Preparation method and application of core-shell P-CoFe2O4(at)GCN photocatalyst

Abstract

The invention belongs to the technical field of composite materials and relates to a preparation method and application of a core-shell P-CoFe2O4(at)GCN photocatalyst. The preparation method comprisesthe following steps: firstly mixing cobalt salt and ferric salt, dropwise adding alkali lye and precipitating to prepare strongly magnetic nanoparticles CoFe2O4; fully dispersing a graphite-type carbonitride precursor and a phosphorus source in distilled water, carrying out solid-liquid separation, drying a solid at 80-100 DEG C for 12-24 h, and grinding to obtain a powder; and finally placing the powder into a muffle furnace, and heating in the air atmosphere at 500-600 DEG C for 2-5 h so as to obtain the photocatalyst. In the invention, the prepared material is also applied to wastewater soas to remove antibiotics. By compound modification of the graphite-type carbonitride, the photocatalytic performance is greatly improved, and the solid-liquid separation problems are solved. The preparation method is simple to operate, and the sources of the raw materials are wide. The surface of the prepared material has a pore structure, and the specific surface area is increased, thus providing more active sites for a photo-catalytic reaction. The result shows that the tetracycline photocatalytic degradation rate of the product is 3.66 times higher than the tetracycline photocatalytic degradation rate of pure graphite-type carbonitride before modification.

Description

technical field

[0001] The invention belongs to the technical field of composite materials, and relates to a graphite carbon nitride photocatalyst, in particular to a core-shell type P-CoFe 2 o 4 The preparation method and application of @GCN photocatalyst. Background technique

[0002] Pharmaceuticals and personal care products (PPCPs) are an emerging pollutant. With the advancement of science and technology, this type of synthetic chemical substance is widely used all over the world. Due to improper handling, this kind of substance is continuously introduced into the In the ecological environment, thus entering the water body, researchers have detected trace amounts of antibiotic pollutants from natural water bodies, which will cause serious harm to human health. Among them, tetracycline antibiotics are one of the PPCPs. Due to their low price, they are widely used in livestock and poultry farming, and their usage accounts for more than half of the total antibiotics. Te...

Examples

Embodiment 1

[0028] A core-shell type P-CoFe 2 o 4 The preparation method of @GCN photocatalyst comprises the following steps:

[0029] a) Fully mix cobalt nitrate and ferric nitrate in equal volume for 0.5h according to the molar concentration ratio of 1:1, the reaction temperature is 35°C, and the stirring rate is 500r·min -1 ;

[0030] b) Slowly add 2mol / L potassium hydroxide solution dropwise to the fully mixed solution until complete precipitation, and react at 80°C for 3h, then rinse with absolute ethanol and distilled water several times, and dry at 60°C for 16h, Strong magnetic nanoparticles CoFe can be prepared 2 o 4 ;

[0031] c) Weigh the prepared CoFe 2 o 4 Add to 80 ml of distilled water, add thiourea and melamine polyphosphate to the mixed solution, fully stir for 5 hours, the stirring rate is 500r·min -1 , CoFe 2 o 4 , The mass ratio of thiourea and melamine polyphosphate is 0.05:1:0.2;

[0032] d) Dry the mixed solution at 80°C for 12 hours after solid-liquid sep...

Embodiment 2

[0037] A core-shell type P-CoFe 2 o 4 The preparation method of @GCN photocatalyst comprises the following steps:

[0038] a) Fully mix cobalt sulfate and ferric chloride in equal volumes at a molar concentration ratio of 1:2 for 0.5h, the reaction temperature is 45°C, and the stirring rate is 600r·min -1 ;

[0039] b) Slowly add 2mol / L ammonia solution dropwise to the fully mixed solution until complete precipitation, and react at 90°C for 4h, then rinse with absolute ethanol and distilled water for several times, and dry at 70°C for 18h. Preparation of strong magnetic nanoparticles CoFe 2 o 4 ;

[0040] c) Weigh the prepared CoFe 2 o 4 Add it to 80 ml of distilled water, add urea and phytic acid to the mixed solution, stir thoroughly for 80 hours, and the stirring rate is 700r·min -1 , CoFe 2 o 4 , The mass ratio of urea and phytic acid is 0.08:1:0.5;

[0041] d) Dry the mixed solution at 90°C for 16 hours after solid-liquid separation, and grind it into powder;

...

Embodiment 3

[0045] A core-shell type P-CoFe 2 o 4 The preparation method of @GCN photocatalyst comprises the following steps:

[0046] a) Fully mix cobalt chloride and ferric chloride in equal volumes according to the molar concentration ratio of 1:2 for 1.0h, the reaction temperature is 55°C, and the stirring rate is 800r·min -1 ;

[0047] b) Slowly add 2mol / L sodium hydroxide solution dropwise to the fully mixed solution until complete precipitation, and react at 90°C for 5h, then rinse with absolute ethanol and distilled water several times, and dry at 80°C for 24h, Strong magnetic nanoparticles CoFe can be prepared 2 o 4 ;

[0048] c) Weigh the prepared CoFe 2 o 4 Add to 80 ml of distilled water, add melamine and melamine polyphosphate to the mixed solution, fully stir for 10h, the stirring speed is 1000r·min -1 , CoFe 2 o 4 , The mass ratio of melamine and melamine polyphosphate is 0.1:1:1;

[0049] d) The mixed solution in step c) is subjected to solid-liquid separation, ...

technical field

[0001] The invention belongs to the technical field of composite materials, and relates to a graphite carbon nitride photocatalyst, in particular to a core-shell type P-CoFe 2 o 4 The preparation method and application of @GCN photocatalyst. Background technique

[0002] Pharmaceuticals and personal care products (PPCPs) are an emerging pollutant. With the advancement of science and technology, this type of synthetic chemical substance is widely used all over the world. Due to improper handling, this kind of substance is continuously introduced into the In the ecological environment, thus entering the water body, researchers have detected trace amounts of antibiotic pollutants from natural water bodies, which will cause serious harm to human health. Among them, tetracycline antibiotics are one of the PPCPs. Due to their low price, they are widely used in livestock and poultry farming, and their usage accounts for more than half of the total antibiotics. Te...

Examples

Embodiment 1

[0028] A core-shell type P-CoFe 2 o 4 The preparation method of @GCN photocatalyst comprises the following steps:

[0029] a) Fully mix cobalt nitrate and ferric nitrate in equal volume for 0.5h according to the molar concentration ratio of 1:1, the reaction temperature is 35°C, and the stirring rate is 500r·min -1 ;

[0030] b) Slowly add 2mol / L potassium hydroxide solution dropwise to the fully mixed solution until complete precipitation, and react at 80°C for 3h, then rinse with absolute ethanol and distilled water several times, and dry at 60°C for 16h, Strong magnetic nanoparticles CoFe can be prepared 2 o 4 ;

[0031] c) Weigh the prepared CoFe 2 o 4 Add to 80 ml of distilled water, add thiourea and melamine polyphosphate to the mixed solution, fully stir for 5 hours, the stirring rate is 500r·min -1 , CoFe 2 o 4 , The mass ratio of thiourea and melamine polyphosphate is 0.05:1:0.2;

[0032] d) Dry the mixed solution at 80°C for 12 hours after solid-liquid sep...

Embodiment 2

[0037] A core-shell type P-CoFe 2 o 4 The preparation method of @GCN photocatalyst comprises the following steps:

[0038] a) Fully mix cobalt sulfate and ferric chloride in equal volumes at a molar concentration ratio of 1:2 for 0.5h, the reaction temperature is 45°C, and the stirring rate is 600r·min -1 ;

[0039] b) Slowly add 2mol / L ammonia solution dropwise to the fully mixed solution until complete precipitation, and react at 90°C for 4h, then rinse with absolute ethanol and distilled water for several times, and dry at 70°C for 18h. Preparation of strong magnetic nanoparticles CoFe 2 o 4 ;

[0040] c) Weigh the prepared CoFe 2 o 4 Add it to 80 ml of distilled water, add urea and phytic acid to the mixed solution, stir thoroughly for 80 hours, and the stirring rate is 700r·min -1 , CoFe 2 o 4 , The mass ratio of urea and phytic acid is 0.08:1:0.5;

[0041] d) Dry the mixed solution at 90°C for 16 hours after solid-liquid separation, and grind it into powder;

...

Embodiment 3

[0045] A core-shell type P-CoFe 2 o 4 The preparation method of @GCN photocatalyst comprises the following steps:

[0046] a) Fully mix cobalt chloride and ferric chloride in equal volumes according to the molar concentration ratio of 1:2 for 1.0h, the reaction temperature is 55°C, and the stirring rate is 800r·min -1 ;

[0047] b) Slowly add 2mol / L sodium hydroxide solution dropwise to the fully mixed solution until complete precipitation, and react at 90°C for 5h, then rinse with absolute ethanol and distilled water several times, and dry at 80°C for 24h, Strong magnetic nanoparticles CoFe can be prepared 2 o 4 ;

[0048] c) Weigh the prepared CoFe 2 o 4 Add to 80 ml of distilled water, add melamine and melamine polyphosphate to the mixed solution, fully stir for 10h, the stirring speed is 1000r·min -1 , CoFe 2 o 4 , The mass ratio of melamine and melamine polyphosphate is 0.1:1:1;

[0049] d) The mixed solution in step c) is subjected to solid-liquid separation, ...

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