CN103588178B - Technology for synthesizing sulfur quantum dots through oil-water interface method - Google Patents
Technology for synthesizing sulfur quantum dots through oil-water interface method Download PDFInfo
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Abstract
The invention discloses a technology for synthesizing sulfur quantum dots through an oil-water interface method. The technology comprises the following steps: 1, preparing metal sulfide quantum dots; 2, preparing a nitric acid solution; and 3, preparing sulfide quantum dots. In the invention, oleic acid is used as a solvent to prepare oil-soluble metal sulfide quantum dots, an n-hexane solution of a metal sulfide and an aqueous solution of nitric acid are mixed as an oil phase and a water phase respectively, nitric acid oxidizes sulfide ions into elemental sulfur in situ at the phase interface, and the metal sulfide quantum dots are adopted as a template to realize the uniform distribution of the particle sizes of the prepared sulfur quantum dots, so the oil-water interface alleviates the reaction speed and realizes the dispersion and small particle sizes of sulfur nano-particles. The technology allows the sulfur quantum dots to be synthesized by adopting the above technical scheme through the oil-water interface reaction with the n-hexane solution of the metal sulfide as the oil phase and the aqueous solution of nitric acid as the water phase, so the technology has the advantages of mild reaction conditions, simple operation, controllable particle size and easy popularization.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, especially a kind of method of water-oil interface method synthesis sulphur quantum dot.
Background technology
Quantum dot (Quantum dots) is made up of a limited number of atom, three dimension are all less than the accurate zero dimensional nanometer materials of 10nm, the motion of its internal electron in all directions is all limited to compared with other nano materials, so quantum confinement effect (quantum confinement effect) is remarkable especially.As a kind of novel semiconductor fluorescence nano material, surface effects, dielectric effect and quantum effect caused by the nanostructure that it is special and have many excellent properties, be able to application and development in fields such as analytical chemistry, luminescent device, biomarker, biological detection and biosensors in recent years.
Sulphur is the main component of traditional Chinese medicine sulphur, is usually used in the dermatosis such as treatment scabies, favus of the scalp, acne, seborrheic dermatitis, rosacea, pityriasis simplex and chronic eczema.Time prepared by the sulphur preparation used clinically at present, raw material sulphur powder used all belongs to micro-nano particle, particle diameter compared with large, size-grade distribution is wide, specific surface area is little, there is the shortcomings such as skin absorption difference, bioavailability is low, bacteriostatic activity is unstable, use is inconvenient, have impact on its curative effect and use to a certain extent.The nano-sulfur (1-100nm) that software engineering researchers invent particle diameter is little, specific surface area is large overcomes some shortcomings of micron sulphur, but sulphur quantum dot has less particle diameter (<10nm), uniform granularity, higher chemically reactive, effectively can solve Problems existing in micro-nano sulphur application process, and there is photoluminescent property, its preparation, characteristic and potential application receive the concern of chemistry and medical territory investigator.
The main method preparing nano-sulfur at present has microemulsion method and chemical Vapor deposition process.Patent name: high-purity nm sulphur preparing process (number of patent application: 03128015.3) disclose a kind of method that chemical vapor infiltration prepares elemental sulfur, this method exists complex operation, cost is high, and the problems such as size distribution is wide, difficult regulation and control; Patent name: (number of patent application: 201010220221.1) disclose a kind of method that microemulsion method prepares elemental sulfur, this method exists reaction system complexity, complex operation, nano-sulfur particle diameter is large, and the problem such as distribute wide for micro-emulsion method for preparing nano-sulfur particles.And the reason that there is this problem to be homogeneous reaction speed fast, nano-sulfur specific surface area is large, makes be easy to absorption between particle and reunite, thus forms large agglomerating particles.
Summary of the invention
It is raw material with metal sulfide quantum dots that the technical problem to be solved in the present invention is to provide a kind of, only needs the method for a kind of water-oil interface method synthesis sulphur quantum dot that can be obtained the fluorescence property that conventional nano sulphur does not have by simple water-oil interface reaction.
To achieve these goals, the present invention is by the following technical solutions:
A method for water-oil interface method synthesis sulphur quantum dot, comprises the following steps:
(1) preparation of metal sulfide quantum dots: add metal chloride in oleic acid, be made into the oleic acid metal chloride mixed solution that concentration is 0.1-0.5mol/L, after 90-170 DEG C of lower magnetic force stirs 25-35min, the oleic acid solutions being dissolved with elemental sulfur that concentration is 0.2-0.6mol/L is added in oleic acid metal chloride mixed solution, described oleic acid metal chloride mixed solution is 2:1 with the volume ratio of the oleic acid solutions being dissolved with elemental sulfur, 55-65min is stirred at 150-320 DEG C of lower magnetic force, obtain metal sulfide quantum dots crude product, in metal sulfide quantum dots crude product, add dehydrated alcohol makes metal sulfide quantum dots precipitate, centrifugation under rotating speed 8000-12000rpm, obtain precipitation absolute ethanol washing more than three times, at 45-55 DEG C, vacuum-drying is carried out to precipitation and namely obtain metal sulfide quantum dots, metal sulfide quantum dots is dissolved in normal hexane, the quality of described metal sulfide quantum dots and the volume ratio of normal hexane are 1:2-4, obtain metal sulfide quantum dots hexane solution,
(2) configuration of salpeter solution: by massfraction be 65% concentrated nitric acid be dissolved in ultrapure water, be namely made into the salpeter solution that concentration is 0.04-0.06mol/L after stirring;
(3) preparation of sulphur quantum dot: metal sulfide quantum dots hexane solution is joined in salpeter solution, in metal sulfide quantum dots hexane solution, the sulfonium ion of metal sulfide quantum dots and the mol ratio of nitric acid are 1:2.67-20, room temperature lower magnetic force stirs 36h and obtains emulsion, obtaining oil phase after carrying out separatory to emulsion is hexane solution containing sulphur quantum dot, rotary evaporation, namely obtains sulphur quantum dot.
Metal in metal chloride described in described step (1) is transition metal.
Described transition metal is Fe, Mn, Zn, Cu, Cd or Ag.
In metal sulfide quantum dots hexane solution described in described step (3), the sulfonium ion of metal sulfide quantum dots and the mol ratio of nitric acid are 1:2.67-10.
The ion-reaction equation of sulfonium ion and salpeter solution is:
3S
2-+8H
++2NO
3 -＝3S↓+2NO↑+4H
2O
The present invention is that oil-soluble metal sulfide quantum dots prepared by solvent with oleic acid, and with the hexane solution of metallic sulfide for oil phase, aqueous nitric acid is aqueous phase, after two-phase mixtures, original position sulfonium ion can be oxidized to elemental sulfur at phase interface place nitric acid, be template with metal sulfide quantum dots, makes the sulphur quantum dot even particle size distribution of preparation, water-oil interface slow down the speed of reaction, make sulphur nanoparticulate dispersed, particle diameter little.
The present invention adopts above technical scheme, is reacted by water-oil interface, with the hexane solution of metallic sulfide for oil phase, take salpeter solution as aqueous phase, and synthesis sulphur quantum dot, whole reaction conditions is gentle, simple to operate, size tunable, is easy to promote.
Accompanying drawing explanation
Illustrate that the present invention is further detailed explanation with embodiment below in conjunction with accompanying drawing:
Fig. 1 is the fluorescence spectrum figure of the ZnS quantum dots prepared in the method for a kind of water-oil interface method synthesis of the present invention sulphur quantum dot;
Fig. 2 is the fluorescence spectrum figure of the sulphur quantum dot that the method for a kind of water-oil interface method synthesis of the present invention sulphur quantum dot is prepared by ZnS quantum dots;
Fig. 3 is the fluorescence spectrum figure of the sulphur quantum dot that the method for a kind of water-oil interface method synthesis of the present invention sulphur quantum dot is prepared by manganese sulfide quantum dot;
Fig. 4 is the fluorescence spectrum figure of the sulphur quantum dot that the method for a kind of water-oil interface method synthesis of the present invention sulphur quantum dot is prepared by cadmiumsulfide quantum dot;
Fig. 5 is the high power transmission electron microscope picture of the method cadmiumsulfide quantum dot of a kind of water-oil interface method synthesis of the present invention sulphur quantum dot;
Fig. 6 is the high power transmission electron microscope picture of the sulphur quantum dot that the method for a kind of water-oil interface method synthesis of the present invention sulphur quantum dot is prepared by cadmiumsulfide quantum dot;
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation:
A method for water-oil interface method synthesis sulphur quantum dot, comprises the following steps:
(1) preparation of metal sulfide quantum dots: add metal chloride in oleic acid, be made into the oleic acid metal chloride mixed solution that concentration is 0.1-0.5mol/L, after 90-170 DEG C of lower magnetic force stirs 25-35min, the oleic acid solutions being dissolved with elemental sulfur that concentration is 0.2-0.6mol/L is added in oleic acid metal chloride mixed solution, described oleic acid metal chloride mixed solution is 2:1 with the volume ratio of the oleic acid solutions being dissolved with elemental sulfur, 55-65min is stirred at 150-320 DEG C of lower magnetic force, obtain metal sulfide quantum dots crude product, in metal sulfide quantum dots crude product, add dehydrated alcohol makes metal sulfide quantum dots precipitate, centrifugation under rotating speed 8000-12000rpm, obtain precipitation absolute ethanol washing more than three times, at 45-55 DEG C, vacuum-drying is carried out to precipitation and namely obtain metal sulfide quantum dots, metal sulfide quantum dots is dissolved in normal hexane, the quality of described metal sulfide quantum dots and the volume ratio of normal hexane are 1:2-4, obtain metal sulfide quantum dots hexane solution,
(2) configuration of salpeter solution: by massfraction be 65% concentrated nitric acid be dissolved in ultrapure water, be namely made into the salpeter solution that concentration is 0.04-0.06mol/L after stirring;
(3) preparation of sulphur quantum dot: metal sulfide quantum dots hexane solution is joined in salpeter solution, in metal sulfide quantum dots hexane solution, the sulfonium ion of metal sulfide quantum dots and the mol ratio of nitric acid are 1:2.67-20, room temperature lower magnetic force stirs 36h and obtains emulsion, obtaining oil phase after carrying out separatory to emulsion is hexane solution containing sulphur quantum dot, rotary evaporation, namely obtains sulphur quantum dot.In metal sulfide quantum dots hexane solution, in sulfonium ion and salpeter solution, the mol ratio of nitrate radical is 1:2.67-20, can ensure that sulfonium ion is all converted into sulphur simple substance.
Metal in metal chloride described in described step (1) is transition metal.
Described transition metal is Fe, Mn, Zn, Cu, Cd or Ag.
In metal sulfide quantum dots hexane solution described in described step (3), the sulfonium ion of metal sulfide quantum dots and the mol ratio of nitric acid are 1:2.67-10.
Embodiment 1
2mmol zinc chloride is joined in 10mL oleic acid, be made into the oleic acid metal chloride mixed solution that concentration is 0.2mol/L, after 170 DEG C of lower magnetic forces stir 30min, the oleic acid solutions being dissolved with elemental sulfur that 5mL concentration is 0.6mol/L is added in oleic acid metal chloride mixed solution, 60min is stirred at 320 DEG C of lower magnetic forces, obtain metal sulfide quantum dots crude product, in metal sulfide quantum dots crude product, add dehydrated alcohol makes metal sulfide quantum dots precipitate, centrifugation under rotating speed 10000rpm, obtain precipitation absolute ethanol washing more than three times, at 50 DEG C, carry out vacuum-drying to precipitation obtain white solid and be ZnS quantum dots, 4.85mg ZnS quantum dots is dissolved in 9.7mL normal hexane, obtain ZnS quantum dots hexane solution, as the oil phase of surface reaction, another compound concentration is the salpeter solution of 0.05mol/L, as the aqueous phase of surface reaction, get 20mL salpeter solution and the mixing of ZnS quantum dots hexane solution, room temperature lower magnetic force stirs 36h and obtains emulsion, obtaining oil phase after carrying out separatory to emulsion is hexane solution containing sulphur quantum dot, rotary evaporation, namely obtains sulphur quantum dot.
As can be seen from Figure 1 ZnS quantum dots has the emission peak of three, and excitation wavelength is 214nm, and maximum emission wavelength is at 491nm.Fig. 2 is the fluorescence spectrum figure of the sulphur quantum dot prepared by ZnS quantum dots, as can be seen from the figure excitation wavelength is at 226nm, emission wavelength is 340nm, these are obviously different from the peak position of ZnS quantum dots, illustrate that ZnS quantum dots and nitric acid reaction generate the sulphur quantum dot with fluorescent characteristic.
Embodiment 2
5mmol Manganous chloride tetrahydrate is joined in 10mL oleic acid, be made into the oleic acid metal chloride mixed solution that concentration is 0.5mol/L, after 120 DEG C of lower magnetic forces stir 25min, the oleic acid solutions being dissolved with elemental sulfur that 5mL concentration is 0.2mol/L is added in oleic acid metal chloride mixed solution, 55min is stirred at 280 DEG C of lower magnetic forces, obtain metal sulfide quantum dots crude product, in metal sulfide quantum dots crude product, add dehydrated alcohol makes metal sulfide quantum dots precipitate, centrifugation under rotating speed 8000rpm, obtain precipitation absolute ethanol washing more than three times, at 45 DEG C, carry out vacuum-drying to precipitation obtain black solid and be manganese sulfide quantum dot, 26.1mg manganese sulfide quantum dot is dissolved in 78.3mL normal hexane, obtain manganese sulfide quantum dot hexane solution, as the oil phase of surface reaction, another compound concentration is the salpeter solution of 0.04mol/L, as the aqueous phase of surface reaction, get 20mL salpeter solution and the mixing of manganese sulfide quantum dot hexane solution, room temperature lower magnetic force stirs 36h and obtains emulsion, obtaining oil phase after carrying out separatory to emulsion is hexane solution containing sulphur quantum dot, rotary evaporation, namely obtains sulphur quantum dot.As can be seen from Figure 1 the excitation wavelength of sulphur quantum dot is at 226nm, and emission wavelength is 340nm.
As can be seen from Figure 3 the excitation wavelength of sulphur quantum dot is at 340nm, and emission wavelength is 428nm, illustrates that the sulphur quantum dot prepared by manganese sulfide quantum dot has fluorescent characteristic.
Embodiment 3
1mmol Cadmium chloride fine powder is joined in 10mL oleic acid, be made into the oleic acid metal chloride mixed solution that concentration is 0.1mol/L, after 90 DEG C of lower magnetic forces stir 35min, the oleic acid solutions being dissolved with elemental sulfur that 5mL concentration is 0.4mol/L is added in oleic acid metal chloride mixed solution, 65min is stirred at 150 DEG C of lower magnetic forces, obtain metal sulfide quantum dots crude product, in metal sulfide quantum dots crude product, add dehydrated alcohol makes metal sulfide quantum dots precipitate, centrifugation under rotating speed 12000rpm, obtain precipitation absolute ethanol washing more than three times, at 55 DEG C, carry out vacuum-drying to precipitation obtain yellow solid and be cadmiumsulfide quantum dot, 8.64mg ZnS quantum dots is dissolved in 34.6mL normal hexane, obtain cadmiumsulfide quantum dot hexane solution, as the oil phase of surface reaction, another compound concentration is the salpeter solution of 0.06mol/L, as the aqueous phase of surface reaction, get 20mL salpeter solution and the mixing of cadmiumsulfide quantum dot hexane solution, room temperature lower magnetic force stirs 36h and obtains emulsion, obtaining oil phase after carrying out separatory to emulsion is hexane solution containing sulphur quantum dot, rotary evaporation, namely obtains sulphur quantum dot.
As can be seen from Figure 4 the excitation wavelength of sulphur quantum dot is at 354nm, and emission wavelength is 431nm, illustrates that sulphur quantum dot prepared by manganese sulfide quantum dot has fluorescent characteristic.Fig. 5 is the high power transmission electron microscope picture of cadmiumsulfide quantum dot, and the median size that can be estimated cadmiumsulfide quantum dot by figure is 2.9nm.Fig. 6 is the high power transmission electron microscope picture that Cadmium Sulfide sulphur quantum dot prepares sulphur quantum dot, and the median size that can be estimated sulphur quantum dot prepared by cadmiumsulfide quantum dot by figure is 1.6nm.
Claims (4)
1. a method for water-oil interface method synthesis sulphur quantum dot, is characterized in that: comprise the following steps:
(1) preparation of metal sulfide quantum dots: add metal chloride in oleic acid, be made into the oleic acid metal chloride mixed solution that concentration is 0.1-0.5mol/L, after 90-170 DEG C of lower magnetic force stirs 25-35min, the oleic acid solutions being dissolved with elemental sulfur that concentration is 0.2-0.6 mol/L is added in oleic acid metal chloride mixed solution, described oleic acid metal chloride mixed solution is 2:1 with the volume ratio of the oleic acid solutions being dissolved with elemental sulfur, 55-65 min is stirred at 150-320 DEG C of lower magnetic force, obtain metal sulfide quantum dots crude product, in metal sulfide quantum dots crude product, add dehydrated alcohol makes metal sulfide quantum dots precipitate, centrifugation under rotating speed 8000-12000rpm, obtain precipitation absolute ethanol washing more than three times, at 45-55 DEG C, vacuum-drying is carried out to precipitation and namely obtain metal sulfide quantum dots, metal sulfide quantum dots is dissolved in normal hexane, the quality of described metal sulfide quantum dots and the volume ratio of normal hexane are 1mg:2-4mL, obtain metal sulfide quantum dots hexane solution,
(2) configuration of salpeter solution: by massfraction be 65% concentrated nitric acid be dissolved in ultrapure water, be namely made into the salpeter solution that concentration is 0.04-0.06 mol/L after stirring;
(3) preparation of sulphur quantum dot: metal sulfide quantum dots hexane solution is joined in salpeter solution, in metal sulfide quantum dots hexane solution, the sulfonium ion of metal sulfide quantum dots and the mol ratio of nitric acid are 1:2.67-20, room temperature lower magnetic force stirs 36h and obtains emulsion, obtaining oil phase after carrying out separatory to emulsion is hexane solution containing sulphur quantum dot, rotary evaporation, namely obtains sulphur quantum dot.
2. the method for water-oil interface method synthesis sulphur quantum dot according to claim 1, is characterized in that: the metal in the metal chloride described in described step (1) is transition metal.
3. the method for water-oil interface method synthesis sulphur quantum dot according to claim 2, is characterized in that: described transition metal is Fe, Mn, Zn, Cu, Cd or Ag.
4. the method for water-oil interface method synthesis sulphur quantum dot according to claim 1, is characterized in that: in the metal sulfide quantum dots hexane solution described in described step (3), the sulfonium ion of metal sulfide quantum dots and the mol ratio of nitric acid are 1:2.67-10.
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| CN110079299B (en) * | 2019-05-08 | 2022-01-04 | 桂林理工大学 | Preparation method of sulfur quantum dot coated bovine serum albumin fluorescent composite nanospheres |
| CN110171806B (en) * | 2019-05-08 | 2022-04-22 | 桂林理工大学 | Preparation method of water-soluble red light sulfur quantum dots |
| CN110129040B (en) * | 2019-05-08 | 2022-02-08 | 桂林理工大学 | Preparation method of water-soluble fluorescent sulfur quantum dots |
| CN110387224B (en) * | 2019-07-23 | 2023-01-24 | 江苏海洋大学 | Method for improving fluorescence property of sulfur quantum dots and application |
| CN111721748A (en) * | 2020-06-30 | 2020-09-29 | 重庆师范大学 | Fluorescent probe for detecting zoledronic acid, preparation method of fluorescent probe, fluorescent sensor, construction method of fluorescent sensor and application of fluorescent sensor |
| CN113025314B (en) * | 2021-03-18 | 2022-11-08 | 中国科学院合肥物质科学研究院 | Simple method for rapidly preparing sulfur quantum dots |
| CN114768830B (en) * | 2022-04-01 | 2023-12-29 | 泰戈特（北京）工程技术有限公司 | Oil-soluble metal sulfide catalyst and preparation method and application thereof |
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