CN106318387A - Preparation method of boron-sulfur doped carbon quantum dots - Google Patents
Preparation method of boron-sulfur doped carbon quantum dots Download PDFInfo
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- CN106318387A CN106318387A CN201610689257.1A CN201610689257A CN106318387A CN 106318387 A CN106318387 A CN 106318387A CN 201610689257 A CN201610689257 A CN 201610689257A CN 106318387 A CN106318387 A CN 106318387A
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- acid sodium
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- 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 boron-sulfur doped carbon quantum dots. The preparation method in sequence comprises the following steps: adding layered double hydroxides (LDH) sieved with a 20-50 mesh sieve into a 4-mercaptophenylboronic acid sodium solution of which the mass percent concentration is 0.1% to 1% as per gram of LDH corresponding to the 1 to 1.5mmol of 4-mercaptophenylboronic acid sodium, stirring for 5 to 6 hours in a constant-temperature water bath at 60 to 70 DEG C, aging for 12 to 24 hours, then carrying out solid-liquid separation, washing precipitates by deionized water for 2 to 3 times, and drying to obtain 4-mercaptophenylboronic acid sodium modified LDH; putting the obtained 4-mercaptophenylboronic acid sodium modified LDH in a vacuum tube furnace, heating to 400 to 600 DEG C under vacuum conditions, carrying out vacuum calcination for 2 to 4 hours, and then cooling to room temperature; adding calcined powder to a hydrochloric acid solution of which the mass percent concentration is 20% to 40% as per gram of the powder corresponding to 10 to 15ml of the hydrochloric acid solution, stirring for 3 to 4 hours under the protection of nitrogen, and carrying out high speed centrifugation when LDH layers are completely dissolved to obtain the boron-sulfur doped carbon quantum dots. The method is simple in material and mild in condition.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to the preparation side of a kind of boron sulfur doping carbon quantum dot
Method.
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 boron sulfur doping carbon quantum dot.
To this end, the invention provides techniques below scheme, the preparation method of a kind of boron sulfur doping carbon quantum dot, include successively
Following steps:
1) according to the amount of the corresponding 1～1.5mmol 4-mercaptophenyl boronic acid sodium of every gram of brucite, the neatly of 20-50 mesh sieve will be crossed
Stone joins in the 4-mercaptophenyl boronic acid sodium solution that mass percent concentration is 0.1%～1%, in 60～70 DEG C of waters bath with thermostatic control
Stirring 5～6h, aging 12～24h, then solid-liquid separation, it is washed with deionized water precipitate 2～3 times, dries, obtain 4-sulfydryl benzene boron
The brucite that acid sodium is modified；
2) brucite that the 4-mercaptophenyl boronic acid sodium obtained is modified is put in vacuum tube furnace, heat under vacuum
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
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 boron 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 4-mercaptophenyl boronic acid sodium is raw material, and this material is tied
Structure is regular, it is possible to obtain the preferable carbon quantum dot of pattern.
2. utilize the special construction of brucite, by anion exchange effect, 4-mercaptophenyl boronic acid root is exchanged to brucite
Interlayer, and it is fixed on interlayer.Guarantee that interlayer Organic substance is being with electric charge point position monomolecular dispersion, shape after 400～600 DEG C of carbonizations
Become granulated carbon structure.
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 4-mercaptophenyl boronic acid sodium, the neatly of 50 mesh sieves will be crossed
Stone joins in the 4-mercaptophenyl boronic acid sodium solution that mass percent concentration is 1%, stirs 6h in 70 DEG C of waters bath with thermostatic control, aging
24h, then solid-liquid separation, be washed with deionized water precipitate 3 times, dries, and obtains the brucite that 4-mercaptophenyl boronic acid sodium is modified；Will
To the modified brucite of 4-mercaptophenyl boronic acid sodium put in vacuum tube furnace, be heated to 600 DEG C under vacuum, vacuum is forged
Burn 4h, be then cooled to room temperature；Powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 40%, every gram
The corresponding 15 milliliters of hydrochloric acid solutions of powder, stir 4h under nitrogen protection, treat that brucite lamella all dissolves, obtain after high speed centrifugation
Boron sulfur doping carbon quantum dot.
Embodiment 2
According to the amount of every gram of commercially available zinc-aluminum hydrotalcite correspondence 1mmol 4-mercaptophenyl boronic acid sodium, the brucite of 20 mesh sieves will be crossed
Join in the 4-mercaptophenyl boronic acid sodium solution that mass percent concentration is 0.1%, 60 DEG C of waters bath with thermostatic control are stirred 5h, aging
12h, then solid-liquid separation, be washed with deionized water precipitate 2 times, dries, and obtains the brucite that 4-mercaptophenyl boronic acid sodium is modified；Will
To the modified brucite of 4-mercaptophenyl boronic acid sodium put in vacuum tube furnace, be heated to 400 DEG C under vacuum, vacuum is forged
Burn 2h, be then cooled to room temperature；Powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 20%, every gram
The corresponding 10 milliliters of hydrochloric acid solutions of powder, stir 3h under nitrogen protection, treat that brucite lamella all dissolves, obtain after high speed centrifugation
Boron 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 4-mercaptophenyl boronic acid sodium, the brucite crossing 50 mesh sieves is joined matter
Amount percent concentration is in the 4-mercaptophenyl boronic acid sodium solution of 0.5%, stirs 6h, aging 24h in 70 DEG C of waters bath with thermostatic control, more solid
Liquid separates, and is washed with deionized water precipitate 3 times, dries, and obtains the brucite that 4-mercaptophenyl boronic acid sodium is modified；The 4-mercapto that will obtain
The brucite of base phenylboric acid sodium modification is put in vacuum tube furnace, is heated to 500 DEG C under vacuum, vacuum calcining 4h, so
After be cooled to room temperature；Powder after calcining is joined in the hydrochloric acid solution that mass percent concentration is 40%, every gram of powder pair
Answer 15 milliliters of hydrochloric acid solutions, stir 4h under nitrogen protection, treat that brucite lamella all dissolves, obtain boron sulfur after high speed centrifugation and mix
Miscellaneous carbon quantum dot.
Claims (1)
1. the preparation method of a boron 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 4-mercaptophenyl boronic acid sodium of every gram of brucite, the brucite crossing 20-50 mesh sieve is added
Enter in the 4-mercaptophenyl boronic acid sodium solution that mass percent concentration is 0.1%～1%, stir in 60～70 DEG C of waters bath with thermostatic control
5～6h, aging 12～24h, then solid-liquid separation, it is washed with deionized water precipitate 2～3 times, dries, obtain 4-mercaptophenyl boronic acid sodium
Modified brucite；
2) brucite that the 4-mercaptophenyl boronic acid sodium obtained is modified is put in vacuum tube furnace, be heated under vacuum
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
Boron sulfur doping carbon quantum dot.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021235024A1 (en) * | 2020-05-21 | 2021-11-25 | 株式会社クレハ | Composition and method for producing same |
| EP4053075A4 (en) * | 2019-10-29 | 2023-03-29 | Kureha Corporation | Carbon quantum dot-containing composition and method for producing same |
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- 2016-08-18 CN CN201610689257.1A patent/CN106318387A/en active Pending
Patent Citations (4)
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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 |
| 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4053075A4 (en) * | 2019-10-29 | 2023-03-29 | Kureha Corporation | Carbon quantum dot-containing composition and method for producing same |
| WO2021235024A1 (en) * | 2020-05-21 | 2021-11-25 | 株式会社クレハ | Composition and method for producing same |
| JPWO2021235024A1 (en) * | 2020-05-21 | 2021-11-25 | ||
| CN115443250A (en) * | 2020-05-21 | 2022-12-06 | 株式会社吴羽 | Composition and method for producing the same |
| JP7265093B2 (en) | 2020-05-21 | 2023-04-25 | 株式会社クレハ | Method for producing the composition |
| CN115443250B (en) * | 2020-05-21 | 2024-05-31 | 株式会社吴羽 | Composition and method for producing same |
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Application publication date: 20170111 |