阅读说明：本技术 一种高性能复合光催化材料的制备方法 (Preparation method of high-performance composite photocatalytic material ) 是由 姚博 于 2019-11-26 设计创作，主要内容包括：本发明属于光催化领域,具体涉及一种高性能复合光催化材料的制备方法,包括如下步骤：步骤1,将电气石加入至蒸馏水中搅拌均匀形成浆料,然后放入球磨机中球磨处理,烘干后得到粒径均匀的电气石粉末；步骤2,将聚乙烯醇加入至电气石粉末中固体搅拌均匀,得到混合粉末,然后加入至蒸馏水中恒温搅拌至完全溶解,得到混合分散液；步骤3,将混合分散液均匀涂覆在基材平板上,恒温快速烘干,冷却形成薄膜层,反复上述涂覆至冷却的步骤2-6次,得到分散膜；步骤4,将钛酸正丁酯加入无水乙醇中搅拌均匀,然后加入至纳米喷雾器中,均匀喷雾在恒温的分散膜表面,形成预制膜；步骤5,将预制膜加入至反应釜中恒温烧结3-6h,冷却后得到复合光催化材料。(The invention belongs to the field of photocatalysis, and particularly relates to a preparation method of a high-performance composite photocatalytic material, which comprises the following steps: step 1, adding tourmaline into distilled water, stirring uniformly to form slurry, then putting the slurry into a ball mill for ball milling treatment, and drying to obtain tourmaline powder with uniform particle size; step 2, adding polyvinyl alcohol into tourmaline powder, uniformly stirring the polyvinyl alcohol and the tourmaline powder to obtain mixed powder, and then adding the mixed powder into distilled water, stirring the mixed powder at constant temperature until the mixed powder is completely dissolved to obtain mixed dispersion liquid; step 3, uniformly coating the mixed dispersion liquid on a substrate flat plate, quickly drying at constant temperature, cooling to form a thin film layer, and repeating the steps from coating to cooling for 2-6 times to obtain a dispersion film; step 4, adding n-butyl titanate into absolute ethyl alcohol, uniformly stirring, then adding into a nano sprayer, and uniformly spraying on the surface of the constant-temperature dispersion film to form a prefabricated film; and 5, adding the prefabricated film into a reaction kettle, sintering at constant temperature for 3-6h, and cooling to obtain the composite photocatalytic material.)

1. A preparation method of a high-performance composite photocatalytic material is characterized by comprising the following steps: the method comprises the following steps:

step 1, adding tourmaline into distilled water, stirring uniformly to form slurry, then putting the slurry into a ball mill for ball milling treatment, and drying to obtain tourmaline powder with uniform particle size;

step 2, adding polyvinyl alcohol into tourmaline powder, uniformly stirring the polyvinyl alcohol and the tourmaline powder to obtain mixed powder, and then adding the mixed powder into distilled water, stirring the mixed powder at constant temperature until the mixed powder is completely dissolved to obtain mixed dispersion liquid;

step 3, uniformly coating the mixed dispersion liquid on a substrate flat plate, quickly drying at constant temperature, cooling to form a thin film layer, and repeating the steps from coating to cooling for 2-6 times to obtain a dispersion film;

step 4, adding n-butyl titanate into absolute ethyl alcohol, uniformly stirring, then adding into a nano sprayer, and uniformly spraying on the surface of the constant-temperature dispersion film to form a prefabricated film;

and 5, adding the prefabricated film into a reaction kettle, sintering at constant temperature for 3-6h, and cooling to obtain the composite photocatalytic material.

2. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: the mass ratio of the tourmaline powder to the distilled water in the step 1 is 3-8:1, the ball milling treatment temperature is 30-60 ℃, the pressure is 10-20MPa, and the drying temperature is 100-.

3. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: the mass ratio of the polyvinyl alcohol to the tourmaline powder in the step 2 is 10-15:3, the stirring speed of solid stirring is 300-700r/min, and the alcoholysis degree of the polyvinyl alcohol is 87-89%.

4. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: the temperature of constant-temperature stirring in the step 2 is 70-80 ℃, the stirring speed is 1000-2000r/min, and the adding amount of the distilled water is 5-8 times of the mass of the polyvinyl alcohol.

5. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: the coating amount in the step 3 is 2-5mL/cm²The constant temperature and rapid drying temperature is 100-120 ℃.

6. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: and the cooling in the step 3 adopts quick air cooling to 10-15 ℃.

7. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: the mass ratio of the n-butyl titanate to the absolute ethyl alcohol in the step 4 is 2:5-8, the stirring speed is 500-1000r/min, and the spray amount of the uniform spray is 20-40mL/m³The constant temperature is 80-100 ℃.

8. The method for preparing the high-performance composite photocatalytic material according to claim 1, wherein: the temperature of the constant temperature sintering in the step 5 is 250-300 ℃.

Technical Field

The invention belongs to the field of photocatalysis, and particularly relates to a preparation method of a high-performance composite photocatalytic material.

Background

The titanium dioxide is a photocatalyst which has high efficiency, no toxicity, stable chemical property, strong photo-oxidation resistance and low price. Titanium dioxide photocatalysis/photoelectrocatalysis technology draws extensive attention in the aspect of toxic and difficult biochemical degradation organic wastewater and waste gas treatment application. The nano titanium dioxide has high degradation efficiency, but can only carry out photocatalytic reaction under the irradiation of ultraviolet light, and the separation rate of photoproduction electrons and holes still needs to be improved. In order to improve the performance of titanium dioxide, preparing a titanium dioxide composite material and changing the application form of the titanium dioxide composite material become one of the key directions of titanium dioxide research. Metals, metal oxides, graphite, organic materials, and the like have all been used to prepare titanium dioxide composites.

The template agent can be used for preparing titanium dioxide with a specific form or for pore-forming titanium dioxide. The titanium dioxide with the pore channel structure has larger specific surface area and stronger mass transfer effect, thereby having stronger photocatalytic performance. Polyethers, surfactants such as polyethylene glycol and cetyltrimethylammonium bromide, and non-surfactants such as glucose are more commonly used templates. Polyaniline is a typical conductive polymer material, and is a research hotspot of conductive polymers due to diversified structures, good environmental stability, easy processing and low price. However, polyaniline has poor solubility and is difficult to form a stable base material structure.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a preparation method of a high-performance composite photocatalytic material, which solves the problem of difficult polyaniline treatment, effectively promotes the electron transfer on the surface of titanium dioxide by using a polymer containing conjugated double bonds generated by a polyvinyl alcohol constant-temperature reaction, realizes a good hole-electron dislocation reaction, and greatly promotes the degradation performance of a surface photocatalytic film.

In order to achieve the technical purpose, the technical scheme of the invention is as follows:

a preparation method of a high-performance composite photocatalytic material comprises the following steps:

step 1, adding tourmaline into distilled water, stirring uniformly to form slurry, then putting the slurry into a ball mill for ball milling treatment, and drying to obtain tourmaline powder with uniform particle size;

step 2, adding polyvinyl alcohol into tourmaline powder, uniformly stirring the polyvinyl alcohol and the tourmaline powder to obtain mixed powder, and then adding the mixed powder into distilled water, stirring the mixed powder at constant temperature until the mixed powder is completely dissolved to obtain mixed dispersion liquid;

step 3, uniformly coating the mixed dispersion liquid on a substrate flat plate, quickly drying at constant temperature, cooling to form a thin film layer, and repeating the steps from coating to cooling for 2-6 times to obtain a dispersion film;

step 4, adding n-butyl titanate into absolute ethyl alcohol, uniformly stirring, then adding into a nano sprayer, and uniformly spraying on the surface of the constant-temperature dispersion film to form a prefabricated film;

and 5, adding the prefabricated film into a reaction kettle, sintering at constant temperature for 3-6h, and cooling to obtain the composite photocatalytic material.

The mass ratio of the tourmaline powder to the distilled water in the step 1 is 3-8:1, the ball milling treatment temperature is 30-60 ℃, the pressure is 10-20MPa, and the drying temperature is 100-.

The mass ratio of the polyvinyl alcohol to the tourmaline powder in the step 2 is 10-15:3, the stirring speed of solid stirring is 300-700r/min, and the alcoholysis degree of the polyvinyl alcohol is 87-89%.

The temperature of constant-temperature stirring in the step 2 is 70-80 ℃, the stirring speed is 1000-2000r/min, and the adding amount of the distilled water is 5-8 times of the mass of the polyvinyl alcohol.

The coating amount in the step 3 is 2-5mL/cm²The constant temperature and rapid drying temperature is 100-120 ℃.

And the cooling in the step 3 adopts quick air cooling to 10-15 ℃.

The mass ratio of the n-butyl titanate to the absolute ethyl alcohol in the step 4 is 2:5-8, the stirring speed is 500-1000r/min, and the spray amount of the uniform spray is 20-40mL/m³The constant temperature is 80-100 ℃.

The temperature of the constant temperature sintering in the step 5 is 250-300 ℃.

From the above description, it can be seen that the present invention has the following advantages:

1. the invention solves the problem of difficult polyaniline treatment, effectively promotes the electron transfer on the surface of titanium dioxide by using the polymer containing conjugated double bonds generated by the constant temperature reaction of polyvinyl alcohol, realizes good hole-electron dislocation reaction, and greatly promotes the degradation performance of the surface photocatalytic film.

2. The invention utilizes the characteristic that the temperature for converting the n-butyl titanate into the anatase titanium dioxide is similar to the temperature for converting the polyvinyl alcohol into the polymer containing the conjugated double bonds, and can realize one-step sintering reaction.

3. According to the invention, the polyvinyl alcohol is used for fastening the tourmaline powder, and the polyvinyl alcohol is used for forming conductivity after reaction, so that electrons generated by the tourmaline powder can be rapidly transferred, and the effect of promoting the surface titanium dioxide film is achieved.

4. According to the invention, the conjugated double-bond polymer is used as a connector, so that the electronic circulation of tourmaline powder and titanium dioxide is realized, the self-cleaning property of the titanium dioxide on the surface is improved, and the degradation efficiency of the titanium dioxide is greatly improved.

Detailed Description

The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.