CN110129040A - A kind of preparation method of water soluble fluorescence sulphur quantum dot - Google Patents
A kind of preparation method of water soluble fluorescence sulphur quantum dot Download PDFInfo
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- CN110129040A CN110129040A CN201910381471.4A CN201910381471A CN110129040A CN 110129040 A CN110129040 A CN 110129040A CN 201910381471 A CN201910381471 A CN 201910381471A CN 110129040 A CN110129040 A CN 110129040A
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Abstract
The invention discloses a kind of preparation methods of water soluble fluorescence sulphur quantum dot.The sodium hydroxide of 1 parts by weight is added to stirring in the deionized water of 10 ~ 30 parts by weight, and, to dissolving, the subsequent continuous stirring of the distillation sulphur powder of polyalcohol and 0.2 ~ 1 parts by weight that 0.5 ~ 1.5 parts by weight are then added 10 minutes obtains mixed liquor；Obtained mixed liquor is poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen, stirs mixed liquor 2 ~ 5 hours under oxygen atmosphere in 50 ~ 99 DEG C, obtains water soluble fluorescence sulphur quantum dot.Water soluble fluorescence sulfur content prepared by the present invention has excellent water solubility and high fluorescence intensity, and its preparation process is simple and quick, and preparation cost is low.The water soluble fluorescence sulphur quantum dot bio-imaging, biological detection, in terms of have a good application prospect.
Description
Technical field
The invention belongs to technical field of nano material, in particular to a kind of preparation method of water soluble fluorescence sulphur quantum dot.
Background technique
Fluorescence quantum is since its unique optical property and small size are in various fields such as bio-imaging, biology inspection
Survey, photoelectric device etc. have shown application potential.Compared with traditional fluorescence semiconductor quantum dots containing metallic element, without gold
The fluorescence quantum Biocompatibility for belonging to element is good, is more suitable for applying in bio-imaging and field of biological detection.Although mesh
It is preceding that there are many fluorescence quantums such as carbon quantum dot, silicon quantum dot, nitrogen carbide quantum dot etc. without metallic element to be synthesized out
Come, but the report in relation to fluorescence sulphur quantum dot is rarely found.Meanwhile it also there are no using oxygen and accelerating to prepare fluorescence sulfur content
The report of point work.
Tellurian simple substance Sulphur ressource is very rich, but there is a problem of that utilization rate is low and wastes serious.Therefore, it explores high
The method of effect has far-reaching theory significance and application value to utilize simple substance Sulphur ressource to prepare water soluble fluorescence sulphur quantum dot.One
Aspect can promote the research and application of fluorescence sulphur quanta point material；On the other hand, the exploitation benefit of simple substance Sulphur ressource can be promoted
With raising added value.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of water soluble fluorescence sulphur quantum dot, the key of the preparation method exists
It is reacted under oxygen atmosphere, oxygen can not only generate water-soluble fluorescence sulfur content with polysulfide fast reaction
Point, and the fluorescence property and yield of fluorescence sulphur quantum dot can be greatly improved.
Specific steps are as follows:
(1) sodium hydroxide of 1 parts by weight is added to stirring in the deionized water of 10 ~ 30 parts by weight and is then added 0.5 to dissolving
The subsequent continuous stirring of the distillation sulphur powder of the polyalcohol of ~ 1.5 parts by weight and 0.2 ~ 1 parts by weight 10 minutes, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 2 ~ 5 hours under oxygen atmosphere in 50 ~ 99 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
The polyalcohol is one of diethylene glycol (DEG), glycerine, ethylene glycol, 1,2- butanediol and trimethylolpropane.
The present invention has many advantages, such as that raw material is easy to get, preparation process is simple and quick, preparation cost is low, is suitable for a large amount of preparations；And
Water soluble fluorescence sulphur quantum dot obtained has excellent water solubility, and aqueous solution can be sent out under 365 nanometers of ultraviolet light irradiations
Strong fluorescence out；Its optical property further is tested with ultraviolet-visible spectrophotometer and Fluorescence Spectrometer, is as a result demonstrate,proved
It is real its with excellent water solubility and high fluorescence intensity；Its size is tested with transmission electron microscope, as a result table
Its bright particle diameter distribution is relatively narrow, and size is 2-5 nanometers；In addition, the water soluble fluorescence sulphur quantum dot is in bio-imaging, biology
Detection, photoelectric device etc. have good application prospect.
Detailed description of the invention
Fig. 1 is the water soluble fluorescence sulphur quantum dot aqueous solution of the preparation of the embodiment of the present invention 1 in daylight and 365 nanometers of ultraviolet lamps
Under photo.
Fig. 2 is the uv-visible absorption spectroscopy of water soluble fluorescence sulphur quantum dot aqueous solution prepared by the embodiment of the present invention 1
Figure.
Fig. 3 is the fluorescence spectra (excitation wavelength of water soluble fluorescence sulphur quantum dot aqueous solution prepared by the embodiment of the present invention 1
It is 340 nanometers).
Fig. 4 is the transmission electron microscope photo of water soluble fluorescence sulphur quantum dot prepared by the embodiment of the present invention 1.
Specific embodiment
Embodiment 1:
(1) 4 grams of sodium hydroxides are added to stirring in 50 grams of deionized waters and 3.3 grams of diethylene glycol (DEG)s and 1.4 grams is then added to dissolving
The subsequent continuous stirring of the sulphur powder that distils 10 minutes, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 5 hours under oxygen atmosphere in 75 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Embodiment 2:
(1) 3 grams of sodium hydroxides are added to stirring in 60 grams of deionized waters and 4.5 grams of diethylene glycol (DEG)s and 1.8 grams is then added to dissolving
The subsequent continuous stirring of the sulphur powder that distils 10 minutes, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 2 hours under oxygen atmosphere in 99 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Embodiment 3:
(1) 2 grams of sodium hydroxides are added to stirring in 25 grams of deionized waters and 1.9 grams of glycerine and 0.7 gram is then added to dissolving
The subsequent continuous stirring of the sulphur powder that distils 10 minutes, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 3.5 hours under oxygen atmosphere in 90 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Embodiment 4:
(1) 1 gram of sodium hydroxide is added to stirring in 30 grams of deionized waters and 1.3 grams of ethylene glycol and 1 gram liter is then added to dissolving
Continue stirring 10 minutes after magnificent sulphur powder, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 5 hours under oxygen atmosphere in 50 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Embodiment 5:
(1) 6 grams of sodium hydroxides are added in 120 grams of deionized waters stirring to dissolving, be then added 3 grams of 1,2- butanediols and
Continue stirring 10 minutes after 1.2 gram liter China sulphur powders, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 4 hours under oxygen atmosphere in 60 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Embodiment 6:
(1) 5 grams of sodium hydroxides are added to stirring in 50 grams of deionized waters and 4 grams of trimethylolpropanes and 2 is then added to dissolving
Continue stirring 10 minutes after gram liter China sulphur powder, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 3 hours under oxygen atmosphere in 80 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Embodiment 7:
(1) 0.5 gram of sodium hydroxide is added to stirring in 10 grams of deionized waters and 0.4 gram of trihydroxy methyl third is then added to dissolving
Continue stirring 10 minutes after alkane and 0.2 gram liter China sulphur powder, obtains mixed liquor.
(2) mixed liquor that step (1) obtains being poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen,
It stirs mixed liquor 4.5 hours under oxygen atmosphere in 55 DEG C, obtains water-soluble fluorescence sulphur quantum dot.
Claims (1)
1. a kind of preparation method of water soluble fluorescence sulphur quantum dot, it is characterised in that specific steps are as follows:
(1) sodium hydroxide of 1 parts by weight is added to stirring in the deionized water of 10 ~ 30 parts by weight and is then added 0.5 to dissolving
The subsequent continuous stirring of the distillation sulphur powder of the polyalcohol of ~ 1.5 parts by weight and 0.2 ~ 1 parts by weight 10 minutes, obtains mixed liquor；
(2) mixed liquor that step (1) obtains is poured into reaction flask, the air in elimination reaction bottle is simultaneously passed through oxygen, makes to mix
It closes liquid to stir 2 ~ 5 hours under oxygen atmosphere in 50 ~ 99 DEG C, obtains water-soluble fluorescence sulphur quantum dot；
The polyalcohol is one of diethylene glycol (DEG), glycerine, ethylene glycol, 1,2- butanediol and trimethylolpropane.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734763A (en) * | 2019-11-08 | 2020-01-31 | 中国石油大学(北京) | sulfur quantum dots, and preparation method and application thereof |
| CN111218272A (en) * | 2020-02-06 | 2020-06-02 | 桂林理工大学 | Preparation method of fluorescent sulfur quantum dots based on sulfur-amine solution |
| CN112852412A (en) * | 2021-01-19 | 2021-05-28 | 中南大学 | Method for rapidly synthesizing high-fluorescence sulfur quantum dots |
| CN113310960A (en) * | 2021-05-26 | 2021-08-27 | 四川中科微纳科技有限公司 | Sulfur quantum dot synthesis method and sulfur quantum dot-based Fe determination method+2And H2O2Method (2) |
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| CN103588178A (en) * | 2013-11-27 | 2014-02-19 | 闽南师范大学 | Technology for synthesizing sulfur quantum dots through oil-water interface method |
| CN106252642A (en) * | 2016-09-22 | 2016-12-21 | 清华大学深圳研究生院 | The preparation method and applications of sulfur nanoparticulate dispersion |
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| CN103588178A (en) * | 2013-11-27 | 2014-02-19 | 闽南师范大学 | Technology for synthesizing sulfur quantum dots through oil-water interface method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110734763A (en) * | 2019-11-08 | 2020-01-31 | 中国石油大学(北京) | sulfur quantum dots, and preparation method and application thereof |
| CN111218272A (en) * | 2020-02-06 | 2020-06-02 | 桂林理工大学 | Preparation method of fluorescent sulfur quantum dots based on sulfur-amine solution |
| CN111218272B (en) * | 2020-02-06 | 2022-02-11 | 桂林理工大学 | Preparation method of fluorescent sulfur quantum dots based on sulfur-amine solution |
| CN112852412A (en) * | 2021-01-19 | 2021-05-28 | 中南大学 | Method for rapidly synthesizing high-fluorescence sulfur quantum dots |
| CN112852412B (en) * | 2021-01-19 | 2022-03-29 | 中南大学 | Method for rapidly synthesizing high-fluorescence sulfur quantum dots |
| CN113310960A (en) * | 2021-05-26 | 2021-08-27 | 四川中科微纳科技有限公司 | Sulfur quantum dot synthesis method and sulfur quantum dot-based Fe determination method+2And H2O2Method (2) |
| CN113310960B (en) * | 2021-05-26 | 2022-06-28 | 四川中科微纳科技有限公司 | Sulfur quantum dot synthesis method and sulfur quantum dot-based Fe determination method2+And H2O2Method (2) |
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Application publication date: 20190816 Assignee: Changsha Houcheng Nanomaterial Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000493 Denomination of invention: A Preparation Method of Water Soluble Fluorescent Sulfur Quantum Dots Granted publication date: 20220208 License type: Common License Record date: 20221229 |
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