network loads the preparation method of three-dimensional bismuthyl carbonate bouquet according to claim 1, which is characterized in that institute in S1
The molar ratio for stating bismuth citrate and urea is 20:3.
4. titanium wire network loads the preparation method of three-dimensional bismuthyl carbonate bouquet according to claim 1, which is characterized in that institute in S2
The temperature for stating hydro-thermal reaction is 160 DEG C, time 5h.
5. titanium wire network loads the preparation method of three-dimensional bismuthyl carbonate bouquet according to claim 1, which is characterized in that institute in S2
The reagent for stating rinse cycle selection is deionized water and dehydrated alcohol.
6. titanium wire network loads the preparation method of three-dimensional bismuthyl carbonate bouquet according to claim 1, which is characterized in that institute in S2
State dry process are as follows: be dried under 60 ~ 80 DEG C of vacuum environment.
7. a kind of titanium wire network loads three-dimensional bismuthyl carbonate bouquet, which is characterized in that pass through any preparation side of claim 1 ~ 6
Method obtains.
8. titanium wire network described in claim 7 loads three-dimensional bismuthyl carbonate bouquet in the application of photoelectric Material Field.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527420A (en) * | 2012-02-17 | 2012-07-04 | 重庆工商大学 | Bismuth subcarbonate photocatalyst and preparation method thereof |
| CN102895963A (en) * | 2012-09-14 | 2013-01-30 | 浙江大学 | Method of loading titanium dioxide nanorod arrays on surface of titanium wire mesh |
| CN104014332A (en) * | 2014-06-10 | 2014-09-03 | 上海大学 | Preparation method for Mn-Ce-W compound oxide integral type denitration catalyst based on titanium wire net |
| CN104923211A (en) * | 2015-05-20 | 2015-09-23 | 中国科学院地球环境研究所 | Bi2O3/(BiO)2CO3 heterojunction catalyst with visible photocatalytic activity and preparation method for Bi2O3/(BiO)2CO3 heterojunction catalyst |
| CN107029770A (en) * | 2017-04-27 | 2017-08-11 | 中南大学 | A kind of preparation method of metastable phase bismuth oxide and its application in photocatalysis degradation organic contaminant |
-
2018
- 2018-10-19 CN CN201811223009.3A patent/CN109317174A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527420A (en) * | 2012-02-17 | 2012-07-04 | 重庆工商大学 | Bismuth subcarbonate photocatalyst and preparation method thereof |
| CN102895963A (en) * | 2012-09-14 | 2013-01-30 | 浙江大学 | Method of loading titanium dioxide nanorod arrays on surface of titanium wire mesh |
| CN104014332A (en) * | 2014-06-10 | 2014-09-03 | 上海大学 | Preparation method for Mn-Ce-W compound oxide integral type denitration catalyst based on titanium wire net |
| CN104923211A (en) * | 2015-05-20 | 2015-09-23 | 中国科学院地球环境研究所 | Bi2O3/(BiO)2CO3 heterojunction catalyst with visible photocatalytic activity and preparation method for Bi2O3/(BiO)2CO3 heterojunction catalyst |
| CN107029770A (en) * | 2017-04-27 | 2017-08-11 | 中南大学 | A kind of preparation method of metastable phase bismuth oxide and its application in photocatalysis degradation organic contaminant |
Non-Patent Citations (3)
| Title |
|---|
| DONG FAN ET.AL: "Growth mechanism and photocatalytic activity of self-organized N-doped (BiO)(2)CO3 hierarchical nanosheet microspheres from bismuth citrate and urea", 《DALTON TRANSACTIONS》 * |
| SUQIN LIU ET.AL: "The effects of citrate ion on morphology and photocatalytic activity of flower-like Bi2O2CO3", 《CERAMICS INTERNATIONAL》 * |
| YANFENGLU ET.AL: "Oxygen vacancy engineering of Bi2O3/Bi2O2CO3 heterojunctions: Implications of the interfacial charge transfer, NO adsorption and removal", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
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