CN104984766A - B/POMs/TiO2 ternary composite photocatalytic material and preparation method thereof - Google Patents

B/POMs/TiO2 ternary composite photocatalytic material and preparation method thereof Download PDF

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CN104984766A
CN104984766A CN201510453806.0A CN201510453806A CN104984766A CN 104984766 A CN104984766 A CN 104984766A CN 201510453806 A CN201510453806 A CN 201510453806A CN 104984766 A CN104984766 A CN 104984766A
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poms
tio
catalysis material
polyacid
tri compound
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CN104984766B (en
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李书军
彭青坡
陈学年
张絜
王若雅
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Henan Normal University
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Abstract

The invention discloses a B/POMs/TiO2 ternary composite photocatalytic material and a preparation method thereof, and belongs to the technical field of synthesis of composite photocatalytic material s. According to the technical scheme adopted by the invention, the key point is that the B/POMs/TiO2 ternary composite photocatalytic material with relatively high catalytic activity is prepared by selecting a sol-gel technology, selecting a proper precursor, and designing and optimizing a synthesis route. Compared with matrix TiO2 and POMs, the prepared B/POMs/TiO2 ternary composite photocatalytic material has a better application prospect in the photocatalytic field because of better visible light absorption activity and higher photocatalytic activity.

Description

One class B/POMs/TiO2 tri compound catalysis material and preparation method thereof
Technical field
The invention belongs to the synthesis technical field of composite photocatalyst material, be specifically related to a class B/POMs/TiO 2tri compound catalysis material and preparation method thereof.
Background technology
Since entering 21 century, the mankind are comfortable with simultaneously easily what enjoy that development in science and technology brings, and face two large crisis of survival also highlight day by day: the exhaustion day by day of the fossil energy such as coal, oil; Living environment runs down, and water body, atmosphere pollution are serious.Photocatalysis technology not only can utilize the pollutant in solar energy degradation water and air can also obtain clean energy resource-hydrogen by decomposition water.Therefore, the scientist of countries in the world drops into very large energy in exploration high-efficiency photocatalysis material.TiO 2be commonly used by people for the fields such as the organic and inorganic pollution of solar cell, photodissociation aquatic products hydrogen, photocatalysis organic reaction, purification of air, degraded owing to having the advantage such as efficient, cheap, stable, become one of catalysis material of most potentiality.But TiO 2there is wider band gap, therefore TiO 2can only ultraviolet light be absorbed, effectively can not utilize solar energy.In addition, TiO in photocatalytic process 2light induced electron and the hole of tool are easy to compound, greatly reduce its photocatalysis efficiency.Above-mentioned two shortcomings seriously constrain TiO 2practical application.
Achievement in research in recent years shows, utilizes specific preparation method to TiO 2carry out the doping of nonmetalloid (nitrogen, sulphur, carbon, phosphorus etc.), can effectively improve its visible light catalysis activity.Boron has the characteristic of electron deficient, and its ionic radius is little, coordination is flexible.The Richard M. Lambert(J. Am. Chem. Soc. 2007,129,13,790 13791 of Britain) and the Yijiao Jiang(ACS Catal. 2014,4,1,451 1457 of Poland) etc. research team find boron doped Ti O 2(B-TiO 2) can visible light catalytic be realized.Shandong University wears beautiful jade (J. Phys. Chem. C 2010,114,19830 – 19834) and Italian Gianfranco Pacchioni(J. Phys. Chem. C 2013,117,13,163 13172 subsequently) etc. team to B-TiO 2structure and electronic structure carried out theoretical research.It is found that, the doping of boron not only achieves the utilization to visible ray, and can by affecting TiO 2lattice structure and pattern, affect TiO 2surface charge and surface acidity improve its photocatalytic activity further.
Polyoxometallate (POMs) has reversible redox property, is also the outstanding catalysis material of a class.But this compounds often has very large solubility to be difficult to recycle in water and in organic solvent.TiO 2/ POMs is a class porous TiO 2the composite (J. Mol. Catal. A 2007,136 – 148) of load polyacid.This kind of material and parent TiO 2comparing with POMs and have lower band gap energy level, and have larger specific surface and porous, is a class heterogeneous photocatalyst.This kind of compound is in photocatalytic process, and POMs can effectively store light induced electron, effectively suppress TiO 2the compound of middle electron-hole, therefore catalytic efficiency improves greatly.
But, at present for B/POMs/TiO 2the synthesis of tri compound catalysis material and photocatalysis research there is not yet relevant report.This kind of material may have B-TiO concurrently 2and TiO 2the advantage of/POMs material, is expected to become more outstanding photochemical catalyst.
Summary of the invention
The technical problem that the present invention solves there is provided a class B/POMs/TiO 2tri compound catalysis material and preparation method thereof, by selecting suitable presoma, and design and optimum synthesis route obtain the B/POMs/TiO with high light catalytic activity 2tri compound catalysis material.
The present invention adopts following technical scheme for solving the problems of the technologies described above: a class B/POMs/TiO 2tri compound catalysis material, it is characterized in that: this tri compound catalysis material is made up of boron, polyacid and titanium dioxide, wherein polyacid is polyoxometallate, and this polyoxometallate is saturated Keggin-type polyacid, saturated Dawson type polyacid or single vacant polyacid.
Further preferably, described saturated Keggin-type polyacid is H 3pW 12o 40.
Further preferably, described saturated Dawson type polyacid is H 6p 2w 18o 62or K 5na 4[P 2w 15o 59(TaO 2) 3].
Further preferably, the vacant polyacid of described list is K 9bW 11o 39.
B/POMs/TiO of the present invention 2the preparation method of tri compound catalysis material, it is characterized in that comprising the following steps: isopropyl titanate and triethyl borate are dissolved in isopropyl alcohol and obtain solution A by (1), POMs is dissolved in deionized water and obtains solution B, under stirring condition, solution B to be dropped in solution A and ultrasonic disperse 10min obtains uniform colloidal sol; (2) in above-mentioned colloidal sol, drip the hydrochloric acid solution that molar concentration is 3mol/L, generate gel; (3) gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in reactor and to be heated to 200 DEG C and keeps 2h; (4) solid step (3) the obtained deionized water of 80 DEG C is repeatedly washed until eluent is in neutral, and the dry 12h of baking oven then product being placed in 50 DEG C obtains B/POMs/TiO 2tri compound catalysis material, wherein POMs is saturated Keggin-type polyacid H 3pW 12o 40or saturated Dawson type polyacid K 5na 4[P 2w 15o 59(TaO 2) 3].
B/POMs/TiO of the present invention 2the preparation method of tri compound catalysis material, it is characterized in that comprising the following steps: isopropyl titanate and triethyl borate are dissolved in isopropyl alcohol and obtain solution A by (1), POMs is dissolved in deionized water and obtains solution B, under stirring condition, solution B to be dropped in solution A and ultrasonic disperse 10min generates gel; (2) gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in reactor and to be heated to 200 DEG C and keeps 2h; (3) solid step (2) the obtained deionized water of 80 DEG C is repeatedly washed until eluent is in neutral, and the dry 12h of baking oven then product being placed in 50 DEG C obtains B/POMs/TiO 2tri compound catalysis material, wherein POMs is saturated Dawson type polyacid H 6p 2w 18o 62or single vacant polyacid K 9bW 11o 39.
The tri compound catalysis material that the present invention obtains is labeled as B/POMs/TiO 2-X-Y, in formula, POMs represents polyoxometallate, can be that saturated Keggin-type polyacid is (as H 3pW 12o 40) and saturated Dawson type polyacid (as H 6p 2w 18o 62or K 5na 4[P 2w 15o 59(TaO 2) 3]), also can be that single vacant polyacid is (as K 9bW 11o 39), X and Y represents the rear molar percentage of B/Ti of ICP test and the mass percentage of POMs respectively, can be controlled by the ratio of each material in preparation process.
The present invention is by selecting suitable presoma, and design and optimum synthesis route obtain the B/POMs/TiO2 tri compound catalysis material with high light catalytic activity, with parent TiO 2compare with POMs, obtained B/POMs/TiO 2tri compound catalysis material shows the photocatalytic activity of better visible absorption and Geng Gao, therefore has good application prospect in photocatalysis field.
Accompanying drawing explanation
Fig. 1 is the tri compound catalysis material B/H of the 2-in-1 one-tenth of the embodiment of the present invention 6p 2w 18o 62/ TiO 2to diffuse spectrogram with the solid of each raw material components, it has good absorption in visible region;
Fig. 2 is the tri compound catalysis material B/H of the 2-in-1 one-tenth of the embodiment of the present invention 6p 2w 18o 62/ TiO 2with the Powder XRD pattern of each raw material components, B/H 6p 2w 18o 62/ TiO 2xRD collection of illustrative plates show main body frame anatase TiO 2characteristic diffraction peak, illustrate that B and POMs disperses in the composite uniformly;
Fig. 3 is the tri compound catalysis material B/H of the 2-in-1 one-tenth of the embodiment of the present invention 6p 2w 18o 62/ TiO 2visible light catalysis activity design sketch, abscissa is the time, and ordinate is degraded residual concentration C 1with initial concentration C 0ratio.
Detailed description of the invention
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
B/H 3pW 12o 40/ TiO 2synthesis
9.0mL isopropyl titanate and 2.3mL triethyl borate are dissolved in 30mL isopropyl alcohol and obtains solution A, by 1.0g H 3pW 12o 40dissolve in 2.0mL deionized water and obtain solution B, under stirring condition, solution B slowly to be dropped in solution A and ultrasonic disperse 10min obtains uniform colloidal sol; Under vigorous stirring, in above-mentioned colloidal sol, dropwise add the hydrochloric acid solution of 3.0M, generate gel; This gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in 50mL reactor and to be heated to 200 DEG C and keeps 2 hours; Washed by obtained solid until eluent is in neutral several times by 80 DEG C of deionized waters, final products are placed in the dry 12 hours obtained product B/H of baking oven of 50 DEG C 3pW 12o 40/ TiO 2tri compound catalysis material.Products obtained therefrom is labeled as B/H 3pW 12o 40/ TiO 2-0.50-0.67, wherein 0.50 and 0.67 represents the molar percentage of B/Ti and H after ICP test respectively 3pW 12o 40mass percentage.
Embodiment 2
B/H 6p 2w 18o 62/ TiO 2synthesis
9.0mL isopropyl titanate and 2.3mL triethyl borate are dissolved in 30mL isopropyl alcohol and obtains solution A, by 1.0g H 6p 2w 18o 62dissolve in 2.0mL deionized water and obtain solution B, under stirring condition, solution B slowly to be dropped in solution A and to continue to be stirred to generation gel after ultrasonic disperse 10min; This gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in 50mL reactor and to be heated to 200 DEG C and keeps 2 hours; Washed by obtained solid until eluent is in neutral several times by 80 DEG C of deionized waters, final products are placed in the dry 12 hours obtained product B/H of baking oven of 50 DEG C 6p 2w 18o 62/ TiO 2tri compound catalysis material.Products obtained therefrom is labeled as B/H 6p 2w 18o 62/ TiO 2-0.50-0.53, wherein 0.50 and 0.53 represents the molar percentage of B/Ti and H after ICP test respectively 6p 2w 18o 62mass percentage.
Embodiment 3
B/K 5na 4[P 2w 15o 59(TaO 2) 3]/TiO 2synthesis
9mL isopropyl titanate and 2.3mL triethyl borate are dissolved in 30mL isopropyl alcohol and obtain solution A, by 1.0g K 5na 4[P 2w 15o 59(TaO 2) 3] be dissolved in 2.0mL deionized water and obtain solution B, under stirring condition, solution B slowly to be dropped in solution A and ultrasonic disperse 10min obtains uniform colloidal sol; Under vigorous stirring, in above-mentioned colloidal sol, dropwise add the hydrochloric acid solution of 3M, generate gel; This gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in 50mL reactor and to be heated to 200 DEG C and keeps 2 hours; Washed by obtained solid until eluent is in neutral several times by 80 DEG C of deionized waters, final products are placed in the dry 12 hours obtained product B/K of baking oven of 50 DEG C 5na 4[P 2w 15o 59(TaO 2) 3]/TiO 2tri compound catalysis material.Products obtained therefrom is labeled as B/K 5na 4[P 2w 15o 59(TaO 2) 3]/TiO 2-0.50-0.50, wherein 0.50 and 0.50 represents the molar percentage of B/Ti and K after ICP test respectively 5na 4[P 2w 15o 59(TaO 2) 3] mass percentage.
Embodiment 4
B/K 9bW 11o 39/ TiO 2synthesis
9.0mL isopropyl titanate and 2.3mL triethyl borate are dissolved in 30mL isopropyl alcohol and obtains solution A, by 1.0g K 9bW 11o 39dissolve in 2.0mL deionized water and obtain solution B, under stirring condition, solution B slowly to be dropped in solution A and ultrasonic disperse 10min obtains gel rapidly; This gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in 50mL reactor and to be heated to 200 DEG C and keeps 2 hours; Washed by obtained solid until eluent is in neutral several times by 80 DEG C of deionized waters, final products are placed in the dry 12 hours obtained product B/K of baking oven of 50 DEG C 9bW 11o 39/ TiO 2tri compound catalysis material.Products obtained therefrom is labeled as B/K 9bW 11o 39/ TiO 2-0.50-0.73, wherein 0.50 and 0.73 represents the molar percentage of B/Ti and K after ICP test respectively 9bW 11o 39mass percentage.
Embodiment 5
The test of photocatalytic activity
The excitation source of light-catalyzed reaction adopts 500W xenon lamp, and be placed on by xenon lamp in cold-trap, be evenly placed in equidistant for 50mL quartz ampoule around cold-trap, reactant liquor is contained in quartz ampoule.Light-catalyzed reaction step is as follows: get the rhodamine B (initial concentration that 50mL newly prepares c 0=10mg/L), add 0.05g catalysis material, use air pump air-blowing, lucifuge 30min, catalysis material is uniformly dispersed in reactant liquor and reaches adsorption-desorption balance.Open light source, every 10min sampling also centrifugation acquisition supernatant liquor, carry out UV-Vis spectrum test.As shown in Figure 3, with B/H 6p 2w 18o 62/ TiO 2for example, demonstrate better photocatalysis effect under visible light illumination, 25min degradation rate reaches 98%, is parent TiO 22.3 times.
Embodiment above describes general principle of the present invention, principal character and advantage; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.

Claims (7)

1. a class B/POMs/TiO 2tri compound catalysis material, it is characterized in that: this tri compound catalysis material is made up of boron, polyacid and titanium dioxide, wherein polyacid is polyoxometallate, and this polyoxometallate is saturated Keggin-type polyacid, saturated Dawson type polyacid or vacant polyacid.
2. B/POMs/TiO according to claim 1 2tri compound catalysis material, is characterized in that: described saturated Keggin-type polyacid is H 3pW 12o 40.
3. B/POMs/TiO according to claim 1 2tri compound catalysis material, is characterized in that: described saturated Dawson type polyacid is H 6p 2w 18o 62or K 5na 4[P 2w 15o 59(TaO 2) 3].
4. B/POMs/TiO according to claim 1 2tri compound catalysis material, is characterized in that: described vacant polyacid is K 9bW 11o 39.
5. a B/POMs/TiO 2the preparation method of tri compound catalysis material, it is characterized in that comprising the following steps: isopropyl titanate and triethyl borate are dissolved in isopropyl alcohol and obtain solution A by (1), POMs is dissolved in deionized water and obtains solution B, under stirring condition, solution B to be dropped in solution A and ultrasonic disperse 10min obtains uniform colloidal sol; (2) in above-mentioned colloidal sol, drip the hydrochloric acid solution that molar concentration is 3mol/L, generate gel; (3) gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in reactor and to be heated to 200 DEG C and keeps 2h; (4) solid step (3) the obtained deionized water of 80 DEG C is repeatedly washed until eluent is in neutral, and the dry 12h of baking oven then product being placed in 50 DEG C obtains B/POMs/TiO 2tri compound catalysis material, wherein POMs is saturated Keggin-type polyacid H 3pW 12o 40or saturated Dawson type polyacid K 5na 4[P 2w 15o 59(TaO 2) 3].
6. a B/POMs/TiO 2the preparation method of tri compound catalysis material, it is characterized in that comprising the following steps: isopropyl titanate and triethyl borate are dissolved in isopropyl alcohol and obtain solution A by (1), POMs is dissolved in deionized water and obtains solution B, under stirring condition, solution B to be dropped in solution A and ultrasonic disperse 10min generates gel; (2) gel is placed in the baking oven ageing 12h of 50 DEG C, products therefrom to be transferred in reactor and to be heated to 200 DEG C and keeps 2h; (3) solid step (2) the obtained deionized water of 80 DEG C is repeatedly washed until eluent is in neutral, and the dry 12h of baking oven then product being placed in 50 DEG C obtains B/POMs/TiO 2tri compound catalysis material, wherein POMs is saturated Dawson type polyacid H 6p 2w 18o 62or single vacant polyacid K 9bW 11o 39.
7. B/POMs/TiO according to claim 1 and 2 2the preparation method of tri compound catalysis material, is characterized in that: obtained B/POMs/TiO 2b and TiO in tri compound catalysis material 2the proportion adjustment of mass percentage by adding materials of Mole percent when POMs.
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CN107591488A (en) * 2016-07-08 2018-01-16 中国科学院苏州纳米技术与纳米仿生研究所 Multi-metal oxygen cluster compound metal complex oxide, its preparation method and application
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CN106362807A (en) * 2016-09-08 2017-02-01 河南师范大学 Visible light driven photocatalysis hydrogen production catalyst as well as preparation method and application thereof
CN106582641A (en) * 2016-12-05 2017-04-26 深圳清华大学研究院 TiO2-based nanometer heterojunction composite photocatalytic material and preparation method thereof
CN109967124A (en) * 2019-02-21 2019-07-05 河南师范大学 The multi-metal oxygen cluster of organic boron covalent modification, preparation method and its application in Photocatalyzed Hydrogen Production field

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