Summary of the invention
The objective of the invention is to propose the method that the auxiliary sonochemistry of a kind of hydro-thermal prepares cobalt sulfide nanocrystalline.This method is simple to operate, the cobalt sulfide nanocrystalline well-crystallized of gained, and particle size dispersion is better.
For achieving the above object, the technical scheme that the present invention adopts is:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 1.16g-5.80g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.58g-2.90g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.5-4.0mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.14mL-0.68mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 10-60min, ultrasonic power 200-500W, ultrasonic temperature 20-80 ℃;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 50%-80%, and sealing afterwards is at 170-210 ℃ of reaction 6-24h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Because the sonochemistry energy produces in the reaction process HTHP, intensive shockwave and high speed jet, having hindered particle becomes big micelle, and the criticality of thermal and hydric environment impels the crystallinity of crystal grain better, makes that the product crystallinity of gained is fine.The cobalt sulfide nanocrystalline pattern of this method preparation is controlled, is the nano bar-shape structure, and diameter is about 10nm; And preparation technology is simple, and is easy to operate, and temperature is low, and energy consumption is little, and preparation cost is lower.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 2.32g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 1.16g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 2.0mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.28mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 30min, ultrasonic power 300W, 80 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 8%, and sealing afterwards is at 190 ℃ of reaction 24h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
The cobalt sulfide nanocrystalline of gained is observed with transmission electron microscope, can be found out that prepared sample is the nano bar-shape structure, diameter is (Fig. 1) about 10nm.
Embodiment 2:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 1.16g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.58g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.5mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.14mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 60min, ultrasonic power 500W, 50 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 80%, and sealing afterwards is at 180 ℃ of reaction 18h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 3:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 5.80g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 2.90g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 4.0mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.68mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 15min, ultrasonic power 200W, 40 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 50%, and sealing afterwards is at 170 ℃ of reaction 20h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 4:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 3.25g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 2.30g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 1.0mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.55mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 20min, ultrasonic power 400W, 20 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 60%, and sealing afterwards is at 200 ℃ of reaction 6h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 5:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 4.60g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 1.65g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 3.0mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.32mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 40min, ultrasonic power 500W, 60 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 70%, and sealing afterwards is at 210 ℃ of reaction 6h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.
Embodiment 6:
1) gets the analytical pure cobalt nitrate hexahydrate (Co (NO of 5.00g
3)
26H
2O) place Erlenmeyer flask, in Erlenmeyer flask, add deionized water, stir, be configured to the red clear solution A of 40mL;
2) get 0.80g YD 30 (EDTA) add stir in the solution A solution B;
3) mass concentration that in solution B, adds 0.8mL is 2% H
2S solution, stir solution C;
4) get (NH of 0.22mL
4)
2S places small beaker, and adds the solution D that deionized water is configured to 40mL;
5) solution C is put into ultrasonic cleaner and shake, dropwise add solution D simultaneously, set ultrasonic time 50min, ultrasonic power 300W, 70 ℃ of ultrasonic temperature;
6) solution behind the ultrasonic reaction is added in the water heating kettle, controlling its packing ratio is 60%, and sealing afterwards is at 200 ℃ of reaction 10h;
7) after reaction finishes, the water heating kettle taking-up is cooled to room temperature, after product was separated, the product after the separation cleaned with deionized water and absolute ethyl alcohol respectively, and the baking oven of putting into 80 ℃ carries out drying, obtains the cobalt sulfide nanocrystalline of black.