Co-Ag3PO4 composite photocatalytic material and preparation method thereof

Abstract

The invention provides a Co-Ag3PO4 composite photocatalytic material and a preparation method of the Co-Ag3PO4 composite photocatalytic material. The preparation method comprises the following steps: firstly, fully compounding silver nitrate and sodium hypophosphite to obtain pure silver phosphate crystals; and then roasting a cobalt source and Ag3PO4 to obtain the Co-Ag3PO4 composite photocatalytic degradation material. Compared with the prior art, the Co-Ag3PO4 composite photocatalytic degradation organic dye solution has the biggest characteristics that a novel catalyst applied to the field of photocatalytic degradation is simple and efficient in preparation process, and the prepared Co-Ag3PO4 composite photocatalytic degradation organic dye solution material is good in performance, perfect in crystal structure, excellent in recycling performance and easy to recycle.

Description

Technical Field

[0001] The present invention relates to the technical field of materials for photocatalytic degradation of organic dye aqueous solutions, and in particular to a Co-Ag3PO4 composite photocatalytic degradation material and a preparation method thereof. Background Art

[0002] With the rapid development of economy and technology, the complex and difficult-to-treat problem of industrial wastewater has become increasingly prominent. Photocatalysis technology is a typical new research field in green chemistry, with many advantages, such as recyclability and environmental friendliness. Using catalysts to degrade wastewater is an effective way to alleviate the current serious environmental problems and energy crisis, and therefore has certain industrial application prospects. However, this technology still has many limitations, such as low conversion efficiency and high application costs. The key to solving these problems is to design and synthesize photocatalysts with high activity, low cost, and high stability. Summary of the Invention

[0003] The present invention aims to address the technical problem of enhancing the reactivity of photocatalytic degradation of organic dyes by preparing a composite photocatalytic material by doping Co with Ag₃PO₄ and providing a simple and efficient preparation method. The present invention produces a high-performance Co-Ag₃PO₄ composite photocatalytic material through programmed temperature calcination. The preparation of this Co-Ag₃PO₄ composite photocatalytic material utilizes readily available and inexpensive raw materials. The addition of Co simplifies the preparation process and conditions, resulting in low cost and high yield.

[0004] The preparation method of the Co-Ag3PO4 composite photocatalytic material of the present invention comprises the following steps:

[0005] (1) Preparation of pure Ag3PO4: Dissolve 1.63 g of silver nitrate (analytical grade) in 64 mL of deionized water and stir continuously for 30 min. Slowly add 1.8 g of NaH2PO4·H2O (analytical grade) to the solution and stir for another hour. Transfer the solution to a centrifuge tube, wash with water, centrifuge three times, and dry in a vacuum oven at 80°C before use.

[0006] (2) Composite reaction: The composite obtained in step (1) was mixed evenly with 1.3 g of cobalt chloride, placed in a tube furnace, and heated to 350° C. at a heating rate of 1° C. / min in a N 2 atmosphere and maintained for 2 h to obtain a calcined product.

[0007] (3) Washing and Drying: The calcined product obtained in step (2) is cooled, taken out, ground, and washed three times by centrifugation with water and ethanol. Finally, the washed product is dried in an oven at 60°C and stored for later use.

[0008] In a specific embodiment of the present invention, the specific types of the raw material cobalt source added in step (1) are as follows: one or more of CoSO4·7H2O and CoCl2·6H2O.

[0009] In another specific embodiment of the present invention, the calcination reaction in step (2) can be prepared using a direct heating method or a programmed temperature heating method; the protective gas uses an H2 atmosphere or an N2 atmosphere; the temperature is raised to 200-400°C at a heating rate of 1-10°C / min, and the heat treatment time is 0.5-3 h. DETAILED DESCRIPTION

[0010] The present invention will be further described below with reference to the following examples, which however are not intended to limit the present invention.

[0011] Example 1

[0012] (1) Preparation of pure Ag3PO4: Dissolve 1.63 g of silver nitrate (analytical grade) in 64 mL of deionized water and stir continuously for 30 min. Weigh 1.8 g of NaH2PO4·H2O (analytical grade) and slowly add it to the solution. Stir for another hour. Transfer the solution to a centrifuge tube, wash with water, centrifuge three times, and dry in a vacuum oven at 80°C before use.

[0013] (2) The composite obtained in step (1) was mixed evenly with 2.91 g of Co(NO3)2·6H2O, placed in a tube furnace, and heated to 350°C at a heating rate of 1°C / min in a N2 atmosphere and maintained for 2 h to obtain a calcined product.

[0014] (3) Washing and Drying: The calcined product obtained in step (2) is cooled, taken out, ground, and washed three times by centrifugation with water and ethanol. Finally, the washed product is dried in an oven at 60°C and stored for later use.

[0015] Example 2

[0016] (1) Adjust the “2.91g Co(NO3)2·6H2O” in step (2) of Implementation Case 1 to “2.81g CoSO4·7H2O”. The remaining steps are the same as Implementation Case 1.

[0017] Example 3

[0018] (1) In Example 1, the step (2) of "heating to 350°C at a heating rate of 1°C / min in a N2 atmosphere and holding for 2 h" was changed to "directly heating to 350°C in a H2 atmosphere and holding for 2 h". The remaining steps were the same as in Example 1.

Claims

1. A Co-Ag3PO4 composite photocatalytic degradation material for liquid organic dyes and its preparation method, characterized in that The method comprises the following steps: (1) Preparation of pure Ag3PO4: Dissolve 1.63g of silver nitrate (analytical grade) in 64mL of deionized water solution and stir continuously for 30min. Weigh 1.8g of NaH2PO4·H2O (analytical grade) and slowly add it to the above solution and stir for another hour. Transfer the above solution into a centrifuge tube, wash with water and centrifuge three times, and dry it in a vacuum oven at 80℃ for later use. (2) Mix the obtained complex with 1.3g of cobalt chloride, place it in a tube furnace, and heat it to 350℃ at a heating rate of 1℃ / min in a N2 atmosphere for 2h to prepare a calcined product. (3) Washing and drying: After cooling the calcined product obtained in step (2), take it out and grind it, wash it with water and ethanol by centrifugation three times. Finally, dry the washed composite in a 60℃ oven for later use.

2. The preparation method according to claim 1, wherein: The cobalt source is one or more of CoSO4·7H2O and CoCl2·6H2O.

3. The preparation method according to claim 1, wherein: The molar ratio of the cobalt source to the silver in the preparation of the complex solution is in the range of 1:3 to 1:

1.

4. The preparation method according to claim 1, wherein: The material can be prepared by direct heating method, programmed heating method or other firing methods; the protective gas can use H2 atmosphere or N2 atmosphere; the temperature is increased to 200-400°C at a heating rate of 1-10°C / min, and the heat treatment time is 0.5-3 h.