CN102285686A - Method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by fast sol-gel method - Google Patents
Method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by fast sol-gel method Download PDFInfo
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Abstract
The invention discloses a method for preparing iron-nitrogen codoped mesoporous nano titanium dioxide by a fast sol-gel method. In the method, a polymer with a molecular weight of 2*10<4>-3*10<6> is used as a template agent, and simultaneously, the template agent reacts with titanium-source hydrolysate to form a hydrogen bond so as to be fast gelated; and simultaneously, an iron source and a nitrogen source are uniformly dispersed in a uniform gel system, and then codoped mesoporous titanium dioxide is obtained by calcination. In the method, the iron element and nitrogen source are codoped and enter crystal lattices of nano titanium dioxide, wherein Fe<3+> becomes a center of capturing photoelectrons, thereby prolonging the survival time of photoholes; nitrogen atoms substitute partial oxygen atoms, so that the forbidden band width of titanium dioxide is reduced, the photoresponse range is enlarged, and titanium dioxide has a certain absorption in a visible light range; and simultaneously, on the basis of the traditional sol-gel method, the defect of long preparation period is overcome by using the method disclosed by the invention. A sample prepared by using high polymers such as polyacrylamide and the like as the template agent has mesopore duct and large specific surface area, and the photocatalysis efficiency is improved.
Description
Technical field
The invention belongs to the preparation technology field of inorganic materials and photocatalytic semiconductor material, relate to the method for a kind of iron-nitrogen co-doped mesohole nano-titanium dioxide, the method for especially a kind of fast sol preparing gel iron-nitrogen co-doped mesohole nano-titanium dioxide.
Background technology
Titanium dioxide is one of a kind of the most frequently used photocatalyst, because of having good thermostability and chemical stability, is widely used in fields such as field of environment protection, photocatalysis hydrogen production, self-cleaning clear wood material.But owing to has the Detitanium-ore-type TiO of better photocatalysis performance
2Energy gap be 3.2eV, only utilizing in the sunlight about 5% ultraviolet ray, thereby solar energy utilization rate is low.Asahi etc. have proposed can reduce energy gap, thereby enlarge the photoresponse scope of titanium dioxide with the part lattice oxygen in the nitrogen doped and substituted titanium dioxide lattice first.Another major issue that needs to be resolved hurrily is to reduce the right recombination rate in light induced electron-hole, promptly improves the survival time of photohole.Thereby this there is scientist propose doped metal ion as improving the survival time of photohole with electronics bonded center.Fe wherein
3+It is a kind of metal ion that effectively is easy to get.Has nano-TiO simultaneously than bigger serface and suitable pore passage structure
2Also be the important channel of improving photocatalysis performance, the nano-TiO that has the mesopore orbit structure in recent years
2Photocatalyst material causes extensive attention.Because of meso-porous nano TiO
2Owing to have big specific surface area and extremely strong advantages such as adsorptive power, aspect degradation of organic substances, shown common nano-TiO
2Incomparable photocatalysis efficiency.
This work is titanium source, Fe (NO with the butyl (tetra) titanate
3)
39H
2O as source of iron, urea as nitrogenous source, polyacrylamide PAM (molecular weight 3,000,000) or polyoxyethylene glycol (molecular weight 20,000) as template, adopt the fast sol gel method to prepare the nitrogen co-doped mesohole nano-titanium dioxide photocatalyst of the iron with visible light activity.Template such as PAM is not only as template in this research, and the hydrogen bond that utilizes amide group in the polyacrylamide and Ti-OH to form has greatly shortened the collosol and gel time.The nano-TiO of preparing simultaneously
2The primary particle size size is not subjected to the shortening of gel time and becomes big, suppresses growing up of crystal grain on the contrary effectively.This method makes gel time shorten in 2 hours from common 3～5 days, has greatly improved conventional efficient.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, the method for a kind of fast sol preparing gel iron-nitrogen co-doped mesohole nano-titanium dioxide is provided, ferro element and nitrogenous source all mix and enter the lattice of nano titanium oxide, wherein Fe in this method
3+Become the center of catching light induced electron, thereby improve the survival time of photohole.Make nitrogen-atoms replace the partial oxygen atom, reduce the energy gap of titanium dioxide, enlarge the photoresponse scope, certain absorption is arranged in visible-range.On the basis of traditional sol-gel method, can overcome the long shortcoming of preparation cycle simultaneously.With high molecular polymers such as polyacrylamides is that the sample that template prepares has mesopore orbit and bigger specific surface area, has improved photocatalysis efficiency.
The objective of the invention is to solve by the following technical programs:
The method of this fast sol preparing gel iron-nitrogen co-doped mesohole nano-titanium dioxide is: adopting molecular weight is 2 * 10
4～3 * 10
6Polymkeric substance as template, simultaneously template reacts with titanium source hydrolyzate, forms hydrogen bond, makes its PhastGel, source of iron and nitrogenous source are dispersed in the gelling system of homogeneous uniformly simultaneously, obtain the mesoporous TiO 2 of codoped after calcining.
Above preparation method specifically may further comprise the steps:
1) under the room temperature, at first mixing solutions to the pH value of regulating dehydrated alcohol, deionized water, nitrogenous source, source of iron with rare nitric acid or dilute hydrochloric acid is 3～4, be 1 according to volume ratio then: (1～4) splashes into the ethanol solution of butyl (tetra) titanate, add massfraction at last and be 0.1～15% the polyacrylamide or the aqueous solution of polyoxyethylene glycol, stir 0.1～2h, obtain gel;
2) gel is placed in the baking oven with 80～100 ℃ of oven dry 2～4h, removes solvent and moisture, xerogel; After xerogel ground, put into crucible in mortar, calcine and remove template at low temperatures, obtain the codoped mesoporous TiO 2.
In the above step 1), the volume ratio of dehydrated alcohol and water is (20～30) in the mixing solutions of dehydrated alcohol, deionized water, nitrogenous source, source of iron: 1.
Above step 2) in, calcining temperature is 350～450 ℃.
Further, more than used nitrogenous source be urea, titanium source and urea mol ratio are (0.90～1.35): 1.More than used source of iron be nine nitric hydrate iron, titanium source and source of iron mol ratio are 1: (0.001～0.01).
The present invention has following beneficial effect than prior art:
1) the present invention has overcome long shortcoming experimental period of Prepared by Sol Gel Method nano titanium oxide, and operation steps is simple, and preparation process is carried out at low temperatures, and envrionment temperature does not have obvious influence;
2) obvious, the electronics-hole-recombination rate reduction of the iron-nitrogen co-doped mesohole nano-titanium dioxide UV, visible light optical absorption edge red shift of the present invention's preparation;
3) iron-crystal grain of nitrogen co-doped mesohole nano-titanium dioxide of the present invention's preparation is little, is that specific surface area is bigger between 10～20nm, at 100～200m
2/ g, and contain the mesopore orbit structure, mean pore size is between 2.9～5.5nm.
Description of drawings
Fig. 1 is the XRD figure of sample, and wherein (a) is the XRD figure of embodiment 1, (b) is the XRD figure of embodiment 2;
Fig. 2 is the low temperature N of embodiment 1 sample
2Adsorption/desorption curve (a) and pore size distribution curve (b);
Fig. 3 is the x-ray photoelectron energy spectrogram of the sample of embodiment 2 preparations, and wherein (a) is the x-ray photoelectron power spectrum of nitrogen element, (b) is the x-ray photoelectron power spectrum of ferro element;
Fig. 4 is photochemical catalysis methyl orange solution (10mg/L) degradation curve of embodiment 1 sample and common nano titanium oxide.
Embodiment
The method of fast sol preparing gel iron of the present invention-nitrogen co-doped mesohole nano-titanium dioxide is that the employing molecular weight is 2 * 10
4～3 * 10
6Polymkeric substance as template, simultaneously template reacts with titanium source hydrolyzate, forms hydrogen bond, makes its PhastGel, source of iron and nitrogenous source are dispersed in the gelling system of homogeneous uniformly simultaneously, obtain the mesoporous TiO 2 of codoped after calcining.It specifically carries out according to following steps:
1) under the room temperature, at first the mixing solutions pH value of regulating dehydrated alcohol, deionized water, nitrogenous source, source of iron with rare nitric acid or dilute hydrochloric acid is 3～4, wherein the volume ratio of dehydrated alcohol and water is (20～30): 1, be 1 according to volume ratio then: (1～4) splashes into the ethanol solution of butyl (tetra) titanate, and then to add massfraction be 0.1～15% the polyacrylamide or the aqueous solution of polyoxyethylene glycol, stir 0.1～2h, obtain wet gel;
2) gel is placed in the baking oven with 80～100 ℃ of oven dry 2～4h, removes solvent and moisture, xerogel; After xerogel ground, put into crucible in mortar, calcine and remove template at low temperatures, obtain the codoped mesoporous TiO 2, wherein calcining temperature is 350～450 ℃.
In preferred embodiment of the present invention, nitrogenous source adopts urea, and titanium source and urea mol ratio are (0.90～1.35): 1.Source of iron adopts nine nitric hydrate iron, and titanium source and source of iron mol ratio are 1: (0.001～0.01).
Below in conjunction with specific embodiment and accompanying drawing the present invention is done and to describe in further detail:
Embodiment 1
(1) at room temperature, get respectively in 280mL dehydrated alcohol, 10mL deionized water, 1.5g urea, the 0.12g nine nitric hydrate iron adding beaker, regulating pH with the rare nitric acid of 5wt% then is 3～4, stirs, and is designated as A;
(2) get a small beaker, add 20mL dehydrated alcohol and 10mL butyl (tetra) titanate respectively, mix, be designated as B;
(3) get 0.1g polyacrylamide (molecular weight is 3,000,000) and add in the 100g deionized water, the preparation mass concentration is about the solution of 0.1wt%, is designated as C;
(4) A is slowly splashed among the B, and constantly stir, add the back, back and continue to stir 10～15 minutes, drip 20mL C liquid then.Add the back and continue to stir 1h, obtain wet gel;
(5) wet gel is put into baking oven 80 ℃ of oven dry down, removed solvent and moisture, obtain wet gel;
(6) xerogel is ground 10min in mortar, take out and put into crucible,, and remove template, obtain product at 350 ℃ of following calcined crystallines.Fig. 1 (a) is the X-ray diffractogram of this sample.
Embodiment 2
(1) at room temperature, get respectively in 200mL dehydrated alcohol, 10mL deionized water, 1.0g urea, the 0.05g nine nitric hydrate iron adding beaker, regulating pH with the rare nitric acid of 5wt% then is 3～4, is designated as A, stirs;
(2) get a small beaker, add 20mL dehydrated alcohol and 10mL butyl (tetra) titanate respectively, mix, be designated as B;
(3) get 15g polyoxyethylene glycol (molecular weight is 20,000) and add in the 100g deionized water, the preparation mass concentration is about the polyglycol solution of 15wt%, is designated as C;
(4) A is slowly splashed among the B, and constantly stir, add the back and continue to stir 10min, slowly be added dropwise to 20mL C liquid then.Add the back and continue to stir 2h, until gel;
(5) wet gel is put into baking oven 90 ℃ of oven dry down, removed solvent and moisture, get xerogel;
(6) xerogel is ground 15min in mortar, take out and put into crucible,, and remove template, obtain the Detitanium-ore-type mesohole nano-titanium dioxide at 400 ℃ of following calcined crystallines.Fig. 1 (b) is the X-ray diffractogram of this sample.
Embodiment 3
Present embodiment specifically carries out according to following steps:
1) under the room temperature, at first mixing solutions to the pH value of regulating dehydrated alcohol, deionized water, nitrogenous source, source of iron with rare nitric acid or dilute hydrochloric acid is 3～4, wherein the volume ratio of dehydrated alcohol and water is 20: 1, be that 1: 1 ethanol solution with butyl (tetra) titanate splashes into according to volume ratio then, and then the adding massfraction is 0.1% polyacrylamide solution, stir 0.1h, obtain gel; Wherein nitrogenous source is a urea, and titanium source and urea mol ratio are 0.90: 1; Source of iron is nine nitric hydrate iron, and titanium source and source of iron mol ratio are 1: 0.001;
2) gel is placed in the baking oven with 80 ℃ of oven dry 4h, removes solvent and moisture, xerogel; After xerogel ground, put into crucible in mortar, calcine and remove template at low temperatures, obtain the codoped mesoporous TiO 2, wherein calcining temperature is 350 ℃.
Embodiment 4
1) under the room temperature, at first mixing solutions to the pH value of regulating dehydrated alcohol, deionized water, nitrogenous source, source of iron with rare nitric acid or dilute hydrochloric acid is 3～4, wherein the volume ratio of dehydrated alcohol and water is 30: 1, be that 1: 4 ethanol solution with butyl (tetra) titanate splashes into according to volume ratio then, and then the adding massfraction is 15% the polyoxyethylene glycol aqueous solution, stir 2h, obtain gel; Nitrogenous source is a urea, and titanium source and urea mol ratio are 1.35: 1; Source of iron is nine nitric hydrate iron, and titanium source and source of iron mol ratio are 1: 0.01;
2) gel is placed in the baking oven with 100 ℃ of oven dry 2h, removes solvent and moisture, xerogel; After xerogel ground, put into crucible in mortar, calcine and remove template at low temperatures, obtain the codoped mesoporous TiO 2, wherein calcining temperature is 450 ℃.
1) under the room temperature, at first mixing solutions to the pH value of regulating dehydrated alcohol, deionized water, nitrogenous source, source of iron with rare nitric acid or dilute hydrochloric acid is 3～4, wherein the volume ratio of dehydrated alcohol and water is 25: 1, be that 1: 3 ethanol solution with butyl (tetra) titanate splashes into according to volume ratio then, and then the adding massfraction is 10% the polyoxyethylene glycol aqueous solution, stirred 1 hour, and obtained gel; Nitrogenous source is a urea, and titanium source and urea mol ratio are 1: 1; Source of iron is nine nitric hydrate iron, and titanium source and source of iron mol ratio are 1: 0.008.
2) gel is placed in the baking oven with 90 ℃ of oven dry 3h, removes solvent and moisture, xerogel; After xerogel ground, put into crucible in mortar, calcine and remove template at low temperatures, obtain the codoped mesoporous TiO 2, wherein calcining temperature is 400 ℃.
Comprehensive above embodiment, it is as follows to analyze Figure of description:
Fig. 1 is respectively the XRD figure of the sample of embodiment 1 and 2, calculates through the Scherrer formula and can get both nanoparticle crystalline primary particle sizes all between 10～20nm, and crystal formation is a Detitanium-ore-type, has good chemical stability and catalytic performance.
Fig. 2 is the N of embodiment 1 preparation sample
2Isothermal adsorption desorption graphic representation (a) and BJH pore size distribution curve (b).From (a), be IV type adsorption isothermal line as can be seen, after relative pressure reaches certain numerical value, N
2Capillary condensation takes place in mesoporous, and adsorptive capacity suddenly rises.After treating that adsorption-condensation finishes, platform appears in adsorption isothermal line.This is the characteristic feature of mesoporous material.This material pore size distribution is narrow as can be seen from the BJH pore size distribution curve, and peak value meets the scope of mesoporous 2～50nm about 4nm, be a kind of mesoporous material, has the ability of good adsorption degradation product.
Fig. 3 is the nitrogen element of sample of embodiment 2 preparation and the x-ray photoelectron power spectrum of ferro element.(a) be the peak of N 1s at the 405.5eV place in, (b) in 716.2eV place be the peak of Fe 2p, in conjunction with the result of the characteristic peak of other species of nothing among the XRD, two figure illustrate that nitrogen element and ferro element have all mixed and have entered TiO
2Lattice in.
Fig. 4 is the data plot of the photocatalytic degradation tropeolin-D of the iron-nitrogen co-doped mesohole nano-titanium dioxide of sample of embodiment 1 preparation and common nano titanium oxide.As can be seen from the figure, iron-nitrogen co-doped mesohole nano-titanium dioxide methyl orange degradation rate behind 1h has reached 83%, and common nano titanium oxide degradation rate behind 3h illustrates after the mixing of ferro element and nitrogen element and improved TiO largely still less than 80%
2Photocatalysis performance, and meso-hole structure has very big specific surface area, to improving photocatalysis efficiency promoter action is arranged, so use the photocatalysis performance that can greatly improve titanium dioxide codoped and mesoporous two kinds of technology the time.
Claims (6)
1. the method for fast sol preparing gel iron-nitrogen co-doped mesohole nano-titanium dioxide is characterized in that, adopting molecular weight is 2 * 10
4～3 * 10
6Polymkeric substance as template, simultaneously template reacts with titanium source hydrolyzate, forms hydrogen bond, makes its PhastGel, source of iron and nitrogenous source are dispersed in the gelling system of homogeneous uniformly simultaneously, obtain the mesoporous TiO 2 of codoped after calcining.
2. the method for fast sol preparing gel iron according to claim 1-nitrogen co-doped mesohole nano-titanium dioxide is characterized in that this method specifically may further comprise the steps:
1) under the room temperature, at first mixing solutions to the pH value of regulating dehydrated alcohol, deionized water, nitrogenous source, source of iron with rare nitric acid or dilute hydrochloric acid is 3～4, be 1 according to volume ratio then: (1～4) splashes into the ethanol solution of butyl (tetra) titanate, and then to add massfraction be 0.1～15% the polyacrylamide or the aqueous solution of polyoxyethylene glycol, stirred 0.1～2 hour, and obtained gel;
2) gel is placed in the baking oven with 80～100 ℃ of oven dry 2～4h, removes solvent and moisture, xerogel; After xerogel ground, put into crucible in mortar, calcine and remove template at low temperatures, obtain the codoped mesoporous TiO 2.
3. the method for fast sol preparing gel iron according to claim 2-nitrogen co-doped mesohole nano-titanium dioxide, it is characterized in that, in the step 1), the volume ratio of dehydrated alcohol and water is (20～30) in the mixing solutions of dehydrated alcohol, deionized water, nitrogenous source, source of iron: 1.
4. the method for fast sol preparing gel iron according to claim 2-nitrogen co-doped mesohole nano-titanium dioxide is characterized in that step 2) in, calcining temperature is 350～450 ℃.
5. the method for fast sol preparing gel iron according to claim 1 and 2-nitrogen co-doped mesohole nano-titanium dioxide is characterized in that used nitrogenous source is a urea, and titanium source and urea mol ratio are (0.90～1.35): 1.
6. the method for fast sol preparing gel iron according to claim 1 and 2-nitrogen co-doped mesohole nano-titanium dioxide is characterized in that, used source of iron is nine nitric hydrate iron, and titanium source and source of iron mol ratio are 1: (0.001～0.01).
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| CN105879893A (en) * | 2014-12-24 | 2016-08-24 | 江南大学 | Preparation method of iron-nitrogen-codoped titanium dioxide visible-light-induced photocatalyst |
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| CN107158638B (en) * | 2017-06-20 | 2019-10-11 | 山东理工大学 | A method of utilizing the methylene blue adsorbed in titanium dioxide degradable particle under solar irradiation |
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