CN112919526A - Preparation method of cuprous oxide nano material - Google Patents

Abstract

The invention discloses a preparation method of a cuprous oxide nano material, which comprises the following steps: selecting CuSO₄·5H₂O is used as a main salt raw material; accurate weighing of CuSO₄·5H₂Dissolving O in deionized water to form a solution A; weighing NaOH and dissolving the NaOH in deionized water to form solution B; mixing the solution A and the solution B, and magnetically stirring to form a solution C; adding ascorbic acid into the solution C, and magnetically stirring to obtain a solution containing yellow precipitates; transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, putting the reaction kettle into a drying box, and cooling the reaction kettle to room temperature along with the furnace after the reaction is finished; pouring out the supernatant of the obtained reaction product to obtain red precipitate containing impurities; placing the red precipitate in a centrifuge tube, and washing with deionized water and absolute ethyl alcohol for three times respectively to obtain pure red precipitate; and putting the pure red precipitate into a drying box, and drying to obtain red powder. The invention adopts a hydrothermal method to synthesize cuprous oxide nano polyhedronPure components, single appearance, high crystallization degree and large specific surface area.

Description

Preparation method of cuprous oxide nano material

Technical Field

The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a cuprous oxide nano material.

Background

Cuprous oxide has an energy band gap of about 2.2eV, is a p-type semiconductor photocatalytic material, has the advantages of no toxicity, good environmental acceptability, low price, high activity and the like compared with other metal oxide semiconductors, is widely concerned by people, and is widely applied to industries such as ceramics, coatings, plastics, glass, organic industrial catalysts and the like.

However, the existing cuprous oxide prepared by various different preparation methods contains Cu and Cu₄O₃In the case of (2), the components are not single enough, and there are problems such as low degradation rate, long degradation time and poor crystallinity.

Therefore, it is necessary to invent a preparation method of cuprous oxide nanomaterial with uniform morphology, pure components and high crystallization degree to solve the above problems.

Disclosure of Invention

Based on the defects of the prior art, the technical problem to be solved by the invention is to provide the preparation method of the cuprous oxide nano material, wherein the cuprous oxide nano polyhedron is synthesized by a hydrothermal method, and the cuprous oxide nano polyhedron has the advantages of pure components, single appearance, high crystallization degree and large specific surface area.

In order to solve the technical problems, the invention is realized by the following technical scheme:

the invention provides a preparation method of a cuprous oxide nano material, which comprises the following steps:

s1, selecting CuSO₄·5H₂O is used as a main salt raw material;

s2, accurately weighing 5mmol of CuSO₄·5H₂Dissolving O in 10ml of deionized water to form a solution A;

s3, weighing 30mmol of NaOH and dissolving in 20ml of deionized water to form a solution B;

s4, mixing the solution A and the solution B, and magnetically stirring for 30min to form a solution C;

s5, adding 25ml of ascorbic acid with the concentration of 0.04mol/l into the solution C, and magnetically stirring for 60min to obtain 55ml of solution containing yellow precipitates;

s6, transferring the reaction kettle into a 100mL reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, putting the reaction kettle into a drying box, setting the reaction temperature at 130 ℃ and the reaction time at 150 ℃, setting the reaction time at 3-7h, and cooling the reaction kettle to room temperature along with the furnace after the reaction is finished;

s7, pouring out the supernatant of the reaction product obtained in the step S4 to obtain red precipitate containing impurities;

s8, placing the red precipitate in a centrifuge tube, and washing the red precipitate with deionized water and absolute ethyl alcohol for three times respectively to obtain pure red precipitate;

s9, putting the pure red precipitate into a drying box, and drying at 60 ℃ for 12h to obtain red powder.

According to the invention, the cuprous oxide nano polyhedron is synthesized by using ascorbic acid as a reducing agent and adopting a hydrothermal method, the cuprous oxide nano polyhedron has the advantages of pure components, single appearance, high crystallization degree and large specific surface area, and meanwhile, the degradation rate of rhodamine B under the irradiation of ultraviolet light reaches 86.12%, so that the cuprous oxide nano polyhedron has the advantages of short degradation time, high degradation rate and low energy consumption.

The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments, together with the accompanying drawings.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.

Fig. 1 is a flow chart of the preparation method of the cuprous oxide nanomaterial of the present invention.

Detailed Description

Other aspects, features and advantages of the present invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings, which form a part of this specification, and which illustrate, by way of example, the principles of the invention. In the referenced drawings, the same or similar components in different drawings are denoted by the same reference numerals.

Example 1:

as shown in fig. 1, the preparation method of the cuprous oxide nanomaterial with uniform morphology, pure components and high crystallization degree specifically comprises the following steps:

s1, selecting CuSO₄·5H₂O is used as a main salt raw material;

s2, accurately weighing 5mmol of CuSO₄·5H₂Dissolving O in 10ml of deionized water to form a solution A;

s3, weighing 30mmol of NaOH and dissolving in 20ml of deionized water to form a solution B;

s4, mixing the solution A and the solution B, and magnetically stirring for 30min to form a solution C;

s5, adding 25ml of ascorbic acid with the concentration of 0.04mol/l into the solution C, and magnetically stirring for 60min to obtain 55ml of solution containing yellow precipitates;

s6, transferring the reaction kettle into a reaction kettle with a 100mL polytetrafluoroethylene lining, sealing the reaction kettle, putting the reaction kettle into a drying box, setting the reaction temperature to be 140 ℃, setting the reaction time to be 3 hours, and cooling the reaction kettle to room temperature along with the furnace after the reaction is finished;

s7, pouring out the supernatant of the reaction product obtained in the step S4 to obtain red precipitate containing impurities;

s8, placing the red precipitate in a centrifuge tube, and washing the red precipitate with deionized water and absolute ethyl alcohol for three times respectively to obtain pure red precipitate;

s9, putting the pure red precipitate into a drying box, and drying at 60 ℃ for 12h to obtain red powder.

Example 2:

unlike the above embodiment, in step S6, the reaction temperature was set to 140 ℃, and the reaction time was set to 5 h.

Example 3:

unlike the above embodiment, in step S6, the reaction temperature was set to 140 ℃, and the reaction time was set to 7 h.

Example 4:

unlike the above-described embodiment, in step S6, the reaction temperature was set to 130 ℃, and the reaction time was set to 5 h.

Example 5:

unlike the above-described embodiment, in step S6, the reaction temperature was set to 150 ℃, and the reaction time was set to 5 h.

The products obtained in the above examples 1 to 5 were collected, and the microscopic morphology of the synthesized product was observed by using a field emission scanning electron microscope, which revealed that:

the cuprous oxide nano material prepared in the embodiment 1 has the advantages of nonuniform grain size and morphology, large and small size and poor dispersibility;

the cuprous oxide nano material prepared in the embodiment 2 has a single crystal grain shape and is in a regular polyhedral shape;

the crystal grains of the cuprous oxide nano material prepared in the embodiment 3 are different in size;

the crystal grains of the cuprous oxide nanomaterial prepared in the embodiment 4 are irregular polyhedrons, different in size, poor in dispersibility and in an aggregation state;

the cuprous oxide nanomaterial prepared in example 5 has excessively large crystal grain size and is not single in shape.

From the above, the cuprous oxide nanomaterial prepared from the data in example 2 has the best quality, and the crystal grain shape is single and regular polyhedral.

Meanwhile, a photochemical reaction instrument and an ultraviolet-visible spectrometer are adopted to test the degradation capability of the product obtained in the example 2 on rhodamine B, and the result shows that the degradation rate of the product obtained in the example 2 on rhodamine B is up to 86.12% under the irradiation of ultraviolet light, so that the method has the advantages of short degradation time, high degradation rate and low energy consumption.

While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.

Claims (1)

1. The preparation method of the cuprous oxide nano material is characterized by comprising the following steps of:

s1, selecting CuSO₄·5H₂O is used as a main salt raw material;

s2, accurately weighing 5mmol of CuSO₄·5H₂Dissolving O in 10ml of deionized water to form a solution A;

s3, weighing 30mmol of NaOH and dissolving in 20ml of deionized water to form a solution B;

s4, mixing the solution A and the solution B, and magnetically stirring for 30min to form a solution C;

s5, adding 25ml of ascorbic acid with the concentration of 0.04mol/l into the solution C, and magnetically stirring for 60min to obtain 55ml of solution containing yellow precipitates;

s6, transferring the reaction kettle into a 100mL reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, putting the reaction kettle into a drying box, setting the reaction temperature at 130 ℃ and the reaction time at 150 ℃, setting the reaction time at 3-7h, and cooling the reaction kettle to room temperature along with the furnace after the reaction is finished;

s7, pouring out the supernatant of the reaction product obtained in the step S4 to obtain red precipitate containing impurities;

s8, placing the red precipitate in a centrifuge tube, and washing the red precipitate with deionized water and absolute ethyl alcohol for three times respectively to obtain pure red precipitate;

s9, putting the pure red precipitate into a drying box, and drying at 60 ℃ for 12h to obtain red powder.

Images