Preparation method for nano-tio 2 thin film, and product and use thereof

Abstract

The present invention belongs to the technical field of catalyst materials. Disclosed are a preparation method for a nano-TiO2 thin film, and a product and the use thereof. The preparation method comprises the following steps: preparing a titanium dioxide sol by using butyl titanate and absolute ethanol as raw materials; loading the titanium dioxide sol onto a glass substrate; and then sequentially drying and sintering the glass substrate loaded with the titanium dioxide sol. The preparation method is simple, uses simple and easily available raw materials, is free of pollution, and is beneficial to industrial production. The loading rate of the nano-TiO2 in the obtained nano-TiO2 thin film is high, thereby resulting in a high utilization rate of solar energy, and enabling efficient photocatalytic degradation of organic pollutants.

Description

Preparation method, product and application of nano-TiO2 film TECHNICAL FIELD

[0001] The present application relates to the technical field of catalyst materials, in particular to a preparation method, product and application of nano-TiO2 film. BACKGROUND

[0002] Municipal landfill leachate is a kind of complex sewage, and relevant research results show that the leachate seriously pollutes surface water and groundwater. The main pollutant in the leachate is organic pollutant, and the concentration of BOD5 and COD can reach tens of thousands of mg / L, which seriously pollutes the environment.

[0003] At present, the research on using metal oxide semiconductor as a catalyst for photocatalytic oxidation degradation of organic wastewater has attracted attention of many scholars at home and abroad. It is reported that more than 300 kinds of organic compounds can be photocatalytically degraded. Nano-TiO2 photocatalyst is a new and rapidly developing high-efficiency spectral catalyst, and has become a research hotspot in environmental protection technology in recent years. However, some key scientific and technical problems of the current photocatalytic technology based on nano-TiO2, such as low quantum yield, low solar energy utilization rate and photocatalyst loading technology, still need to be solved.

[0004] SUMMARY

[0005] Therefore, the present application aims to provide a preparation method, product and application of nano-TiO2 film, and the nano-TiO2 film provided by the present application has high loading rate of photocatalyst and high solar energy utilization rate, and can efficiently degrade organic pollutants.

[0006] In order to achieve the above-mentioned purpose, the present application provides the following technical solutions.

[0007] One of the technical solutions of the present application is a preparation method of nano-TiO2 film, comprising the following steps:

[0008] Titanium dioxide sol is prepared by using butyl titanate and anhydrous ethanol as raw materials, the titanium dioxide sol is loaded on a glass substrate, and then the glass substrate loaded with the titanium dioxide sol is sequentially dried and sintered.

[0009] The second technical solution of the present application is a nano-TiO2 film prepared by the above preparation method.

[0010] The third technical solution of the present application is an application of the above nano-TiO2 film in photocatalytic degradation of organic pollutants.

[0011] The present application discloses the following technical effects:

[0012] The preparation method is simple, raw materials are simple and easy to obtain, and pollution is avoided, so that industrial production is facilitated.

[0013] The nano TiO2 thin film has high loading rate of nano TiO2, so that the utilization rate of solar energy is high, and the organic pollutants can be efficiently photocatalytically degraded. DETAILED DESCRIPTION

[0014] Various exemplary embodiments of the present application will now be described in detail, which should be considered in a descriptive sense only and not for purposes of limitation to the application described. Rather, certain aspects, features and embodiments of the present application are directed to novel methods, procedures, compositions and systems that are novel, unobvious, and / or improved implementations of particular described aspects of the present application.

[0015] It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. Additionally, the use of the term "about" in relation to a value or range of values is intended to include each and every value falling within the range and each and every value falling within the range as well as the range itself. The upper and lower limits of these smaller ranges can independently be included or excluded in the range.

[0016] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application, the preferred methods and materials are described. All publications mentioned herein are incorporated by reference to disclose and describe the methods and / or materials in connection with which the publications are cited. The citation of any reference is not an admission that it is prior art with respect to the present application. All documents mentioned herein are incorporated by reference.

[0017] Many modifications and variations of this application description will be apparent to those of ordinary skill in the art from the foregoing description. Such modifications and variations are intended to fall within the scope of the application. Other embodiments will be apparent to those skilled in the art from consideration of the specification and practice of the application disclosed herein. The specification and examples given are exemplary only. It is to be understood that the application is not limited in any way by the specific details of that specification.

[0018] As used herein, the terms "comprise", "comprising", "include", "including", "have", "having" and the like are open-ended and do not exclude additional elements or steps.

[0019] One of the technical solutions of the present application is a preparation method of a nano TiO2 thin film, comprising the following steps:

[0020] Titanium dioxide sol is prepared by using butyl titanate and anhydrous ethanol as raw materials, the titanium dioxide sol is loaded on a glass substrate, and then the glass substrate loaded with the titanium dioxide sol is sequentially dried and sintered.

[0021] In some embodiments of the present application, the method for preparing the titanium dioxide sol from butyl titanate and anhydrous ethanol is method 1 or method 2:

[0022] The method 1 is: mixing butyl titanate and anhydrous ethanol, then adding dropwise into an acidic aqueous solution under stirring, continuing to stir until a colloidal solution is formed after the dropwise adding is completed;

[0023] The method 2 is: adding a dispersant and a stabilizer into anhydrous ethanol in sequence, stirring until a uniform transparent solution is formed, then adding dropwise butyl titanate and water into the transparent solution in sequence under stirring until a colloidal solution is formed.

[0024] In some embodiments of the present application, in the method 1, the mass ratio of butyl titanate to anhydrous ethanol is (2-5):(3-7); the acidic aqueous solution is a hydrochloric acid solution; the pH of the acidic aqueous solution is 4; the dropwise adding amount of the acidic aqueous solution is to make the pH of the reaction system be 5-6.

[0025] In some embodiments of the present application, in the method 2, the dispersant is polyethylene glycol-40; the stabilizer is triethanolamine; the volume ratio of butyl titanate, anhydrous ethanol, polyethylene glycol-400 and triethanolamine is 5:20:5:6.

[0026] In some embodiments of the present application, before the titanium dioxide sol is loaded on the glass substrate, a step of pretreating the glass substrate is further included; the pretreatment is sequentially performing oil removal treatment, alkali treatment, acid treatment and alcohol treatment on the glass substrate; the oil removal treatment is soaking the glass substrate in an oil removal agent to remove oil, the oil removal agent can be selected from the oil removal agents commonly used by those skilled in the art, which can achieve the effect of removing oil on the surface of the glass substrate; the alkali treatment is soaking the glass substrate after the oil removal treatment in 1wt% sodium hydroxide; the acid treatment is soaking the glass substrate after the alkali treatment in hydrochloric acid with a pH of 2; the alcohol treatment is wetting the glass substrate after the acid treatment with anhydrous ethanol.

[0027] In some embodiments of the present application, after the alcohol treatment, a step of air-drying at room temperature is further included.

[0028] In some embodiments of the present application, the method for loading the titanium dioxide sol on the glass substrate can be selected from the methods well known to those skilled in the art, such as impregnation, rotation or spraying.

[0029] In some embodiments of the present application, when the method for preparing the titanium dioxide sol is the method 1, the sintering is heating to 450℃ at a speed of 10℃ / min and keeping for 60min;

[0030] When the method for preparing the titanium dioxide sol is method 2, the sintering is: after being kept at 100℃ for 30 min, the temperature is increased to 400℃ at a rate of 5℃ / min and kept at 400℃ for 1 h, and then kept at 550℃ for 1 h.

[0031] The second technical solution of the present application is the nano-TiO2 film prepared by the above preparation method.

[0032] The third technical solution of the present application is the application of the above nano-TiO2 film in photocatalytic degradation of organic pollutants.

[0033] In order to better understand the present application, the content of the present application is further illustrated below in combination with examples, but the content of the present application is not limited to the examples below.

[0034] The raw materials and reagents used in the examples can be obtained through commercial channels if no special instructions are given.

[0035] The glass substrate used in the examples is a pretreated glass substrate, and the pretreatment is as follows: the glass substrate is soaked in a degreasing agent to remove oil (the degreasing agent is selected from the degreasing agents commonly used by those skilled in the art, which can achieve the effect of removing oil on the surface of the glass substrate), washed with water, soaked in 1wt% sodium hydroxide after the degreasing treatment of the glass substrate, washed with water, soaked in 2 pH hydrochloric acid after the alkali treatment of the glass substrate, washed with water, and the acid-treated glass substrate is wetted with anhydrous ethanol and dried at room temperature.

[0036] Example 1

[0037] Step 1. 5 mL of butyl titanate and 7 mL of anhydrous ethanol are mixed, and then the pH of the reaction system is adjusted to 5 by adding the mixture dropwise into a hydrochloric acid solution with a pH of 4 under stirring. After the dropwise addition is completed, the stirring is continued until a colloidal solution is formed.

[0038] Step 2. The glass cylinder (open at both ends) is immersed in the colloidal solution obtained in step 1, and after the colloidal solution is loaded on the wall of the glass cylinder, the glass cylinder is naturally air-dried, and then placed in a muffle furnace and heated to 450℃ at a rate of 10℃ / min and kept at 450℃ for 60 min, and then naturally cooled to room temperature to obtain a glass cylinder loaded with a TiO2 film.

[0039] Example 2

[0040] Step 1. 5 mL of polyethylene glycol-400 and 6 mL of triethanolamine are sequentially added to 20 mL of anhydrous ethanol, and stirred until a uniform transparent solution is formed. Then, 5 mL of butyl titanate is added dropwise into the transparent solution under stirring, and then water is added dropwise until a colloidal solution is formed.

[0041] Step 2. The glass sheet was immersed in the colloidal solution obtained in step 1, then the glass sheet was pulled at a speed of 5 cm / min, dried at 100℃ for 5 min, cooled at room temperature for 5 min, the pulling operation was repeated for 3 times, then put into a controllable temperature furnace, heated from room temperature to 100℃ for 30 min, then heated to 400℃ at a rate of 5℃ / min for 1 h, then transferred into a muffle furnace and heated at 550℃ for 1 h, and naturally cooled to room temperature to obtain a glass sheet loaded with TiO2 film.

[0042] The above only describes the preferred embodiments of the present application, and it should be noted that for those skilled in the art, some improvements and refinements can be made without departing from the principles of the present application, and these improvements and refinements should also be considered as the protection scope of the present application.

Claims

1. A method for preparing a nano-TiO2 film, characterized in that, The method comprises the following steps: Titanium dioxide sol is prepared by using butyl titanate and anhydrous ethanol as raw materials, the titanium dioxide sol is loaded on a glass substrate, and then the glass substrate loaded with the titanium dioxide sol is sequentially dried and sintered.

2. The method for preparing nano-TiO2 thin films according to claim 1, characterized in that, The method for preparing the titanium dioxide sol by using butyl titanate and anhydrous ethanol as raw materials is method 1 or method 2: The method 1 is that butyl titanate and anhydrous ethanol are mixed, then the mixture is added dropwise into an acidic aqueous solution under stirring, and the stirring is continued until a colloidal solution is formed after the dropwise addition is completed; The method 2 is that a dispersant and a stabilizer are sequentially added into anhydrous ethanol, the mixture is stirred until a uniform transparent solution is formed, then butyl titanate and water are sequentially added dropwise into the transparent solution under stirring until a colloidal solution is formed.

3. The method according to claim 2, wherein the method is characterized by, In the method 1, the mass ratio of the butyl titanate to the anhydrous ethanol is (2-5):(3-7), the acidic aqueous solution is a hydrochloric acid solution, the pH of the acidic aqueous solution is 4, and the dropwise addition amount of the acidic aqueous solution is such that the pH of the reaction system is 5-6.

4. The method for preparing nano-TiO2 thin films according to claim 2, characterized in that, In the method 2, the dispersant is polyethylene glycol-400, the stabilizer is triethanolamine, and the volume ratio of the butyl titanate, the anhydrous ethanol, the polyethylene glycol-400 and the triethanolamine is 5:20:5:

6.

5. The method for preparing nano-TiO2 thin films according to claim 1, characterized in that, Before the titanium dioxide sol is loaded on the glass substrate, a step of pretreating the glass substrate is further included; the pretreatment is that the glass substrate is sequentially subjected to oil removal treatment, alkali treatment, acid treatment and alcohol treatment.

6. The method for preparing nano-TiO2 thin films according to claim 1, characterized in that, When the method for preparing the titanium dioxide sol is the method 1, the sintering is heating at a speed of 10 ℃ / min to 450 ℃ and then maintaining the temperature for 60 min; When the method for preparing the titanium dioxide sol is the method 2, the sintering is maintaining the temperature at 100 ℃ for 30 min, then heating at a speed of 5 ℃ / min to 400 ℃ and maintaining the temperature for 1 h, and then maintaining the temperature at 550 ℃ for 1 h.

7. A nano-TiO2 film prepared by the method according to any one of claims 1-6.

8. Application of the nano-TiO2 film according to claim 7 to photocatalytic degradation of organic pollutants.