阅读说明：本技术 一种高效处理污水的光催化剂的制备方法 (Preparation method of photocatalyst for efficiently treating sewage ) 是由 卢定泽 蒋国俊 王东旭 文毅 崔世博 闫梓颀 于 2019-07-29 设计创作，主要内容包括：本发明公开了一种高效处理污水的光催化剂的制备方法,采用水热法制备出二硫化钼花状纳米片,在常温常压条件下,通过原位沉积法将磷酸银和二硫化钼有效复合,制备出均匀生长在花状二硫化钼纳米片上的磷酸银复合光催化剂。本发明将金属硫化物前驱体引入到反应体系中,一步法实现了构筑Ag<Sub>3</Sub>PO<Sub>4</Sub>/MoS<Sub>2</Sub>光催化剂颗粒尺寸以及负载量的调控；本方法的制备原料易得,操作简单。(The invention discloses a preparation method of a photocatalyst for efficiently treating sewage, which is characterized in that a hydrothermal method is adopted to prepare flower-shaped molybdenum disulfide nanosheets, and silver phosphate and molybdenum disulfide are effectively compounded through an in-situ deposition method under the conditions of normal temperature and normal pressure to prepare a silver phosphate composite photocatalyst uniformly growing on the flower-shaped molybdenum disulfide nanosheets. The invention introduces the metal sulfide precursor into the reaction system, and realizes the construction of Ag by one step 3 PO 4 /MoS 2 Regulating and controlling the size and the loading capacity of photocatalyst particles; the preparation method has the advantages of easily obtained raw materials and simple operation.)

1. A preparation method of a photocatalyst for efficiently treating sewage is characterized by comprising the following steps:

step 1, preparing a solution containing ammonium molybdate tetrahydrate and thioacetamide, and heating and drying the mixed solution to obtain flower-shaped MoS₂The MoS obtained₂Dissolving in distilled water, and performing ultrasonic treatment;

step 2, the MoS obtained in the step 1 is processed₂Adding AgNO into the solution in sequence₃Dissolving the solid and distilled water in stirring to AgNO₃MoS of (1)₂Sequentially adding anhydrous disodium hydrogen phosphate solid and distilled water into the solution, and stirring to dissolve to obtain a mixed solution;

step 3, heating the mixed solution obtained in the step 2, taking out the mixed solution after heating, removing supernatant, reserving precipitate for later use, and centrifugally washing the obtained precipitate with deionized water and absolute ethyl alcohol in sequence;

step 4, after the washing is finished, drying the precipitate obtained in the step 3, and grinding precipitate powder to obtain the Ag₃PO₄/MoS₂A photocatalyst.

2. The method for preparing the photocatalyst for efficiently treating sewage according to claim 1, wherein the step 1 is specifically carried out according to the following steps:

1.1, preparing 1-60 mL of a mixed solution of ammonium molybdate and thioacetamide with the mass fraction of 1-20%;

step 1.2, heating and drying the mixed solution obtained in the step 1.1 at the temperature of 150-250 ℃ for 0.5-3 h to obtain flower-shaped MoS₂；

Step 1.3, taking 0.01-10 g of MoS₂Adding 5-100 mL of distilled water, and carrying out ultrasonic treatment for 0.5-3 h to obtain MoS₂And (4) suspending the solution.

3. The method for preparing the photocatalyst for efficiently treating sewage according to claim 1, wherein the step 2 is specifically performed according to the following steps:

step 2.1, to the MoS obtained in step 1₂Slowly adding 0.1-10 g of AgNO into the suspension₃Adding 5-100 mL of distilled water into the solid, and magnetically stirring for 1-15 h until the solid is dissolved;

step 2.2, adding AgNO obtained in step 2.1₃And MoS₂Adding 0.1-5 g of anhydrous disodium hydrogen phosphate solid into the mixed solution, adding 1-30 mL of distilled water, and magnetically stirring for 1-3 h until the solid is dissolved to obtain the mixed solution.

4. The method for preparing the photocatalyst for efficiently treating sewage according to claim 1, wherein the step 3 is specifically performed according to the following steps:

step 3.1, heating the mixed solution obtained in the step 2 at 160-220 ℃ for 3-96 h;

step 3.2, after the heating is finished, taking out the mixed solution obtained in the step 3.1, removing supernatant liquid, and reserving precipitate for later use;

and 3.3, centrifugally washing the precipitate obtained in the step 3.2 by using deionized water and absolute ethyl alcohol until the pH value of the supernatant is 5-7.

5. The method for preparing the photocatalyst for efficiently treating sewage according to claim 1, wherein the step 4 is specifically performed according to the following steps:

step 4.1, after the washing is finished, drying the precipitate obtained in the step 4 at the temperature of 40-80 ℃ for 2-12 h;

step 4.2, grinding the dried precipitate obtained in the step 4.1 into powder to obtain Ag₃PO₄/MoS₂A photocatalyst.

Technical Field

The invention belongs to the technical field of sewage treatment, and relates to a preparation method of a photocatalyst for efficiently treating sewage.

Background

In order to solve the problems of environmental pollution and energy crisis which have become more serious in recent years, the photocatalytic technology has attracted more and more attention from experts and scholars. Photocatalytic technology can utilize clean, sustainable solar energy and also degrade and decompose pollutants in air or water. Improving the performance of the photocatalyst is the key point for improving the photocatalytic technology. Among numerous photocatalysts, silver phosphate has been widely studied due to its wide visible light response range and extremely high light absorption performance. However, the large-scale use of silver phosphate is limited by the disadvantages of low separation efficiency of photogenerated carriers. It has been found that by recombining two semiconductors, the transfer of photogenerated electrons or holes from one semiconductor to the other increases the separation of photogenerated carriers, thereby increasing photocatalytic activity. Preparing a flower-shaped molybdenum disulfide nanosheet by a hydrothermal method, and effectively compounding silver phosphate and molybdenum disulfide by an in-situ deposition method under the conditions of normal temperature and normal pressure to prepare the silver phosphate composite photocatalyst uniformly growing on the flower-shaped molybdenum disulfide nanosheet.

Disclosure of Invention

The invention aims to provide a preparation method of a photocatalyst for efficiently treating sewage, which solves the problem of complex and fussy preparation process in the prior art.

The technical scheme adopted by the invention is that the preparation method of the photocatalyst for efficiently treating the sewage is implemented according to the following steps:

step 1, preparing a solution containing ammonium molybdate tetrahydrate and thioacetamide, and heating and drying the mixed solution to obtain flower-shaped MoS₂The MoS obtained₂Dissolving in distilled water, and performing ultrasonic treatment;

step 2, the MoS obtained in the step 1 is processed₂Adding AgNO into the solution in sequence₃Dissolving the solid and distilled water in stirring to AgNO₃And MoS₂Sequentially adding anhydrous disodium hydrogen phosphate solid and distilled water into the mixed solution, and stirring to dissolve to obtain a mixed solution;

step 3, heating the AgNO obtained in step 2₃And MoS₂After the mixed solution is heated, taking out the mixed solution, removing supernatant, reserving precipitate for later use, and centrifugally washing the obtained precipitate by using deionized water and absolute ethyl alcohol in sequence;

step 4, after the washing is finished, drying the precipitate obtained in the step 3, and grinding the precipitate powderTo obtain Ag₃PO₄/MoS₂A photocatalyst.

The invention is also characterized in that:

the step 1 is implemented according to the following steps:

1.1, preparing 1-60 mL of a mixed solution of ammonium molybdate and thioacetamide with the mass fraction of 1-20%;

step 1.2, heating and drying the mixed solution obtained in the step 1.1 at the temperature of 150-250 ℃ for 0.5-3 h to obtain flower-shaped MoS₂；

Step 1.3, taking 0.01-10 g of MoS₂Adding 5-100 mL of distilled water, and carrying out ultrasonic treatment for 0.5-3 h to obtain MoS₂And (4) suspending the solution.

The step 2 is implemented according to the following steps:

step 2.1, to the MoS obtained in step 1₂Slowly adding 0.1-10 g of AgNO into the suspension₃Adding 5-100 mL of distilled water into the solid, and magnetically stirring for 1-15 h until the solid is dissolved;

step 2.2, adding AgNO obtained in step 2.1₃And MoS₂Adding 0.1-5 g of anhydrous disodium hydrogen phosphate solid into the mixed solution, adding 1-30 mL of distilled water, and magnetically stirring for 1-3 h until the solid is dissolved to obtain a mixed solution;

step 3 is specifically implemented according to the following steps:

step 3.1, heating the mixed solution obtained in the step 2 at 160-220 ℃ for 3-96 h;

step 3.2, after the heating is finished, taking out the mixed solution obtained in the step 3.1, removing supernatant liquid, and reserving precipitate for later use;

and 3.3, centrifugally washing the precipitate obtained in the step 3.2 by using deionized water and absolute ethyl alcohol until the pH value of the supernatant is 5-7.

Step 4 is specifically implemented according to the following steps:

step 4.1, after the washing is finished, drying the precipitate obtained in the step 4 at the temperature of 40-80 ℃ for 2-12 h;

step 4.2, grinding the dried precipitate obtained in the step 4.1 into powder to obtain Ag₃PO₄/MoS₂A photocatalyst.

The invention has the beneficial effects that:

1. the preparation method of the photocatalyst for efficiently treating sewage introduces the metal sulfide precursor into the reaction system, and realizes the construction of Ag by one step₃PO₄/MoS₂And (3) regulation and control of the particle size and the loading amount of the photocatalyst. The method has the advantages of easily available raw materials and simple operation.

2. The preparation method of the photocatalyst for efficiently treating sewage has the advantages of easily available raw materials and simple operation.

Drawings

FIG. 1 is a flow chart of example 1 of a method for preparing a photocatalyst for efficiently treating wastewater according to the present invention;

FIG. 2 is a TEM image of example 1 of a method for preparing a photocatalyst for efficiently treating wastewater according to the present invention;

FIG. 3 is an evaluation diagram of photocatalytic degradation of rhodamine B in example 1 of the method for preparing a photocatalyst for efficiently treating wastewater according to the present invention;

Detailed Description

The invention is described in detail below with reference to fig. 1 and the specific embodiments, and the specific operation steps are shown in fig. 1.