CN103130267A - Preparation method for visible-light response black titanium dioxide photocatalyst - Google Patents
Preparation method for visible-light response black titanium dioxide photocatalyst Download PDFInfo
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- CN103130267A CN103130267A CN2013100529839A CN201310052983A CN103130267A CN 103130267 A CN103130267 A CN 103130267A CN 2013100529839 A CN2013100529839 A CN 2013100529839A CN 201310052983 A CN201310052983 A CN 201310052983A CN 103130267 A CN103130267 A CN 103130267A
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Abstract
The invention discloses a preparation method for visible-light response black titanium dioxide photocatalyst. Glacial acetic acid and amide are adopted as solvents. Metal lithium salt is adopted as promoter. Titanium sheets are adopted as titanium sources. Ionic liquid is added as a structure-directing agent. A composition is achieved in one step by the adoption of a solvothermal method. The particle diameter of the prepared product is about 100 nm. Compared with other titanium dioxide, the visible-light response black titanium dioxide photocatalyst is black in color. The visible-light response black titanium dioxide photocatalyst displays good performance for degrading organic dyes under visible light. The preparation method for the visible-light response black titanium dioxide photocatalyst has the advantages that the chemical reagents which are used by the preparation method for the visible-light response black titanium dioxide photocatalyst are frequently-used reagents, low in price, easy to achieve, simple in method and technology, and capable of expanding anatase phase titanium dioxide to a visible-light response range. Meanwhile, the photocatalyst can degrade low-concentration dye wastewater under visible-light, and display the same high activity in a system of the low-concentration dye wastewater and phenolic substance.
Description
Technical field
The invention discloses a kind of preparation method of visible-light-responsive photocatalyst, be specially a kind of preparation method of visible light-responded black titanium dioxide photocatalyst.Synthesize and utilize one step of solvent-thermal method to make, the gained catalyzer has the premium properties of efficient degradation lower concentration organic dye, and degraded has better effects to phenols sewage.
Background technology
Along with the growth of demographic and economic, environment and energy problem become two large factors of restriction human development.Semiconductor light-catalyst has unique advantage in dye wastewater treatment using and photolysis water hydrogen.Compare with the conventional process waster water process, photochemical catalysis has the advantages such as reaction conditions gentleness, energy consumption be low, pollution-free, has very important application prospect aspect environment and the energy.More and more to the research of semiconductor light-catalyst, well-known in recent years, TiO
2Due to cheapness, nontoxic, the advantage such as stable is used photocatalyst widely.But Anatase TiO
2Energy gap is 3.2eV, and it only can absorb UV-light (account for sunlight 4%), and quantum yield is low, can not be used for the actual production dye wastewater treatment.But TiO
2Because himself color is white, do not possess visible light-responded ability, the utilising efficiency in natural light is lower.Exploitation visible-light response type TiO
2Become improve light utilization efficiency solve environmental pollution in the urgent need to.
Summary of the invention
The object of the invention is to for the existing defective of prior art and satisfying the market needs, provide a kind of titanium dioxide optical catalyst of black Detitanium-ore-type simple, the expensive low novel preparation method of productive rate.
Black octahedrite type titanium dioxide photocatalyst provided by the present invention, adopting glacial acetic acid and acid amides is solvent, the metal lithium salts is auxiliary agent, and use the titanium sheet to be the titanium source, add ionic liquid as structure directing agent, utilize the solvent-thermal method one-step synthesis, prepared product cut size is in about 100nm, is black than other its color of titanium dioxide.It demonstrates the performance of good degradating organic dye under visible light.
The gained catalyzer has the premium properties of efficient degradation lower concentration organic dye, and degraded has better effects to phenols sewage.
A kind of preparation method of visible light-responded black titanium dioxide photocatalyst comprises the steps:
1) be transferred in 50mL tetrafluoroethylene water heating kettle after adding a certain amount of Lithium acetate dihydrate to stir to clarify in 30mL glacial acetic acid and amide solvent, add the titanium sheet as the titanium source, and add the 1-methyl of 2mL-3-tetrafluoroborate ionic liquid;
2) water heating kettle is reacted 8-48h under 150-220 ℃ of condition, after deionized water and ethanol respectively wash three times, obtain the titanium dioxide optical catalyst of the Detitanium-ore-type of black at 80 ℃ of lower vacuum-drying 12h.
In step 1), in 30mL glacial acetic acid and acid amides mixed solvent, the volume of each component is: 1-2:2-1.Preferred ratio has: glacial acetic acid 10mL, acid amides 20mL; Glacial acetic acid 12mL, acid amides 18mL; Glacial acetic acid 15mL, acid amides 15mL; Glacial acetic acid 18mL, acid amides 12mL; Glacial acetic acid 20mL, acid amides 10mL.
Described acid amides is a kind of in methane amide, ethanamide, DMF, N,N-dimethylacetamide and benzamide.
In step 1), described Lithium acetate dihydrate quality is 0.2-1.0g, and preferred Lithium acetate dihydrate quality is 0.2g, 0.4g, 0.6g and 1.0g, and more preferred Lithium acetate dihydrate quality is 0.6g.
Step 2) in, the Heating temperature of preferred water heating kettle is 150 ℃, 180 ℃, 200 ℃, 220 ℃, and the reaction times is 8h, 12h, 24h, 48h.The more preferred reaction times is 24h.
The titanium dioxide optical catalyst that the present invention makes is applied to degradation of dye waste water, and described dyestuff comprises tropeolin-D, methylene blue, rhodamine B, fluorescent yellow, Congo red.
The titanium dioxide optical catalyst that the present invention makes is applied to the degrading phenol material, described aldehydes matter comprises phenol, 4-chlorophenol (4CP), 2-chlorophenol (2CP), 4-chloro-3-methylphenol (4C3MP), 2,4-chlorophenesic acid (2,4-DCP), 2,4, the 6-Trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP).
The product of the present invention's preparation carries out structural characterization by following means: adopt the X-ray diffraction of measuring on Rigaku Rigaku D/Max-RB type X-ray diffractometer to carry out the structural analysis of sample; The stereoscan photograph that adopts Japanese JEOL JSM-6380LV type scanning electron microscope to obtain, the transmission electron microscope photo that adopts Japanese JEOL JEM-2100 type transmission electron microscope to obtain.
The present invention compared with prior art, have the following advantages and outstanding effect: chemical reagent used in the present invention is common agents, cheap and easy to get, method technique is simple, and anatase phase titanium dioxide is extended to visible light-responded scope.Simultaneously, this photocatalyst is at visible luminous energy degraded lower concentration waste water from dyestuff, and demonstrates equally high reactivity in the system that lower concentration waste water from dyestuff and aldehydes matter mix.
Description of drawings
Fig. 1 is the XRD figure spectrum of the photocatalyst sample of prepared black anatase titania;
Fig. 2 is the high resolution scanning Electronic Speculum figure of prepared black anatase titania photocatalyst sample;
Fig. 3 is transmission electron microscope picture and the single crystal diffraction figure of prepared black anatase titania photocatalyst sample;
Fig. 4 is that the black anatase titania photocatalyst sample that makes is to waste water from dyestuff degradation process figure.
Embodiment
Be doing further in detail, illustrating clearly and completely of how realizing below in conjunction with specific embodiment to the present invention, listed embodiment only is further described the present invention, and is not thereby limiting the invention:
Embodiment 1
Add in 12mL glacial acetic acid and 18mL methane amide and be transferred in 50mL tetrafluoroethylene reactor after the 0.2g Lithium acetate dihydrate stirs to clarify, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 3
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 24h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 4
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 48h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 5
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 6
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 7
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 8
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 24h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 9
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 220 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 10
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 48h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 11
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 220 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 12
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL methane amide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 13
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL N,N-dimethylacetamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 14
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL N,N-dimethylacetamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 15
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL N,N-dimethylacetamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 24h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 16
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 48h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 17
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL N,N-dimethylacetamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 18
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 19
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 24h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 21
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 220 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 22
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 48h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 23
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 220 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 24
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL ethanamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 25
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 26
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 27
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.2g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 24h under 180 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 28
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 48h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 29
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.4g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 31
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 32
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle was reacted 24 hours under 200 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 33
Be transferred in 50mL tetrafluoroethylene reactor after adding the 0.6g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 220 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 34
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 12mL glacial acetic acid and 18mL DMF, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 48h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
Embodiment 35
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 18mL glacial acetic acid and 12mL benzamide, add the titanium sheet as the titanium source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 8h under 220 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the titanium dioxide optical catalyst of the Detitanium-ore-type of black at 80 ℃ of lower vacuum-drying 12h.
Embodiment 36
Be transferred in 50mL tetrafluoroethylene reactor after adding the 1.0g Lithium acetate dihydrate to stir to clarify in 10mL glacial acetic acid and 20mL benzamide, add the titanium sheet as the source, and add 2mL1-methyl-3-tetrafluoroborate ionic liquid.Water heating kettle is reacted 12h under 150 ℃ of conditions; After deionized water and ethanol respectively wash three times, obtain the black octahedrite type titanium dioxide photocatalyst at 80 ℃ of lower vacuum-drying 12h.
What this method was synthetic as can be drawn from Figure 1 is the titanium dioxide of Detitanium-ore-type.
As can be seen from Figure 2 Electronic Speculum figure be cluster together.
Can obtain this kind material from Fig. 3 is monocrystalline.
Black titanium dioxide has good activity at degradation of contaminant as can be seen from Figure 4.
Claims (11)
1. the preparation method of a visible light-responded black titanium dioxide photocatalyst, is characterized in that: comprise the steps:
1) be transferred in 50mL tetrafluoroethylene water heating kettle after adding a certain amount of Lithium acetate dihydrate to stir to clarify in 30mL glacial acetic acid and amide solvent, add the titanium sheet as the titanium source, and add the 1-methyl of 2mL-3-tetrafluoroborate ionic liquid;
2) water heating kettle was reacted 8-48 hour under 150-220 ℃ of condition; After deionized water and ethanol respectively wash three times, obtain the titanium dioxide optical catalyst of the Detitanium-ore-type of black at 80 ℃ of lower vacuum-drying 12h.
2. the preparation method of a kind of visible light-responded black titanium dioxide photocatalyst according to claim 1, it is characterized in that: in step 1), in 30mL glacial acetic acid and acid amides mixed solvent, the volume of each component is: 1-2:2-1.
3. the preparation method of a kind of visible light-responded black titanium dioxide photocatalyst according to claim 2, it is characterized in that: in step 1), in 30mL glacial acetic acid and acid amides mixed solvent, the volume of each component is: glacial acetic acid 10mL, acid amides 20mL; Glacial acetic acid 12mL, acid amides 18mL; Glacial acetic acid 15mL, acid amides 15mL; Glacial acetic acid 18mL, acid amides 12mL; Glacial acetic acid 20mL, acid amides 10mL.
4. the preparation method of a kind of visible light-responded black titanium dioxide photocatalyst according to claim 1, it is characterized in that: described acid amides is methane amide, ethanamide, N, a kind of in dinethylformamide, N,N-dimethylacetamide and benzamide.
5. the preparation method of a kind of visible light-responded black titanium dioxide photocatalyst according to claim 1, it is characterized in that: in step 1), described Lithium acetate dihydrate quality is 0.2-1.0g.
6. the preparation method of a kind of visible light-responded black titanium dioxide photocatalyst according to claim 5, it is characterized in that: described Lithium acetate dihydrate quality is 0.2g, 0.4g, 0.6g and 1.0g.
7. want the preparation method of 6 described a kind of visible light-responded black titanium dioxide photocatalysts according to right, it is characterized in that: described Lithium acetate dihydrate quality is 0.6g.
8. want the preparation method of 1 described a kind of visible light-responded black titanium dioxide photocatalyst according to right, it is characterized in that: step 2) in, the Heating temperature of described water heating kettle is 150 ℃, 180 ℃, 200 ℃, 220 ℃, and the reaction times is 8h, 12h, 24h, 48h.
9. want the preparation method of 8 described a kind of visible light-responded black titanium dioxide photocatalysts according to right, it is characterized in that: the described reaction times is 24h.
10. want the preparation method of 1 described a kind of visible light-responded black titanium dioxide photocatalyst according to right, it is characterized in that: the titanium dioxide optical catalyst that makes is applied to degradation of dye waste water, and described dyestuff comprises tropeolin-D, methylene blue, rhodamine B, fluorescent yellow and Congo red.
11. want the preparation method of 1 described a kind of visible light-responded black titanium dioxide photocatalyst according to right, it is characterized in that the titanium dioxide optical catalyst that makes is applied to the degrading phenol material, described aldehydes matter comprises phenol, 4-chlorophenol, 2-chlorophenol, 4-chloro-3-methylphenol, 2,4-chlorophenesic acid and 2,4,6-Trichlorophenol and pentachlorophenol.
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Cited By (13)
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| CN103833075A (en) * | 2014-03-31 | 2014-06-04 | 中国科学院新疆理化技术研究所 | Preparation method for controllable micropore or mesoporous anatase titanium dioxide |
| CN103866314A (en) * | 2014-02-28 | 2014-06-18 | 南京航空航天大学 | Preparation method and application of visible light response black titanium dioxide nano-film |
| CN103864142A (en) * | 2014-03-20 | 2014-06-18 | 南京工业大学 | Method for preparing anatase phase titanium dioxide nanowire array by one-step method |
| CN104477986A (en) * | 2014-12-14 | 2015-04-01 | 桂林理工大学 | Preparation method of black titanium diode nanotube |
| CN104843780A (en) * | 2015-04-30 | 2015-08-19 | 景德镇陶瓷学院 | Preparation method of anatase black nano titanium oxide powder |
| CN105731930A (en) * | 2016-02-23 | 2016-07-06 | 西北永新涂料有限公司 | Photocatalyst super-water-resistant attapulgite clay air purification plaster |
| CN105885557A (en) * | 2016-05-12 | 2016-08-24 | 盐城工学院 | Antibacterial and self-cleaning wall body coating and preparation method thereof |
| CN106115777A (en) * | 2016-06-15 | 2016-11-16 | 南开大学 | The preparation method of a kind of titanium dioxide ultrathin nanometer page and the application in lithium ion battery thereof |
| CN106185864A (en) * | 2016-07-10 | 2016-12-07 | 九江学院 | A kind of preparation method of titanium dioxide nano-belts |
| CN107138161A (en) * | 2017-07-17 | 2017-09-08 | 上海友兰科技有限公司 | A kind of preparation method for the black titanium dioxide that adulterates |
| CN110624527A (en) * | 2019-10-14 | 2019-12-31 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of three-dimensional colored titanium dioxide photocatalytic material, product and application thereof |
| GB2596291A (en) * | 2020-06-22 | 2021-12-29 | Nanomox Ltd | Method for producing metal and/or metalloid compounds in an ionic liquid |
| CN115707657A (en) * | 2022-11-30 | 2023-02-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method and product application of titanium dioxide nano material |
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| CN103866314B (en) * | 2014-02-28 | 2016-08-17 | 南京航空航天大学 | The preparation method and application of visible light-responded black titanium dioxide nano thin-film |
| CN103866314A (en) * | 2014-02-28 | 2014-06-18 | 南京航空航天大学 | Preparation method and application of visible light response black titanium dioxide nano-film |
| CN103864142A (en) * | 2014-03-20 | 2014-06-18 | 南京工业大学 | Method for preparing anatase phase titanium dioxide nanowire array by one-step method |
| CN103864142B (en) * | 2014-03-20 | 2015-09-02 | 南京工业大学 | Method for preparing anatase phase titanium dioxide nanowire array by one-step method |
| CN103833075B (en) * | 2014-03-31 | 2015-08-05 | 中国科学院新疆理化技术研究所 | The preparation method of a kind of controllable micropore or mesoporous anatase titanium dioxide |
| CN103833075A (en) * | 2014-03-31 | 2014-06-04 | 中国科学院新疆理化技术研究所 | Preparation method for controllable micropore or mesoporous anatase titanium dioxide |
| CN104477986A (en) * | 2014-12-14 | 2015-04-01 | 桂林理工大学 | Preparation method of black titanium diode nanotube |
| CN104477986B (en) * | 2014-12-14 | 2016-01-20 | 深圳孔雀科技开发有限公司 | A kind of preparation method of black titanium dioxide nanotube |
| CN104843780A (en) * | 2015-04-30 | 2015-08-19 | 景德镇陶瓷学院 | Preparation method of anatase black nano titanium oxide powder |
| CN104843780B (en) * | 2015-04-30 | 2016-06-22 | 景德镇陶瓷大学 | A kind of preparation method of anatase black nano titanium oxide powder |
| CN105731930B (en) * | 2016-02-23 | 2018-05-08 | 西北永新涂料有限公司 | The super water-fast attapulgite clay air purification plaster of photocatalyst |
| CN105731930A (en) * | 2016-02-23 | 2016-07-06 | 西北永新涂料有限公司 | Photocatalyst super-water-resistant attapulgite clay air purification plaster |
| CN105885557A (en) * | 2016-05-12 | 2016-08-24 | 盐城工学院 | Antibacterial and self-cleaning wall body coating and preparation method thereof |
| CN106115777A (en) * | 2016-06-15 | 2016-11-16 | 南开大学 | The preparation method of a kind of titanium dioxide ultrathin nanometer page and the application in lithium ion battery thereof |
| CN106185864A (en) * | 2016-07-10 | 2016-12-07 | 九江学院 | A kind of preparation method of titanium dioxide nano-belts |
| CN107138161A (en) * | 2017-07-17 | 2017-09-08 | 上海友兰科技有限公司 | A kind of preparation method for the black titanium dioxide that adulterates |
| CN107138161B (en) * | 2017-07-17 | 2020-04-03 | 上海友兰科技有限公司 | Preparation method of doped black titanium dioxide |
| CN110624527A (en) * | 2019-10-14 | 2019-12-31 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of three-dimensional colored titanium dioxide photocatalytic material, product and application thereof |
| GB2596291A (en) * | 2020-06-22 | 2021-12-29 | Nanomox Ltd | Method for producing metal and/or metalloid compounds in an ionic liquid |
| WO2021260360A1 (en) * | 2020-06-22 | 2021-12-30 | Nanomox Ltd | Method for producing metal and/or metalloid compounds in an ionic liquid |
| CN116018319A (en) * | 2020-06-22 | 2023-04-25 | 纳诺姆有限公司 | Method for producing metal and/or metalloid compounds in ionic liquids |
| CN115707657A (en) * | 2022-11-30 | 2023-02-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method and product application of titanium dioxide nano material |
| CN115707657B (en) * | 2022-11-30 | 2024-03-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method and productization application of titanium dioxide nano material |
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