阅读说明：本技术 一种二氧化锡/聚苯胺纳米线复合光催化剂的制备方法 (Preparation method of tin dioxide/polyaniline nanowire composite photocatalyst ) 是由 孙丰强 杨思娴 李超贤 苏秋瑶 何谷平 于 2020-05-08 设计创作，主要内容包括：本发明属于材料化学领域,具体涉及一种二氧化锡/聚苯胺纳米线复合光催化剂的制备方法,包括以下步骤：S1.制备聚苯胺纳米线；S2.将步骤S1制备得到的聚苯胺纳米线与二氧化锡前驱体溶液混合并搅拌均匀得到混合悬浊液,其中混合悬浊液中Sn<Sup>2+</Sup>与聚苯胺纳米线的质量比为：(4～30):1；S3.将步骤S2得到的混合悬浊液置于紫外灯下辐射,保留沉淀物纯化即得。制得的二氧化锡/聚苯胺纳米线复合光催化剂具有光催化性能优异,性能稳定等特点。在降解有机污染物方面有较好的应用前景。(The invention belongs to the field of material chemistry, and particularly relates to a preparation method of a tin dioxide/polyaniline nanowire composite photocatalyst, which comprises the following steps: s1, preparing polyaniline nanowires; s2, mixing the polyaniline nanowires prepared in the step S1 with a tin dioxide precursor solution, and uniformly stirring to obtain a mixed suspension, wherein Sn is contained in the mixed suspension 2+ The mass ratio of the polyaniline nano-wire to the polyaniline nano-wire is as follows: (4-30) 1; and S3, placing the mixed suspension obtained in the step S2 under an ultraviolet lamp for radiation, and keeping the precipitate for purification. The prepared stannic oxide/polyaniline nanowire composite photocatalyst has the characteristics of excellent photocatalytic performance, stable performance and the like. Has better effect on degrading organic pollutantsAnd the application prospect is good.)

1. A preparation method of a tin dioxide/polyaniline nanowire composite photocatalyst is characterized by comprising the following steps:

s1, preparing polyaniline nanowires;

s2, mixing the polyaniline nanowires prepared in the step S1 with a tin dioxide precursor solution, and uniformly stirring to obtain a mixed suspension, wherein Sn is contained in the mixed suspension²⁺The mass ratio of the polyaniline nano-wire to the polyaniline nano-wire is as follows: (4-30): 1;

and S3, placing the mixed suspension obtained in the step S2 under an ultraviolet lamp for radiation, and keeping the precipitate for purification.

2. The method for preparing the tin dioxide/polyaniline nanowire composite photocatalyst as claimed in claim 1, wherein in the step S3, the power of the ultraviolet lamp is 1-200W, the dominant wavelength range is 250-380 nm, and the irradiation intensity is 0.05-2.0 mW/cm²The irradiation time is 0.1-24 h.

3. The method for preparing the tin dioxide/polyaniline nanowire composite photocatalyst as claimed in claim 1, wherein in the step S1, the polyaniline nanowire is prepared by oxidizing aniline in an acidic medium with an oxidant.

4. The method for preparing the tin dioxide/polyaniline nanowire composite photocatalyst as claimed in claim 3, wherein the acidic medium is one of a nitric acid solution, an acetic acid solution, a hydrochloric acid solution, a sulfuric acid solution and a formic acid solution.

5. The preparation method of the tin dioxide/polyaniline nanowire composite photocatalyst as claimed in claim 3, wherein the molar ratio of the aniline to the oxidant is 1: (0.1-10).

6. The method for preparing the tin dioxide/polyaniline nanowire composite photocatalyst as claimed in claim 1, wherein in the step S2, the tin dioxide precursor solution is prepared by dissolving a divalent tin ion salt in a non-oxidizing acid solution with a concentration of 0.01-10 mol/L.

7. The preparation method of the tin dioxide/polyaniline nanowire composite photocatalyst as claimed in claim 6, wherein the stannous ion salt is one or more of stannous chloride, stannous sulfate and stannous nitrate.

8. The tin dioxide/polyaniline nanowire composite photocatalyst prepared by the preparation method of the tin dioxide/polyaniline nanowire composite photocatalyst as described in any one of claims 1 to 7.

9. The use of the tin dioxide/polyaniline nanowire composite photocatalyst as described in claim 8 in sewage treatment.

10. The application of the tin dioxide/polyaniline nanowire composite photocatalyst in sewage treatment according to claim 9 is characterized by being applied to degradation of rhodamine B.

Technical Field

The invention belongs to the field of material chemistry, and particularly relates to a preparation method of a tin dioxide/polyaniline nanowire composite photocatalyst.

Technical Field

The dye is used as an important chemical raw material and widely applied to the fields of food, textile, papermaking and the like. During the production and use of the dye, a large amount of waste water is generated, and the traditional biochemical treatment method is difficult to effectively degrade the dye. The photocatalytic degradation technology is an effective way for environmental management and obtaining clean energy, the photocatalyst can be effectively applied to the degradation of organic matters in various waste water and waste gas, and the development of the high-efficiency photocatalyst draws general attention in recent years.

Semiconductor oxide SnO₂Is a commonly used semiconductor photocatalyst material. However, it is usually SnO with a large band gap width (3.6eV) and different particle sizes₂The catalyst has different specific surface areas, and the specific surface areas directly influence the catalytic performance of the catalyst, so that the reduction of the forbidden band width and the increase of the specific surface areas are very important for enhancing the photocatalytic capability. When tin dioxide is used alone as a photocatalyst, the activity is generally low and the application is limited to some extent. The recombination is a method for effectively improving the photocatalytic activity of the material, and the electron-hole transfer in a system can be improved and the photocatalytic activity is enhanced through the recombination of semiconductors.

Polyaniline (PANI) is a common conductive polymer material, and has a conjugated structure, so that the polyaniline has special proton doping property, environmental stability and high doping conductivity, which attracts extensive attention, but the polyaniline is difficult to characterize and process at a later stage, and is not beneficial to practical popularization and application. The composite modification technology can effectively improve the processing performance and continuously broaden the application field of the conductive polyaniline.

The research on photochemical method is less in the preparation of semiconductor materials, and the exploration of photochemical synthesis of semiconductors, especially semiconductor composite materials, is a very challenging and important topic. China, 201210218542.7[ P ]. 2012-10-03), a preparation method of a tin dioxide/polyaniline composite material adopts a sol-gel method to prepare a tin dioxide nano powder material, and then adopts a microemulsion in-situ polymerization method to prepare the tin dioxide/polyaniline composite material, but the synthesis process of the tin dioxide is difficult to control, the stability is poor, and organic alcohol is adopted as a solvent and is not friendly to the environment. In the prior art, tin dioxide is synthesized by photochemical method, then aniline and oxidant are added into acid solution dispersed with tin dioxide, and the tin dioxide/polyaniline composite material is prepared by in-situ chemical oxidation polymerization method, but the appearance is difficult to control. Meanwhile, when the existing tin dioxide/polyaniline composite material is prepared, tin dioxide is prepared firstly and then polyaniline is compounded, so that polyaniline is easy to cover the surface of tin dioxide, and when the composite material is used as a photocatalytic material, the surface active sites of tin dioxide are not covered, so that the enhancement effect is influenced.

Disclosure of Invention

The invention aims to overcome the problems in the prior art and provides a preparation method of a tin dioxide/polyaniline nanowire composite photocatalyst with a regular morphology and application of the photocatalyst prepared by the method in anhydrous treatment.

The purpose of the invention is realized by the following technical scheme:

a preparation method of a tin dioxide/polyaniline nanowire composite photocatalyst comprises the following steps:

s1, preparing polyaniline nanowires;

s2, mixing the polyaniline nanowires prepared in the step S1 with a tin dioxide precursor solution, and uniformly stirring to obtain a mixed suspension, wherein Sn is contained in the mixed suspension²⁺The mass ratio of the polyaniline nano-wire to the polyaniline nano-wire is as follows: (4-30) 1;

and S3, placing the mixed suspension obtained in the step S2 under an ultraviolet lamp for radiation, and keeping the precipitate for purification.

Preferably, in the step S3, the power of the ultraviolet lamp is 1-200W, the dominant wavelength range is 250-380 nm, and the irradiation intensity is 0.05-2.0 mW/cm²The irradiation time is 0.1-24 h.

Preferably, in the step S1, the polyaniline nanowires are prepared by oxidizing aniline with an oxidant in an acidic medium.

Preferably, the acidic medium is one of a nitric acid solution, an acetic acid solution, a hydrochloric acid solution, a sulfuric acid solution and a formic acid solution.

Preferably, the oxidant is one or more of ammonium persulfate, potassium persulfate, sodium persulfate, potassium ferricyanide, copper chloride, potassium dichromate, potassium permanganate, ferric trichloride, silver nitrate and hydrogen peroxide.

Preferably, the molar ratio of aniline to oxidant is 1: (0.1-10).

Preferably, in the step S2, the tin dioxide precursor solution is prepared by dissolving a divalent tin ion salt in a non-oxidizing acid solution with a concentration of 0.01 to 10 mol/L.

Preferably, the divalent tin ion salt is one or more of stannous chloride, stannous sulfate and stannous nitrate.

The tin dioxide/polyaniline nanowire composite photocatalyst is prepared by the preparation method of the tin dioxide/polyaniline nanowire composite photocatalyst.

The tin dioxide/polyaniline nanowire composite photocatalyst is applied to sewage treatment.

The tin dioxide/polyaniline nanowire composite photocatalyst is applied to degradation of rhodamine B.

Compared with the prior art, the invention has the following technical effects:

according to the preparation method of the tin dioxide/polyaniline nanowire composite photocatalyst, the polyaniline nanowire with a regular shape is prepared, and then the tin dioxide is compounded with the polyaniline nanowire by a photochemical method to obtain the composite material, so that the limitation that the shape is difficult to control can be overcome, and the coverage of active sites on the surface of the tin dioxide can be avoided. The method has the advantages of mild reaction conditions, environment-friendly aqueous system, energy conservation, low consumption, easy control of reaction, high material utilization rate, less waste liquid and simple equipment, and can react at room temperature. The prepared stannic oxide/polyaniline nanowire composite photocatalyst has the characteristics of excellent photocatalytic performance, stable performance and the like. Has better application prospect in the aspect of degrading organic pollutants.

Drawings

FIG. 1 is an SEM representation of polyaniline nanowires;

FIG. 2 is an SEM representation of a tin dioxide/polyaniline nanowire binary composite material;

FIG. 3 shows FT-IR during synthesis, where curve a is FT-IR of PANI and curve b is SnO₂FT-IR plot of/PANI; curve c is SnO₂FT-IR diagram of (1);

FIG. 4 is a graph showing the degradation rate of rhodamine B during the preparation of a tin dioxide/polyaniline nanowire binary composite material under illumination;

FIG. 5 is a graph showing the degradation rate of rhodamine B as a function of the amount of polyaniline used in a tin dioxide/polyaniline nanowire binary composite material.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below with reference to specific examples and comparative examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.

Unless otherwise specified, the devices used in the present examples, comparative examples and experimental examples were all conventional experimental devices, the materials and reagents used were commercially available without specific reference, and the experimental methods without specific reference were also conventional experimental methods.