CN101559368B - Visible light active boron-nickel co-doped titanium dioxide solid solution catalyst and preparation method thereof - Google Patents
Visible light active boron-nickel co-doped titanium dioxide solid solution catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention relates to visible light active boron-nickel co-doped titanium dioxide solid solution catalyst and a preparation method thereof. The method uses titanium tetrachloride, boron-containing compound and soluble nickel salt as raw materials to prepare the material of the visible light active boron-nickel co-doped titanium dioxide solid solution catalyst by a spray pyrogenation method at atemperature of between 500 and 700 DEG C. The boron-nickel co-doped titanium dioxide solid solution synthesized by the method has high purity, good dispersion, has higher visible light photocatalysti c activity, and can be particularly used in the field of environmental pollution treatment. The method has simple process, easily-controlled condition, lower requirement on equipment and low cost, andis convenient for further enlargement of production.
Description
Technical field
The present invention relates to a kind of visible light active boron-nickel co-doped titanium dioxide solid solution catalyst and preparation method, belong to wet chemistry and make field of nanometer material technology.
Background technology
In recent years, as a kind of cheapness, stable, nontoxic, photochemical catalyst that catalytic performance is good, TiO
2Become the focus of photocatalysis technology area research.But because TiO
2Greater band gap (3.0～3.2eV), can only can not be made full use of solar energy by the following ultraviolet excitation of 387nm, and light-catalyzed reaction efficient is not high, has limited its real world applications.In order to expand TiO
2To the response of visible light, improve the efficient of utilizing sunshine, people are to TiO
2Photochemical catalyst has carried out a large amount of study on the modification, for example adopts that dye sensitization, noble metal loading, semiconductor are compound, metal ion and method such as nonmetallic ion-doped.Wherein, to TiO
2Doping vario-property is to improve the main means of its visible light catalytic ability.Early-stage Study focuses mostly on and mixes at metal ion (Fe, Co, Ni, La etc.), but introducing metal ion forms the carrier complex centre easily, reduce photocatalysis efficiency, and catalyst stability is not high.Subsequently, because mixing, nonmetallic ion (S, N, C, I etc.) can replace TiO
2In the part of O atom, semi-conductive valence band location is raise, dwindle the semiconductor energy gap, make it absorb band edge red shift and improve its catalytic activity, thereby become the focus of research at visible region.Except to TiO
2Carry out the doping of single-element, in recent years, nano-TiO
2Codope becomes TiO just day by day
2The research focus of photocatalysis field has excellent research and is worth and prospect.Many researchers are to codope TiO
2Study, the result shows, when doping elements is suitable, and can be at TiO
2The forbidden band in introduce doped energy-band, its forbidden band is narrowed, the less photon of energy can excitation electron generation transition, can absorbing wavelength long light, the photoresponse scope has been widened in the red shift of light absorption band edge, improve quantum efficiency, thereby helped the raising of photocatalysis efficiency.On single basis of mixing, light absorption red shift degree further strengthens, visible light-responded enhancing as the codope of S-N, B-S etc.; Codopes such as N and Fe, La and Ta can produce synergy, further improve photoresponse scope and photocatalytic activity; Zr doped Ti O
2Can significantly improve the catalytic capability of photochemical catalyst.About B and Ni codope TiO
2Bibliographical information is not seen in the research of photochemical catalyst as yet.
Have not yet to see patent report about the boron-nickel co-doped titanium dioxide Preparation of Catalyst, domestic about relating to codope TiO
2The patent of catalyst only limits to prepare N-In codope, N-S codope, N-Sn codope.As being precursor with the titanate esters, be adulterant with nitrogen-containing compound, indium salt, adopt the hydrolytic precipitation legal system be equipped with anatase mutually with the rutile nanometer N-In codope photochemical catalyst of mixed crystal (application number is 200710059504.0, and publication number is CN101130160) mutually; With the titanate esters is precursor, is adulterant with nitrogen-containing compound, pink salt, prepares the nano-photocatalyst (application number is 200710057891, and publication number is 101108336) of anatase phase with the hydrolysis precipitation method; The nano titanium oxide (application number is 200610040382, and publication number is 1850618) that is equipped with nitrogen and sulfur two-component doped type by the hydrolytic precipitation legal system.
The present invention utilizes spray pyrolysis to prepare the boron-nickel co-doped titanium dioxide solid solution catalyst material, and this material has very high visible light photocatalysis active, in the environmental pollution improvement field very big application potential is arranged; Technology of the present invention is simple, and condition is easily controlled, and is lower to the equipment requirement, being convenient to further extension and producing.
Summary of the invention
The object of the present invention is to provide synthetic boron-nickel co-doped titanium dioxide solid solution catalysis material of a kind of employing spray pyrolysis and preparation method, this boron-nickel co-doped titanium dioxide material has good visible light responsible photocatalytic performance.
Realize a kind of boron-nickel co-doped titanium dioxide photochemical catalyst of above-mentioned purpose, it is characterized in that: being precursor with the titanium tetrachloride, is adulterant with boron-containing compound, nickel salt, prepares the B-Ni codope TiO of anatase phase with spray pyrolysis
2Photochemical catalyst, this catalyst is formed in Quality Percentage, and the content of B is 0.99%, and the content of Ni is 0.7%, and all the other are TiO
2This catalyst is the micron ball of diameter in 0.5～10 mu m range.
The preparation method of described boron-nickel co-doped titanium dioxide photochemical catalyst, its preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 5-20mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration boron-containing compounds and divalent nickel salt solution, the content of solubility boron-containing compound is 5-20mmol/L in the solution, the content of nickel ion is 0.5-2mmol/L in the solution, and the molar content of boron compound is 10 times of molar content of nickel ion in the solution, and described solubility boron-containing compound is boric acid or sodium borohydride;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1, and the titanium ion molar concentration equates with the boron-containing compound molar concentration;
Step 4, the solution of step 3 gained is poured in the container of ultrasonic nebulizer, spray pyrolysis in 500～700 ℃ of air atmospheres reacted 0.5～2 hour;
Step 6, with the product of step 5 50 ℃ dry 3～10 hours down, can obtain flaxen boron-nickel co-doped titanium dioxide photocatalyst material.
Among the preparation method of boron-nickel co-doped titanium dioxide of the present invention, described divalent nickel salt is nickelous sulfate, nickel chloride or nickel nitrate.
Advantage of the present invention:
1, synthetic route is simple, and lower to the equipment requirement, whole technical process is controlled easily, the needs of realistic production;
2, He Cheng boron-nickel co-doped titanium dioxide solid solution material purity height, the particle size size is even, good dispersion;
3, the boron-nickel co-doped titanium dioxide solid solution material has very high visible light photocatalysis active, in the environmental pollution improvement field very big application potential is arranged.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of 10,000 times of amplifications of the boron-nickel co-doped titanium dioxide solid solution for preparing of the present invention
Fig. 2 is the scanning electron microscope diagram of 30,000 times of amplifications of the boron-nickel co-doped titanium dioxide solid solution for preparing of the present invention
Fig. 3 is the XRD figure of the boron-nickel co-doped titanium dioxide solid solution for preparing of the present invention
Fig. 4 is the XPS figure of the boron-nickel co-doped titanium dioxide solid solution for preparing of the present invention
Fig. 5 is the NO gas degraded-time graph of boron-nickel co-doped titanium dioxide solid solution under the simulated solar light action that the present invention prepares
The gained boron-nickel co-doped titanium dioxide solid solution is through observing (seeing Fig. 1) under 10,000 times of amplifications of scanning electron microscope diagram (JSM-5600), boron-nickel co-doped titanium dioxide solid solution is made up of the microballoon of diameter at 0.5～10 μ m, and preferably purity is arranged. Observed result (seeing Fig. 2) under 30,000 times of amplifications of SEM illustrates that the titanium dioxide solid solution microballoon is hollow-core construction. Gained boron-nickel co-doped titanium dioxide solid solution sample is tested through XRD, the characteristic peak of (seeing Fig. 3) in the diffracting spectrum and titanium dioxide standard diffracting spectrum (TiO2JCPDS 84-1285) peak value coincide. Gained boron-nickel co-doped titanium dioxide solid solution sample is tested through XPS, and XPS spectrum (seeing Fig. 4) illustrates that boron and nickel successfully are entrained in the titanium dioxide lattice, and wherein the mass content of B is that the mass content of 0.99%, Ni is 0.7%, and all the other are TiO2 It is the NO gas of 400ppb that the gained boron-nickel co-doped titanium dioxide solid solution catalyst is separated initial concentration in the decline of simulated solar light action, and degraded-time graph (seeing Fig. 5) illustrates that boron-nickel co-doped titanium dioxide solid solution catalyst has good visible light responsible photocatalytic activity.
The specific embodiment
Embodiment 1
Preparation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst, preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 5mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration boric acid and nickel chloride solution, the content of solution mesoboric acid is 5mmol/L; The content of nickel chloride is 0.5mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1;
Step 4, pour in the container of ultrasonic nebulizer at the solution of step 3 gained, spray pyrolysis in 500 ℃ of air atmospheres reacted 1 hour;
Step 6, with the product of step 5 50 ℃ dry 3 hours down, can obtain flaxen boron-nickel co-doped titanium dioxide solid solution photocatalyst material.
Gained boron-nickel co-doped titanium dioxide solid solution photocatalyst material is observed (see figure 1) down through 10,000 times of amplifications of scanning electron microscope diagram (JSM-5600), and boron-nickel co-doped titanium dioxide is made up of at the microballoon of 0.5～10 μ m diameter, and purity is preferably arranged.Observed result (see figure 2) explanation titanium dioxide solid solution microballoon under 30,000 times of amplifications of SEM is a hollow-core construction.Gained boron-nickel co-doped titanium dioxide solid solution sample is tested through XRD, the characteristic peak of (see figure 3) and titanium dioxide standard diffracting spectrum (TiO in the diffracting spectrum
2JCPDS 84-1285) peak value coincide.Gained boron-nickel co-doped titanium dioxide sample is tested through XPS, and XPS spectrum (see figure 4) explanation boron and nickel successfully are entrained in the titanium dioxide lattice.Wherein the mass content of B is 0.99%, and the mass content of Ni is 0.7%, and all the other are TiO
2The gained boron-nickel co-doped titanium dioxide solid solution catalyst descends at the simulated solar light action and separates the NO gas that initial concentration is 400ppb, and degraded-time graph (see figure 5) explanation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst has good visible light responsible photocatalytic activity.
Embodiment 2
Preparation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst, preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 20mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration boric acid and nickel chloride solution, the content of solution mesoboric acid is 20mmol/L; The content of nickel chloride is 2mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1;
Step 4, pour in the container of ultrasonic nebulizer at the solution of step 3 gained, spray pyrolysis in 600 ℃ of air atmospheres reacted 2 hours;
Step 6, with the product of step 5 50 ℃ dry 10 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide solid solution photocatalyst material.
Embodiment 3
Preparation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst, preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 10mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration sodium borohydrides and nickel sulfate solution, the content of sodium borohydride is 10mmol/L in the solution; The content of nickelous sulfate is 1mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1;
Step 4, pour in the container of ultrasonic nebulizer at the solution of step 3 gained, spray pyrolysis in 700 ℃ of air atmospheres reacted 0.5 hour;
Step 6, with the product of step 5 50 ℃ dry 5 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide solid solution photocatalyst material.
Embodiment 4
Preparation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst, preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 20mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration sodium borohydrides and nickel sulfate solution, the content of sodium borohydride is 20mmol/L in the solution; The content of nickelous sulfate is 2mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1;
Step 4, pour in the container of ultrasonic nebulizer at the solution of step 3 gained, spray pyrolysis in 700 ℃ of air atmospheres reacted 2 hours;
Step 6, with the product of step 5 50 ℃ dry 10 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide solid solution photocatalyst material.
Preparation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst, preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 5mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration boric acid and nickel nitrate solution, the content of solution mesoboric acid is 5mmol/L; The content of nickel ion is 0.5mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1;
Step 4, pour in the container of ultrasonic nebulizer at the solution of step 3 gained, spray pyrolysis in 600 ℃ of air atmospheres reacted 2 hours;
Step 6, with the product of step 5 50 ℃ dry 5 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide solid solution photocatalyst material.
Embodiment 6
Preparation boron-nickel co-doped titanium dioxide solid solution photochemical catalyst, preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 20mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration sodium borohydrides and nickel nitrate solution, the content of sodium borohydride is 20mmol/L in the solution; The content of nickel ion is 2mmol/L in the solution;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1;
Step 4, pour in the container of ultrasonic nebulizer at the solution of step 3 gained, spray pyrolysis in 700 ℃ of air atmospheres reacted 2 hours;
Step 6, with the product of step 5 50 ℃ dry 3 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide solid solution photocatalyst material.
Degraded-the time graph of the composition of embodiment 2～6 gained samples, pattern, structure, XPS spectrum and degraded NO gas is identical with embodiment 1.
Claims (3)
1. boron-nickel co-doped titanium dioxide photochemical catalyst is characterized in that: this catalyst is formed in Quality Percentage, and the content of B is 0.99%, and the content of Ni is 0.7%, and all the other are TiO
2, catalyst is the micron ball of diameter in 0.5～10 mu m range, preparation as follows, and preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 5-20mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration boron-containing compounds and divalent nickel salt solution, the content of solubility boron-containing compound is 5-20mmol/L in the solution, the content of nickel ion is 0.5-2mmol/L in the solution, and the molar content of boron compound is 10 times of molar content of nickel ion in the solution, and described solubility boron-containing compound is boric acid or sodium borohydride;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1, and the titanium ion molar concentration equates with the boron-containing compound molar concentration;
Step 4, the solution of step 3 gained is poured in the container of ultrasonic nebulizer, spray pyrolysis in 500～700 ℃ of air atmospheres reacted 0.5～2 hour;
Step 5, after the course of reaction of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product more than 3 times;
Step 6, with the product of step 5 50 ℃ dry 3～10 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide photocatalyst material.
2. the preparation method of the described boron-nickel co-doped titanium dioxide photochemical catalyst of claim 1 is characterized in that preparation process is:
Step 1, employing titanium tetrachloride are raw material, under stirring condition, are configured to titanium tetrachloride solution with 4 ℃ of distilled water, and the content of titanium ion is 5-20mmol/L in the solution;
Step 2, in another container, with 4 ℃ of distilled water configuration boron-containing compounds and divalent nickel salt solution, the content of solubility boron-containing compound is 5-20mmol/L in the solution, the content of nickel ion is 0.5-2mmol/L in the solution, and the molar content of boron compound is 10 times of molar content of nickel ion in the solution, and described solubility boron-containing compound is boric acid or sodium borohydride;
Step 3, be under the stirring condition at the solution of step 1 gained, the solution of step 2 gained poured in the solution of step 1 gained, the volume ratio of two kinds of solution is 1: 1, and the titanium ion molar concentration equates with the boron-containing compound molar concentration;
Step 4, the solution of step 3 gained is poured in the container of ultrasonic nebulizer, spray pyrolysis in 500～700 ℃ of air atmospheres reacted 0.5～2 hour;
Step 5, after the course of reaction of step 4 finishes, solid product is filtered, and with distilled water or ethanol drip washing product more than 3 times;
Step 6, with the product of step 5 50 ℃ dry 3～10 hours down, promptly obtain flaxen boron-nickel co-doped titanium dioxide photocatalyst material.
3. the preparation method of boron-nickel co-doped titanium dioxide photochemical catalyst according to claim 2 is characterized in that: described divalent nickel salt is nickelous sulfate, nickel chloride or nickel nitrate.
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| CN102500375B (en) * | 2011-09-28 | 2013-10-30 | 江苏科技大学 | Method for preparing titanium dioxide codoped with boron and metal element |
| CN103007968B (en) * | 2012-12-21 | 2014-12-03 | 华中师范大学 | Method for preparing bismuth oxychloride micro-sphere photocatalyst by ultrasonic spraying method |
| CN103252240A (en) * | 2013-04-07 | 2013-08-21 | 华东理工大学 | A solvothermal method for solid solution catalyst NixM1-x-yMgyO (M is Ce, co, sn, mn) used for dry gas reforming of CH4-CO2 |
| CN103877694B (en) * | 2014-03-13 | 2016-05-25 | 江苏大学 | A kind of TiO2The method of the organic pollution visible ray anaerobic degradation of nano material mediation |
| CN104611768B (en) * | 2014-12-31 | 2017-08-25 | 上海师范大学 | A kind of ullrasonic spraying drying prepares mesoporous single crystals TiO2Method |
| CN106582657B (en) * | 2016-12-21 | 2019-01-15 | 郑州师范学院 | A kind of TiO2- M-B cooperative photocatalysis agent and its preparation method and application |
| CN106861732A (en) * | 2017-01-25 | 2017-06-20 | 平顶山学院 | A kind of boron nickel titanium dioxide/nitridation carbon composite photocatalyst, and application thereof and preparation method |
| CN106824237A (en) * | 2017-03-15 | 2017-06-13 | 哈尔滨师范大学 | Ta‑F‑P‑TiO2Nano-photocatalyst and preparation method thereof |
| CN107282033B (en) * | 2017-06-28 | 2018-09-21 | 天津朗华科技发展有限公司 | A kind of photochemical catalyst and preparation method thereof for air V OC processing |
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| CN1600424A (en) * | 2003-09-22 | 2005-03-30 | 中国科学院化学研究所 | Photocatalyst responding to visible light, and preparation method and application |
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