CN106318383A - Preparation method of sulfur-doped carbon quantum dots - Google Patents
Preparation method of sulfur-doped carbon quantum dots Download PDFInfo
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- CN106318383A CN106318383A CN201610685133.6A CN201610685133A CN106318383A CN 106318383 A CN106318383 A CN 106318383A CN 201610685133 A CN201610685133 A CN 201610685133A CN 106318383 A CN106318383 A CN 106318383A
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- methyl
- brucite
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- mercaptopropionic acid
- hydrotalcite
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a preparation method of sulfur-doped carbon quantum dots. The preparation method sequentially comprises the following steps that 20-50 mesh of hydrotalcite is added to a 2-methyl-2-mercapto sodium propionate solution with the mass percentage concentration of 0.1%-1% based on the dosage that each gram of hydrotalcite corresponds to 1-1.5 mmol 2-methyl-2-mercaptopropionic acid, stirring is performed in a constant temperature water bath of 60-70 DEG C for 5-6 hours, ageing is performed for 12-24 hours, then solid-liquid separation is performed, a precipitate is washed with deionized water for 2-3 times, and drying is performed to obtain 2-methyl-2-mercapto sodium propionate modified hydrotalcite; the obtained 2-methyl-2-mercapto sodium propionate modified hydrotalcite is put in a vacuum tubular furnace, heating is performed under the vacuum condition to reach 400-600 DEG C, vacuum calcination is performed for 2-4 hours, and then cooling is performed to reach room temperature; the calcined powder is added to a hydrochloric acid solution with the mass percentage concentration of 20%-40%, each gram of powder corresponds to 10-15 ml hydrochloric acid solution, stirring is performed for 3-4 hours under nitrogen protection, and the sulfur-doped carbon quantum dots are obtained after a hydrotalcite layer is completely dissolved and high-speed centrifugation is performed. The materials adopted by the method are simple, and the conditions are mild.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to the preparation method of a kind of sulfur doping carbon quantum dot.
Background technology
Quantum dot is at the nanometer semiconductor structure that exciton is held onto on three direction in spaces.This constraint can be returned
Tie in electrostatic potential (by outside electrode, doping, strain, impurity produces), the interface of two kinds of different semi-conducting materials (such as:
In group quantum dot), the surface (such as: semiconductor nanocrystal) of quasiconductor, or the combination of above three.Quantum dot has
The quantized power spectrum separated.Corresponding wave function is spatially positioned in quantum dot, but extends in several lattice period.
It is unit that one quantum dot has a small amount of electronics of (1-100) integer, electric hole or electronics electricity hole pair, i.e. its electricity carried
The integral multiple of electric charge.
Carbon quantum dot is similar with various metal quantum points, and carbon quantum dot can emit a brilliant light in the case of illumination.
Before it has application in the widest field including improvement biosensor, medical imaging devices and small light emitting diode
Scape.Because carbon nano-particles has the biggest surface area, so scientists thinks this nanoparticle phase for a long time always
Than macroscopical carbon, there is the most peculiar chemical and physical features.
Quantum dot usually extracts from the mixture of lead, cadmium and silicon, but these quantum dots are the most poisonous, to ring
Also there is the biggest harm in border.So scientists seeks to extract quantum dot in the compound that some are optimum.Opposing metallic quantum
For Dian, carbon quantum dot nonhazardous effect, the harm to environment is the least, and preparation cost is cheap.Its research represents luminescence and receives
Rice corpuscles research enters a new stage.
Layered di-hydroxyl composite metal oxidate (Layered Double Hydroxides is called for short LDH), also known as neatly
Stone, is the important inorganic functional material of a class.The layer structure of its uniqueness and laminate element and the adjustable degeneration of interlayer anion
Get more and more people's extensive concerning, introduce new object anion through ion exchange to interlayer and layer structure and composition can be made to produce phase
The change answered, thus a big class can be prepared there is the functional material of special nature.Hydrotalcite material belongs to anion type laminated
Compound.Lamellar compound refers to have layer structure, interlayer ion has a compounds of interchangeability, utilizes laminarization
Intercalation that compound main body is had under highly polar molecular action and the interchangeability of interlayer ion, by some functional visitors
Body material introduces bedding void and laminate distance is strutted thus form layer-pillared compound.
Brucite chemical structure of general formula is: [M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O], wherein M2+For Mg2+、Ni2+、
Mn2+、Zn2+、Ca2+、Fe2+、Cu2+Deng divalent metal；M3+For Al3+、Cr3+、Fe3+、Co3+Deng trivalent metal cation；
An-For anion, such as CO3 2-、NO3 -、Cl-、OH-、SO4 2-、PO4 3-、C6H4(COO)2 2-Etc. inorganic and organic ion and complexation from
Son, when interlevel inorganic anion is different, and the interlamellar spacing of brucite is different.
Summary of the invention
It is an object of the invention to as overcoming complicated process of preparation in prior art, expensive etc. deficiency, it is provided that a kind of
The preparation method of sulfur doping carbon quantum dot.
To this end, the invention provides techniques below scheme, the preparation method of a kind of sulfur doping carbon quantum dot, include successively as
Lower step:
1) according to the amount of the corresponding 1～1.5mmol 2-methyl-2 mercaptopropionic acid sodium of every gram of brucite, by 20-50 mesh sieve
Brucite join in 2-methyl-2 mercaptopropionic acid sodium solution that mass percent concentration is 0.1%～1%, 60～70
DEG C water bath with thermostatic control stirs 5～6h, aging 12～24h, then solid-liquid separation, it is washed with deionized water precipitate 2～3 times, dries,
To the brucite that 2-methyl-2 mercaptopropionic acid sodium is modified；
2) brucite that the 2-obtained methyl-2 mercaptopropionic acid sodium is modified is put in vacuum tube furnace, at vacuum condition
Under be heated to 400～600 DEG C, vacuum calcining 2～4h, be then cooled to room temperature；
3) powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 20%～40%, every gram of powder
Corresponding 10～15 milliliters of hydrochloric acid solutions, stirring 3～4h, treats that brucite lamella all dissolves, after high speed centrifugation under nitrogen protection
Obtain sulfur doping carbon quantum dot.
Compared with prior art, the present invention has a following useful technique effect:
1. preparing this quanta point material source simple, utilizing acylate 2-methyl-2 mercaptopropionic acid sodium is raw material, this thing
Matter compound with regular structure, it is possible to obtain the preferable carbon quantum dot of pattern.
2. utilize the special construction of brucite, by anion exchange effect, 2-methyl-2 mercaptopropionic acid root is exchanged to
Hydrotalcite layers, and it is fixed on interlayer.Guarantee that interlayer Organic substance is being with electric charge point position monomolecular dispersion, at 400～600 DEG C of carbon
Granulated carbon structure is formed after change.
3. the material after carbonization is after overpickling, brucite itself destructurized, and metal-oxide is molten by acid
Solving, the charcoal quantum dot of interlayer presents naturally, and process is simple, gentle.
Detailed description of the invention
Describe the present invention in detail below in conjunction with embodiment, but the present invention is not limited to this.
Embodiment 1
According to the amount of every gram of commercially available magnesium aluminum-hydrotalcite correspondence 1.5mmol 2-methyl-2 mercaptopropionic acid sodium, by 50 mesh sieves
Brucite join in 2-methyl-2 mercaptopropionic acid sodium solution that mass percent concentration is 1%, in 70 DEG C of waters bath with thermostatic control
Stirring 6h, aging 24h, then solid-liquid separation, it is washed with deionized water precipitate 3 times, dries, obtain 2-methyl-2 mercaptopropionic acid sodium
Modified brucite；The brucite that the 2-obtained methyl-2 mercaptopropionic acid sodium is modified is put in vacuum tube furnace, at vacuum bar
600 DEG C it are heated under part, vacuum calcining 4h, it is then cooled to room temperature；Powder after calcining is joined mass percent concentration
It is in the hydrochloric acid solution of 40%, every gram of corresponding 15 milliliters of hydrochloric acid solutions of powder, stir 4h under nitrogen protection, treat brucite lamella
All dissolve, after high speed centrifugation, obtain sulfur doping carbon quantum dot.
Embodiment 2
According to the amount of every gram of commercially available zinc-aluminum hydrotalcite correspondence 1mmol 2-methyl-2 mercaptopropionic acid sodium, 20 mesh sieves will be crossed
Brucite joins in 2-methyl-2 mercaptopropionic acid sodium solution that mass percent concentration is 0.1%, in 60 DEG C of waters bath with thermostatic control
Stirring 5h, aging 12h, then solid-liquid separation, it is washed with deionized water precipitate 2 times, dries, obtain 2-methyl-2 mercaptopropionic acid sodium
Modified brucite；The brucite that the 2-obtained methyl-2 mercaptopropionic acid sodium is modified is put in vacuum tube furnace, at vacuum bar
400 DEG C it are heated under part, vacuum calcining 2h, it is then cooled to room temperature；Powder after calcining is joined mass percent concentration
It is in the hydrochloric acid solution of 20%, every gram of corresponding 10 milliliters of hydrochloric acid solutions of powder, stir 3h under nitrogen protection, treat brucite lamella
All dissolve, after high speed centrifugation, obtain sulfur doping carbon quantum dot.
Embodiment 3
It is first according to document (Hydrotalcite by Hydrothermal Method synthesizes, applied chemistry, 2001,18,70-72) synthesis and prepares magnalium
Type brucite；Brucite is crossed 40 mesh sieves, standby.
According to the amount of every gram of brucite correspondence 1mmol 2-methyl-2 mercaptopropionic acid sodium, the brucite crossing 50 mesh sieves is added
Enter in 2-methyl-2 mercaptopropionic acid sodium solution that mass percent concentration is 0.5%, 70 DEG C of waters bath with thermostatic control stirred 6h,
Aging 24h, then solid-liquid separation, be washed with deionized water precipitate 3 times, dries, and obtains the water that 2-methyl-2 mercaptopropionic acid sodium is modified
Talcum；The brucite that the 2-obtained methyl-2 mercaptopropionic acid sodium is modified is put in vacuum tube furnace, heats under vacuum
To 500 DEG C, vacuum calcining 4h, it is then cooled to room temperature；Powder after calcining is joined mass percent concentration is 40%
In hydrochloric acid solution, every gram of corresponding 15 milliliters of hydrochloric acid solutions of powder, stir 4h under nitrogen protection, treat that brucite lamella is the most molten
Solve, after high speed centrifugation, obtain sulfur doping carbon quantum dot.
Claims (1)
1. the preparation method of a sulfur doping carbon quantum dot, it is characterised in that: in turn include the following steps:
1) according to the amount of the corresponding 1～1.5mmol 2-methyl-2 mercaptopropionic acid sodium of every gram of brucite, the water of 20-50 mesh sieve will be crossed
Talcum joins in 2-methyl-2 mercaptopropionic acid sodium solution that mass percent concentration is 0.1%～1%, 60～70 DEG C of perseverances
Tepidarium stirs 5～6h, aging 12～24h, then solid-liquid separation, it is washed with deionized water precipitate 2～3 times, dries, obtain 2-
The brucite that methyl-2 mercaptopropionic acid sodium is modified；
2) brucite that the 2-obtained methyl-2 mercaptopropionic acid sodium is modified is put in vacuum tube furnace, add under vacuum
Hot to 400～600 DEG C, vacuum calcining 2～4h, it is then cooled to room temperature；
3) powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 20%～40%, every gram of powder correspondence
10～15 milliliters of hydrochloric acid solutions, stirring 3～4h, treats that brucite lamella all dissolves, obtains after high speed centrifugation under nitrogen protection
Sulfur doping carbon quantum dot.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114300274A (en) * | 2022-01-24 | 2022-04-08 | 西北民族大学 | Boron-sulfur co-doped porous carbon material and preparation method and application thereof |
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| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN104140084A (en) * | 2014-08-01 | 2014-11-12 | 中国人民解放军国防科学技术大学 | Method for preparing carbon nitride quantum dots |
| CN104817063A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen- and phosphorus-doped graphene |
| CN104974749A (en) * | 2014-04-04 | 2015-10-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitrogen-doped carbon quantum dot with high fluorescence quantum yield and preparation method and application of nitrogen-doped carbon quantum dot |
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- 2016-08-18 CN CN201610685133.6A patent/CN106318383A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497762A (en) * | 2013-06-26 | 2014-01-08 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN104974749A (en) * | 2014-04-04 | 2015-10-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitrogen-doped carbon quantum dot with high fluorescence quantum yield and preparation method and application of nitrogen-doped carbon quantum dot |
| CN104140084A (en) * | 2014-08-01 | 2014-11-12 | 中国人民解放军国防科学技术大学 | Method for preparing carbon nitride quantum dots |
| CN104817063A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen- and phosphorus-doped graphene |
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| 史文颖等，: ""二维限域空间内碳点的制备及性能调控"", 《中国化学会第30届学术年会摘要集-第二十一分会：Π-共轭材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114300274A (en) * | 2022-01-24 | 2022-04-08 | 西北民族大学 | Boron-sulfur co-doped porous carbon material and preparation method and application thereof |
| CN114300274B (en) * | 2022-01-24 | 2023-07-14 | 西北民族大学 | Boron-sulfur co-doped porous carbon material and preparation method and application thereof |
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