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Hollow shell-type titanium dioxide nano-material, silver-loaded hollow shell-type titanium dioxide nano-material, and preparation method thereof

A technology of titanium dioxide and nano-materials, applied in the field of inorganic nano-photocatalyst materials and their preparation, can solve the problems of low separation efficiency, unsuitability, and difficult degradation of photogenerated carriers, so as to improve photocatalytic reactivity, avoid easy agglomeration, The effect of improving separation efficiency

Active Publication Date: 2019-06-18
NORTHEAST GASOLINEEUM UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

But TiO 2 As a photocatalyst, there are two main problems: (1) TiO 2 The semiconductor band gap determines that it can only absorb light sources with a wavelength less than 387nm, the absorption rate of visible light is very poor, and the utilization rate of solar energy is low; (2) The separation efficiency of photogenerated carriers is low, and the utilization rate of photogenerated electrons is low
[0004] Chinese patent application CN201710683148.3 discloses a preparation method and application of a molybdenum disulfide-coated titanium dioxide hollow core-shell structure composite photocatalyst, although the composite photocatalyst prepared by the patent application can quickly and efficiently convert 4-nitrophenol It is reduced to 4-aminophenol, but this only converts the nitro group on the phenol into an amino group, but does not degrade the phenol body. As we all know, the reduction of nitro group is relatively easy, but the degradation of phenol is very difficult. Therefore, the patent The composite photocatalyst applied for is not suitable for treating phenol-containing wastewater; in addition, molybdenum disulfide is a sheet-like substance, and the loaded sheet-like substance (such as molybdenum disulfide, graphene oxide, etc.) is likely to cause the load and titanium dioxide. Severe agglomeration, serious loss of specific surface area of ​​the catalyst, thus affecting the degradation effect of the composite photocatalyst
Chinese patent application CN201310259237.7 discloses a silver-loaded nano-titanium dioxide photocatalyst and its preparation method, but the silver-loaded nano-titanium dioxide photocatalyst prepared by the patent application has poor degradation efficiency to methylene blue (MB). In the same period, the MB degradation can only reach about 70%; and as we all know, among the common refractory pollutants such as phenol, methylene blue (MB), rhodamine B (RhB) and methyl orange (MO), phenol is the most Refractory to degradation, MB is the easiest to degrade; therefore, the silver-loaded nano-titanium dioxide photocatalyst prepared by this patent application is also not suitable as a photocatalyst for treating phenol-containing wastewater

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  • Hollow shell-type titanium dioxide nano-material, silver-loaded hollow shell-type titanium dioxide nano-material, and preparation method thereof
  • Hollow shell-type titanium dioxide nano-material, silver-loaded hollow shell-type titanium dioxide nano-material, and preparation method thereof
  • Hollow shell-type titanium dioxide nano-material, silver-loaded hollow shell-type titanium dioxide nano-material, and preparation method thereof

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preparation example Construction

[0040] The present invention provides a kind of preparation method of hollow shell type titania nanometer material in the first aspect, described method comprises the following steps:

[0041] (1) Mix the resorcinol formaldehyde resin dispersion liquid and ammonia water with absolute ethanol to obtain a mixed liquid, and then add tetrabutyl titanate (butyl titanate) dropwise into the mixed liquid for reaction to obtain Reaction product solution; the volume ratio of the absolute ethanol, the resorcinol formaldehyde resin dispersion (RF dispersion), the ammonia water and the tetrabutyl titanate is (40~50): (4~ 6): (0.1~0.4): (0.75~1.5) (for example, 40:4:0.1:0.75, 40:4:0.2:0.75, 40:4:0.3:0.75, 40:4:0.4:0.75, 45: 5:0.1:1, 45:5:0.2:1, 45:5:0.3:1, 45:5:0.4:1, 50:6:0.1:1.5, 50:6:0.2:1.5, 50:6: 0.3:1.5 or 50:6:0.4:1.5); in the present invention, the ammonia water is an aqueous solution of ammonia, such as an aqueous solution containing 25 to 28 wt% of ammonia; in the present inventi...

Embodiment 1

[0067] Example 1: Hollow TiO 2 and the preparation experiment of HT@Ag.

[0068] ① Preparation of RF dispersion: Add 0.35mL of ammonia water to a solution of 40mL of distilled water and 16mL of absolute ethanol, put it in a three-necked flask, put the three-necked flask into a heat-collecting constant temperature magnetic stirrer, stir at room temperature for 1 hour, and add 0.4g Resorcinol, continue to stir for 0.5h, heat up to 30°C, add 0.56mL formaldehyde solution, react for 24h, centrifuge and wash three times with a mixed solution of absolute ethanol and distilled water to obtain a sample, then disperse in 40mL absolute ethanol to obtain RF dispersion liquid for use.

[0069] ②RF@TiO 2 Preparation: Take four 5mL RF dispersions and place them in 45mL of absolute ethanol and 0.10mL, 0.20mL, 0.30mL, and 0.35mL of ammonia solution, ultrasonically treat them for 0.5h, place them in a three-necked flask, and put the three-necked flask into the set In a thermal constant tempe...

Embodiment 2

[0078] Example 2: Hollow TiO 2 (HT) Experiments on the degradation of phenol.

[0079] Weigh 20 mg of the four HT nanoparticles in Example 1, respectively, and disperse them in four parts of 40 mL of phenol suspension solutions with a concentration of 400 μmol / L, and stir the four parts of phenol suspension solutions containing HT nanoparticles in a dark environment After 30 minutes to reach the adsorption-desorption equilibrium of phenol on the surface of the composite nanoparticles, turn on the high-pressure mercury lamp, take out 2mL of the suspension and centrifuge the catalyst after different time of illumination (taking a sample every 15min or 30min), and use the supernatant Liquid is analyzed (ultraviolet-visible spectrophotometer UV1900 / UV1901PCS), the ultraviolet-visible absorption spectrum figure of phenol and its intermediate product is as follows Figure 6 As shown, in the figure, the ultraviolet absorption peak corresponding to phenol is at 270nm, the abscissa Wa...

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Abstract

The invention relates to a hollow shell-type titanium dioxide nano-material, a silver-loaded hollow shell-type titanium dioxide nano-material, and a preparation method thereof. The preparation methodof the hollow shell-type titanium dioxide nano-material comprises following steps: absolute ethyl alcohol is adopted for uniform mixing of RF dispersion liquid and ammoniacal liquor, tetrabutyl titanate is added for reaction, and then centrifugation separation, washing, drying, and two step roasting are carried out so as to obtain the hollow shell-type titanium dioxide nano-material; wherein the volume ratio of the absolute ethyl alcohol, dispersion liquid, ammoniacal liquor, and tetrabutyl titanate is controlled to be (40-50) : (4-6) : (0.1-0.4) : (0.75-1.5). According to the preparation method, ultraviolet light radiation sedimentation method is adopted for precipitation of silver onto the surface of the hollow shell-type titanium dioxide nano-material so as to obtain the silver-loaded hollow shell-type titanium dioxide nano-material. The hollow shell-type titanium dioxide nano-material and the silver-loaded hollow shell-type titanium dioxide nano-material are anatase crystal form, and are high in degradation efficiency on phenol.

Description

technical field [0001] The invention belongs to the field of inorganic nano photocatalyst materials and preparation thereof, and in particular relates to a hollow shell type titanium dioxide nanometer material, a silver loaded hollow shell type titanium dioxide nanometer material and a preparation method thereof. Background technique [0002] The discharge of phenolic wastewater from industries such as petrochemical, pharmaceutical, pesticide, and papermaking has posed a serious threat to the environment, and high concentrations of phenolic wastewater can corrode skin and mucous membranes and damage the biological central nervous system. The traditional treatment methods of phenol-containing wastewater are: extraction method, adsorption method, chemical precipitation method, chemical oxidation method, etc., but these methods will cause secondary pollution to a certain extent, and the energy consumption is large, and the degradation is not complete. Under the environment of a...

Claims

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Application Information

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IPC IPC(8): C01G23/053B82Y40/00B01J23/50B01J35/10C02F1/30C02F101/34
Inventor 王雪芹王俊磊宋华柳艳修张娇静王园园
Owner NORTHEAST GASOLINEEUM UNIV