CN1555916A - Preparation method of photocatalytic active fluorine adulterated titanium dioxide nano material - Google Patents
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Abstract
A F doped nano-class TiO2 material with photocatalytic activity is prepared by doping F into TiO2 crystal. It features that its energy gap can be triggered by visual light, realizing the full-frequency absorption to visual light for increasing its light quantum efficiency.
Description
Technical Field
The invention relates to a preparation method of a nano material, in particular to a preparation method of a fluorine-doped titanium dioxide nano material with photocatalytic activity, belonging to the field of inorganic nano photocatalytic materials.
Background
Titanium dioxide semiconductor photocatalysisOxidation technology is a new modern technology. Because it can widely use natural energy-solar energy, and has the outstanding characteristics of low energy consumption, mild reaction condition, simple operation, capability of reducing secondary pollution and the like, it is increasingly paid attention to, and has wide application prospect. In recent years, semiconductor photocatalysis has become one of the research hotspots in the fields of photochemistry and environmental protection. The application of the compound in wastewater treatment has been reported in many documents. A large number of researches prove that dyes, surfactants, organic halides, pesticides, cyanides, phenols, polychlorinated biphenyls, polycyclic aromatic hydrocarbons and the like can be effectively catalyzed, degraded, decolorized, detoxified and mineralized into inorganic small molecular substances, so that the pollution to the environment is eliminated. In practical applications, TiO2The photocatalytic material has been used in the fields of water and air purification devices, self-cleaning glass surfaces, antibacterial photocatalytic ceramic tiles and the like, and has produced great economic, environmental and social benefits.
TiO2The forbidden band width of the light absorption band is 3.2eV, and the light absorption range is limited to the ultraviolet region (the wavelength is less than 380 nm). But the part of light can not reach 5 percent of the total energy of the sunlight irradiating the ground, and the TiO is used for the current2The quantum efficiency is not higher than 28%, so the utilization efficiency of the solar energy is only about 1%, and the utilization of the solar energy is greatly limited. How to solve TiO2Dependence on Ultraviolet (UV) (4.5% in sunlight), modifying the catalyst to red shift its photoresponse wavelength to visible region (46% in sunlight radiation), so that it can directly use the sunlight radiation, and is TiO2The key point of the photocatalytic oxidation technology is entering the practical stage. And TiO 22The catalyst is not high in activity, and is deactivated because excited valence band holes and conduction band electrons generated after being irradiated by light are easy to recombine. According to the third law of thermodynamics, all physical systems have different degrees of irregularity except at absolute zero degrees. The actual crystal is of an approximate space lattice structure and always has one or more structural defects. When traces of impurities are incorporated into the crystal, impurity defects may form, the presence of these defects acting as photocatalyst TiO2The activity plays an important role.
Found by literature search, ChinaThe patent publication numbers are: CN 1438071a, patent name: surface fluorineA process for improving the photocatalytic activity of titanium oxide by chemical treatment features that the surface of titanium oxide is immersed in the aqueous solution of organic acid containing fluorine to increase the number of organic groups containing fluorine on the surface of titanium oxide, so decreasing the recombination between photo-generated electrons and holes. However, this material focuses on the suppression of the recombination of photo-generated electrons and holes by using fluorine-containing strong electron groups. Because the fluorine element is bonded with the carbon element and then appears on the surface of the material in a chemical adsorption state, and does not enter the TiO2In the crystal, therefore, TiO cannot be reduced2The forbidden band width of the light source is not enough to use visible light.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a fluorine-doped titanium dioxide nano material with photocatalytic activity. The method is used for preparing TiO through a simpler preparation process2The fluorine doping can reduce the forbidden band width to the extent of the available visible light range (400-800nm) to improve the light quantum efficiency. The preparation method has the advantages of simplifying production and preparation processes and reducing production cost.
The invention is realized by the following technical scheme: the invention adopts fluorine doping technology to synthesize fluorine-doped modified titanium dioxide nano material, fluorine is doped in crystal lattice of titanium dioxide crystal, and fluorine is doped in crystal gap, wherein the weight percentage of 3 elements in the fluorine-doped titanium dioxide nano material is as follows: the content of titanium is 44.6-52.7%; the oxygen content is 16.7-39.4%; the content of fluorine accounts for 7.9 to 38.7 percent.
Such doping will act as follows for the catalyst:
① the p orbital of fluorine atom and the 2p orbital of O atom form new molecular orbitals after hybridization, while TiO2The valence band of (A) is basically composed of the 2p orbital of the O atom, and the hybridization of the p orbital of the fluorine atom and the 2p orbital of the O atom to form a new molecular orbital is larger than that of the 2p orbital of the original O atomHigh energy per unit area, and TiO2The height of the conduction band is not changed, thereby reducing TiO2The forbidden band width of the solar energy collector enables the light absorption of the solar energy collector to be red-shifted to the whole visible light region, and the visible light part in solar light radiation can be directly utilized.
② impurities are introduced into the crystal to cause defects, which can effectively capture photo-generated electrons, inhibit the recombination of electrons and holes, prolong the service life of holes, and improve the photocatalytic activity of titanium dioxide.
The invention is further described in detail below, comprising the steps of:
(a) adding a titanium precursor into a proper amount of aqueous solution of fluorine dopant, and fully and uniformly mixing to generate a white precipitate;
(b) the precursor of the titanium is inorganic salt or titanium alkoxide of titanium. If the precursor of the titanium is inorganic salt of the titanium, the white precipitate is generated and then is washed by deionized water until the concentration of anions (such as chloride ions and sulfate ions) is less than 0.5mg/L, and then the precipitate is filtered and collected; this is not required if the titanium precursor is a titanium alkoxide;
(c) drying the white precipitate at a certain temperature, and then grinding to obtain solid powder;
(d) and carrying out heat treatment on the solid powder, and calcining the solid powder in an air atmosphere at the temperature of 300-700 ℃ to obtain the fluorine-doped titanium dioxide nano material.
The titanium precursor comprises titanium alkoxide and inorganic titanium salt, wherein the titanium alkoxide comprises one or a combination of tetrabutyl titanate, isopropyl titanate and ethyl titanate; the inorganic salt of titanium is one or two of titanium chloride, titanium sulfate and the like.
The fluorine doping agent is as follows: HF or fluorine-containing salts.
The drying time from the white precipitate to the solid dried substance is not less than 20 minutes, and the drying temperature is not more than 200 ℃. The white precipitate is dried by direct heating or natural drying. The optimal drying temperature is 100-150 ℃, the optimal drying time is 5-10 hours, and the optimal drying mode is direct heating drying.
The solid powder heat treatment has the temperature rise speed of 1-40 ℃/min, the heat preservation time of 0.5-6 hours and the temperature reduction speed of 15-40 ℃/min. The optimal temperature rising speed is 3-10 ℃/min, the optimal heat preservation time is 0.5-3 hours, and the optimal temperature reduction speed is 20-30 ℃/min.
The fluorine-doped titanium dioxide nano catalyst material is in an anatase type or coexists in the anatase type and the rutile type. The fluorine-doped titanium dioxide nano catalyst material has a forbidden bandwidth which can be excited by visible light irradiation, thereby realizing full-frequency absorption of visible light, and obviously improving the modified TiO2The photon efficiency of the material. The light source can be natural light, artificial simulated sunlight or ultraviolet light source.
The preparation method of the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under visible light comprises the steps of adding a small amount of fluorine dopant into water to prepare a fluorine dopant aqueous solution, then dropwise adding the aqueous solution into a titanium precursor solution to generate a white precipitate, drying the white precipitate for removing water at 100-150 ℃ under a direct heating and drying condition for 2-10 hours, grinding to obtain solid powder, carrying out heat treatment on the solid powder, calcining at 300-700 ℃ in an air atmosphere to form a crystal form, and finally cooling to room temperature to obtain the fluorine-doped titanium dioxide nano catalyst material.
The photocatalytic activity test of the fluorine-doped titanium dioxide nano catalyst material is characterized by decomposing phenol in water by the fluorine-doped titanium dioxide nano catalyst material under the irradiation of visible light. Phenol is an organic matter with strong toxicity, and the waste water containing phenol is a pollutant with wide source and serious harm, and is widely existed in the waste water of industries such as steel, petrochemical industry, plastics, synthetic fibers, urban gas and the like, and the pollution problem caused by the waste water is more and more prominent. Therefore, the present invention selects it as a simulated polluting compound. Photocatalytic oxidation separation of phenolThe solution is based on the following chemical reaction: photocatalytic activity of fluorine-doped titanium dioxide nano catalyst material for decomposing phenol in waterThe test was carried out using a 1000 ml photocatalytic reactor at normal temperature and pressure. The process for measuring the photocatalytic activity of the fluorine-doped titanium dioxide nano catalyst material comprises the following steps: weighing 500 ml of prepared 20mg/L phenol solution, adding into a photocatalytic reactor, adding 0.35 g of accurately weighed fluorine-doped titanium dioxide nano catalyst material, and stirring by strong magnetic force. Before the photocatalysis experiment, phenol and the fluorine-doped titanium dioxide nano catalyst material in the reactor reach adsorption balance. The initial concentration of phenol in the reactor after equilibrium adsorption was reached was about 19mg/L, whichremained constant until the 1000W xenon lamp (with a 420nm filter) was turned on. The initial temperature in the reactor was 25. + -. 1 ℃. In order to keep the temperature in the reactor constant, a circulating water cooling device is arranged outside the reactor. In the reaction process, strong magnetic stirring is always adopted in the reactor. The phenol concentration was measured by 4-aminoantipyrine spectrophotometry, and the change in phenol concentration was measured by sampling every 20 minutes after the reaction. The phenol concentration gradually decreases along with the progress of the photocatalytic reaction, and the degradation reaction is a first-order reaction and conforms to a first-order reaction kinetic equation ln (C)0/Ct)＝kt，C0As initial phenol concentration, CtK is the first order reaction kinetic apparent rate constant for the phenol concentration at which the reaction proceeded to t. The prepared fluorine-doped titanium dioxide nano catalyst material and commercial titanium dioxide powder (Shanghai chemical reagent company, chemical purity) are used for measuring catalytic oxidation activity by the method.
The invention has substantive characteristics and remarkable progress. The fluorine-doped titanium dioxide nano catalyst material prepared by the preparation method has forbidden bandwidth which can be excited by visible light irradiation, realizes full-frequency absorption of visible light, and can remarkably improve the modified TiO2The photon efficiency of the material; meanwhile, the preparation method is simple and has the prospect of industrial production.
Drawings
Fig. 1 is a graph comparing uv-vis absorption spectra of a fluorine-doped titanium dioxide nanocatalyst material with high catalytic activity and titanium dioxide powder (modelP25, Degussa, germany). The measuring instrument is a VARIANCary 500UV-vis spectrophotometer.
Detailed Description
In order to confirm the light absorption performance of the fluorine-doped titanium dioxide nano powder catalyst having high catalytic activity in visible light, ultraviolet-visible absorption spectrum (UV-Vis) was measured. The measuring instrument is a VARIAN Cary 500UV-vis spectrophotometer. The weight percentages of 3 elements in the fluorine-doped titanium dioxide nano material of the following embodiment are all selected according to the following ranges; the titanium accounts for 44.6 to 52.7 percent, the oxygen accounts for 16.7 to 39.4 percent, and the fluorine accounts for 7.9 to 38.7 percent.
Example 1
15ml of hydrogen fluoride solution (0.5M/L) were reacted with 20ml of tetrabutyl titanate (mass% of>98.0%) until a white precipitate was formed. Directly heating the white precipitate in an oven, treating at 120 deg.C for 4 hr, and evaporating to remove water and alcohol substances generated in reaction to obtain solid dry substance. And grinding the solid dried substance to make the particles uniform and reduce soft agglomeration. And (3) placing the mixture into a muffle furnace after grinding, and calcining the mixture for 2 hours at 285 ℃ to obtain the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under visible light. In a catalytic activity test, the apparent rate constant of the first-order reaction kinetics of the catalyst material for catalyzing and degrading phenol is 1.00 multiplied by 10-3min-1And the apparent rate constant k of the first-order reaction kinetics of the degradation of phenol under the same conditions of the experiment is 0 under the condition of visible light of the common commercial titanium dioxide, so that the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under the visible light is formed after the heat treatment for 2 hours.
The ultraviolet-visible absorption spectra (UV-Vis) of the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity and the titanium dioxide powder (P25, Degussa) are shown in fig. 1, and the fluorine-doped titanium dioxide nano catalyst material and the titanium dioxide powder (P25, Degussa) have almost equally strong absorption in the ultraviolet region; in the visible light region, the light absorption of the fluorine-doped titanium dioxide nano-catalyst material is significantly higher than that of titanium dioxide powder (P25, Degussa). This is attributed to the fluorine doping technique red-shifts the photoresponsive wavelength into the visible region, enhancing the absorption of visible light.
Example 2
15ml of hydrogen fluoride solution (0.5M/L) was reacted with 20ml of titanium sulfate (mass% of>40.0%) until a white precipitate was formed. After rinsing the resulting white precipitate with deionized water, the resulting solution was washed until the anion (sulfate ion) concentration was less than 0.5 mg/L. Directly heating the white precipitate in an oven, treating at 120 deg.C for 4 hr, and evaporating to remove water and alcohol substances generated in reaction to obtain solid dry substance. And grinding the solid dried substance to make the particles uniform and reduce soft agglomeration. And (3) placing the mixture into a muffle furnace after grinding, and calcining the mixture for 2 hours at 285 ℃ to obtain the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under visible light. In a catalytic activity test, the apparent rate constant of the first-order reaction kinetics of the catalyst material for catalyzing and degrading phenol is 0.95 multiplied by 10-3min-1And the apparent rate constant k of the first-order reaction kinetics of the degradation of phenol under the same conditions of the experiment is 0 under the condition of visible light of the common commercial titanium dioxide, so that the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under the visible light is formed after the heat treatment for 2 hours.
Example 3
15ml of hydrogen fluoride solution (0.5M/L) was reacted with 20ml of titanium chloride (mass% of>99.9%) until a white precipitate was formed. After rinsing the resulting white precipitate with deionized water, the resulting solution was washed until the anion (chloride ion) concentration was less than 0.5 mg/L. Directly heating the white precipitate in an oven, treating at 120 deg.C for 4 hr, and evaporating to remove water and alcohol substances generated in reaction to obtain solid dry substance. And grinding the solid dried substance to make the particles uniform and reduce soft agglomeration. And (3) placing the mixture into a muffle furnace after grinding, and calcining the mixture for 2 hours at 285 ℃ to obtain the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under visible light. In the test of catalytic activity, the catalysisThe first-order reaction kinetic apparent rate constant of the catalyst material for catalyzing and degrading phenol is k ═ 0.96 multiplied by 10-3min-1And the apparent rate constant k of the first-order reaction kinetics of the degradation of phenol under the same conditions of the experiment is 0 under the condition of visible light of the common commercial titanium dioxide, so that the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under the visible light is formed after the heat treatment for 2 hours.
Example 4
15ml of hydrogen fluoride solution (0.5M/L) were reacted with 20ml of tetrabutyl titanate (mass% of>98.0%) until a white precipitate was formed. Heating the white precipitate in oven directly, treating at 120 deg.C for 4 hr, evaporating to remove water and part of alcohol substances generated in reaction to obtain solid dry substance. And grinding the obtained solid dried substance to ensure that the particles are uniform and soft agglomeration is reduced. And (3) placing the mixture into a muffle furnace after grinding, and calcining the mixture for 1 hour, 2 hours and 3 hours at 285 ℃ respectively to obtain the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under visible light. In a catalytic activity test, the apparent rate constants of first-order reaction kinetics of the catalyst material for catalyzing and degrading phenol are respectively 0.80 multiplied by 10-3min-1、1.00×10-3min-1、0.66×10-3min-1. It can be seen that after heat treatment, the fluorine-doped titanium dioxide nano catalyst material with high catalytic activity under visible light is formed.
Claims (9)
1. A method for preparing a fluorine-doped titanium dioxide nano material with photocatalytic activity is characterized in that the method adopts a fluorine doping technology to synthesize the fluorine-doped modified titanium dioxide nano material, fluorine elements are doped into crystal lattices of titanium dioxide crystals, and the fluorine elements are doped into crystal gaps of the titanium dioxide crystals, wherein the weight percentage of 3 elements in the fluorine-doped titanium dioxide nano material is as follows: the titanium accounts for 44.6 to 52.7 percent, the oxygen accounts for 16.7 to 39.4 percent, and the fluorine accounts for 7.9 to 38.7 percent.
2. The process for the preparation of photocatalytically active fluorine-doped titanium dioxide nanomaterial according to claim 1, characterized in that the process of the present invention is further defined as follows, the process comprising the specific steps of:
(a) adding a titanium precursor into a proper amount of aqueous solution of fluorine dopant, and fully and uniformly mixing to generate a white precipitate;
(b) if the precursor of the titanium is inorganic salt of the titanium, washing the titanium precursor with deionized water after generating a white precipitate until the concentration of anions is less than 0.5mg/L, then filtering, and collecting the precipitate washed with the deionized water, wherein if the precursor of the titanium is titanium alkoxide, the washing treatment is not needed;
(c) drying the white precipitate at a certain temperature, and grinding to obtain a solid dried substance;
(d) and (3) carrying out heat treatment on the solid dried substance, and calcining the solid dried substance in the air atmosphere at the temperature of 300-700 ℃ to obtain the fluorine-doped titanium dioxide nano material.
3. The method for producing a photocatalytically active fluorine-doped titanium dioxide nanomaterial according to claim 1 or 2, wherein the produced fluorine-doped titanium dioxide nanomaterial is in an anatase form or coexists in an anatase form and a rutile form, and fluorine is doped in both crystal lattices and crystal gaps of the titanium dioxide crystal material.
4. The method of claim 1 or 2, wherein the fluorine-doped titanium dioxide nanomaterial has catalyticactivity under both visible light and ultraviolet light, and the light source used is natural light, artificial simulated sunlight or ultraviolet light.
5. The method for preparing the photocatalytically active fluorine-doped titanium dioxide nanomaterial according to claim 2, wherein the titanium precursor comprises titanium alkoxide and inorganic titanium salt, and the titanium alkoxide comprises one or a combination of two of tetrabutyl titanate, isopropyl titanate and ethyl titanate; the inorganic salt of titanium is one or two of titanium chloride and titanium sulfate.
6. The method of claim 2, wherein the fluorine dopant is selected from the group consisting of: HF or fluorine-containing salts.
7. The process for producing a photocatalytically active fluorine-doped titanium dioxide nanomaterial according to claim 2, wherein the drying time of the white precipitate to the solid dried substance is 20 minutes or more and the drying temperature is 200 ℃ or less.
8. The process for preparing photocatalytically active fluorine-doped titanium dioxide nanomaterials of claim 2 or 7, wherein the white precipitate is dried by direct heating or natural drying.
9. The method for preparing the photocatalytic active fluorine-doped titanium dioxide nanomaterial according to claim 2, wherein the temperature rise rate of the heat treatment is 1-40 ℃/min, the heat preservation time is 0.5-6 hours, and the temperature drop rate is 15-40 ℃/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327966C (en) * | 2005-08-25 | 2007-07-25 | 上海交通大学 | Process for preparing fluorine blended metal oxide catalyst |
| CN102218335A (en) * | 2011-06-13 | 2011-10-19 | 华东理工大学 | Preparation method of hydrophobic immobilized photocatalyst with solar photocatalysis activity |
| CN102266792A (en) * | 2011-06-13 | 2011-12-07 | 华东理工大学 | Synthesis method for visible photocatalyst by modifying titanium dioxide by using ammonium fluoride |
| CN101632936B (en) * | 2008-07-25 | 2013-04-17 | 中国科学院福建物质结构研究所 | Visible light response catalyst and preparation and application thereof |
| CN104609468A (en) * | 2013-11-04 | 2015-05-13 | 天津大学 | Method for preparing anatase type titanium dioxide having porous hexagonal prism morphology, and applications of anatase type titanium dioxide having porous hexagonal prism morphology |
| CN108499582A (en) * | 2018-04-04 | 2018-09-07 | 昆明理工大学 | A kind of preparation method of composite photo-catalyst |
| CN109967062A (en) * | 2019-03-11 | 2019-07-05 | 浙江万里学院 | A kind of high energy crystal face exposure TiO2The preparation method of photochemical catalyst |
| CN111744512A (en) * | 2020-07-30 | 2020-10-09 | 内蒙古工业大学 | Narrow forbidden band low valence band modified TiO2Method for preparing photocatalyst |
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2003
- 2003-12-30 CN CN 200310109845 patent/CN1259128C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327966C (en) * | 2005-08-25 | 2007-07-25 | 上海交通大学 | Process for preparing fluorine blended metal oxide catalyst |
| CN101632936B (en) * | 2008-07-25 | 2013-04-17 | 中国科学院福建物质结构研究所 | Visible light response catalyst and preparation and application thereof |
| CN102218335A (en) * | 2011-06-13 | 2011-10-19 | 华东理工大学 | Preparation method of hydrophobic immobilized photocatalyst with solar photocatalysis activity |
| CN102266792A (en) * | 2011-06-13 | 2011-12-07 | 华东理工大学 | Synthesis method for visible photocatalyst by modifying titanium dioxide by using ammonium fluoride |
| CN102218335B (en) * | 2011-06-13 | 2013-01-16 | 华东理工大学 | Preparation method of hydrophobic immobilized photocatalyst with solar photocatalysis activity |
| CN102266792B (en) * | 2011-06-13 | 2013-01-16 | 华东理工大学 | Synthesis method for visible photocatalyst by modifying titanium dioxide by using ammonium fluoride |
| CN104609468A (en) * | 2013-11-04 | 2015-05-13 | 天津大学 | Method for preparing anatase type titanium dioxide having porous hexagonal prism morphology, and applications of anatase type titanium dioxide having porous hexagonal prism morphology |
| CN104609468B (en) * | 2013-11-04 | 2016-11-02 | 天津大学 | A kind of method preparing the anatase titanium dioxide with porous hexagon looks and application thereof |
| CN108499582A (en) * | 2018-04-04 | 2018-09-07 | 昆明理工大学 | A kind of preparation method of composite photo-catalyst |
| CN109967062A (en) * | 2019-03-11 | 2019-07-05 | 浙江万里学院 | A kind of high energy crystal face exposure TiO2The preparation method of photochemical catalyst |
| CN111744512A (en) * | 2020-07-30 | 2020-10-09 | 内蒙古工业大学 | Narrow forbidden band low valence band modified TiO2Method for preparing photocatalyst |
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