CN112279293A - Preparation method of copper sulfide nano material - Google Patents
Preparation method of copper sulfide nano material Download PDFInfo
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- CN112279293A CN112279293A CN202011205892.0A CN202011205892A CN112279293A CN 112279293 A CN112279293 A CN 112279293A CN 202011205892 A CN202011205892 A CN 202011205892A CN 112279293 A CN112279293 A CN 112279293A
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- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The embodiment of the invention discloses a preparation method of a copper sulfide nano material, which comprises the following steps: dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously; putting the obtained product into a constant-temperature water bath kettle, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process; transferring the obtained substance into a high-pressure hydrothermal reaction kettle, putting the high-pressure hydrothermal reaction kettle into an oven with the temperature of 130-; and taking the obtained product out of the high-pressure reaction kettle, washing the product for a plurality of times by absolute ethyl alcohol, then carrying out centrifugal separation, and finally drying the product to obtain the nano copper sulfide. According to the preparation method of the copper sulfide nano material, the crystallization process is directly controlled through the temperature difference, the process is simple and controllable, and the prepared copper sulfide nano rod is uniform in particle size and strong in stability.
Description
Technical Field
The invention relates to the field of preparation of copper sulfide nano materials, in particular to a preparation method of a copper sulfide nano material.
Background
The copper sulfide is an inorganic compound, is a sulfide of divalent copper, has a chemical formula of CuS, is black brown, is extremely insoluble, has good catalytic activity, visible light absorption, photoinduced power generation, three-order nonlinear polarizability, three-order nonlinear response speed and other properties, and has good application prospects in the fields of solar cells, photoelectric switches, gas sensors and the like.
In recent years, with the development of nanotechnology, nanomaterials are more and more concerned by researchers in various fields, and the properties of the nanomaterials are obviously changed due to the particularity of the nanomaterials, and the changes are embodied as five effects: dielectric confinement effects, volume effects, surface effects, macroscopic quantum tunneling effects, and quantum size effects. These five effects result in nanomaterials that exhibit unusual properties, both in physical and chemical nature.
Copper sulfide nano-material is an important semiconductor material, and is widely applied to thermocouples, optical recording, optical filters, solar cells, dry powder coating, fluorescent materials and superconductors, and particularly, rapid ionic conductivity shown at high temperature is of great interest to many researchers.
According to the appearance of the copper sulfide nanocrystal material, the copper sulfide nanocrystal material is divided into a plurality of nanoparticles, nanorods, nanowires, nanotubes, nanoflowers and the like, and can be synthesized by a hydrothermal method, a wet chemical synthesis method, a template method, a microwave method and the like. However, no matter which synthesis method is selected, the problems of complex synthesis process, uneven nano particle size, poor stability, difficult control, high cost and the like exist.
Disclosure of Invention
The invention aims to solve the technical problems that most of the existing synthetic methods of nano copper sulfide have the problems of complex synthetic process, uneven nano particle size, poor stability, difficulty in control and higher cost, and provides a preparation method of a copper sulfide nano material.
In order to solve the technical problem, the invention provides a preparation method of a copper sulfide nano material, which comprises the following steps:
step one, dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously;
step two: putting the obtained substance in the step one into a constant-temperature water bath, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process;
step three: transferring the obtained substance in the step two into a high-pressure hydrothermal reaction kettle, putting the high-pressure hydrothermal reaction kettle into an oven with the temperature of 130-;
step four: and (3) taking the obtained substance in the third step out of the high-pressure reaction kettle, washing the obtained substance for a plurality of times by using absolute ethyl alcohol, then carrying out centrifugal separation, and finally drying the obtained product to obtain the nano copper sulfide.
Further, in the first step, the mass ratio of the sodium sulfide, the copper chloride and the dilute hydrochloric acid is as follows: 1:1:(2-2.5).
Further, in the second step, the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 hours.
Further, in step three, the ratio of the amount of the substance of chloroform to the amount of the substance of dilute hydrochloric acid in step one was 1: 1.
Further, in the fourth step, after centrifugal separation, the nano copper sulfide is spread out in a drying oven for drying, the thickness of the spread nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, and the drying temperature is 60 ℃.
Furthermore, the prepared nano copper sulfide is in a nano rod shape, and the width is 80-90 nm.
The embodiment of the invention has the following beneficial effects: according to the preparation method of the copper sulfide nano material, the crystallization process is directly controlled through the temperature difference, the process is simple and controllable, and the prepared copper sulfide nano rod is uniform in particle size and strong in stability.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a copper sulfide nano material, which comprises the following steps:
the method comprises the following steps: dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously; the mass ratio of the added sodium sulfide, copper chloride and dilute hydrochloric acid is as follows: 1:1:(2-2.5).
Step two: putting the obtained substance in the step one into a constant-temperature water bath, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process; the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 h.
Step three: transferring the obtained substance in the step two into a high-pressure hydrothermal reaction kettle, putting the high-pressure hydrothermal reaction kettle into an oven with the temperature of 130-; the ratio of the amount of chloroform added to the amount of dilute hydrochloric acid in step one was 1: 1.
Step four: and (3) taking the obtained substance in the third step out of the high-pressure reaction kettle, washing the obtained substance for a plurality of times by absolute ethyl alcohol, then carrying out centrifugal separation, spreading the nano copper sulfide in a drying box for drying after the centrifugal separation, wherein the thickness of the spread nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, the drying temperature is 60 ℃, and the nano copper sulfide can be obtained after drying.
The method mainly controls the grain size and uniformity of the prepared nano copper sulfide crystal by a three-step cooling hydrothermal method in the three steps, the crystal form can have other disordered shapes due to overhigh temperature or temperature difference, and the crystallization degree is not high due to overlow temperature or temperature difference. The three temperatures selected in the application are just proper, the prepared nano copper sulfide is in a nanorod shape, the width is 80-90nm, and the nano copper sulfide is loaded on activated carbon to prepare a loaded catalyst due to large specific surface area, so that the loaded catalyst is used for treating sewage and coal-fired flue gas, has a great adsorption effect and has an excellent effect.
Example 1
Dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously; the mass ratio of the added sodium sulfide, copper chloride and dilute hydrochloric acid is as follows: 1:1:2.5. Putting the obtained product into a constant-temperature water bath kettle, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process; the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 h. Then transferring the mixture subjected to heating reflux treatment into a high-pressure hydrothermal reaction kettle, putting the mixture into a drying oven at 140 ℃ for reaction for 12 hours, adjusting the temperature of the drying oven to 110 ℃, reacting for 5 hours, adjusting the temperature of the drying oven to 70 ℃, reacting for 5 hours, opening the high-pressure reaction kettle, adding trichloromethane, introducing nitrogen into the drying oven at the same time, and continuously cooling to room temperature; the ratio of the amount of chloroform added to the amount of dilute hydrochloric acid in step one was 1: 1. And finally, taking out the nano copper sulfide from the high-pressure reaction kettle, washing the nano copper sulfide for a plurality of times by absolute ethyl alcohol, then carrying out centrifugal separation, spreading the spread nano copper sulfide in a drying box for drying after the centrifugal separation, wherein the thickness of the spread nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, the drying temperature is 60 ℃, and drying to obtain the nano copper sulfide.
Example 2
Dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously; the mass ratio of the added sodium sulfide, copper chloride and dilute hydrochloric acid is as follows: 1:1:2. Putting the obtained product into a constant-temperature water bath kettle, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process; the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 h. Then transferring the mixture subjected to heating reflux treatment into a high-pressure hydrothermal reaction kettle, putting the mixture into a drying oven at the temperature of 130 ℃ for reaction for 12 hours, adjusting the temperature of the drying oven to 100 ℃, reacting for 5 hours, adjusting the temperature of the drying oven to 60 ℃, reacting for 5 hours, opening the high-pressure reaction kettle, adding trichloromethane, introducing nitrogen into the drying oven at the same time, and continuously cooling to the room temperature; the ratio of the amount of chloroform added to the amount of dilute hydrochloric acid in step one was 1: 1. And finally, taking out the nano copper sulfide from the high-pressure reaction kettle, washing the nano copper sulfide for a plurality of times by absolute ethyl alcohol, then carrying out centrifugal separation, spreading the spread nano copper sulfide in a drying box for drying after the centrifugal separation, wherein the thickness of the spread nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, the drying temperature is 60 ℃, and drying to obtain the nano copper sulfide.
Example 3
Dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously; the mass ratio of the added sodium sulfide, copper chloride and dilute hydrochloric acid is as follows: 1:1:2.5. Putting the obtained product into a constant-temperature water bath kettle, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process; the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 h. Then transferring the mixture subjected to heating reflux treatment into a high-pressure hydrothermal reaction kettle, putting the mixture into a 135 ℃ drying oven for reaction for 12 hours, adjusting the temperature of the drying oven to 105 ℃, reacting for 5 hours, adjusting the temperature of the drying oven to 65 ℃, reacting for 5 hours, opening the high-pressure reaction kettle, adding trichloromethane, introducing nitrogen into the drying oven at the same time, and continuously cooling to room temperature; the ratio of the amount of chloroform added to the amount of dilute hydrochloric acid in step one was 1: 1. And finally, taking out the nano copper sulfide from the high-pressure reaction kettle, washing the nano copper sulfide for a plurality of times by absolute ethyl alcohol, then carrying out centrifugal separation, spreading the spread nano copper sulfide in a drying box for drying after the centrifugal separation, wherein the thickness of the spread nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, the drying temperature is 60 ℃, and drying to obtain the nano copper sulfide.
Example 4
Dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously; the mass ratio of the added sodium sulfide, copper chloride and dilute hydrochloric acid is as follows: 1:1:2.3. Putting the obtained product into a constant-temperature water bath kettle, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process; the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 h. Then transferring the mixture subjected to heating reflux treatment into a high-pressure hydrothermal reaction kettle, putting the mixture into a drying oven at 140 ℃ for reaction for 12 hours, adjusting the temperature of the drying oven to 105 ℃, reacting for 5 hours, adjusting the temperature of the drying oven to 60 ℃, reacting for 5 hours, opening the high-pressure reaction kettle, adding trichloromethane, introducing nitrogen into the drying oven at the same time, and continuously cooling to room temperature; the ratio of the amount of chloroform added to the amount of dilute hydrochloric acid in step one was 1: 1. And finally, taking out the nano copper sulfide from the high-pressure reaction kettle, washing the nano copper sulfide for a plurality of times by absolute ethyl alcohol, then carrying out centrifugal separation, spreading the spread nano copper sulfide in a drying box for drying after the centrifugal separation, wherein the thickness of the spread nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, the drying temperature is 60 ℃, and drying to obtain the nano copper sulfide.
The embodiment of the invention has the following beneficial effects: according to the preparation method of the copper sulfide nano material, the crystallization process is directly controlled through the temperature difference, the process is simple and controllable, and the prepared copper sulfide nano rod is uniform in particle size and strong in stability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A preparation method of a copper sulfide nano material is characterized by comprising the following steps:
the method comprises the following steps: dissolving sodium sulfide and copper chloride into a dilute hydrochloric acid solution simultaneously;
step two: putting the obtained substance in the step one into a constant-temperature water bath, carrying out heating reflux treatment, and continuously stirring in the heating reflux treatment process;
step three: transferring the obtained substance in the step two into a high-pressure hydrothermal reaction kettle, putting the high-pressure hydrothermal reaction kettle into an oven with the temperature of 130-;
step four: and (3) taking the obtained substance in the third step out of the high-pressure reaction kettle, washing the obtained substance for a plurality of times by using absolute ethyl alcohol, then carrying out centrifugal separation, and finally drying the obtained product to obtain the nano copper sulfide.
2. The method for preparing copper sulfide nano material according to claim 1, wherein in the first step, the ratio of the amount of sodium sulfide, copper chloride and dilute hydrochloric acid is as follows: 1:1:(2-2.5).
3. The method for preparing the copper sulfide nano material according to the claim 1, wherein in the second step, the heating temperature of the heating reflux treatment is 100 ℃, and the treatment time is 3 h.
4. The method for preparing copper sulfide nanomaterial according to claim 1, wherein the ratio of the amount of chloroform added in step three to the amount of dilute hydrochloric acid in step one is 1: 1.
5. The method for preparing the copper sulfide nano material according to the claim 1, wherein in the fourth step, after the centrifugal separation, the nano copper sulfide is spread out in a drying oven for drying, the thickness of the spread-out nano copper sulfide is not more than 0.5cm, the drying time is not less than 5h, and the drying temperature is 60 ℃.
6. The method for preparing copper sulfide nano-material according to any one of claims 1 to 5, wherein the prepared nano copper sulfide is in a shape of nano-rod with a width of 80 to 90 nm.
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