CN111747384A - Method for preparing low-toxicity molybdenum diselenide by ultrasonic wave - Google Patents
Method for preparing low-toxicity molybdenum diselenide by ultrasonic wave Download PDFInfo
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- CN111747384A CN111747384A CN202010610747.4A CN202010610747A CN111747384A CN 111747384 A CN111747384 A CN 111747384A CN 202010610747 A CN202010610747 A CN 202010610747A CN 111747384 A CN111747384 A CN 111747384A
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- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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Abstract
The invention belongs to the field of nano material preparation methods, and particularly relates to a method for preparing low-toxicity molybdenum diselenide by ultrasonic waves, which has the technical key points that: adding selenium powder and sodium molybdate into a polytetrafluoroethylene inner container, adding deionized water and hydrazine hydrate, uniformly stirring, carrying out hydrothermal reaction, naturally cooling, and repeatedly washing with deionized water until the mixture is neutral. Preparing a mixed liquid of deionized water and organic alcohols, adding the prepared molybdenum diselenide powder into the organic mixed solution for ultrasonic dispersion, centrifugally washing the mixed solution by the deionized water, and drying the washed mixed solution at 60 ℃ to obtain the product. The prepared carbon-coated molybdenum diselenide has excellent dispersibility in water and has a great application value in the fields of biological medicines and the like.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing low-toxicity molybdenum diselenide by ultrasonic waves.
Background
Molybdenum diselenide has been widely studied as one of transition metal compounds in various fields such as optoelectronics, medicine, batteries, and the like. Molybdenum diselenide has lower cytotoxicity than graphene and its analogs. Selenium and molybdenum are essential trace elements for human body, and the toxicity of molybdenum diselenide is lower than that of other two-dimensional transition metal double-halide materials. As an inorganic material, the normal molybdenum diselenide has poor biocompatibility to human body, so that the search for a processing method of a molybdenum diselenide nano material with good biocompatibility and multiple functions is urgent.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for preparing low-toxicity molybdenum diselenide by ultrasonic waves. The research on the influence of the carbon-doped molybdenum diselenide nano particles on biocompatibility and the reduction of the toxicity of the carbon-doped molybdenum diselenide nano particles are of great significance.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing low-toxicity molybdenum diselenide by ultrasonic waves comprises the steps of adding molybdenum diselenide into a mixed liquid of deionized water and organic alcohols, dispersing by ultrasonic waves, washing by deionized water, and drying.
The molybdenum selenide can be prepared by the following method: selenium powder, sodium molybdate, hydrazine hydrate and deionized water are mixed to carry out hydrothermal reaction (the mixture can be fully and uniformly stirred in a polytetrafluoroethylene liner to realize mixing, and then the hydrothermal reaction is directly carried out), and after natural cooling, the mixture is repeatedly washed by the deionized water to be neutral.
Wherein the mass ratio of the selenium powder to the sodium molybdate is preferably 1: 1-2. The volume ratio of hydrazine hydrate to distilled water is 1: 5-10. The conditions of the hydrothermal reaction are preferably 180 ℃ and 220 ℃ for 12-24 h.
The organic alcohol can be any one or more of ethanol, polyethylene glycol and isopropanol, and the volume ratio of the organic alcohol to the deionized water is 1: 1-5.
The mass ratio of the molybdenum selenide to the organic alcohol is preferably 1: 100-1000.
The frequency of ultrasonic wave in the ultrasonic dispersion is preferably 20-40KHZ, the power is preferably 200-1500W, the dispersion time is preferably 2-4h, and the ultrasonic wave is dried at 60 ℃ after centrifugal washing by deionized water.
The principle of the invention is as follows:
high-power ultrasound is adopted in the preparation process of the molybdenum diselenide nano material, and pyrolysis and ultrasonic dispersion in the cavitation process play a leading role. The ultrasonic cavitation phenomenon of ultrasonic waves is utilized to release huge energy, and cavitation bubbles generate a local high-temperature high-pressure environment at the moment of explosion. The organic mixture is subjected to chemical bond breakage, water phase combustion or thermal decomposition in the cavitation bubbles under the conditions, and the formation of the carbide on the surface of the molybdenum diselenide is promoted. The prepared carbon-coated molybdenum diselenide has excellent dispersibility in water and has a great application value in the fields of biological medicines and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. the ultrasonic technology is simple, safe, low in cost and high in biocompatibility of the product.
2. The carbon content on the surface is adjustable: the carbon content of the surface of the molybdenum diselenide can be adjusted according to the proportion of the organic mixed solution, so that the biocompatibility of the material is adjusted. The covering carbonized layer increases with the increase of organic solvent, and the biocompatibility becomes better.
Drawings
Fig. 1 is a graph comparing biocompatibility before molybdenum diselenide treatment in example 1.
Fig. 2 is a graph comparing biocompatibility after molybdenum diselenide treatment of example 1.
Fig. 3 is a Scanning Electron Microscope (SEM) image of molybdenum diselenide of example 1.
Fig. 4 is a Transmission Electron Microscope (TEM) image of molybdenum diselenide of example 1.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
Example 1: adding 0.5g of selenium powder, 0.765g of sodium molybdate, 5mL of hydrazine hydrate and 40mL of deionized water into a polytetrafluoroethylene inner container, and fully and uniformly stirring. Carrying out hydrothermal reaction for 12h at 200 ℃, naturally cooling, and repeatedly washing with deionized water until the solution is neutral. 100mL of a mixed solution of isopropanol (50mL) and deionized water (50mL) was prepared, and the volume ratio of the isopropanol to the deionized water was 1: 1. Adding the prepared molybdenum diselenide into a mixed organic solution, wherein the mass ratio of the molybdenum diselenide to the organic alcohol is 1: 500. dispersing for 2h by ultrasonic waves with the frequency of 40KHZ and the power of 1500W, centrifugally washing by deionized water, and drying at 60 ℃ to obtain the product.
Normal and carbon doped MoSe2After the nanoparticles are treated with dimethyl sulfoxide with different concentrations for 48 hours, the survival rate of KH-2 cells is detected by using an MTT method. FIGS. 1 and 2 show normal MoSe at different concentrations2The survival rate of the nanoparticles to KH-2 cells is reduced to 64.4 percent when the concentration reaches 100 mu g/mL. And carbon-doped MoSe2The nano-particles have good inhibition effect on the proliferation of KH-2 cells, the cell survival rate under different concentrations almost reaches 100 percent, and the result shows that the carbon-doped MoSe2Nano particles are more common than ordinary MoSe2The nanoparticles have better biocompatibility. Fig. 3 and 4 show that the obtained product has porous surface topography, and the dimension reaches the nanometer level.
Table 1 shows the EDS carbon content detection result of the product, and the result shows that the product contains rich carbon elements.
TABLE 1 elemental distribution of molybdenum diselenide obtained by the preparation
Example 2: adding 0.5g of selenium powder, 0.765g of sodium molybdate, 8mL of hydrazine hydrate and 40mL of deionized water into a polytetrafluoroethylene inner container, and fully and uniformly stirring. Carrying out hydrothermal reaction for 12h at 210 ℃, naturally cooling, and repeatedly washing with deionized water until the solution is neutral. 100mL of a mixed solution of deionized water (50mL), ethanol (20mL) and isopropanol (30mL) is prepared, and the volume ratio of the organic alcohol to the deionized water is 1: 1. Adding the prepared molybdenum diselenide into a mixed organic solution, wherein the mass ratio of the molybdenum diselenide to the organic alcohol is 1: 200. dispersing for 3h by using ultrasonic waves with the frequency of 40KHZ and the power of 1500W, centrifugally washing by using deionized water, and drying at 60 ℃ to obtain the product. The obtained product has a 24-hour KH-2 cell survival rate of over 96%.
Example 3: adding 0.5g of selenium powder, 0.765g of sodium molybdate, 5mL of hydrazine hydrate and 40mL of deionized water into a polytetrafluoroethylene inner container, and fully and uniformly stirring. Carrying out hydrothermal reaction for 12h at 200 ℃, naturally cooling, and repeatedly washing with deionized water until the solution is neutral. 100mL of a mixed solution of deionized water (80mL), polyethylene glycol 400(10mL) and isopropanol (10mL) is prepared, and the volume ratio of the organic alcohol to the deionized water is 1: 4. Adding the prepared molybdenum diselenide into a mixed organic solution, wherein the mass ratio of the molybdenum diselenide to the organic alcohol is 1: 800. dispersing for 4h by using ultrasonic waves with the frequency of 40KHZ and the power of 500W, centrifugally washing by using deionized water, and drying at 60 ℃ to obtain the product. The obtained product has a KH-2 cell survival rate of over 98% in 24 hours.
Example 4: adding 0.5g of selenium powder, 0.765g of sodium molybdate, 5mL of hydrazine hydrate and 40mL of deionized water into a polytetrafluoroethylene inner container, and fully and uniformly stirring. Carrying out hydrothermal reaction for 12h at 220 ℃, naturally cooling, and repeatedly washing with deionized water until the solution is neutral. 100mL of a mixed solution of deionized water (80mL), polyethylene glycol 400(5mL) and ethanol (15mL) is prepared, and the volume ratio of the organic alcohol to the deionized water is 1: 4. Adding the prepared molybdenum diselenide into a mixed organic solution, wherein the mass ratio of the molybdenum diselenide to the organic alcohol is 1: 600. ultrasonic dispersion is carried out for 2h at the frequency of 20KHZ and the power of 1000W, and the product is obtained after centrifugal washing by deionized water and drying at the temperature of 60 ℃. The obtained product has a KH-2 cell survival rate of over 97% in 24 hours.
Example 5: adding 0.5g of selenium powder, 0.765g of sodium molybdate, 5mL of hydrazine hydrate and 50mL of deionized water into a polytetrafluoroethylene inner container, and fully and uniformly stirring. Carrying out hydrothermal reaction for 12h at 190 ℃, naturally cooling, and repeatedly washing with deionized water until the solution is neutral. 100mL of a mixed solution of deionized water (60mL), polyethylene glycol 400(5mL), ethanol (15mL) and isopropanol (20mL) is prepared, and the volume ratio of the organic alcohol to the deionized water is 1: 3. Adding the prepared molybdenum diselenide into a mixed organic solution, wherein the mass ratio of the molybdenum diselenide to the organic alcohol is 1: 1000. ultrasonic dispersion is carried out for 4 hours at the frequency of 30KHZ and the power of 1500W, and the product is obtained after centrifugal washing by deionized water and drying at the temperature of 60 ℃. The obtained product has a KH-2 cell survival rate of over 99% in 24 hours.
In summary, the invention adopts the ultrasonic technology to disperse the molybdenum diselenide nano particles, utilizes the ultrasonic cavitation phenomenon of ultrasonic waves to release huge energy, and cavitation bubbles generate local high-temperature and high-pressure environment at the moment of explosion. The organic mixture is subjected to chemical bond breakage, water phase combustion or thermal decomposition in the cavitation bubbles under the conditions, so that the surfaces of the molybdenum diselenide particles contain carbon elements with good biocompatibility. Molybdenum diselenide has lower cytotoxicity than graphene and its analogs. Selenium and molybdenum are essential trace elements for human body, and the toxicity of molybdenum diselenide is lower than that of other two-dimensional transition metal double-halide materials. As an inorganic material, the normal molybdenum diselenide has poor biocompatibility to human bodies, and the research on the influence of the carbon-doped molybdenum diselenide nano particles on the biocompatibility has important significance in reducing the toxicity of the carbon-doped molybdenum diselenide nano particles. The prepared carbon-coated molybdenum diselenide has excellent dispersibility in water and has a great application value in the fields of biological medicines and the like.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing low-toxicity molybdenum diselenide by ultrasonic waves is characterized in that molybdenum diselenide is added into mixed liquid of deionized water and organic alcohols, ultrasonic waves are dispersed, and the molybdenum diselenide is obtained by drying after being washed by the deionized water.
2. The ultrasonic method for preparing molybdenum diselenide with low toxicity according to claim 1, wherein the molybdenum diselenide is prepared by the following method: selenium powder, sodium molybdate, hydrazine hydrate and deionized water are mixed for hydrothermal reaction, and the mixture is naturally cooled and repeatedly washed by the deionized water until the mixture is neutral.
3. The ultrasonic method for preparing molybdenum diselenide with low toxicity according to claim 2, wherein the mass ratio of the selenium powder to the sodium molybdate is 1: 1-2.
4. The method for preparing the low-toxicity molybdenum diselenide by the ultrasonic waves as claimed in claim 2 or 3, wherein the selenium powder, the sodium molybdate, the hydrazine hydrate and the deionized water are fully and uniformly stirred in a polytetrafluoroethylene liner and then subjected to hydrothermal reaction.
5. The method for ultrasonically preparing molybdenum diselenide with low toxicity according to claim 2 or 3, wherein the hydrothermal reaction is carried out at the temperature of 180 ℃ and 220 ℃ for 12 h.
6. The ultrasonic method for preparing molybdenum diselenide with low toxicity according to claim 1, wherein the organic alcohol is any one or more of ethanol, polyethylene glycol and isopropanol.
7. The ultrasonic method for preparing molybdenum diselenide with low toxicity according to claim 1 or 6, wherein the volume ratio of the organic alcohol to the deionized water is 1: 1-5.
8. The ultrasonic method for preparing low-toxicity molybdenum diselenide according to claim 1 or 6, wherein the mass ratio of molybdenum selenide to organic alcohols is 1: 100-1000.
9. The method for ultrasonically preparing molybdenum diselenide with low toxicity as claimed in claim 1, wherein the ultrasonic frequency in the ultrasonic dispersion is 20-40KHZ, and the power is 200-.
10. The method for ultrasonically preparing molybdenum diselenide with low toxicity according to claim 1 or 9, wherein the time for ultrasonic dispersion is 2-4 h.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992281A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Nanometer flower-shaped MoSe2 and preparation method thereof |
| CN103692763A (en) * | 2013-12-06 | 2014-04-02 | 深圳先进技术研究院 | Peeling method of two-dimensional layered nano material |
| CN105524617A (en) * | 2015-12-21 | 2016-04-27 | 东南大学 | Preparation method of molybdenum selenide quantum dots |
| CN107226476A (en) * | 2016-09-28 | 2017-10-03 | 西安交通大学 | Two-dimensional thin-layer material coated on surface of microsphere and simple stripping method thereof |
| CN109449004A (en) * | 2018-09-26 | 2019-03-08 | 哈尔滨理工大学 | A kind of preparation method of two selenizings molybdenum nanometer sheet ball-graphene composite material |
| CN109970034A (en) * | 2019-04-29 | 2019-07-05 | 四川大学锦城学院 | A kind of ultrathin nanometer hollow sphere MoSe2The preparation method of material |
| US10414668B1 (en) * | 2017-11-27 | 2019-09-17 | United States Of America As Represented By The Secretary Of The Air Force | Exfoliating layered transition metal dichalcogenides |
-
2020
- 2020-06-29 CN CN202010610747.4A patent/CN111747384B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992281A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Nanometer flower-shaped MoSe2 and preparation method thereof |
| CN103692763A (en) * | 2013-12-06 | 2014-04-02 | 深圳先进技术研究院 | Peeling method of two-dimensional layered nano material |
| CN105524617A (en) * | 2015-12-21 | 2016-04-27 | 东南大学 | Preparation method of molybdenum selenide quantum dots |
| CN107226476A (en) * | 2016-09-28 | 2017-10-03 | 西安交通大学 | Two-dimensional thin-layer material coated on surface of microsphere and simple stripping method thereof |
| US10414668B1 (en) * | 2017-11-27 | 2019-09-17 | United States Of America As Represented By The Secretary Of The Air Force | Exfoliating layered transition metal dichalcogenides |
| CN109449004A (en) * | 2018-09-26 | 2019-03-08 | 哈尔滨理工大学 | A kind of preparation method of two selenizings molybdenum nanometer sheet ball-graphene composite material |
| CN109970034A (en) * | 2019-04-29 | 2019-07-05 | 四川大学锦城学院 | A kind of ultrathin nanometer hollow sphere MoSe2The preparation method of material |
Non-Patent Citations (1)
| Title |
|---|
| 亢淑梅等: "《超声波钢包精炼应用基础》", 31 October 2014 * |
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