CN105618049B - A kind of doping preparation method in situ of visible light-responsible titanium dioxide - Google Patents
A kind of doping preparation method in situ of visible light-responsible titanium dioxide Download PDFInfo
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- CN105618049B CN105618049B CN201510980755.7A CN201510980755A CN105618049B CN 105618049 B CN105618049 B CN 105618049B CN 201510980755 A CN201510980755 A CN 201510980755A CN 105618049 B CN105618049 B CN 105618049B
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- 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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
Abstract
The invention discloses a kind of doping preparation methods in situ of visible light-responsible titanium dioxide, including titanium ion solution will be configured, on the basis of titanium ion mole 100~400% nitrogen doping source, 0.5~2% metal-doped source, 0.5~1.5% doping auxiliary agent, 100~300% precipitating reagent are separately added into solution, stirring 1h obtains reaction precursor liquid；By precursor liquid centrifuge washing to precipitation, precipitation is settled to 1L, then adds in the peptizing aid of titanium ion mole 0.5~2%, the peptizing agent of titanium ion mole 1~3% is added dropwise to generating vitreosol；Colloidal sol is added in into closed hydrothermal reaction kettle and carries out crystallization to get to the titanium dioxide of visible light catalysis activity.This method preparation process is simple, is not required to high-temperature process, is easy to use.
Description
Technical field
The present invention relates to a kind of doping preparation methods in situ of visible light-responsible titanium dioxide, belong to photochemical catalyst and prepare skill
Art field.
Background technology
Titanium dioxide (TiO2) it is a kind of wide bandgap semiconductor, it, can be by most organic matter ore deposits under illumination effect
It is melted into as carbon dioxide and water, therefore the field of environment protection such as air pollution indoors, water body purification, antibacterial and deodouring are widely used
Prospect.But TiO2Intrinsic energy gap for 3.2eV, can only be reacted using ultraviolet light, therefore limit such material
Use in daily life.Therefore, to TiO2It is modified, makes it have visible light activity, be to promote TiO2Photocatalysis material
Expect the inexorable trend of application field.
In TiO2Method of modifying in, ion doping is wherein simple and effective means.Research shows that due to can be simultaneously
In TiO2The position at top of valence band and conduction band bottom introduces impurity energy level, metallic element and nitrogen codope TiO simultaneously2It can show
Go out and adulterate TiO than one pack system2Higher visible light catalysis activity, while the metal ion of suitable concentration can become catching for electronics
Center is obtained, improves the separative efficiency of photo-generated carrier.Hongqi Sun, Guanliang Zhou, Shizhen Liu, et al.,
Chemical Engineering Journal, 2013 (231):18-25. is prepared for N at 400 DEG C by the high-temperature process of 4h
With the nano-TiO of Fe, Ni, Ag, Pt codope2Powder, degradation experiment show codope TiO2TiO is adulterated than one pack system2Have
Higher visible light catalysis activity.D.Dolat, S.Mozia, R.J.Wrobel, et al., Applied Catalysis B：
Environmental, 2015 (162):Precursors are handled 4h at 800 DEG C and are prepared for N and Fe, Co, Ni by 310-318.
The TiO of codope2Powder and corresponding single doping TiO2Powder, by measuring CO in acetic acid degradation experiment2Generating rate,
It was found that codope TiO2TiO is adulterated compared to single2With superior visible light activity.
But N and metallic element codope TiO at present2Preparation need to be heated at high temperature more, not only high energy consumption, while high
Temperature can cause the reunion of titanium dioxide, reduce performance, and be heat-treated the TiO prepared2For powder, and powder is in actual use
Disperseed or loaded, not only increase processing step, while the going out phenomena such as adding in and cladding can be caused of dispersant
It is existing, reduce properties of product.Therefore, develop it is a kind of it is simple for process, be not required to high-temperature process, can directly use visible light-responded two
The preparation method of titanium oxide is of great significance for promoting the application of photocatalysis material of titanium dioxide in daily life.
Invention content
The purpose of the present invention is to provide a kind of preparation process it is simple, be not required to high-temperature process, wieldy visible ray is rung
Answer the doping preparation method in situ of titanium dioxide.
The purpose of the present invention is what is realized by following technical proposals.
A kind of doping preparation method in situ of visible light-responsible titanium dioxide, includes the following steps：
Step 1：A certain amount of titanium source is added in 1L water and configures the titanium ion solution of 0.3~1.5mol/L, then with
On the basis of titanium ion mole, the nitrogen doping source of addition 100~400% into solution, 0.5~2% metal-doped source, 0.5
~1.5% doping auxiliary agent, 100~300% precipitating reagent, stirring 1h obtain reaction precursor liquid；
Step 2：Precursor liquid deionized water centrifuge washing in step 1 is precipitated for 5 times, added in into precipitation go from
Sub- water is settled to 1L, then adds in the peptizing aid of titanium ion mole 0.5~2%, be added dropwise later titanium ion mole 1~
3% peptizing agent is to generating vitreosol；
Step 3：The colloidal sol obtained in step 2 is added in into closed hydrothermal reaction kettle and carries out crystallization to get to visible ray
The titanium dioxide of catalytic activity.
Further, the titanium source is one kind in titanyl sulfate, titanium tetrachloride or butyl titanate.
Further, the nitrogen doping source is one kind in urea, triethylamine or nitroguanidine.
Further, the metal-doped source is one kind in ferrous sulfate or nickel nitrate.
Further, the doping auxiliary agent is dodecyl hydroxypropyl sulfobetaines, dodecyl ethyoxyl sulfobetaines
One kind in alkali or dodecyl azochlorosulfonate propyl lycine.
Further, the precipitating reagent is one kind in KOH or sodium carbonate.
Further, the peptizing aid is one kind in ethylene glycol or glycerine.
Further, the peptizing agent is oxalic acid.
Further, hydrothermal crystallizing temperature is 50~80 DEG C, and the time is 0.5~3h.
The beneficial effects of the present invention are：
1) by controlling hydrothermal crystallization process, the synchronization N doping of hydrothermal synthesis is realized, under the conditions of low-temperature hydrothermal in fact
The codope in situ of nitrogen and metallic element is showed, prepared material has good visible light photocatalysis performance, avoids
Conventional high-temperature heat treatment process is reunited caused by preparing nitrogen and metal-doped titanium dioxide and Phenomena of Grain Growth, while can be with
Effectively reduce production cost.
2) by synchronous N doping technique, it is molten that one-step method is prepared for the visible light-responsible titanium dioxide that can directly use
Glue avoids traditional optically catalytic TiO 2 powder body material auxiliary agent packet caused by introducing dispersant during twice dispersing
The problems such as covering and being difficult to monodisperse ensures that the performance of visible light-responsible titanium dioxide gives full play to, has good applicability.
Description of the drawings
Attached drawing described herein is used to provide further understanding of the present invention, and forms the part of the application, not
Inappropriate limitation of the present invention is formed, in the accompanying drawings：
Fig. 1 is the XRD diagram of the nitrogen iron codope titanium dioxide colloidal sol prepared by embodiment 1.
Fig. 2 is the Uv-vis abosrption spectrograms of the nitrogen iron codope titanium dioxide colloidal sol prepared by embodiment 2.
Fig. 3 is the transmission electron microscope photo of the nitrogen iron codope titanium dioxide colloidal sol prepared by embodiment 1.
After nitrogen iron codope titanium dioxide colloidal sol spraying film forming of the attached drawing 4 synthesized by embodiment 1, under visible light to benzene
Removal effect data.
Specific embodiment
Below in conjunction with attached drawing and specific embodiment, the present invention will be described in detail, herein illustrative examples of the invention
And explanation is used for explaining the present invention, but not as a limitation of the invention.
A kind of doping preparation method in situ of visible light-responsible titanium dioxide, includes the following steps：
Step 1：One kind in a certain amount of titanyl sulfate, titanium tetrachloride, butyl titanate is mixed into 1L water and is configured
Go out the titanium ion solution of 0.3~1.5mol/L, then on the basis of titanium ion mole, 100~400% are added in into solution
Nitrogen doping source (one kind in urea, triethylamine, nitroguanidine), 0.5~2% metal-doped source is (in ferrous sulfate, nickel nitrate
It is a kind of), 0.5~1.5% doping auxiliary agent (dodecyl hydroxypropyl sulfobetaines, dodecyl ethyoxyl sulfobetaines,
One kind in dodecyl azochlorosulfonate propyl lycine), 100~300% precipitating reagent (one kind in KOH, sodium carbonate), stirring 1h is obtained
To reaction precursor liquid；
Step 2：By the deionized water centrifuge washing 5 times of the precursor liquid in step 1, precipitated, add in and go into precipitation
Ionized water is settled to 1L, then adds in the peptizing aid one kind of glycerine (ethylene glycol) of titanium ion mole 0.5~2%,
The oxalic acid of titanium ion mole 1~3% is added dropwise later to generating vitreosol；
Step 3：The colloidal sol obtained in step 2 is added in into closed hydrothermal reaction kettle and carries out crystallization, wherein, hydrothermal crystallizing
Condition is：Temperature is 50~80 DEG C, and the time is 0.5~3h.
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Embodiment 1：
The titanyl sulfate of 0.3mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
The urea of addition 100% into solution, 0.5% ferrous sulfate, 0.5% dodecyl hydroxypropyl sulfobetaines, 100%
KOH, precursor liquid centrifuge washing 5 times precipitated, deionized water added in into precipitation, be settled to 1L, Ran Houjia by stirring 1h
Enter the ethylene glycol of titanium ion mole 0.5%, the oxalic acid generation vitreosol of titanium ion mole 1% is added dropwise later, then will
Colloidal sol is heated to 80 DEG C of crystallization 2h in closed water heating kettle and obtains the titanium dioxide with visible light catalysis activity.
Fig. 1 show the XRD diagram of the nitrogen iron codope titanium dioxide colloidal sol prepared by embodiment 1, Fig. 1 as it can be seen that prepare
The titanium dioxide Anatase higher for photocatalytic activity, well-crystallized, without other dephasigns, it was demonstrated that synthesis technology stability is good
It is good.
Fig. 3 show the transmission electron microscope photo of the nitrogen iron codope titanium dioxide colloidal sol prepared by embodiment 1, such as
Shown in figure, obtained nano-titanium dioxide is uniformly dispersed, and mainly to be about 100nm, the fusiformis sol particle of wide about 20nm is deposited
, particle almost all exists in the form of monodisperse, have good dispersibility, effectively prevent the cladding that twice dispersing is brought
The problems such as, a step is prepared for can be directly as the photocatalyst sol that photocatalytic product uses.
After nitrogen iron codope titanium dioxide colloidal sol spraying film forming of the attached drawing 4 synthesized by embodiment 1, under visible light to benzene
Removal effect data, as seen from the figure, the colloidal sol film forming after, 4h can be degradable by the benzene of 20ppm, there is good visible ray
Photocatalysis performance has broad prospect of application in depollution of environment field.
Embodiment 2：
The titanium tetrachloride of 0.5mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
The triethylamine of addition 150% into solution, 0.8% ferrous sulfate, 1% dodecyl ethyoxyl sulfobetaines, 150%
KOH, precursor liquid centrifuge washing 5 times precipitated, deionized water added in into precipitation, be settled to 1L, Ran Houjia by stirring 1h
Enter the ethylene glycol of titanium ion mole 1%, the oxalic acid generation vitreosol of titanium ion mole 2% is added dropwise later, it then will be molten
Glue is heated to 50 DEG C of crystallization 3h in closed water heating kettle and obtains the titanium dioxide with visible light catalysis activity.
Fig. 2 is the Uv-vis abosrption spectrograms of prepared nitrogen iron codope titanium dioxide colloidal sol；As shown in the figure, with not mixing
Miscellaneous titanium dioxide is compared, and obtained nitrogen iron codope titanium dioxide has the visible ray of 400~600nm wave-length coverages stronger
Absorbability efficiently solves dependence of the titanium dioxide to ultraviolet light by the technique, makes it under conditions of general visible
There can be good photocatalysis performance.
Embodiment 3：
The butyl titanate of 1mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
300% nitroguanidine, 2% nickel nitrate, 1.5% dodecyl azochlorosulfonate propyl lycine, 200% carbonic acid are added in into solution
Precursor liquid centrifuge washing 5 times is precipitated, deionized water is added in into precipitation, be settled to 1L, then add in by sodium, stirring 1h
The oxalic acid generation vitreosol of titanium ion mole 3% is added dropwise, then by colloidal sol in the glycerine of titanium ion mole 1% later
80 DEG C of crystallization 0.5h are heated in closed water heating kettle and obtain the titanium dioxide with visible light catalysis activity.
Embodiment 4：
The titanyl sulfate of 1.5mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
400% nitroguanidine, 2% nickel nitrate, 1.0% dodecyl azochlorosulfonate propyl lycine, 150% carbonic acid are added in into solution
Precursor liquid centrifuge washing 5 times is precipitated, deionized water is added in into precipitation, be settled to 1L, then add in by sodium, stirring 1h
The oxalic acid generation vitreosol of titanium ion mole 2.5% is added dropwise in the glycerine of titanium ion mole 2% later, then will be molten
Glue is heated to 60 DEG C of crystallization 2h in closed water heating kettle and obtains the titanium dioxide with visible light catalysis activity.
Embodiment 5：
The titanyl sulfate of 0.8mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
The nitroguanidine of addition 250% into solution, 1.8% nickel nitrate, 1.2% dodecyl hydroxypropyl sulfobetaines, 300%
Sodium carbonate, precursor liquid centrifuge washing 5 times precipitated, deionized water added in into precipitation, be settled to 1L, so by stirring 1h
The ethylene glycol of titanium ion mole 1.8% is added in afterwards, and the oxalic acid generation vitreosol of titanium ion mole 1.5% is added dropwise later,
Then colloidal sol in closed water heating kettle is heated to 70 DEG C of crystallization 1.5h and obtains the nanometer titanium dioxide with visible light catalysis activity
Titanium.
Embodiment 6：
The titanyl sulfate of 1.3mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
The nitroguanidine of addition 300% into solution, 1.2% ferrous sulfate, 1.5% dodecyl hydroxypropyl sulfobetaines,
Precursor liquid centrifuge washing 5 times is precipitated, deionized water is added in into precipitation, be settled to by 180% sodium carbonate, stirring 1h
Then 1L adds in the ethylene glycol of titanium ion mole 1.3%, the oxalic acid generation that titanium ion mole 2.3% is added dropwise later is transparent
Then colloidal sol in closed water heating kettle is heated to 75 DEG C of crystallization 1h and obtains the titanium dioxide with visible light catalysis activity by colloidal sol
Titanium.
Embodiment 7：
The titanium tetrachloride of 0.8mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
The nitroguanidine of addition 250% into solution, 1.8% nickel nitrate, 1.2% dodecyl hydroxypropyl sulfobetaines, 300%
Sodium carbonate, precursor liquid centrifuge washing 5 times precipitated, deionized water added in into precipitation, be settled to 1L, so by stirring 1h
The glycerine of titanium ion mole 1.2% is added in afterwards, and the oxalic acid generation vitreosol of titanium ion mole 1.5% is added dropwise later,
Then colloidal sol in closed water heating kettle is heated to 70 DEG C of crystallization 1.5h and obtains the titanium dioxide with visible light catalysis activity.
Embodiment 8：
The titanium tetrachloride of 0.6mol is taken to add in 1L water and obtains titanium ion solution, then on the basis of titanium ion mole,
The urea of addition 200% into solution, 1.3% nickel nitrate, 0.8% dodecyl hydroxypropyl sulfobetaines, 250%
Precursor liquid centrifuge washing 5 times is precipitated, deionized water is added in into precipitation, be settled to 1L, then add in by KOH, stirring 1h
The ethylene glycol of titanium ion mole 1.8% is added dropwise the oxalic acid generation vitreosol of titanium ion mole 1.5%, then will later
Colloidal sol is heated to 60 DEG C of crystallization 2.5h in closed water heating kettle and obtains the titanium dioxide with visible light catalysis activity.
Embodiment 9：
The butyl titanate of 1.4mol is taken to add in 1L water and obtains titanium ion solution, then using titanium ion mole as base
Standard, the nitroguanidine of addition 250% into solution, 1.0% nickel nitrate, 1.2% dodecyl ethyoxyl sulfobetaines,
Precursor liquid centrifuge washing 5 times is precipitated, deionized water is added in into precipitation, be settled to 1L by 300% KOH, stirring 1h,
Then the glycerine of titanium ion mole 1.8% is added in, the oxalic acid generation that titanium ion mole 1.5% is added dropwise later is transparent molten
Then colloidal sol in closed water heating kettle is heated to 50 DEG C of crystallization 3h and obtains the titanium dioxide with visible light catalysis activity by glue.
Embodiment 10：
The butyl titanate of 0.7mol is taken to add in 1L water and obtains titanium ion solution, then using titanium ion mole as base
Standard, the nitroguanidine of addition 180% into solution, 1.6% ferrous sulfate, 0.6% dodecyl azochlorosulfonate propyl lycine,
Precursor liquid centrifuge washing 5 times is precipitated, deionized water is added in into precipitation, be settled to by 220% sodium carbonate, stirring 1h
Then 1L adds in the ethylene glycol of titanium ion mole 1.8%, the oxalic acid generation that titanium ion mole 2.8% is added dropwise later is transparent
Then colloidal sol in closed water heating kettle is heated to 50 DEG C of crystallization 2.5h and obtains the titanium dioxide with visible light catalysis activity by colloidal sol
Titanium.
Claims (3)
1. the doping preparation method in situ of a kind of visible light-responsible titanium dioxide, which is characterized in that include the following steps：
Step 1：Will a certain amount of titanyl sulfate, titanium tetrachloride or butyl titanate titanium source add in 1L water configure 0.3~
Then on the basis of titanium ion mole, 100~400% N doping is added in into solution for the titanium ion solution of 1.5mol/L
Source, 0.5~2% metal-doped source, 0.5~1.5% doping auxiliary agent, 100~300% precipitating reagent stir to get reaction
Precursor liquid；
Step 2：Precursor liquid in step 1 with deionized water centrifuge washing is precipitated, deionized water is added in into precipitation, it is fixed
Hold to 1L, then add in the ethylene glycol of titanium ion mole 0.5~2% or the peptizing aid of glycerine, titanium ion is added dropwise later
The peptizing agent of mole 1~3% is to generating vitreosol；
Step 3：The colloidal sol obtained in step 2 is added in into closed hydrothermal reaction kettle and carries out crystallization, hydrothermal crystallizing temperature is 50
~80 DEG C, the time is 0.5~3h；Obtain the titanium dioxide of visible light catalysis activity；
The metal-doped source is one kind in ferrous sulfate or nickel nitrate；
The doping auxiliary agent is dodecyl hydroxypropyl sulfobetaines, dodecyl ethyoxyl sulfobetaines or dodecyl
One kind in azochlorosulfonate propyl lycine；
The peptizing agent is oxalic acid.
A kind of 2. doping preparation method in situ of visible light-responsible titanium dioxide as described in claim 1, which is characterized in that institute
Nitrogen doping source is stated as one kind in urea, triethylamine or nitroguanidine.
A kind of 3. doping preparation method in situ of visible light-responsible titanium dioxide as described in claim 1, which is characterized in that institute
Precipitating reagent is stated as one kind in KOH or sodium carbonate.
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