阅读说明：本技术 一种高活性光催化颗粒的制备方法 (Preparation method of high-activity photocatalytic particles ) 是由 朱盼盼 于 2019-12-06 设计创作，主要内容包括：本发明属于光催化领域,具体涉及一种高活性催化颗粒的制备方法,所述高活性光催化颗粒利用钛酸正丁酯包裹至纳米一氧化钛表面。并经过水解转化为二氧化钛,形成以一氧化钛为核心、二氧化钛为包裹层的多钛光催化颗粒。本发明解决了二氧化钛颗粒量子产率低的问题,利用一氧化钛作为内层,二氧化钛作为包裹层,形成的钛氧颗粒,产生氧缺特性,大大提升了表面二氧化钛的活性,有效的提升了光催化降解效率。(The invention belongs to the field of photocatalysis, and particularly relates to a preparation method of high-activity catalytic particles. And is converted into titanium dioxide through hydrolysis to form the multi-titanium photocatalytic particles taking titanium monoxide as a core and titanium dioxide as a coating layer. The invention solves the problem of low quantum yield of titanium dioxide particles, and the titanium oxide is used as the inner layer and the titanium dioxide is used as the wrapping layer to form titanium oxide particles with oxygen deficiency characteristics, thereby greatly improving the activity of the titanium dioxide on the surface and effectively improving the photocatalytic degradation efficiency.)

1. A preparation method of high-activity photocatalytic particles is characterized by comprising the following steps: the high-activity photocatalytic particles are wrapped on the surface of the nano titanium oxide by using n-butyl titanate. And is converted into titanium dioxide through hydrolysis to form the multi-titanium photocatalytic particles taking titanium monoxide as a core and titanium dioxide as a coating layer.

2. The method for preparing highly active photocatalytic particles according to claim 1, characterized in that: the method comprises the following steps:

step 1, adding titanium monoxide into a ball mill, adding a small amount of distilled water, stirring to form slurry, carrying out ball milling reaction for 2-5h, sealing and blow-drying by adopting hot nitrogen, and cooling to obtain nano titanium monoxide;

step 2, slowly adding the nano-titanium monoxide into the n-butyl titanate for low-temperature microwave reaction for 2-5 hours, and stirring to form suspension slurry;

step 3, simultaneously spraying the suspension slurry and distilled water in a constant-temperature reaction kettle for constant-temperature reaction for 1-3h, and circularly spraying to form particle suspended matters;

and 4, blowing and collecting the particle suspended matters at constant temperature to obtain the photocatalytic particles.

3. The method for preparing highly active photocatalytic particles according to claim 2, characterized in that: in the step 1, the adding amount of the Zhejiang distilled water is 5-10% of the mass of the titanium monoxide, the pressure of the ball milling reaction is 2-6MPa, and the temperature is 40-60 ℃.

4. The method for preparing highly active photocatalytic particles according to claim 2, characterized in that: the temperature of the hot nitrogen in the step 1 is 100-120 ℃, and the flow rate of the hot nitrogen for drying is 5-20 mL/min.

5. The method for preparing highly active photocatalytic particles according to claim 2, characterized in that: the mass ratio of the nano titanium oxide to the n-butyl titanate in the step 2 is 1:5-8, the adding speed of the nano titanium oxide is 1-2g/min, the low-temperature microwave temperature is 10-20 ℃, the microwave power is 400-800W, and the stirring speed is 2000-4000 r/min.

6. The method for preparing highly active photocatalytic particles according to claim 2, characterized in that: the mass ratio of the distilled water to the suspension slurry in the step 3 is 1:10-15, the spraying speed of the distilled water is 1-2mL/min, the spraying speed of the suspension slurry is 3-6mL/min, the temperature of the constant temperature reaction is 60-80 ℃, and the pressure is 1-2 MPa.

7. The method for preparing highly active photocatalytic particles according to claim 2, characterized in that: the spraying speed of the circulating spraying in the step 3 is 50-80mL/min, the temperature is 100-120 ℃, and the constant-temperature reaction kettle adopts a nitrogen atmosphere.

8. The method for preparing highly active photocatalytic particles according to claim 2, characterized in that: the temperature of the constant-temperature purging in the step 4 is 100-120 ℃.

Technical Field

The invention belongs to the field of photocatalysis, and particularly relates to a preparation method of high-activity catalytic particles.

Background

In recent years, semiconductor photocatalysts have important application in the field of environmental pollution treatment, and titanium dioxide is a representative photocatalyst and is a photocatalyst which is widely applied at present. Theoretically, titanium dioxide has the advantages of high photocatalytic activity, good stability, no toxicity, low cost and the like. In addition, the photocatalytic reaction of titanium dioxide can be carried out under normal temperature and pressure conditions.

However, in practice, the titanium dioxide photocatalysis is still in the laboratory stage, and there are still many technical difficulties in practical application. The titanium dioxide is difficult to form rapid degradation under low photocatalytic treatment efficiency, and the inactivation phenomenon is easy to occur under the condition of high concentration.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a preparation method of high-activity photocatalytic particles, which solves the problem of low quantum yield of titanium dioxide particles, and the titanium dioxide is used as an inner layer and a wrapping layer to form titanium oxide particles with oxygen deficiency characteristics, so that the activity of the titanium dioxide on the surface is greatly improved, and the photocatalytic degradation efficiency is effectively improved.

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

a preparation method of high-activity photocatalytic particles is provided, wherein the high-activity photocatalytic particles are coated on the surface of nano titanium monoxide by utilizing n-butyl titanate. And is converted into titanium dioxide through hydrolysis to form the multi-titanium photocatalytic particles taking titanium monoxide as a core and titanium dioxide as a coating layer.

The method comprises the following steps:

step 1, adding titanium monoxide into a ball mill, adding a small amount of distilled water, stirring to form slurry, carrying out ball milling reaction for 2-5h, sealing and blow-drying by adopting hot nitrogen, and cooling to obtain nano titanium monoxide;

step 2, slowly adding the nano-titanium monoxide into the n-butyl titanate for low-temperature microwave reaction for 2-5 hours, and stirring to form suspension slurry;

step 3, simultaneously spraying the suspension slurry and distilled water in a constant-temperature reaction kettle for constant-temperature reaction for 1-3h, and circularly spraying to form particle suspended matters;

and 4, blowing and collecting the particle suspended matters at constant temperature to obtain the photocatalytic particles.

In the step 1, the adding amount of the Zhejiang distilled water is 5-10% of the mass of the titanium monoxide, the pressure of the ball milling reaction is 2-6MPa, and the temperature is 40-60 ℃.

The temperature of the hot nitrogen in the step 1 is 100-120 ℃, and the flow rate of the hot nitrogen for drying is 5-20 mL/min.

The mass ratio of the nano titanium oxide to the n-butyl titanate in the step 2 is 1:5-8, the adding speed of the nano titanium oxide is 1-2g/min, the low-temperature microwave temperature is 10-20 ℃, the microwave power is 400-800W, and the stirring speed is 2000-4000 r/min.

The mass ratio of the distilled water to the suspension slurry in the step 3 is 1:10-15, the spraying speed of the distilled water is 1-2mL/min, the spraying speed of the suspension slurry is 3-6mL/min, the temperature of the constant temperature reaction is 60-80 ℃, and the pressure is 1-2 MPa.

The spraying speed of the circulating spraying in the step 3 is 50-80mL/min, the temperature is 100-120 ℃, and the constant-temperature reaction kettle adopts a nitrogen atmosphere.

The temperature of the constant-temperature purging in the step 4 is 100-120 ℃.

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

1. the invention solves the problem of low quantum yield of titanium dioxide particles, and the titanium oxide is used as the inner layer and the titanium dioxide is used as the wrapping layer to form titanium oxide particles with oxygen deficiency characteristics, thereby greatly improving the activity of the titanium dioxide on the surface and effectively improving the photocatalytic degradation efficiency.

2. The invention realizes that the tetrabutyl titanate forms a liquid film on the surface of the titanium monoxide particles by utilizing the combination of the tetrabutyl titanate and the nano titanium monoxide, and the liquid film is converted into the titanium dioxide particles by hydrolysis, thereby realizing the titanium dioxide particles taking the titanium monoxide as the core.

3. The method carries out constant-temperature hydrolysis reaction in a nitrogen environment, prevents oxygen in the air from influencing the titanium monoxide, and ensures the integrity of the titanium monoxide.

Detailed Description

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