CN107519902A - The preparation method of chlorine doped titanium dioxide photocatalyst - Google Patents
The preparation method of chlorine doped titanium dioxide photocatalyst Download PDFInfo
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- CN107519902A CN107519902A CN201610459116.0A CN201610459116A CN107519902A CN 107519902 A CN107519902 A CN 107519902A CN 201610459116 A CN201610459116 A CN 201610459116A CN 107519902 A CN107519902 A CN 107519902A
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- China
- Prior art keywords
- titanium dioxide
- preparation
- milling
- doped titanium
- dioxide photocatalyst
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 26
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000000460 chlorine Substances 0.000 title claims abstract description 21
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 238000001238 wet grinding Methods 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 4
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 abstract description 22
- 229960003405 ciprofloxacin Drugs 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000012798 spherical particle Substances 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 5
- 239000000178 monomer Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000012698 light-induced step-growth polymerization Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- -1 trihydroxy methyl Chemical group 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- 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
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- 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)
- Catalysts (AREA)
Abstract
This application discloses a kind of preparation method of chlorine doped titanium dioxide photocatalyst, including step：(1), titania powder, sodium chloride and absolute ethyl alcohol are mixed and carry out ball milling, obtains wet-milling；The mass ratio of titania powder and sodium chloride is (2.6~3):1.(2), wet-milling is dried, then calcined 5~7 hours under the conditions of 600~800 DEG C.The titanium dioxide crystal spherical particle size that the present invention is obtained is uniform.The titanium dioxide of chlorine doping reaches more than 87% to the degradation rate of Ciprofloxacin waste water.
Description
Technical field
The application belongs to technical field of waste water processing, more particularly to a kind of preparation of chlorine doped titanium dioxide photocatalyst
Method.
Background technology
Cadmium selenide is the direct band-gap semicondictor material that energy gap is 1.7eV, has cubic zinc blende and six side's fibre zinc
It two kinds of crystal structures of ore deposit, wherein cube phase structure is metastable state, can be only present in lower temperature, be changed into hexagonal phase knot during high temperature
Structure.Cadmium selenide at normal temperatures can simultaneously exist cube and six sides, two kinds of crystalline phases.Cadmium selenide nano-crystal is ground in semiconductor nano
Study carefully most extensively, the best a kind of II-VI group semiconductor nano of application prospect, because it has important optically nonlinearity
Matter, luminosity and other physicochemical characteristics and enjoy attracting attention for common people.As a kind of very important semi-conducting material,
Through in various light-emitting devices, laser and infrared detector, the neck such as infrared window and nonlinear optical material and light sensor
The wide application prospect of domain views.Particularly cadmium selenide can absorb visible ray well, thus it is photochemical catalyst
Preferred material.
Cadmium selenide easily photoetch, photostability is poor, and the light absorbs threshold value of titanium dioxide is confined to ultraviolet light and gone, sun profit
Low with rate, these deficiencies strongly limit the performance of their performances.
The content of the invention
It is an object of the invention to provide a kind of preparation method of chlorine doped titanium dioxide photocatalyst, to overcome existing skill
Deficiency in art.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of preparation method of chlorine doped titanium dioxide photocatalyst, including step：
(1), titania powder, sodium chloride and absolute ethyl alcohol are mixed and carry out ball milling, obtains wet-milling,；
The mass ratio of titania powder and sodium chloride is (2.6~3):1.
(2), wet-milling is dried, then calcined 5~7 hours under the conditions of 600~800 DEG C.
Preferably, in the preparation method of above-mentioned chlorine doped titanium dioxide photocatalyst, in step (1), ball radius 4
~6mm, ratio of grinding media to material are (7~10)：1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours.
Preferably, in the preparation method of above-mentioned chlorine doped titanium dioxide photocatalyst, in step (1), titanium dioxide
The mass ratio of powder and sodium chloride is (2.6~3):1
Preferably, in the preparation method of above-mentioned chlorine doped titanium dioxide photocatalyst, in step (2), drying temperature
For 50~60 DEG C, drying time 2~4 hours.
Compared with prior art, the advantage of the invention is that：The titanium dioxide crystal spheric granules chi that the present invention is obtained
It is very little uniform.The titanium dioxide of chlorine doping reaches more than 87% to the degradation rate of Ciprofloxacin waste water.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
Embodiment 1
The preparation method of chlorine doped titanium dioxide photocatalyst
(1), titania powder, sodium chloride and absolute ethyl alcohol are mixed and carry out ball milling, acquisition wet-milling, ball radius 4~
6mm, ratio of grinding media to material are (7~10)：1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours；
The mass ratio of titania powder and sodium chloride is 2.8:1.
(2), wet-milling is carried out to drying 2 hours at 60 DEG C, then calcined 5 hours under the conditions of 800 DEG C.
XRD and XPS shows titanium dioxide of the synthesized nano material for doping chlorine.The titanium dioxide obtained is brilliant
Body spherical particle size is uniform.
The titanium dioxide of chlorine doping reaches more than 87% to the degradation rate of Ciprofloxacin waste water.
(3), by Ciprofloxacin template molecule, acrylamide function monomer, azo-bis-isobutyl cyanide and the propylene of trihydroxy methyl three
Acid esters is dissolved in the mixed solution of methanol and water, is stirred, and obtains precursor solution；
The volume ratio of methanol and water is 8:3；
Ciprofloxacin template molecule, acrylamide, azo-bis-isobutyl cyanide, the mass ratio of tri methylol triacrylate are 1:
2:6:3。
(4), precursor solution is added in chlorine is titania-doped, under ultraviolet light light-induced polymerization 4 hours, mistake
Filter, wash and dry, obtain polymer；
(5) polymer, is subjected to surname extraction 48 hours with the mixed liquor of methanol and acetic acid, obtains optically catalytic TiO 2
Agent.
The volume ratio of methanol and acetic acid is 10：1.
XRD and XPS shows that success blot arrives in the hole of acrylamide function monomer and Ciprofloxacin template molecule
Titanium dioxide base material surface.
The catalyst reaches more than 73% to the degradation rate of Ciprofloxacin.
Embodiment 2
The preparation method of chlorine doped titanium dioxide photocatalyst
(1), titania powder, sodium chloride and absolute ethyl alcohol are mixed and carry out ball milling, acquisition wet-milling, ball radius 4~
6mm, ratio of grinding media to material are (7~10)：1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours；
The mass ratio of titania powder and sodium chloride is 2.8:1.
(2), wet-milling is carried out to drying 4 hours at 50 DEG C, then calcined 7 hours under the conditions of 600 DEG C.
(3), by Ciprofloxacin template molecule, acrylamide function monomer, azo-bis-isobutyl cyanide and the propylene of trihydroxy methyl three
Acid esters is dissolved in the mixed solution of methanol and water, is stirred, and obtains precursor solution；
The volume ratio of methanol and water is 7:3；
Ciprofloxacin template molecule, acrylamide, azo-bis-isobutyl cyanide, the mass ratio of tri methylol triacrylate are 1:
2:5:3。
(4), precursor solution is added in chlorine is titania-doped, under ultraviolet light light-induced polymerization 4 hours, mistake
Filter, wash and dry, obtain polymer；
(5) polymer, is subjected to surname extraction 48 hours with the mixed liquor of methanol and acetic acid, obtains optically catalytic TiO 2
Agent.
The volume ratio of methanol and acetic acid is 9：1.
XRD and XPS shows that success blot arrives in the hole of acrylamide function monomer and Ciprofloxacin template molecule
Titanium dioxide base material surface.
The catalyst reaches 75% to the degradation rate of Ciprofloxacin.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (4)
1. a kind of preparation method of chlorine doped titanium dioxide photocatalyst, it is characterised in that including step：
(1), titania powder, sodium chloride and absolute ethyl alcohol are mixed and carry out ball milling, obtains wet-milling,；
The mass ratio of titania powder and sodium chloride is (2.6~3):1.
(2), wet-milling is dried, then calcined 5~7 hours under the conditions of 600~800 DEG C.
2. the preparation method of chlorine doped titanium dioxide photocatalyst according to claim 1, it is characterised in that：Step (1)
In, 4~6mm of ball radius, ratio of grinding media to material is (7~10)：1,500~600 turns/min of rotational speed of ball-mill, Ball-milling Time 5~7 hours.
3. the preparation method of chlorine doped titanium dioxide photocatalyst according to claim 1, it is characterised in that：Step (1)
In, the mass ratio of titania powder and sodium chloride is (2.6~3):1 .
4. the preparation method of chlorine doped titanium dioxide photocatalyst according to claim 1, it is characterised in that：Step (2)
In, drying temperature is 50~60 DEG C, drying time 2~4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610459116.0A CN107519902A (en) | 2016-06-22 | 2016-06-22 | The preparation method of chlorine doped titanium dioxide photocatalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610459116.0A CN107519902A (en) | 2016-06-22 | 2016-06-22 | The preparation method of chlorine doped titanium dioxide photocatalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107519902A true CN107519902A (en) | 2017-12-29 |
Family
ID=60733737
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610459116.0A Withdrawn CN107519902A (en) | 2016-06-22 | 2016-06-22 | The preparation method of chlorine doped titanium dioxide photocatalyst |
Country Status (1)
| Country | Link |
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| CN (1) | CN107519902A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113003651A (en) * | 2021-03-17 | 2021-06-22 | 东北大学 | Method for catalytic degradation of thiocyanate radicals in wastewater by visible light |
| CN113184901A (en) * | 2021-04-22 | 2021-07-30 | 西安交通大学 | Chlorine-doped titanium dioxide/carbon porous structure and preparation method thereof |
| CN115970713A (en) * | 2023-01-31 | 2023-04-18 | 山西大学 | Grinding preparation method and application of halogen-doped metal oxide nanoenzyme |
-
2016
- 2016-06-22 CN CN201610459116.0A patent/CN107519902A/en not_active Withdrawn
Non-Patent Citations (1)
| Title |
|---|
| 刘馨琳: "镉/钛基纳米复合半导体材料的制备及其光催化性能研究", 《中国博士学位论文全文数据库 信息科技辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113003651A (en) * | 2021-03-17 | 2021-06-22 | 东北大学 | Method for catalytic degradation of thiocyanate radicals in wastewater by visible light |
| CN113003651B (en) * | 2021-03-17 | 2022-05-03 | 东北大学 | Method for catalytic degradation of thiocyanate radicals in wastewater by visible light |
| CN113184901A (en) * | 2021-04-22 | 2021-07-30 | 西安交通大学 | Chlorine-doped titanium dioxide/carbon porous structure and preparation method thereof |
| CN113184901B (en) * | 2021-04-22 | 2023-06-27 | 西安交通大学 | Chlorine doped titanium dioxide/carbon porous structure and preparation method thereof |
| CN115970713A (en) * | 2023-01-31 | 2023-04-18 | 山西大学 | Grinding preparation method and application of halogen-doped metal oxide nanoenzyme |
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Application publication date: 20171229 |