CN110683571B - Preparation method of flower-shaped cuprous sulfide micron particles - Google Patents
Preparation method of flower-shaped cuprous sulfide micron particles Download PDFInfo
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- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a preparation method of flower-shaped cuprous sulfide micron particles. After preparing a copper sulfate pentahydrate aqueous solution, a sodium hydroxide aqueous solution and a glucose aqueous solution respectively, firstly dropwise adding the sodium hydroxide aqueous solution into the copper sulfate pentahydrate aqueous solution according to a proportion, then violently stirring to obtain a mixed solution, then adding the glucose aqueous solution into the stirred mixed solution, then carrying out centrifugal cleaning on the obtained intermediate reaction liquid, dispersing the obtained solid into deionized water, then adding sodium sulfide powder into the intermediate product dispersion liquid, violently shaking the intermediate product dispersion liquid, and standing after the intermediate product dispersion liquid is completely blackened to obtain a product in the final reaction liquid; wherein the product is spherical with a diameter of 2-3 μm, and the spherical material is composed of multiple petal-shaped sheets with a thickness of 35-40 nm. The method has the characteristics of time saving, energy saving and low cost, and the prepared product is very easy to be widely and commercially applied to the fields of photo-thermal conversion, thin-film solar photovoltaic, catalysis, biosensors and the like.
Description
Technical Field
The invention relates to a preparation method of micron particles, in particular to a preparation method of flower-shaped cuprous sulfide micron particles.
Background
Cuprous sulfide (Cu) with good chemical and thermal stability2S) is a narrow-bandgap p-type semiconductor material, and has great application potential in the fields of photo-thermal conversion, thin-film solar photovoltaic, catalysis, biosensors and the like. In practical application, the micro-morphology, structure and size of the cuprous sulfide directly influence the performance of the cuprous sulfide. Thus, some beneficial attempts and efforts have been made to obtain cuprous sulfide in micro-nano dimensions, such as the title "Two-step synthesis of novel Cu2S nanofluwers for field emission application ", Materials Letters, 2014, 137: 56-58 ("two-step synthesis of novel cuprous sulfide nanoflowers and their field emission applications", volume 137, pages 56-58 of materials bulletin 2014). Cuprous sulfide is referred to herein as flower-like micro-particles; the preparation method adopts a hydrothermal-solvent synthesis method, and the specific process comprises the steps of mixing copper chloride powder and thiourea powder in an ethanol solution for reaction to form a slurry-like substance, and then carrying out the reactionTransferring the mixture into a reaction kettle to react for 6 hours at the temperature of 160 ℃ to obtain a product. Although the preparation method is relatively simple and can prepare a large amount of flower-shaped cuprous sulfide micron particles, the preparation method has the defects of long time consumption and relatively large energy consumption.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a time-saving and energy-saving preparation method of flower-shaped cuprous sulfide micron particles.
In order to solve the technical problem, the technical scheme adopted by the invention is that the preparation method of the flower-shaped cuprous sulfide micron particles adopts an ion exchange method, and particularly comprises the following main steps:
step 1, respectively preparing 200-300g/L copper sulfate pentahydrate aqueous solution, 100-150g/L sodium hydroxide aqueous solution and 150-250g/L glucose aqueous solution;
step 2, firstly, according to the volume ratio of the blue vitriol aqueous solution, the sodium hydroxide aqueous solution and the glucose aqueous solution of 0.8-1.2: 0.8-1.2: 0.8-1.2, adding the sodium hydroxide aqueous solution into the copper sulfate pentahydrate aqueous solution drop by drop, stirring vigorously for at least 3min to obtain a mixed solution, placing the mixed solution at 45-55 ℃, stirring for at least 3min, adding the glucose aqueous solution into the mixed solution under the stirring state, and reacting under stirring for at least 25min to obtain an intermediate reaction solution;
step 3, firstly, centrifugally cleaning the intermediate reaction solution, dispersing the obtained solid into deionized water to obtain an intermediate product dispersion solution, then adding 0.1-0.3g of sodium sulfide powder into 10-15g/L of the intermediate product dispersion solution, violently shaking the intermediate product dispersion solution, and standing for at least 8min after the intermediate product dispersion solution is completely blackened to obtain flower-shaped cuprous sulfide micron particles in the final reaction solution;
wherein the flower-shaped cuprous sulfide micron particles are spherical with the diameter of 2-3 mu m, and the spheres are composed of a plurality of petal-shaped sheets with the thickness of 35-40 nm.
As a further improvement of the preparation method of the flower-shaped cuprous sulfide micron particles:
preferably, the flower-like cuprous sulfide micro-particles in the final reaction solution are centrifugally cleaned, and then the obtained flower-like cuprous sulfide micro-particles are dispersed in deionized water.
Preferably, the stirring rate during vigorous stirring is 800-.
Preferably, the centrifugal washing times of the intermediate reaction solution and the flower-like cuprous sulfide micro-particles in the final reaction solution are 2-4 times.
Preferably, the rotational speed of centrifugal separation is 2000-6000r/min and the time is 2-6min during centrifugal cleaning.
Preferably, the cleaning agent is deionized water during centrifugal cleaning.
Compared with the prior art, the beneficial effects are that:
firstly, the prepared product is respectively characterized by using a scanning electron microscope and an X-ray diffractometer, and the result shows that the product is spherical with the diameter of 2-3 mu m, and the spherical object consists of a plurality of petal-shaped sheets with the thickness of 35-40 nm; the composition of the spherical object composed of a plurality of petal-shaped sheets with the thickness of 35-40nm is cuprous sulfide. The product assembled by the cuprous sulfide of the petal-shaped sheets is characterized in that the cuprous sulfide and a large number of two-dimensional sheets with nanometer-scale thickness are staggered and crossed to form the microspheres, so that multiple reflections can occur between the sheets when light waves irradiate the surfaces of the two-dimensional sheets, the absorption and utilization of light are greatly increased, and the huge specific surface area of the two-dimensional sheets is more favorable for adsorbing organic pollutants in photocatalysis application.
Secondly, the preparation method is simple, scientific and efficient. The method is easy for large-batch industrial preparation of the product, namely the flower-shaped cuprous sulfide micron particles, and has the characteristics of time saving, energy saving and low cost; and the prepared product is easy to be widely applied to the fields of photo-thermal conversion, thin film solar photovoltaic, catalysis, biosensors and the like in a commercialized mode.
Drawings
Fig. 1 is one of the results of characterization of the product obtained by the preparation method using a Scanning Electron Microscope (SEM). Fig. 1, a, is an SEM image of the product, from which it can be seen that the product is spherical in shape with a uniform size; panel b is a high magnification SEM image of the product shown in panel a, showing that the spherical product is composed of a large number of petal-shaped pieces.
Fig. 2 is one of the results of characterization of the obtained product using an X-ray diffraction (XRD) instrument. And comparing the spectral line of the product in the XRD spectrogram with a standard cuprous sulfide XRD curve at the bottom of the XRD spectrogram, and confirming that the component of the product is cuprous sulfide with a cubic structure.
Detailed Description
The preferred embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
First commercially available or manufactured on its own:
copper sulfate pentahydrate aqueous solution;
an aqueous sodium hydroxide solution;
an aqueous glucose solution;
deionized water;
sodium sulfide powder.
Then:
example 1
The preparation method comprises the following specific steps:
step 1, preparing 200g/L copper sulfate pentahydrate aqueous solution, 150g/L sodium hydroxide aqueous solution and 150g/L glucose aqueous solution respectively.
Step 2, firstly, according to the volume ratio of the blue vitriol aqueous solution, the sodium hydroxide aqueous solution and the glucose aqueous solution of 0.8: 1.2: 0.8, dropwise adding the sodium hydroxide aqueous solution into the copper sulfate pentahydrate aqueous solution, and violently stirring for 3 min; wherein the stirring speed during vigorous stirring is 1000r/min, and a mixed solution is obtained. And stirring the mixed solution at 45 ℃ for 7min, adding a glucose aqueous solution into the mixed solution under a stirring state, and stirring to react for 25min to obtain an intermediate reaction solution.
Step 3, firstly, carrying out centrifugal cleaning on the intermediate reaction liquid for 2 times, and then dispersing the obtained solid into deionized water; wherein, during centrifugal cleaning, the rotating speed of centrifugal separation is 2000r/min, the time is 6min, and the cleaning agent during centrifugal cleaning is deionized water, so as to obtain the intermediate product dispersion liquid. And adding 0.3g of sodium sulfide powder into 10g/L of the intermediate product dispersion liquid, violently shaking the intermediate product dispersion liquid, and standing for 8min after the intermediate product dispersion liquid is completely blackened to obtain the flower-shaped cuprous sulfide micron particles in the final reaction liquid. Then, carrying out 2 times of centrifugal cleaning on the flower-shaped cuprous sulfide micron particles in the final reaction solution; wherein, the rotational speed of centrifugal separation is 2000r/min and the time is 6min during centrifugal cleaning, the cleaning agent during centrifugal cleaning is deionized water, flower-shaped cuprous sulfide micron particles similar to those shown in figure 1 and shown in a curve in figure 2 are prepared, and then the obtained flower-shaped cuprous sulfide micron particles are dispersed in the deionized water.
Example 2
The preparation method comprises the following specific steps:
step 1, respectively preparing 225g/L copper sulfate pentahydrate aqueous solution, 138g/L sodium hydroxide aqueous solution and 175g/L glucose aqueous solution.
Step 2, firstly, according to the volume ratio of the blue vitriol aqueous solution, the sodium hydroxide aqueous solution and the glucose aqueous solution of 0.9: 1.1: 0.9, dropwise adding the sodium hydroxide aqueous solution into the copper sulfate pentahydrate aqueous solution, and violently stirring for 4 min; wherein the stirring speed during vigorous stirring is 950r/min, and a mixed solution is obtained. And stirring the mixed solution at 48 ℃ for 6min, adding a glucose aqueous solution into the mixed solution under a stirring state, and stirring to react for 28min to obtain an intermediate reaction solution.
Step 3, firstly, centrifugally cleaning the intermediate reaction liquid for 2 times, and then dispersing the obtained solid into deionized water; wherein, during centrifugal cleaning, the rotating speed of centrifugal separation is 3000r/min, the time is 5min, and the cleaning agent during centrifugal cleaning is deionized water, so as to obtain the intermediate product dispersion liquid. And adding 0.25g of sodium sulfide powder into 11g/L of the intermediate product dispersion liquid, violently shaking the intermediate product dispersion liquid, and standing for 9min after the intermediate product dispersion liquid is completely blackened to obtain the flower-shaped cuprous sulfide micron particles in the final reaction liquid. Then, carrying out 2 times of centrifugal cleaning on the flower-shaped cuprous sulfide micron particles in the final reaction solution; wherein, the rotational speed of centrifugal separation is 3000r/min and the time is 5min during centrifugal cleaning, the cleaning agent during centrifugal cleaning is deionized water, flower-shaped cuprous sulfide micron particles similar to those shown in figure 1 and shown by the curve in figure 2 are prepared, and then the obtained flower-shaped cuprous sulfide micron particles are dispersed in the deionized water.
Example 3
The preparation method comprises the following specific steps:
step 1, preparing 250g/L of blue vitriol aqueous solution, 125g/L of sodium hydroxide aqueous solution and 200g/L of glucose aqueous solution respectively.
Step 2, firstly, mixing copper sulfate pentahydrate aqueous solution, sodium hydroxide aqueous solution and glucose aqueous solution according to the volume ratio of 1: 1: 1, dropwise adding a sodium hydroxide aqueous solution into a copper sulfate pentahydrate aqueous solution, and violently stirring for 5 min; wherein the stirring speed during vigorous stirring is 900r/min, and a mixed solution is obtained. And stirring the mixed solution at 50 ℃ for 5min, adding a glucose aqueous solution into the mixed solution under a stirring state, and stirring to react for 30min to obtain an intermediate reaction solution.
Step 3, firstly, centrifugally cleaning the intermediate reaction solution for 3 times, and then dispersing the obtained solid into deionized water; wherein, during centrifugal cleaning, the rotating speed of centrifugal separation is 4000r/min, the time is 4min, and the cleaning agent during centrifugal cleaning is deionized water, so as to obtain the intermediate product dispersion liquid. And adding 0.2g of sodium sulfide powder into 12g/L of the intermediate product dispersion liquid, violently shaking the intermediate product dispersion liquid, and standing for 10min after the intermediate product dispersion liquid is completely blackened to obtain the flower-shaped cuprous sulfide micron particles in the final reaction liquid. Then, carrying out 3 times of centrifugal cleaning on the flower-shaped cuprous sulfide micron particles in the final reaction solution; wherein, the rotational speed of centrifugal separation is 4000r/min and the time is 4min during centrifugal cleaning, the cleaning agent during centrifugal cleaning is deionized water, flower-shaped cuprous sulfide micro-particles shown in figure 1 and shown in a curve in figure 2 are prepared, and then the obtained flower-shaped cuprous sulfide micro-particles are dispersed in the deionized water.
Example 4
The preparation method comprises the following specific steps:
step 1, 275g/L of blue vitriol aqueous solution, 113g/L of sodium hydroxide aqueous solution and 225g/L of glucose aqueous solution are prepared respectively.
Step 2, firstly, according to the volume ratio of the blue vitriol aqueous solution, the sodium hydroxide aqueous solution and the glucose aqueous solution of 1.1: 0.9: 1.1, adding the sodium hydroxide aqueous solution into the copper sulfate pentahydrate aqueous solution drop by drop, and stirring vigorously for 6 min; wherein the stirring speed during vigorous stirring is 850r/min, and a mixed solution is obtained. And stirring the mixed solution at 53 deg.C for 4min, adding glucose aqueous solution under stirring, and stirring for reaction for 33min to obtain intermediate reaction solution.
Step 3, firstly, centrifugally cleaning the intermediate reaction solution for 3 times, and then dispersing the obtained solid into deionized water; wherein, during centrifugal cleaning, the rotating speed of centrifugal separation is 5000r/min, the time is 3min, and the cleaning agent during centrifugal cleaning is deionized water, so as to obtain an intermediate product dispersion liquid. And adding 0.15g of sodium sulfide powder into 13g/L of the intermediate product dispersion liquid, violently shaking the intermediate product dispersion liquid, and standing for 11min after the intermediate product dispersion liquid is completely blackened to obtain the flower-shaped cuprous sulfide micron particles in the final reaction liquid. Then, carrying out 3 times of centrifugal cleaning on the flower-shaped cuprous sulfide micron particles in the final reaction solution; wherein, the rotational speed of centrifugal separation is 5000r/min and the time is 3min during centrifugal cleaning, the cleaning agent during centrifugal cleaning is deionized water, flower-shaped cuprous sulfide micron particles similar to those shown in figure 1 and shown in a curve in figure 2 are prepared, and then the obtained flower-shaped cuprous sulfide micron particles are dispersed in the deionized water.
Example 5
The preparation method comprises the following specific steps:
step 1, preparing 300g/L of copper sulfate pentahydrate aqueous solution, 100g/L of sodium hydroxide aqueous solution and 250g/L of glucose aqueous solution respectively.
Step 2, firstly, mixing copper sulfate pentahydrate aqueous solution, sodium hydroxide aqueous solution and glucose aqueous solution according to the volume ratio of 1.2: 0.8: 1.2, dropwise adding a sodium hydroxide aqueous solution into a copper sulfate pentahydrate aqueous solution, and violently stirring for 7 min; wherein the stirring speed during vigorous stirring is 800r/min, and a mixed solution is obtained. And stirring the mixed solution at 55 ℃ for 3min, adding a glucose aqueous solution into the mixed solution under a stirring state, and stirring to react for 35min to obtain an intermediate reaction solution.
Step 3, firstly, carrying out centrifugal cleaning on the intermediate reaction liquid for 4 times, and then dispersing the obtained solid into deionized water; wherein, during centrifugal cleaning, the rotating speed of centrifugal separation is 6000r/min, the time is 2min, and the cleaning agent during centrifugal cleaning is deionized water, so as to obtain the intermediate product dispersion liquid. And adding 0.1g of sodium sulfide powder into 15g/L of the intermediate product dispersion liquid, violently shaking the intermediate product dispersion liquid, and standing for 12min after the intermediate product dispersion liquid is completely blackened to obtain the flower-shaped cuprous sulfide micron particles in the final reaction liquid. Then, carrying out centrifugal cleaning on the flower-like cuprous sulfide micron particles in the final reaction solution for 4 times; wherein, the rotational speed of the centrifugal separation is 6000r/min and the time is 2min during the centrifugal cleaning, the cleaning agent during the centrifugal cleaning is deionized water, the flower-shaped cuprous sulfide micron particles similar to those shown in figure 1 and shown in the curve of figure 2 are prepared, and then the obtained flower-shaped cuprous sulfide micron particles are dispersed in the deionized water.
It is apparent that those skilled in the art can make various modifications and variations to the method for preparing the flower-shaped cuprous sulfide micro-particles of the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (6)
1. A preparation method of flower-shaped cuprous sulfide micron particles adopts an ion exchange method, and is characterized by mainly comprising the following steps:
step 1, respectively preparing 200-300g/L copper sulfate pentahydrate aqueous solution, 100-150g/L sodium hydroxide aqueous solution and 150-250g/L glucose aqueous solution;
step 2, firstly, according to the volume ratio of the blue vitriol aqueous solution, the sodium hydroxide aqueous solution and the glucose aqueous solution of 0.8-1.2: 0.8-1.2: 0.8-1.2, adding the sodium hydroxide aqueous solution into the copper sulfate pentahydrate aqueous solution drop by drop, stirring vigorously for at least 3min to obtain a mixed solution, placing the mixed solution at 45-55 ℃, stirring for at least 3min, adding the glucose aqueous solution into the mixed solution under the stirring state, and reacting under stirring for at least 25min to obtain an intermediate reaction solution;
step 3, firstly, centrifugally cleaning the intermediate reaction solution, dispersing the obtained solid into deionized water to obtain an intermediate product dispersion solution, then adding 0.1-0.3g of sodium sulfide powder into 10-15g/L of the intermediate product dispersion solution, violently shaking the intermediate product dispersion solution, and standing for at least 8min after the intermediate product dispersion solution is completely blackened to obtain flower-shaped cuprous sulfide micron particles in the final reaction solution;
wherein the flower-shaped cuprous sulfide micron particles are spherical with the diameter of 2-3 mu m, and the spheres are composed of a plurality of petal-shaped sheets with the thickness of 35-40 nm.
2. The method for preparing the flower-like cuprous sulfide micron particles according to claim 1, wherein the flower-like cuprous sulfide micron particles in the final reaction solution are centrifugally cleaned, and then the obtained flower-like cuprous sulfide micron particles are dispersed in deionized water.
3. The method for preparing flower-like cuprous sulfide micron particles as claimed in claim 1, wherein the stirring speed during vigorous stirring is 800-1000 r/min.
4. The method for producing flower-like cuprous sulfide micro particles according to claim 1 or 2, wherein the number of times of centrifugal washing of the intermediate reaction solution and the flower-like cuprous sulfide micro particles in the final reaction solution is 2-4 times.
5. The method for preparing flower-shaped cuprous sulfide micron particles as claimed in claim 4, wherein the rotation speed of centrifugal separation is 2000-6000r/min and the time is 2-6 min.
6. The method for preparing flower-like cuprous sulfide micron particles, according to claim 5, wherein when centrifugally cleaning, the cleaning agent is deionized water.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04349117A (en) * | 1991-05-27 | 1992-12-03 | Mitsubishi Materials Corp | Production of cuprous sulfide |
| CN104495908A (en) * | 2014-12-31 | 2015-04-08 | 湖南稀土金属材料研究院 | Preparation method of cuprous sulfide powder, and cuprous sulfide powder |
| CN109516492A (en) * | 2018-12-18 | 2019-03-26 | 合肥学院 | A kind of Cu2The preparation method of S micro nanocrystalline |
| CN110127749A (en) * | 2019-05-28 | 2019-08-16 | 昆明理工大学 | A kind of preparation method of the cuprous sulfide nano flower of cupric defect |
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2019
- 2019-09-27 CN CN201910920837.0A patent/CN110683571B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04349117A (en) * | 1991-05-27 | 1992-12-03 | Mitsubishi Materials Corp | Production of cuprous sulfide |
| CN104495908A (en) * | 2014-12-31 | 2015-04-08 | 湖南稀土金属材料研究院 | Preparation method of cuprous sulfide powder, and cuprous sulfide powder |
| CN109516492A (en) * | 2018-12-18 | 2019-03-26 | 合肥学院 | A kind of Cu2The preparation method of S micro nanocrystalline |
| CN110127749A (en) * | 2019-05-28 | 2019-08-16 | 昆明理工大学 | A kind of preparation method of the cuprous sulfide nano flower of cupric defect |
Non-Patent Citations (1)
| Title |
|---|
| 沉淀转化法制备非化学计量化合物Cu2-xS的物相研究;陈建波等;《稀有金属与硬质合金》;20151231;第43卷(第6期);第56-58页 * |
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