CN104028292A - N-TiO2/C and N-TiO2 and preparation method thereof - Google Patents
N-TiO2/C and N-TiO2 and preparation method thereof Download PDFInfo
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Abstract
The invention relates to N-TiO2/C and N-TiO2 and a preparation method thereof, and particularly discloses a method for preparing nitrogen-doped titanium oxide and a nano-composite of nitrogen-doped titanium oxide with carbon through heat treatment in air. The preparation method comprises the following steps: (1) mixing 10wt% of a tetramethylammonium hydroxide water solution with ethylene glycol, adding isopropyl titanate, uniformly stirring, and performing hydrothermal treatment on an obtained solution for 8 hours at 200 DEG C; (2) centrifuging and cleaning a hydrothermal product which is obtained in the step (1) in ethanol and deionized water, and drying in the air at 70 DEG C; and (3) performing heat treatment on a dried product which is obtained in the step (2) for 2 hours in the air at 250 to 550 DEG C, so as to obtain the nano-composite of nitrogen-doped titanium oxide/carbon or nitrogen-doped titanium oxide. The nano-composite of the nitrogen-doped titanium oxide/carbon and nitrogen-doped titanium oxide, which are obtained by using the preparation method, have the advantage of high nitrogen content and have visible light catalytic activity, and an absorption spectrum is expanded to a visible light region. The adopted preparation method has the advantages of simplicity, convenience, easiness in implementation, high safety factor, low cost and the like.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide nano material, especially a kind of nano-complex (N-TiO of nitrogen adulterated TiOx/carbon
2/ C) or nitrogen adulterated TiOx (N-TiO
2) preparation method, belong to the preparation field of chemical material, aspect photocatalytic degradation pollutant, having very important purposes.
Background technology
Low owing to having cost, nontoxic, chemical synthesis is convenient, the characteristics such as Heat stability is good, and titanium oxide is a kind of very common photochemical catalyst.Titanium oxide has three kinds of crystal formations, rutile, anatase and brockites.Wherein, anatase is the most frequently used photochemical catalyst.The principle of photocatalysis to degrade organic matter is, under illumination condition, in incident photon, energy is higher than the photon of energy gap by valence band Electron absorption, and then electron transition is to conduction band.Light induced electron is transferred to dyestuff from the conduction band of titanium oxide, dyestuff generation oxidation reaction, so that oxidized.The energy gap of anatase is 3.2eV, the oxidized titanium of ultraviolet luminous energy that only has wavelength to be less than 380nm absorbs, and the energy of ultraviolet light only accounts for 7% of sun nature spectrum, therefore, the anatase that common synthetic method obtains is very low to the utilization ratio of light, is necessary to improve the response of anatase to visible light wave range.
For improving the response of anatase titanium oxide to whole natural daylight wave band, can improve from following two aspects, the one, pattern regulation and control, the 2nd, chemical regulation.Pattern regulation and control are mainly by increasing the specific area of titanium oxide, increasing porosity increases titanium oxide to the absorption of dyestuff or exposes particular crystal plane, as enlivening face, [100] or [101] etc. carry out for example, the photodissociation to organic dyestuff (: methylene blue, methylene orange, pinkish red etc.) of accelerating oxidation titanium.Pattern regulation and control do not relate to the energy gap that changes titanium oxide, therefore little on the enhancing impact of light absorption.And another kind of method, chemical regulation, thus be mainly that the energy gap that changes titanium oxide by doping reaches the absorption to visible ray.Doping is conventional method, comprises doping metals and nonmetal.From the angle of application, metal cost compare is high, thus to nonmetalloid C, H, S, the doping research of N is many.But, titanium oxide is being carried out to C, H, during N doping, the most frequently used method is to heat-treat under special atmosphere.Such as, nitrogen adulterated TiOx is generally that titanium oxide is carried out to high-temperature heat treatment under nitrogen atmosphere, and hydrogen doping titanium oxide is heat treatment titanium oxide under hydrogen shield.Except experiment working condition being required to height, also there is safety problem in the heat treatment of carrying out under special atmosphere, whole process production cost also increases greatly.Therefore, at relative low temperature, and do not need special atmosphere, such as adulterating under air conditions, become a study hotspot.
Meanwhile, research discovery, simple nitrogen adulterated TiOx, although titanium oxide energy gap is narrowed down, has widened its spectral response range, and the hole that doping is introduced, unintentionally for carrier provides complex centre, causes photo-generated carrier utilization ratio to reduce.For addressing this problem, can carry out modification to the titanium oxide of nitrogen doping.Such as, nitrogen adulterated TiOx and carbon are carried out compound.Material with carbon element is because the characteristic of its powerful Electronic saving ability and metal conduction band can be accepted light induced electron.Research is found, after the coated titanium oxide of carbon nanomaterial, because the fermi level between carbon and titanium oxide is poor, causes electronics to carbon nanomaterial direction generation enrichment, has therefore promoted the separation of photohole-electronics, and the photocatalysis efficiency of titanium oxide is improved.But, at present relative less with the compound research of carbon for nitrogen adulterated TiOx, and existing preparation method's reaction condition is not gentle, and higher to requirement for experiment condition.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of N-TiO is provided
2/ C and N-TiO
2and preparation method thereof.Utilize incomplete hydro-thermal reaction to prepare predecessor, follow-up heat treatment process is controlled TiO
2doping vario-property, different temperatures obtains the TiO that different chemical forms
2product, i.e. N-TiO
2/ C or N-TiO
2.
The preparation method of the nano-complex of nitrogen adulterated TiOx or itself and carbon comprises the steps:
1) tetramethyl ammonium hydroxide solution is joined in ethylene glycol, the volume ratio of tetramethyl ammonium hydroxide solution and ethylene glycol is 1:3, the two adds isopropyl titanate after stirring, the volume that titanium isopropoxide solution adds is 1/10 of tetramethyl oxyammonia solution, continues to be stirred to acquisition homogeneous solution under room temperature;
2) homogeneous solution obtaining in step 1) is moved in polytetrafluoroethylene (PTFE) water heating kettle liner, with stainless steel outer sleeve sealing, then hydro-thermal reaction 8h at 200 ℃, naturally cools to room temperature;
3) utilize acetone, alcohol and deionized water eccentric cleaning step 2 respectively) product that obtains, and dry in air ambient;
4) desciccate step 3) being obtained is heat-treated, and heat treatment temperature is 250 ~ 550 ℃, and heat treatment time is 2h, and heat treatment atmosphere is air atmosphere, obtains the nano-complex of nitrogen adulterated TiOx or nitrogen adulterated TiOx/carbon.
Described tetramethyl ammonium hydroxide solution is 10wt% tetramethylammonium hydroxide aqueous solution.
When described heat treatment temperature is 250 ~ 400 ℃, obtain the nano-complex of nitrogen adulterated TiOx/carbon; When heat treatment temperature is 400 ~ 550 ℃, obtain nitrogen adulterated TiOx.
The nano-complex nitrogen content of nitrogen adulterated TiOx/carbon prepared by described preparation method is 2.23 ~ 3.32%, and carbon content is 19 ~ 23%, and specific area is 55 ~ 80m
2/ g, in the nano-complex of described nitrogen adulterated TiOx/carbon, titanium oxide is anatase crystal.
Nitrogen adulterated TiOx nitrogen content prepared by described preparation method is 1.94 ~ 2.56%, and specific area is 45 ~ 58m
2/ g, in described nitrogen adulterated TiOx, titanium oxide is anatase crystal.
It is high that the nano-complex of nitrogen adulterated TiOx/carbon that the present invention obtains and nitrogen adulterated TiOx have nitrogen content, and absorption spectra is extended to and can, by light region, has the advantages such as visible light photocatalysis active.The preparation method who adopts heat-treats under air atmosphere, has avoided the inconvenience that heat treatment is brought under special atmosphere (as hydrogen, nitrogen, indifferent gas), and whole preparation process is simple and easy to do, and safety coefficient is high, and cost is low.And by controlling heat treatment temperature, can obtain very easily N-TiO
2/ C or N-TiO
2and the control of realization to its nitrogen content, carbon content.
Accompanying drawing explanation
The XRD collection of illustrative plates of the nitrogen adulterated TiOx/carbon nano-complex of Fig. 1 the inventive method example 1 preparation;
The high-resolution photo of the nitrogen adulterated TiOx/carbon nano-complex of Fig. 2 the inventive method example 1 preparation;
XPS score and the N1s open score of the nitrogen adulterated TiOx/carbon nano-complex of Fig. 3 the inventive method example 1 preparation;
The ultraviolet-ray visible absorbing spectrum of the nitrogen adulterated TiOx/carbon nano-complex of Fig. 4 the inventive method example 1 preparation;
The XRD collection of illustrative plates of the nitrogen adulterated TiOx of Fig. 5 the inventive method example 3 preparations;
XPS score and the N1s open score of the nitrogen adulterated TiOx of Fig. 6 the inventive method example 3 preparations;
The Raman collection of illustrative plates of the nitrogen adulterated TiOx of Fig. 7 the inventive method example 3 preparations;
The ultraviolet-ray visible absorbing spectrum of the nitrogen adulterated TiOx of Fig. 8 the inventive method example 3 preparations.
The specific embodiment
Below by specific embodiment, the invention will be further described, but therefore do not limit the scope of the invention.After having read the content of the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modification falls into the scope of the claims in the present invention equally.
embodiment 1
Nitrogen adulterated TiOx/carbon nano-complex is as shown in Figures 1 to 4 to adopt following methods prepare and obtain:
1) 10mL tetramethyl ammonium hydroxide solution is joined in 30mL ethylene glycol and stirs 10min, then add 1mL isopropyl titanate, under room temperature, stir 0.5h, obtain homogeneous solution.
2) homogeneous solution obtaining in step 1) is moved into the polytetrafluoroethylene (PTFE) that volume is 80mL
In water heating kettle liner, after stainless steel outer sleeve sealing, hydro-thermal reaction 8h at 200 ℃, from
So be cooled to room temperature.
3) utilize acetone, alcohol and deionized water 1 step 2 of eccentric cleaning respectively) obtain
Product, and dry 10h in 70 ℃ of air ambients.
4) desciccate step 3) being obtained is heat-treated.Heat treatment temperature is 250 ℃, heat
Processing time is 2h, and heat treatment atmosphere is air atmosphere, obtains receiving of nitrogen adulterated TiOx/carbon
Rice compound.
Fig. 1 is the XRD collection of illustrative plates of the nitrogen adulterated TiOx/carbon nano-complex of example 1 preparation, as can be seen from Figure, the product obtaining is anatase crystal, although crystallinity is poor, but in 2 θ=25.3,37.9,48.15, the diffraction maximum at 54.05,55.28 ° of places such as grade can be corresponding one by one with anatase JCPDS card No.84-1285.
Fig. 2 is the high resolution electron microscopy photo of the nitrogen adulterated TiOx/carbon nano-complex of example 1 preparation, can observe carbon and the crystal grain of crystallite dimension between 3 ~ 8nm of disordering in figure.The analysis of lattice diffraction fringe can obtain, and the crystal grain in white circle is anatase crystal grain.
Fig. 3 is the XPS collection of illustrative plates of the nitrogen adulterated TiOx/carbon nano-complex of example 1 preparation, have nitrogen, and nitrogen content is higher in the product that wherein in embedded N1s spectrogram, strong electronics shows to obtain in conjunction with peak.And analyze and learn, the doped forms of nitrogen is gapped nitrogen both, has again replacement nitrogen.
Fig. 4 is the ultraviolet-ray visible absorbing spectrum of the nitrogen adulterated TiOx/carbon nano-complex of example 1 preparation, in figure, can learn, prepared nitrogen adulterated TiOx/carbon nano-complex all has obvious absorption in whole ultraviolet-visible region, corresponding to the appearance of black of product.Can predict the visible light photocatalysis active of product.
embodiment 2
Nitrogen adulterated TiOx/carbon nano-complex is to adopt following methods prepare and obtain:
1) 10mL tetramethyl ammonium hydroxide solution is joined in 30mL ethylene glycol and stirs 10min, then add 1mL isopropyl titanate, under room temperature, stir 0.5h, obtain homogeneous solution.
2) homogeneous solution obtaining in step 1) is moved into the polytetrafluoroethylene (PTFE) that volume is 80mL
In water heating kettle liner, after stainless steel outer sleeve sealing, hydro-thermal reaction 8h at 200 ℃, from
So be cooled to room temperature.
3) utilize acetone, alcohol and deionized water 1 step 2 of eccentric cleaning respectively) obtain
Product, and dry 10h in 70 ℃ of air ambients.
4) desciccate step 3) being obtained is heat-treated.Heat treatment temperature is 350 ℃, heat
Processing time is 2h, and heat treatment atmosphere is air atmosphere, obtains receiving of nitrogen adulterated TiOx/carbon
Rice compound.
embodiment 3
A nitrogen adulterated TiOx as shown in Fig. 5 to Fig. 8 is to adopt following methods prepare and obtain:
1) 10mL tetramethyl ammonium hydroxide solution is joined in 30mL ethylene glycol and stirs 10min, then add 1mL isopropyl titanate, under room temperature, stir 0.5h, obtain homogeneous solution.
2) homogeneous solution obtaining in step 1) is moved into the polytetrafluoroethylene (PTFE) that volume is 80mL
In water heating kettle liner, after stainless steel outer sleeve sealing, hydro-thermal reaction 8h at 200 ℃, from
So be cooled to room temperature.
3) utilize acetone, alcohol and deionized water 1 step 2 of eccentric cleaning respectively) obtain
Product, and dry 10h in 70 ℃ of air ambients.
4) desciccate step 3) being obtained is heat-treated.Heat treatment temperature is 450 ℃, heat
Processing time is 2h, and heat treatment atmosphere is air atmosphere, obtains nitrogen adulterated TiOx.
Fig. 5 is the XRD collection of illustrative plates of the nitrogen adulterated TiOx of example 3 preparations, as can be seen from Figure, the product obtaining is Anatase titanium oxide, and crystallinity is good, in 2 θ=25.3,37.9,48.15, the diffraction maximum at 54.05,55.28 ° of places such as grade can be corresponding one by one with anatase JCPDS card No.84-1285.
Fig. 6 is the XPS collection of illustrative plates of the nitrogen adulterated TiOx of example 3 preparations, wherein in embedded N1s spectrogram, can observe electronics in conjunction with peak, have nitrogen, and nitrogen content is higher in the product that shows to obtain.And analyze and learn, the doped forms of nitrogen is gapped nitrogen both, has again replacement nitrogen.
Fig. 7 is the Raman collection of illustrative plates of the nitrogen adulterated TiOx of example 3 preparations, 100 ~ 700 cm
-1between anatase structured corresponding to product of the peak that produces, wherein wave number is 580cm
-1the peak at place has characterized the existence of nitrogen.Meanwhile, 1000 ~ 2000 cm
-1between without Raman peaks, show in product not carbon containing, be nitrogen adulterated TiOx.
Fig. 8 is the ultraviolet-ray visible absorbing spectrum of the nitrogen adulterated TiOx of example 3 preparations, in figure, can learn, prepared its absorption region of nitrogen adulterated TiOx, than pure zirconia titanium, is extended to visibility region by ultraviolet region, echoes mutually with the yellow appearance of product.And, " absorption tail " (450 ~ 550nm) that absorption spectra produces with typical nitrogen doped products.Can predict the visible light photocatalysis active of product.
embodiment 4
A nitrogen adulterated TiOx of the present invention is to adopt following methods prepare and obtain:
1) 10mL tetramethyl ammonium hydroxide solution is joined in 30mL ethylene glycol and stirs 10min, then add 1mL isopropyl titanate, under room temperature, stir 0.5h, obtain homogeneous solution.
2) homogeneous solution obtaining in step 1) is moved into the polytetrafluoroethylene (PTFE) that volume is 80mL
In water heating kettle liner, after stainless steel outer sleeve sealing, hydro-thermal reaction 8h at 200 ℃, from
So be cooled to room temperature.
3) utilize acetone, alcohol and deionized water 1 step 2 of eccentric cleaning respectively) obtain
Product, and dry 10h in 70 ℃ of air ambients.
4) desciccate step 3) being obtained is heat-treated.Heat treatment temperature is 550 ℃, heat
Processing time is 2h, and heat treatment atmosphere is air atmosphere, obtains nitrogen adulterated TiOx.
Claims (5)
1. a preparation method for the nano-complex of nitrogen adulterated TiOx or itself and carbon, is characterized in that, comprises the steps:
1) tetramethyl ammonium hydroxide solution is joined in ethylene glycol, the volume ratio of tetramethyl ammonium hydroxide solution and ethylene glycol is 1:3, the two adds isopropyl titanate after stirring, the volume that titanium isopropoxide solution adds is 1/10 of tetramethyl oxyammonia solution, continues to be stirred to acquisition homogeneous solution under room temperature;
2) homogeneous solution obtaining in step 1) is moved in polytetrafluoroethylene (PTFE) water heating kettle liner, with stainless steel outer sleeve sealing, then hydro-thermal reaction 8h at 200 ℃, naturally cools to room temperature;
3) utilize acetone, alcohol and deionized water eccentric cleaning step 2 respectively) product that obtains, and dry in air ambient;
4) desciccate step 3) being obtained is heat-treated, and heat treatment temperature is 250 ~ 550 ℃, and heat treatment time is 2h, and heat treatment atmosphere is air atmosphere, obtains the nano-complex of nitrogen adulterated TiOx or nitrogen adulterated TiOx/carbon.
2. preparation method according to claim 1, is characterized in that described tetramethyl ammonium hydroxide solution is 10wt% tetramethylammonium hydroxide aqueous solution.
3. preparation method according to claim 1, while it is characterized in that described heat treatment temperature is 250 ~ 400 ℃, obtains the nano-complex of nitrogen adulterated TiOx/carbon; When heat treatment temperature is 400 ~ 550 ℃, obtain nitrogen adulterated TiOx.
4. a nano-complex for nitrogen adulterated TiOx/carbon that as claimed in claim 1 prepared by preparation method, is characterized in that: the nano-complex nitrogen content of described nitrogen adulterated TiOx/carbon is 2.23 ~ 3.32%, carbon content is 19 ~ 23%, and specific area is 55 ~ 80m
2/ g, in the nano-complex of described nitrogen adulterated TiOx/carbon, titanium oxide is anatase crystal.
5. the nitrogen adulterated TiOx that as claimed in claim 1 prepared by preparation method, is characterized in that: described nitrogen adulterated TiOx nitrogen content is 1.94 ~ 2.56%, and specific area is 45 ~ 58m
2/ g, in described nitrogen adulterated TiOx, titanium oxide is anatase crystal.
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| CN112850784A (en) * | 2021-02-26 | 2021-05-28 | 中国检验检疫科学研究院 | Synthetic method and application of flaky TiO nano material |
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| CN105680019A (en) * | 2016-03-16 | 2016-06-15 | 江苏乐能电池股份有限公司 | Preparation method of high-rate ternary material |
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| CN108246335A (en) * | 2018-01-31 | 2018-07-06 | 辽宁工程技术大学 | A kind of nitrogen-Ag doped with nano TiO2The preparation method of powder |
| CN108246335B (en) * | 2018-01-31 | 2020-03-31 | 辽宁工程技术大学 | Nitrogen-silver doped nano TiO2Method for preparing powder |
| CN109718823A (en) * | 2018-12-10 | 2019-05-07 | 齐鲁工业大学 | N-doped TiO2/ C composite and the preparation method and application thereof |
| CN109718823B (en) * | 2018-12-10 | 2021-10-26 | 齐鲁工业大学 | N-doped TiO2/C composite material and preparation method and application thereof |
| CN112850784A (en) * | 2021-02-26 | 2021-05-28 | 中国检验检疫科学研究院 | Synthetic method and application of flaky TiO nano material |
| CN113181950A (en) * | 2021-04-29 | 2021-07-30 | 浙江大学 | Photocatalyst for degrading antibiotics in water by activating persulfate under assistance of visible light |
| CN113181950B (en) * | 2021-04-29 | 2022-08-23 | 浙江大学 | Photocatalyst for degrading antibiotics in water by activating persulfate under assistance of visible light |
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