CN110270363A - A kind of preparation method and application of Li, C, N ternary codoping titanium dioxide nano material - Google Patents
A kind of preparation method and application of Li, C, N ternary codoping titanium dioxide nano material Download PDFInfo
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- CN110270363A CN110270363A CN201910604660.3A CN201910604660A CN110270363A CN 110270363 A CN110270363 A CN 110270363A CN 201910604660 A CN201910604660 A CN 201910604660A CN 110270363 A CN110270363 A CN 110270363A
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- titanium dioxide
- ternary
- nano material
- dioxide nano
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 36
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 29
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002071 nanotube Substances 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 15
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003911 water pollution 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a kind of preparation method and applications of Li, C, N ternary codoping titanium dioxide nano material, and steps are as follows: (1) by lithium nitrate and urea co-dissolve in dehydrated alcohol, nanotube TiO is added2, magnetic agitation mixing until dehydrated alcohol volatilize completely, obtain mixture；(2) mixture in step (1) is placed in crucible, calcining at constant temperature under inert gas obtains ternary codoping titanium dioxide nano material.The present invention uses nanotube TiO2For presoma, one-step method is the titanium dioxide nano material that Li, C, N ternary codope is prepared, simple process, it is easy industrialization, significantly during presoma crystal structure and pattern change while realizing ternary codope, doped chemical can be evenly distributed in titanium dioxide matrix, to obtain the titanic oxide material of fine structure, function admirable.
Description
Technical field
The present invention relates to nano material preparation and catalysis technical fields, and in particular to a kind of Li, C, N ternary codope dioxy
Change the preparation method and application of titanium nano material.
Background technique
TiO2Belong to wide bandgap semiconductor, under ultraviolet lighting, TiO2It can be with harmful in photo-catalyst, effectively degradation air
Micro organic pollutant in gas, removal water pollution.In order to utilize a large amount of visible light in solar spectrum, to TiO2It carries out
Doping is a kind of extensive method [Feng C, Wang Y, Zhang J, Yu L, Li D, Yang J, et al. of report
The effect of infrared light on visible light photocatalytic activity: An
intensive contrast between Pt-doped TiO2 and N-doped TiO2. Appl Catal B
Environ. 2012;113-114:61-71.].Zhuan Weibin etc. by then carrying out electric heating sintering in copper surface depositing colloidal,
The excellent N doping TiO of processability2Powder [is participated in: Zhuan Weibin, Liu Yue, Li Heliang, Wu Bo, a kind of N doping TiO2The preparation of powder
Method, CN107670681A].Pan Xiaoyang etc. uses sol-gal process, is prepared into using carbonitride as template, carbon source and nitrogen source
To a kind of N doping TiO-C material, for nitro reducing catalyst [referring to Pan Xiaoyang, Long Peiqing, Yi Zhiguo, a kind of N doping
TiO-C material, preparation method and application, CN107983384A].Above method can make TiO2The light abstraction width of material
It is expanded from ultraviolet light to visible light, while showing the activity of apparent catalyzing and degrading pollutant by visible light.But the above method is equal
One or two kinds of element dopings are only realized, and there are problems that metal-doped to be uniformly distributed.Most as ionic radius
Small Li ion, it is relatively easy to adulterate；It introduces nonmetallic C, N doping simultaneously again, needs a kind of relatively brilliant preparation method.
Summary of the invention
The invention proposes a kind of preparation method and applications of Li, C, N ternary codoping titanium dioxide nano material, pass through
Disperse dopant in situ in nanotube titanium dioxide surfaces externally and internally, then carry out high-temperature calcination, is prepared a kind of with visible
The titanium dioxide nano material of Li, C, N codope of photoresponse.
Realize the technical scheme is that
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
(1) by lithium nitrate and urea co-dissolve in dehydrated alcohol, nanotube TiO is added2, magnetic agitation mixing is until anhydrous
Ethyl alcohol volatilizees completely, obtains mixture；
(2) mixture in step (1) is placed in crucible, calcining at constant temperature under inert gas obtains ternary codope titanium dioxide
Nano material.
Nanotube TiO in the step (1)2The preparation method comprises the following steps: by TiO2Polytetrafluoroethyl-ne alkene reaction is mixed in aqueous slkali
In device, magnetic agitation reaction is filtered, washed to neutrality, is dried to obtain nanotube TiO2。
Aqueous slkali is concentration 8-20molL-1NaOH solution, magnetic agitation temperature be 100-150 DEG C, time 20-
30h。
Lithium nitrate and nanotube TiO in the step (1)2Mass ratio be (0.06-0.6): 1.
Calcination temperature is 300-700 DEG C in the step (2), calcination time 1-6h.
Application of the ternary codoping titanium dioxide nano material of preparation in visible light photocatalytic degradation.
The beneficial effects of the present invention are: the present invention uses nanotube TiO2For presoma, one-step method be prepared Li, C,
The titanium dioxide nano material of N ternary codope, simple process are easy industrialization, significantly in presoma crystal knot
During structure and pattern change while realizing ternary codope, doped chemical can be distributed in titanium dioxide matrix
It is even, to obtain the titanic oxide material of fine structure, function admirable.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is 1 nanotube TiO of the embodiment of the present invention2Electron microscope.
Fig. 2 is 1 nanotube TiO of the embodiment of the present invention2XRD diagram.
Fig. 3 is the XRD diagram of Li, C, N ternary codoping titanium dioxide nano material prepared by the embodiment of the present invention 4.
Fig. 4 is the electron microscope of ternary codoping titanium dioxide nano material prepared by embodiment 4.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
(1) 100 mL are measured-1 10mol·L-1NaOH solution and TiO2It is mixed in polytetrafluoroethylene (PTFE) reactor, controls temperature
120 degree magnetic agitation 25 hours, filtered after cooled to room temperature, washing to pH be neutrality, drying nanotube is prepared
TiO2。
(2) 0.5g lithium nitrate and 1g urea co-dissolve are weighed in dehydrated alcohol, 5g nanotube TiO is then added2, magnetic force
It is uniformly mixed, until dehydrated alcohol all volatilizees.
(3) mixture obtained in step (2) is placed in crucible, calcined 2 hours for 300 degree under inert gas protection, from
It is so cooled to room temperature, that is, Li, C, N codoping titanium dioxide nano material is prepared.
Fig. 1 is preparation-obtained nanotube TiO in step (1)2Electron microscope.It can be seen that material prepared one
Tie up nanotube-shaped, caliber is about 6nm, and pipe range is up to hundreds of nanometers.The tubular structure makes nanotube TiO2Large specific surface area, it is interior
Outer wall can adsorb lithium nitrate and urea.
Fig. 2 is preparation-obtained nanotube TiO in step (1)2XRD diagram.9oThere is apparent nanotube TiO2's
Characteristic diffraction peak belongs to rhombic system.
Embodiment 2
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination temperature in step (3) is 400 degree.
Embodiment 3
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination temperature in step (3) is 500 degree.
Embodiment 4
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination temperature in step (3) is 600 degree.
Fig. 3 is the XRD diagram of preparation-obtained Li, C, N ternary the codoping titanium dioxide nano material of embodiment 4.By
High-temperature calcination, nanotube TiO2Orthorhombic structure change, the crystal structure of material prepared is with anatase TiO2For
It is main.18o、33oThere is the diffraction maximum of Li salt, illustrates that Li ion is scattered in Li, C, N ternary codope titanium dioxide well and receives
In rice material.
Fig. 4 is the electron microscope of preparation-obtained Li, C, N ternary the codoping titanium dioxide nano material of embodiment 4, can be with
See nanotubes TiO2Pattern from tubulose variation be nano particle, 30 ~ 50nm of particle size.
Embodiment 5
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination temperature in step (3) is 700 degree.
Embodiment 6
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination time in step (3) is 3 hours.
Embodiment 7
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination time in step (3) is 4 hours.
Embodiment 8
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination time in step (3) is 5 hours.
Embodiment 9
A kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, steps are as follows:
Difference from example 1 is that: the calcination time in step (3) is 6 hours.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of Li, C, N ternary codoping titanium dioxide nano material, it is characterised in that steps are as follows:
(1) by lithium nitrate and urea co-dissolve in dehydrated alcohol, nanotube TiO is added2, magnetic agitation mixing, mixed
Object；
(2) mixture in step (1) is placed in crucible, calcining at constant temperature under inert gas obtains ternary codope titanium dioxide
Nano material.
2. the preparation method of Li, C, N ternary codoping titanium dioxide nano material according to claim 1, feature exist
In nanotube TiO in the step (1)2The preparation method comprises the following steps: by TiO2It is mixed in polytetrafluoroethylene (PTFE) reactor with aqueous slkali,
Magnetic agitation reaction, is filtered, washed to neutrality, is dried to obtain nanotube TiO2。
3. the preparation method of Li, C, N ternary codoping titanium dioxide nano material according to claim 2, feature exist
In: the aqueous slkali is concentration 8-20molL-1NaOH solution, magnetic agitation temperature be 100-150 DEG C, time 20-
30h。
4. the preparation method of Li, C, N ternary codoping titanium dioxide nano material according to claim 1, feature exist
In: lithium nitrate and nanotube TiO in the step (1)2Mass ratio be (0.06-0.6): 1.
5. the preparation method of Li, C, N ternary codoping titanium dioxide nano material according to claim 1, feature exist
In: calcination temperature is 300-700 DEG C in the step (2), calcination time 1-6h.
6. ternary codoping titanium dioxide nano material the answering in visible light photocatalytic degradation of any one of claim 1-6 preparation
With.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444724A (en) * | 2008-12-24 | 2009-06-03 | 南开大学 | Method for preparing high activity non-metallic ion co-doped titanium dioxide photochemical catalyst |
| US20120308630A1 (en) * | 2011-05-04 | 2012-12-06 | Averett Steward B | Titanium dioxide photocatalytic compositions and uses thereof |
| CN103861631A (en) * | 2014-03-12 | 2014-06-18 | 北京理工大学 | Preparation method of nitrogen-doped titanium dioxide nanoribbon visible light photocatalyst |
| CN108275719A (en) * | 2018-01-30 | 2018-07-13 | 北京工业大学 | A kind of TiO that Phase Proportion is controllable2The preparation and application of heterojunction material |
-
2019
- 2019-07-05 CN CN201910604660.3A patent/CN110270363A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444724A (en) * | 2008-12-24 | 2009-06-03 | 南开大学 | Method for preparing high activity non-metallic ion co-doped titanium dioxide photochemical catalyst |
| US20120308630A1 (en) * | 2011-05-04 | 2012-12-06 | Averett Steward B | Titanium dioxide photocatalytic compositions and uses thereof |
| CN103861631A (en) * | 2014-03-12 | 2014-06-18 | 北京理工大学 | Preparation method of nitrogen-doped titanium dioxide nanoribbon visible light photocatalyst |
| CN108275719A (en) * | 2018-01-30 | 2018-07-13 | 北京工业大学 | A kind of TiO that Phase Proportion is controllable2The preparation and application of heterojunction material |
Non-Patent Citations (2)
| Title |
|---|
| CHUNCHENG CHEN ET AL.: "Photocatalytic Degradation of Organic Pollutants by Co-Doped TiO2 Under Visible Light Irradiation", 《CURRENT ORGANIC CHEMISTRY》 * |
| 石海洋 等: "金属修饰Ｎ掺杂TiO2的制备及其光催化性能研究", 《化工新型材料》 * |
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