Photocatalyst with broadband spectrum response and preparation method thereof

A photocatalyst and broad spectrum technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of insufficient light response range, low quantum efficiency of composite materials, etc., to improve catalytic performance , the effect of broadening the spectral response range and increasing the lifespan

Inactive Publication Date: 2017-11-07

江苏科来材料科技有限公司

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AI-Extracted Technical Summary

Problems solved by technology

However, the quantum efficiency of the composite material of this method...

Method used

The present invention has combined the method for ion doping and semiconductor compound, Fe, N doping and bismuth tungstate titanium dioxide are combined, improve catalytic efficiency on the one hand, on the other hand the spectral response range of photocataly...

Abstract

The invention provides a preparation method for a photocatalyst with broadband spectrum response. The photocatalyst with broadband spectrum response is a nitrogen iron-doped bismuth tungstate compound titanium dioxide nano-particle or nano-tube. The preparation method for the photocatalyst with broadband spectrum response comprises the following steps: preparing a titanium dioxide nanometer material; doping nitrogen and iron into the titanium dioxide nanometer material; and preparing the nitrogen iron-doped bismuth tungstate compound titanium dioxide nanometer material. The invention combines ion doping modifying and semiconductor compound modifying techniques for expanding the ultraviolet part of the photocatalyst with broadband spectrum response scope below 387nm to a near-infrared band, the visible light and near-infrared light response of the nanometer titanium dioxide photocatalyst is realized and the catalytic activity of the nanometer carbon dioxide photocatalyst is enhanced.

Application Domain

Physical/chemical process catalysts

Technology Topic

BroadbandSemiconductor +13

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Examples

Experimental program(3)

Example Embodiment

[0064] A preparation method of a photocatalyst with wide spectral response, the photocatalyst with wide spectral response is nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterial, and the preparation method of the photocatalyst with wide spectral response is as follows:

[0065] 1. Preparation of titanium dioxide nanomaterials; the titanium dioxide nanomaterials are titanium dioxide nanoparticles or titanium dioxide nanotubes;

[0066] 2. Nitrogen-iron doping of titanium dioxide nanomaterials;

[0067] 3. Preparation of nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterials.

[0068] Wherein, in the step 1), nano-titanium dioxide nanoparticles can be prepared by evaporative condensation method, sol-gel method, and hydrothermal method, or titanium dioxide nanotubes can be prepared by hydrothermal method, template method, anodization method, and crystal powder digestion method. However, the preparation of titania nanoparticles or titania nanotubes is not limited to these methods.

[0069] Wherein, the steps of preparing titanium dioxide nanotubes by hydrothermal method are as follows:

[0070] 1.1), the TiO 2 The powder particles are dissolved in the NaOH solution and stirred until well mixed;

[0071] 1.2), put the above-mentioned solution into the autoclave, the temperature is 120~180 ℃ constant temperature for 48h, and then naturally cooled to room temperature;

[0072] 1.3), put the cooled sample into the centrifuge for centrifugation, and then add deionized water until the pH value is nearly neutral;

[0073] 1.4), wash the sample with hydrochloric acid solution, and then wash the sample with deionized water until the pH value is near neutral;

[0074] 1.5), use a centrifuge to separate, and obtain titanium dioxide nanotubes after drying.

[0075] Preferably, the concentration of the NaOH solution in step 1.1) is 5-15 mol/L.

[0076] Preferably, TiO in step 1.1) 2 The mass fraction in the NaOH solution is 5-9% wt.

[0077] Preferably, the autoclave used in step 1.2) is a polytetrafluoroethylene lined autoclave.

[0078] Preferably, the concentration of the hydrochloric acid solution in step 1.4) is 0.1 mol/L.

[0079] Preferably, the drying temperature in step 1.5) is 60-100°C.

[0080] Wherein, the step 2) the method for doping titanium dioxide nanomaterials with nitrogen and iron has the following steps:

[0081] 2.1), put the titanium dioxide nanomaterial prepared in step 1) into the ferric nitrate solution and soak;

[0082] 2.2) Put the above materials into a tube furnace, maintain an ammonia gas atmosphere, and heat to obtain a titanium dioxide nanomaterial co-doped with iron and nitrogen.

[0083] Preferably, the concentration of the ferric nitrate solution in the step 2.1) is 0.05-0.2 mol/L.

[0084] Preferably, the soaking time in the step 2.1) is 24h.

[0085] Preferably, the heating temperature in the step 2.2) is 400-500°C, and the heating is performed for 2-3 hours.

[0086] Among them, a nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterial is prepared by a hydrothermal method.

[0087] Preferably, the steps of preparing nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterials are as follows:

[0088] 3.1), the Bi (NO 3 ) 3.5H 2 O and Na 2 WO 4.2H 2 O was dissolved in the ethylene glycol solution and stirred until fully mixed;

[0089] 3.2), the above-mentioned solution is moved into the hydrothermal reactor, and wherein step 2) is put into the prepared titanium dioxide nanomaterial, and the reaction is naturally cooled to room temperature after finishing;

[0090] 3.3), rinse the obtained product alternately with deionized water and absolute ethanol, and then put it into a drying oven to dry, to obtain nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterials.

[0091] Preferably, in step 3.1) Bi(NO 3 ) 3.5H 2 O and Na 2 WO 4.2H 2 O is respectively dissolved in ethylene glycol solution, and the mass fractions are 0.5-1% wt and 0.2-0.4% wt respectively.

[0092] Preferably, in step 3.2), the hydrothermal reaction is performed for 10 to 20 hours, and the temperature is 120 to 200°C.

[0093] Preferably, the hydrothermal reactor in step 3.2) is a hydrothermal reactor containing polytetrafluoroethylene lining.

[0094] Preferably, in step 3.3), the sample is washed alternately with deionized water and absolute ethanol for 5 to 8 times.

[0095] Preferably, the drying conditions in step 3.3) are drying in a drying oven at 50-90° C. for 12 hours.

[0096] The photocatalyst with broad spectral response prepared by the method of the invention is a nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterial.

[0097] The nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterial has the following structure: Fe replaces part of tetravalent Ti in the form of ferric iron 4+ TiO is present 2 In the lattice, N-substituted O intercalates into TiO 2 lattice, forming an N-Ti-O grid structure. Titanium dioxide exists in the form of anatase phase, bismuth tungstate exists in orthorhombic system, and bismuth tungstate is uniformly dispersed on titanium dioxide, and the two form a heterojunction structure.

[0098] In the nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanomaterial, the content of bismuth tungstate is 15-25%.

[0099] Preferably, the content of bismuth tungstate is 20%.

Example Embodiment

[0100] Example 1

[0101] A broad spectral response photocatalyst prepared by:

[0102] 1. Preparation of TiO2 Nanotubes

[0103] 1.1, the TiO 2 The powder particles were dissolved in 10mol/L NaOH solution and stirred until fully mixed; TiO 2 The mass fraction in NaOH solution is 7%wt;

[0104] 1.2. Put the above solution into an autoclave containing a polytetrafluoroethylene lining, keep the temperature at 160°C for 48h, and then naturally cool to room temperature;

[0105] 1.3. Put the cooled sample into a centrifuge for centrifugation, and then add deionized water until the pH value is nearly neutral;

[0106] 1.4. Wash the sample with hydrochloric acid solution with a concentration of 0.1mol/L, and then wash the sample with deionized water until the pH value is nearly neutral;

[0107] 1.5. Use a centrifuge to separate, and obtain titanium dioxide nanotubes after drying at 80 °C;

[0108] 2. Nitrogen-iron doping of titanium dioxide nanotubes

[0109] 2.1. Put the titanium dioxide nanotubes prepared in step 1 into a ferric nitrate solution with a concentration of 0.1 mol/L, and soak for 24 hours;

[0110] 2.2. Put the above samples into a tube furnace, maintain an ammonia atmosphere, and heat at a temperature of 450°C for 2 hours to obtain iron and nitrogen co-doped titanium dioxide nanotubes;

[0111] 3. Preparation of bismuth tungstate composite titanium dioxide nanotubes

[0112] 3.1. The Bi (NO3 ) 3.5H 2 O and Na 2 WO 4.2H 2 O was dissolved in ethylene glycol solution, the mass fractions were 1%wt and 0.3%wt, respectively, and stirred until fully mixed;

[0113] 3.2, the above solution is moved into the hydrothermal reactor containing the polytetrafluoroethylene lining, and the titanium dioxide nanotubes prepared in step 2 are placed therein, and the reaction is naturally cooled to room temperature after finishing;

[0114] 3.3. Rinse the sample alternately with deionized water and absolute ethanol for 8 times, and then put it in a drying oven at 90°C for drying for 12 hours to obtain nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanotubes.

[0115] The product prepared in this example is confirmed to be the target product nitrogen-iron-doped bismuth tungstate composite titanium dioxide nanotube through XRD and EDS phase analysis. Its absorption spectrum is shown in figure 1 and figure 2. from figure 1 It can be seen that compared with titanium dioxide and single-ion-doped titanium dioxide (respectively, composite bismuth tungstate alone and nitrogen and iron doping alone), the present invention has higher absorption capacity and absorption efficiency in the range of ultraviolet to visible light. from figure 2 It can be seen that, compared with the composite of titanium dioxide and single semiconductor, the present invention has higher absorption capacity and absorption efficiency in the range of visible light to near-infrared light.

[0116] From the perspective of absorption spectrum, the photocatalyst prepared by the invention produces near-infrared absorption on the one hand, realizes broad-spectrum photocatalysis, and realizes the support of electrons and holes in different semiconductors due to the generation of coupled heterojunctions. The efficient separation of currents increases the photocatalytic efficiency.

Example Embodiment

[0117] Example 2

[0118] 1. Preparation of TiO2 Nanotubes

[0119] 1.1, the TiO 2 The powder particles were dissolved in 15mol/L NaOH solution and stirred until fully mixed; TiO 2 The mass fraction in NaOH solution is 5%wt;

[0120] 1.2. Put the above solution into an autoclave containing a polytetrafluoroethylene lining, keep the temperature at 180°C for 48h, and then naturally cool to room temperature;

[0121] 1.3. Put the cooled sample into a centrifuge for centrifugation, and then add deionized water until the pH value is nearly neutral;

[0122] 1.4. Wash the sample with hydrochloric acid solution with a concentration of 0.1mol/L, and then wash the sample with deionized water until the pH value is nearly neutral;

[0123] 1.5. Use a centrifuge to separate, and obtain titanium dioxide nanotubes after drying at 100 °C;

[0124] 2. Nitrogen-iron doping of titanium dioxide nanotubes

[0125] 2.1. Put the titanium dioxide nanotubes prepared in step 1 into a ferric nitrate solution with a concentration of 0.2mol/L, and soak for 24h;

[0126] 2.2. Put the above samples into a tube furnace, maintain an ammonia atmosphere, and heat at a temperature of 500 ° C for 2 hours to obtain iron and nitrogen co-doped titanium dioxide nanotubes;

[0127] 3. Preparation of bismuth tungstate composite titanium dioxide nanotubes

[0128] 3.1. The Bi (NO 3 ) 3.5H 2 O and Na 2 WO 4.2H 2 O was dissolved in ethylene glycol solution, the mass fractions were 0.5%wt and 0.4%wt, respectively, and stirred until fully mixed;

[0129] 3.2, the above solution is moved into the hydrothermal reactor containing the polytetrafluoroethylene lining, and the titanium dioxide nanotubes prepared in step 2 are placed therein, and the reaction is naturally cooled to room temperature after finishing;

[0130] 3.3. Rinse the sample alternately with deionized water and anhydrous ethanol for 5 times, and then put it in a drying oven at 50°C for 12 hours to obtain bismuth tungstate composite titanium dioxide nanotubes.

PUM

Property	Measurement	Unit
Concentration	0.05 ~ 0.2	mol/l
Concentration	0.1	mol/l

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Classification and recommendation of technical efficacy words

Improve catalytic performance
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Photocatalyst with broadband spectrum response and preparation method thereof

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

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