CN106350066A - Method for preparing carbon quantum dots doped with phosphorus and chlorine - Google Patents
Method for preparing carbon quantum dots doped with phosphorus and chlorine Download PDFInfo
- Publication number
- CN106350066A CN106350066A CN201610687226.2A CN201610687226A CN106350066A CN 106350066 A CN106350066 A CN 106350066A CN 201610687226 A CN201610687226 A CN 201610687226A CN 106350066 A CN106350066 A CN 106350066A
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- Prior art keywords
- sodium
- chloromethane
- hydrotalcite
- phosphorous acid
- acid solution
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/72—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing halogen, e.g. halophosphates
- C09K11/727—Aluminates; Silicates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention discloses a method for preparing carbon quantum dots doped with phosphorus and chlorine. The method sequentially includes steps of adding hydrotalcite into sodium chloromethane phosphorous acid solution according to certain quantities, stirring the hydrotalcite and the sodium chloromethane phosphorous acid solution in constant-temperature water bath at the temperature of 60-70 DEG C for 5-6 h, aging the hydrotalcite and the sodium chloromethane phosphorous acid solution for 12-25 h, separating solid from liquid, washing precipitates by the aid of deionized water by 2-3 times and drying the precipitates to obtain hydrotalcite modified by sodium chloromethane phosphorous acid; placing the obtained hydrotalcite modified by the sodium chloromethane phosphorous acid into a vacuum tube furnace, heating the hydrotalcite modified by the sodium chloromethane phosphorous acid under vacuum conditions until the temperature of the hydrotalcite modified by the sodium chloromethane phosphorous acid reaches 400-600 DEG C, calcining the hydrotalcite modified by the sodium chloromethane phosphorous acid under vacuum conditions for 2-4 h and then cooling the hydrotalcite modified by the sodium chloromethane phosphorous acid until the temperature of the hydrotalcite modified by the sodium chloromethane phosphorous acid reaches the room temperature; adding calcined powder into hydrochloric acid solution with the mass percent concentration of 20%-40%, stirring the powder and the hydrochloric acid solution under the protection of nitrogen for 3-4 h, completely dissolving hydrotalcite lamellas and then centrifuging solution at high speeds to obtain the carbon quantum dots doped with the phosphorus and the chlorine. Each gram of the hydrotalcite added into the sodium chloromethane phosphorous acid solution corresponds to 1-1.5 mmol of the sodium chloromethane phosphorous acid, the mass percent concentration of the sodium chloromethane phosphorous acid solution is 0.1%-1%, and the hydrotalcite is sieved by the aid of sieves with the sizes of 20-50 meshes. Each gram of the sintered powder corresponds to 10-15 milliliters of the hydrochloric acid solution. The method has the advantages of simple materials and mild conditions.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, more particularly, to a kind of preparation side of phosphorus chlorine doping carbon quantum dot
Method.
Background technology
Quantum dot is in 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, adulterate, strain, impurity produces), the interface of two kinds of different semi-conducting materials (for example:
From in group quantum dot), the surface (for example: semiconductor nanocrystal) of quasiconductor, or the combination of above three.Quantum dot has
Detached quantized power spectrum.Corresponding wave function is spatially positioned in quantum dot, but extends in several lattice period.
One quantum dot has a small amount of electronics of (1-100) integer, electric hole or electronics electricity hole pair, and the electricity that is, it is carried is unit
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 very wide field including improving biosensor, medical imaging devices and small light emitting diode
Scape.Because carbon nano-particles have very big surface area, scientists think this nanoparticle phase always for a long time
The macroscopical carbon of ratio, has very peculiar chemical and physical features.
Quantum dot is usually extract from the mixture of lead, cadmium and silicon, but these quantum dots are typically poisonous, to ring
Also there is very big harm in border.So scientists seek to extract quantum dot in some optimum compounds.Opposing metallic quantum
For point, carbon quantum dot nonhazardouss act on, the harm very little to environment, and preparation cost is cheap.Its research represents luminous receiving
Rice corpuscles research enters a new stage.
Layered di-hydroxyl composite metal oxidate (layered double hydroxides, abbreviation ldh), also known as neatly
Stone, is the important inorganic functional material of a class.Its unique layer structure and the adjustable degeneration of laminate element and interlayer anion
Get more and more people's extensive concerning, introducing new object anion through ion exchange to interlayer can make layer structure and composition produce phase
The change answered, thus the functional material that a big class has special nature can be prepared.Hydrotalcite material belongs to anion type laminated
Compound.Lamellar compound refers to have layer structure, interlayer ion has a class compound of interchangeability, using laminarization
Intercalation and the interchangeability of interlayer ion that compound main body has under highly polar molecular action, by some features visitor
Body material introduces bedding void and struts laminate distance thus forming 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, the interlamellar spacing of brucite is different.
Content of the invention
The purpose of the present invention is for overcoming the shortcomings of complicated process of preparation in prior art, expensive etc., providing one kind
The preparation method of phosphorus chlorine doping carbon quantum dot.
For this reason, the invention provides technical scheme below, a kind of preparation method of phosphorus chlorine doping carbon quantum dot, including successively
Following steps:
1) according to the amount of the corresponding 1～1.5mmol chloromethyl phosphonous acid sodium of every gram of brucite, the neatly of 20-50 mesh sieve will be crossed
Stone is added in the chloromethyl phosphonous 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 chloromethyl Asia phosphine
The modified brucite of sour sodium；
2) the modified brucite of the chloromethyl obtaining phosphonous acid sodium is put in vacuum tube furnace, heat under vacuum
To 400～600 DEG C, vacuum calcining 2～4h, it is subsequently cooled to room temperature；
3) powder after calcining is added in the hydrochloric acid solution that mass percent concentration is 20%～40%, every gram of powder
Corresponding 10～15 milliliters of hydrochloric acid solutions, stir 3～4h under nitrogen protection, treat that brucite lamella all dissolves, after high speed centrifugation
Obtain phosphorus chlorine doping carbon quantum dot.
Compared with prior art, the present invention has a following beneficial technique effect:
1. prepare this quanta point material source simple, be raw material using acylate chloromethyl phosphonous acid sodium, 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, chloromethyl phosphonous acid root is exchanged to by brucite by anion exchange effect
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 granule carbon structure.
3. the material after carbonization is after through overpickling, brucite itself destructurized, metal-oxide is molten by acid
Solution, the charcoal quantum dot of interlayer presents naturally, and process is simple, gentle.
Specific embodiment
To describe the present invention in detail with reference to embodiment, but the present invention is not limited to this.
Embodiment 1
Correspond to the amount of 1.5mmol chloromethyl phosphonous acid sodium according to every gram of commercially available magnesium aluminum-hydrotalcite, the neatly of 50 mesh sieves will be crossed
Stone is added in the chloromethyl phosphonous 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, are washed with deionized water precipitate 3 times, dry, and obtain the modified brucite of chloromethyl phosphonous acid sodium；Will
To the modified brucite of chloromethyl phosphonous acid sodium put in vacuum tube furnace, be heated to 600 DEG C under vacuum, vacuum is forged
Burn 4h, be subsequently cooled to room temperature；Powder after calcining is added in the hydrochloric acid solution that mass percent concentration is 40%, every gram
Powder corresponds to 15 milliliters of hydrochloric acid solutions, stirs 4h under nitrogen protection, treats that brucite lamella all dissolves, obtain after high speed centrifugation
Phosphorus chlorine doping carbon quantum dot.
Embodiment 2
Correspond to the amount of 1mmol chloromethyl phosphonous acid sodium according to every gram of commercially available zinc-aluminum hydrotalcite, the brucite of 20 mesh sieves will be crossed
It is added in the chloromethyl phosphonous 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, are washed with deionized water precipitate 2 times, dry, and obtain the modified brucite of chloromethyl phosphonous acid sodium；Will
To the modified brucite of chloromethyl phosphonous acid sodium put in vacuum tube furnace, be heated to 400 DEG C under vacuum, vacuum is forged
Burn 2h, be subsequently cooled to room temperature；Powder after calcining is added in the hydrochloric acid solution that mass percent concentration is 20%, every gram
Powder corresponds to 10 milliliters of hydrochloric acid solutions, stirs 3h under nitrogen protection, treats that brucite lamella all dissolves, obtain after high speed centrifugation
Phosphorus chlorine 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 magnalium is obtained
Type brucite；Brucite is crossed 40 mesh sieves, standby.
According to the amount of the corresponding 1mmol chloromethyl phosphonous acid sodium of every gram of brucite, the brucite crossing 50 mesh sieves is added to matter
Amount percent concentration is in 0.5% chloromethyl phosphonous acid sodium solution, 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 modified brucite of chloromethyl phosphonous acid sodium；By the chloromethane obtaining
The modified brucite of base phosphonous acid sodium 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 added 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 phosphorus chlorine after high speed centrifugation and mix
Miscellaneous carbon quantum dot.
Claims (1)
1. a kind of phosphorus chlorine adulterate carbon quantum dot preparation method it is characterised in that: in turn include the following steps:
1) according to the amount of the corresponding 1～1.5mmol chloromethyl phosphonous acid sodium of every gram of brucite, the brucite crossing 20-50 mesh sieve is added
Enter in the chloromethyl phosphonous acid sodium solution being 0.1%～1% to mass percent concentration, 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, dry, obtain chloromethyl phosphonous acid sodium
Modified brucite；
2) the modified brucite of the chloromethyl obtaining phosphonous acid sodium is put in vacuum tube furnace, be heated under vacuum
400～600 DEG C, vacuum calcining 2～4h, it is subsequently cooled to room temperature；
3) powder after calcining is added in the hydrochloric acid solution that mass percent concentration is 20%～40%, every gram of powder corresponds to
10～15 milliliters of hydrochloric acid solutions, stir 3～4h under nitrogen protection, treat that brucite lamella all dissolves, obtain after high speed centrifugation
Phosphorus chlorine doping carbon quantum dot.
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| CN201610687226.2A CN106350066A (en) | 2016-08-18 | 2016-08-18 | Method for preparing carbon quantum dots doped with phosphorus and chlorine |
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| CN201610687226.2A CN106350066A (en) | 2016-08-18 | 2016-08-18 | Method for preparing carbon quantum dots doped with phosphorus and chlorine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321945A (en) * | 2021-06-22 | 2021-08-31 | 华南农业大学 | Preparation method and application of carbon quantum dot regulated aluminum phosphite crystal |
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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 |
-
2016
- 2016-08-18 CN CN201610687226.2A patent/CN106350066A/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 |
Non-Patent Citations (1)
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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》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113321945A (en) * | 2021-06-22 | 2021-08-31 | 华南农业大学 | Preparation method and application of carbon quantum dot regulated aluminum phosphite crystal |
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