CN106000378A - Preparation method of C nano-material doped titanium dioxide nanorod catalyst - Google Patents
Preparation method of C nano-material doped titanium dioxide nanorod catalyst Download PDFInfo
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- CN106000378A CN106000378A CN201610362270.6A CN201610362270A CN106000378A CN 106000378 A CN106000378 A CN 106000378A CN 201610362270 A CN201610362270 A CN 201610362270A CN 106000378 A CN106000378 A CN 106000378A
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- Prior art keywords
- nano
- titanium dioxide
- material doped
- doped titanium
- preparation
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 39
- 239000002073 nanorod Substances 0.000 title claims abstract description 33
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 30
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229950000845 politef Drugs 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000975 dye Substances 0.000 abstract description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract 3
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 description 5
- 235000001727 glucose Nutrition 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 150000002304 glucoses Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000926 separation method 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of a C nano-material doped titanium dioxide nanorod catalyst. The preparation method is characterized in that titanium dioxide nanorods and a C nano-material are prepared at first, and then a reflux condensation method is adopted to finish preparation of doping the C nano-material into the titanium dioxide nanorods. In the preparation process, different volume fractions of C in the titanium dioxide nanorods are controlled to ensure that a doped photocatalytic material can respond to visible light, excellent photocatalytic performance is achieved in comparison with conventional titanium dioxide, the C nano-material doped titanium dioxide nanorod catalyst can serve as a photocatalytic material under visible light and enable an organic dyestuff to be completely degraded within 2 h, and has a very good application prospect in the field of photocatalytic treatment of organic pollutants.
Description
Technical field
The present invention relates to photocatalyst material technology, particularly to C nano material doped titanium dioxide nano-rod method for preparing catalyst.
Background technology
Quasiconductor TiO2Catalysis material is studied widely because it has higher photocatalytic activity and avirulence, but pure TiO2Material energy gap is relatively big, only could produce electron-hole pair under ultraviolet excitation, and then carry out photocatalytic degradation reaction, thus be restricted in actual applications.It addition, use ion doping can effectively solve TiO2Problem with gap length such that it is able to by excited by visible light, improve the utilization rate to visible ray.
Metal-doped, nonmetal doping and element codope are existing to use more means under study for action, at TiO2Some metal ions of middle doping or nonmetallic ion, cause TiO2Absorption band generation red shift, therefore can make full use of sunlight, thus improve pure TiO2The defect not enough to sunlight utilization rate.The doping of nonmetalloid can improve the photocatalysis efficiency of titanium dioxide.C doping can reduce TiO2Energy gap, thus improve its photocatalysis performance.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of C nano material doped titanium dioxide nano-rod catalyst, improve the utilization rate to visible ray, improve the pure titinium dioxide defect to sunlight utilization rate deficiency, improve the photocatalysis performance of titanium dioxide.
The present invention realizes above-mentioned purpose by the following technical solutions.C nano material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that comprise the steps:
1) preparation of titanium dioxide nano-rod:
Titanium dioxide is evenly spread in sodium hydrate aqueous solution, above-mentioned aqueous solution is transferred in autoclave, and puts into drying baker, at 120 DEG C, heat 24 h；Take out autoclave and be cooled to room temperature；It is centrifugally separating to obtain white precipitate, clean through deionized water, and in the high speed centrifuge that rotating speed is 10000 r/min, it is centrifuged 5 min, to obtain transferring in autoclave after moist product is scattered in deionized water, place into and drying baker heats at 200 DEG C 24 h, take out autoclave and naturally cool to room temperature；Finally it is centrifuged separating and with deionized water rinsing, the most available through 60 DEG C of vacuum drying；
2) preparation of C nano material:
Weigh glucose with sodium hydroxide in beaker, in beaker, add deionized water and a little magneton, magnetic stirring apparatus stirs；The clear solution obtained all is poured in stainless steel cauldron, tightening stainless steel cauldron to be placed in electric drying oven with forced convection, drying baker temperature is arranged on 100-200 DEG C, reacted 4 ~ 5 h, take out and be cooled to room temperature, making clear solution become tan liquid；By the brown liquid of acquisition centrifugal 10-30 min in the high speed centrifuge that rotating speed is 10000 r/min, removing insoluble particles big in reactant liquor, gained supernatant is carbon nanomaterial solution；
3) preparation of the material doped titanium dioxide nano-rod of C nano:
Add distilled water and C nano material to titanium dioxide nano-rod, 60 DEG C of water-baths with condensing unit are reacted 24 h, then in rotating speed is 10000 r/min high speed centrifuges after centrifugal 5 min, is dried at 60 DEG C of vacuum drying ovens, complete preparation.
Preferably, described autoclave is 100 mL teflon-lined rustless steel autoclaves.
Preferably, described white precipitate is TiO 2 precursor.
Preferably, the pH value that in described step 1), deionized water cleans is 10.5.
Preferably, described step 2) in weigh the ratio of glucose and sodium hydroxide be 10 1.
Preferably, described step 2) in add deionized water be 10-30 mL.
Preferably, described stainless steel cauldron is 50 mL politef stainless steel cauldrons.
Preferably, described step 2) in brown liquid it be also possible to use the membrane filtration that aperture is 0.22 m.
Preferably, the rotating speed of described little magneton is 450-500 r/min.
Beneficial effects of the present invention :The present invention passes through hydro-thermal reaction method, prepares titanium dioxide nano-rod catalyst and C nano material.In preparation process, by controlling the ratio of the different volumes of C in titanium dioxide nano-rod, after doping, catalysis material can have response to visible ray, more existing titanium dioxide has the photocatalysis performance of excellence, can be as photocatalyst material under visible ray, degradation of organic dyes can be made in 2 h complete, in photocatalysis treatment organic pollution field, there is good application prospect under the effect of visible ray.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1 :One better embodiment of the present invention, C nano material doped titanium dioxide nano-rod method for preparing catalyst, the steps include:
1) preparation of titanium dioxide nano-rod:
By 2 g P25Evenly spread in the sodium hydrate aqueous solution of 10 M of 80 mL；Above-mentioned solution is transferred in 100 mL teflon-lined rustless steel autoclaves, and put it in drying baker, at 120 DEG C, heat 24 h；Take out autoclave and be cooled to room temperature；Be performing centrifugal separation on obtaining white precipitate TiO 2 precursor, and with deionized water clean to pH be 10.5；Product centrifugal 5 min in the high speed centrifuge that rotating speed is 10000 r/min that will obtain again, moist product 1 g will be obtained be scattered in 40 mL deionized waters, it is then transferred in 50 mL teflon-lined rustless steel autoclaves, and put in drying baker, at 200 DEG C, heat 24 h；Take out autoclave and also naturally cool to room temperature, centrifugation with deionized water rinsing, i.e. can get titanium dioxide nano-rod through 60 DEG C of vacuum drying.
2) preparation of C nano material:
Weigh 1.0 g glucoses and 0.1 g sodium hydroxide in the beaker of 250 mL.In beaker, add 15 mL deionized waters and the little magneton that rotating speed is 450-500 r/min stirs 10 min on magnetic stirring apparatus.The clear solution obtained all is poured in the politef stainless steel cauldron of 30 mL, tighten stainless steel cauldron.The stainless steel cauldron that will be equipped with reactant liquor is placed in electric drying oven with forced convection, drying baker temperature is set to 160 DEG C, after reacted 4 h, take out stainless steel cauldron and be cooled to room temperature, treat that clear solution becomes tan liquid, the brown liquid of acquisition is centrifuged in the high speed centrifuge that rotating speed is 10000 r/min 10-30 min or the membrane filtration using aperture to be 0.22 m again, removes insoluble particles big in reactant liquor.Gained supernatant is C nano material solution.
3) C(carbon) nano material doping titanium dioxide nano rod preparation:
Take 0.5 g titanium dioxide (TiO2) nanometer rods is added thereto to 19 mL distilled water and 1 mL
C nano material.In 60 DEG C of water-baths with condensing unit, react 24 h, in rotating speed is 10000 r/min high speed centrifuges after centrifugal 5 min, is dried through 60 DEG C of vacuum drying ovens, obtains C nano material doped titanium dioxide nano-rod catalyst.
Embodiment 2 :Another better embodiment of the present invention, C nano material doped titanium dioxide nano-rod method for preparing catalyst, its step 1) is same as in Example 1；Step 2) in brown liquid use aperture to be the membrane filtration of 0.22 m.Other are same as in Example 1.
Step 3) takes 0.5 g titanium dioxide (TiO2) rod is added thereto to 19 mL distilled water and 2 mL
C nano material.In 60 DEG C of water-baths with condensing unit, react 24 h, in rotating speed is 10000 r/min high speed centrifuges after centrifugal 5 min, is dried through 60 DEG C of vacuum drying ovens, obtains C nano material doped titanium dioxide nano-rod catalyst.
Embodiment 3 :Another better embodiment of the present invention, C nano material doped titanium dioxide nano-rod method for preparing catalyst, its step 1) and step 2) same as in Example 1.The C nano material added in step 3) is 3 mL, and other are identical.
Embodiment 4 :Another better embodiment of the present invention, C nano material doped titanium dioxide nano-rod method for preparing catalyst, its step 1) and step 2) same as in Example 1.The C nano material added in step 3) is 4 mL, and other are identical.
Claims (9)
1.C nano material doping titanium dioxide nano rod method for preparing catalyst, it is characterised in that comprise the steps:
1) preparation of titanium dioxide nano-rod:
Titanium dioxide is evenly spread in sodium hydrate aqueous solution, above-mentioned aqueous solution is transferred in autoclave, and puts into drying baker, at 120 DEG C, heat 24 h；Take out autoclave and be cooled to room temperature；It is centrifugally separating to obtain white precipitate, clean through deionized water, and in the high speed centrifuge that rotating speed is 10000 r/min, it is centrifuged 5 min, to obtain transferring in autoclave after moist product is scattered in deionized water, place into and drying baker heats at 200 DEG C 24 h, take out autoclave and naturally cool to room temperature；Finally it is centrifuged separating and with deionized water rinsing, the most available through 60 DEG C of vacuum drying；
2) preparation of C nano material:
Weigh glucose with sodium hydroxide in beaker, in beaker, add deionized water and a little magneton, magnetic stirring apparatus stirs；The clear solution obtained all is poured in stainless steel cauldron, tightening stainless steel cauldron to be placed in electric drying oven with forced convection, drying baker temperature is arranged on 100-200 DEG C, reacted 4 ~ 5h, take out and be cooled to room temperature, making clear solution become tan liquid；By the brown liquid of acquisition centrifugal 10-30 min in the high speed centrifuge that rotating speed is 10000 r/min, removing insoluble particles big in reactant liquor, gained supernatant is carbon nanomaterial solution；
3) preparation of the material doped titanium dioxide nano-rod of C nano:
Add distilled water and C nano material to titanium dioxide nano-rod, 60 DEG C of water-baths with condensing unit are reacted 24 h, then in rotating speed is 10000 r/min high speed centrifuges after centrifugal 5 min, 60
DEG C vacuum drying oven is dried, and completes preparation.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that described autoclave is 100 mL teflon-lined rustless steel autoclaves.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that described white precipitate is TiO 2 precursor.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that the pH value that in described step 1), deionized water cleans is 10.5.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that described step 2) in weigh the ratio of glucose and sodium hydroxide be 10 1.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that described step 2) in add deionized water be 10-30 mL.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that described stainless steel cauldron is 50 mL politef stainless steel cauldrons.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that described step 2) in brown liquid it be also possible to use the membrane filtration that aperture is 0.22 m.
C nano the most according to claim 1 material doped titanium dioxide nano-rod method for preparing catalyst, it is characterised in that the rotating speed of described little magneton is 450-500 r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610362270.6A CN106000378A (en) | 2016-05-30 | 2016-05-30 | Preparation method of C nano-material doped titanium dioxide nanorod catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610362270.6A CN106000378A (en) | 2016-05-30 | 2016-05-30 | Preparation method of C nano-material doped titanium dioxide nanorod catalyst |
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| CN106000378A true CN106000378A (en) | 2016-10-12 |
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| CN201610362270.6A Pending CN106000378A (en) | 2016-05-30 | 2016-05-30 | Preparation method of C nano-material doped titanium dioxide nanorod catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111097400A (en) * | 2019-12-30 | 2020-05-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of C-doped titanium dioxide nanobelt |
| CN114749198A (en) * | 2021-12-27 | 2022-07-15 | 西北民族大学 | Nano C-TiO2NBSMethod for preparing photocatalyst |
-
2016
- 2016-05-30 CN CN201610362270.6A patent/CN106000378A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111097400A (en) * | 2019-12-30 | 2020-05-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of C-doped titanium dioxide nanobelt |
| CN114749198A (en) * | 2021-12-27 | 2022-07-15 | 西北民族大学 | Nano C-TiO2NBSMethod for preparing photocatalyst |
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Application publication date: 20161012 |