CN108300458A - A kind of metalloporphyrin organic frame quantum dot and preparation method thereof - Google Patents
A kind of metalloporphyrin organic frame quantum dot and preparation method thereof Download PDFInfo
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- CN108300458A CN108300458A CN201810319832.8A CN201810319832A CN108300458A CN 108300458 A CN108300458 A CN 108300458A CN 201810319832 A CN201810319832 A CN 201810319832A CN 108300458 A CN108300458 A CN 108300458A
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Abstract
The invention discloses a kind of metalloporphyrin organic frame quantum dot and preparation method thereof, the chemical formula of the quantum dot is Cu5C56H48N8O16.Preparation method is copper acetate monohydrate solid, dodecyl solid sodium sulfate and 5, and the acetic acid solution of 10,15,20 four (4 pyridyl group) porphyrins is added in deionized water, 20oA period of time is stood under C, and metalloporphyrin organic frame quantum dot solution is made；Above-mentioned aqueous solution is dropped on copper mesh and is spontaneously dried, metalloporphyrin organic frame quantum dot is made.The preparation method is simple and efficient, and favorable reproducibility, low energy consumption, convenient for batch production, and meets environmental-friendly requirement；Metalloporphyrin organic frame quantum dot size obtained by this method is uniform, good dispersion, and substance is novel, and application potential is higher.
Description
Technical field
The present invention relates to a kind of quantum dots, and in particular to a kind of metalloporphyrin organic frame quantum dot and preparation method thereof,
Belong to metal-organic framework material field.
Background technology
Metal organic frame（MOF）Material be organic ligand by be coordinated with metal ion and its cluster one
The porous orderly nano material of kind.The arrangement of its organic ligand and metal ion or cluster has apparent directionality, can be with shape
At different frame pore structures, to show different absorption properties, optical property, electromagnetic property etc..MOF nanometers
Material have many advantages, such as it is porous orderly, structure and function is adjustable, dielectricity is adjustable, obtained in fields such as sensing, biomedicine, optics
To extensive use.MOF nano materials type is more at present, can be divided into zero dimension, one-dimensional, two-dimentional, three-dimensional, zero dimension from configuration aspects
MOF nano materials have unique physicochemical properties, such as quantum size effect, skin effect etc..With development in science and technology, light
Electrical part present small size, large capacity, lighting development trend, metal organic frame quantum dot is as a kind of important zero dimension
Semi-conducting material, due to have the advantages that porosity height, large specific surface area, be easily worked it is integrated, and its laser, memory,
The application prospect in the fields such as energy storage so that metal organic frame quantum dot and preparation method thereof becomes micro-, receives field of photoelectric devices
Research Emphasis.
Porphyrin is a kind of tetrapyrrole macrocyclic compound of conjugation, and it is all that the fragrant macrocyclic structure of 18 pi-electrons conjugation makes it show
More properties and function.The material not only plays key in the transmission of the photosynthesis oxygen of nature, electron-transport, energy transmission
Effect, and its fragrant macrocyclic structure and multiple tooth coordination ability assign their fabulous self organization abilities, allow its material science,
The fields such as medicine, chemical catalysis, Organic Light Emitting Diode and solar cell are widely used.Currently, metal organic frame
Nano material uses top-down preparation method, and this method is complicated for operation, efficiency is low, and the cost is relatively high, and repetitive rate is low,
It is not suitable for producing in batches.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of metalloporphyrin organic frame quantum
Point and preparation method thereof, which is prepared by the way of auxiliary agent assisted self assembling from bottom to top, and this method is simply high
Effect, is convenient for batch production at favorable reproducibility, and metalloporphyrin organic frame quantum dot size obtained by this method is uniform, dispersibility
It is good, it is cheap.
In order to achieve the above object, the present invention uses following technical scheme：
A kind of metalloporphyrin organic frame quantum dot, chemical formula Cu5C56H48N8O16。
Further, the size of the metalloporphyrin organic frame quantum dot is 5nm 10nm.
The preparation method of the metalloporphyrin organic frame quantum dot, includes the following steps：
S1）Copper acetate monohydrate and dodecyl sodium sulphate are dissolved separately in deionized water, copper acetate monohydrate is made
Solution and dodecyl metabisulfite solution；4- pyridyl group porphyrins are completely dissolved in acetic acid again, are made 5,10,15,20- tetra-
(4- pyridyl groups) porphyrin acetic acid solution；
S2）First copper acetate monohydrate solution and dodecyl metabisulfite solution are uniformly mixed, are then added dropwise 5,10,
15,20- tetra- (4- pyridyl groups) porphyrin acetic acid solutions are stirred to uniformly mixed；
S3）By the mixed liquor of step S2 20oConstant temperature under C stands reaction 5h-24h to get to metalloporphyrin organic frame quantum
Point aqueous solution；
S4）The metalloporphyrin organic frame quantum dot aqueous solution of step S3 is dropped on copper mesh, is spontaneously dried, metal is made
Porphyrin organic frame quantum dot.
Further, the copper acetate monohydrate solution in step S2 mixed solutions, dodecyl metabisulfite solution and 5,
10,15,20- tetra-（4- pyridyl groups）The concentration ratio of porphyrin acetic acid solution is 1mM-2mM:3.5mM-4mM:0.01mM-0.04mM.
Further, the copper acetate monohydrate solution in step S2, dodecyl metabisulfite solution and 5,10,15,20-
Four（4- pyridyl groups）The volume ratio of porphyrin acetic acid solution is 15:15:1.
Further, the copper mesh of step S4 is that copper mesh carbon supports film.
Compared with prior art, technical scheme of the present invention has the following advantages that：
1. the preparation method of the present invention is simple and efficient, favorable reproducibility, convenient for batch production, and meet environmental-friendly requirement.
2. the metalloporphyrin organic frame quantum dot being prepared by preparation method of the present invention, size uniformity, dispersibility
It is good and cheap.
Description of the drawings
Fig. 1 is the low power transmission electron microscope picture that the embodiment of the present invention 1 reacts metalloporphyrin organic frame quantum dot obtained by 5h.
Fig. 2 is the high power transmission electron microscope picture that the embodiment of the present invention 1 reacts metalloporphyrin organic frame quantum dot obtained by 5h.
Fig. 3 is the low power transmission electron microscope picture of metalloporphyrin organic frame quantum dot obtained by the reaction for 24 hours of the embodiment of the present invention 1.
Fig. 4 is the low power transmission electron microscope picture that the embodiment of the present invention 2 reacts metalloporphyrin organic frame quantum dot obtained by 5h.
Fig. 5 is the low power transmission electron microscope picture that the embodiment of the present invention 3 reacts metalloporphyrin organic frame quantum dot obtained by 5h.
Specific implementation mode
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.The embodiment is shown
Example is shown in the accompanying drawings, specific reality of the specific embodiment described in following embodiments of the present invention only as the present invention
Apply the exemplary illustration of mode, it is intended to for explaining the present invention, and be not configured to limitation of the present invention.
Embodiment 1
A kind of preparation method of metalloporphyrin organic frame quantum dot, includes the following steps：
S1）By the copper acetate monohydrate aqueous solution of a concentration of 3.34 mM of 6ml and the lauryl sodium sulfate of 8 mM of 6ml
Aqueous solution uniformly mixes, then by 5,10,15,20- tetra-（4- pyridyl groups）Porphyrin is added in acetic acid, is configured to a concentration of 1mM
Solution, and the 0.4ml solution is taken to instill dropwise in copper acetate monohydrate and lauryl sodium sulfate mixed solution, mixing is equal
It is even；
S2）Mixed liquor is rested on 20 immediatelyoIn C baking ovens or low temperature thermostat bath, start timing, reaction 5h-24h to get to
Metalloporphyrin organic frame quantum dot aqueous solution；
S3）The metalloporphyrin organic frame quantum dot aqueous solution of step S2 is dropped to copper mesh carbon to support on film, is spontaneously dried,
Porphyryl metal organic frame quantum dot is made.
Copper mesh carbon after above-mentioned dry is supported to carry out observation shooting, black nano under film transfer to transmission electron microscope
Particle, that is, porphyryl metal organic frame quantum dot, size are 5nm 10nm.
The chemical formula of 1 gained metalloporphyrin organic frame quantum dot of above-described embodiment is Cu5C56H48N8O16。
Fig. 1 is that gained metalloporphyrin organic frame quantum dot low power transmitted electron is aobvious after 1 isothermal reaction 5h of above-described embodiment
Micro mirror figure, Fig. 2 are its high power transmission electron microscope figure, show the lattice of the crystal structure, show obtained metalloporphyrin
Organic frame quantum dot size is uniform, good dispersion.
Fig. 3 is the low power transmission electron microscope of gained metalloporphyrin organic frame quantum dot after 1 isothermal reaction of above-described embodiment for 24 hours
Scheme, it is found that metalloporphyrin organic frame quantum dot size obtained is 5nm 10nm in figure, and metalloporphyrin in unit area
The number of organic frame quantum dot increases.
Embodiment 2
A kind of preparation method of metalloporphyrin organic frame quantum dot, includes the following steps：
S1）By the copper acetate monohydrate aqueous solution of a concentration of 3mM of 6ml and the lauryl sodium sulfate aqueous solution of the 8mM of 6ml
Uniformly mixing, then by 5,10,15,20- tetra-（4- pyridyl groups）Porphyrin is added in acetic acid, is configured to the solution of a concentration of 1mM,
And the 0.4ml solution is taken to instill dropwise in copper acetate monohydrate and lauryl sodium sulfate mixed solution, it is uniformly mixed；
S2）Mixed liquor is rested on 20 immediatelyoIn C baking ovens or low temperature thermostat bath, start timing, reaction 5h-24h to get to
Metalloporphyrin organic frame quantum dot aqueous solution；
S3）The metalloporphyrin organic frame quantum dot aqueous solution of step S2 is dropped to copper mesh carbon to support on film, is spontaneously dried,
Porphyryl metal organic frame quantum dot is made.
Copper mesh carbon after above-mentioned dry is supported to carry out observation shooting, black nano under film transfer to transmission electron microscope
Particle, that is, porphyryl metal organic frame quantum dot, size are 5nm 10nm.
The chemical formula of 2 gained metalloporphyrin organic frame quantum dot of above-described embodiment is Cu5C56H48N8O16。
Fig. 4 is the low power transmission electron microscope of gained metalloporphyrin organic frame quantum dot after 2 isothermal reaction 5h of above-described embodiment
Figure, metalloporphyrin organic frame quantum dot size is uniform, good dispersion.
Embodiment 3
A kind of preparation method of metalloporphyrin organic frame quantum dot, wherein step S1-S3 steps corresponding to above-described embodiment 1
Rapid identical, copper acetate monohydrate solution concentration is 4mM in only step S1.Support film transfer to saturating in copper mesh carbon after above-mentioned dry
It penetrates and carries out observation shooting under electron microscope, black nano particle, that is, metalloporphyrin organic frame quantum dot, size 5nm
10nm。
The chemical formula of 3 gained metalloporphyrin organic frame quantum dot of above-described embodiment is Cu5C56H48N8O16。
Fig. 5 is the low power transmission electron microscope of gained metalloporphyrin organic frame quantum dot after 3 isothermal reaction 5h of above-described embodiment
Figure, metalloporphyrin organic frame quantum dot size is uniform, good dispersion.
The present invention provides a kind of efficiently easy metalloporphyrin organic frame quantum dot preparation method, favorable reproducibility,
And reacted in solution environmental, convenient for batch production, meet environmental-friendly requirement, the metalloporphyrin prepared by the above method
Organic frame quantum dot size is 5nm 10nm, size uniformity, good dispersion, and cheap, cost reduction.
It should be noted that above-described embodiment is that the present invention will be described rather than limits the invention, and
Those skilled in the art can design alternative embodiment without departing from the scope of the appended claims.In claim
In, word "comprising" does not exclude the presence of data or step not listed in the claims.
Claims (6)
1. a kind of metalloporphyrin organic frame quantum dot, it is characterised in that：The chemical formula of the metalloporphyrin organic frame is：
Cu5C56H48N8O16。
2. metalloporphyrin organic frame quantum dot according to claim 1, it is characterised in that：The metalloporphyrin has machine frame
The size of frame quantum dot is 5nm-10nm.
3. the preparation method of metalloporphyrin organic frame quantum dot described in claim 1, which is characterized in that including following step
Suddenly：
S1）Copper acetate monohydrate and dodecyl sodium sulphate are dissolved separately in deionized water, copper acetate monohydrate is made
Solution and dodecyl metabisulfite solution；4- pyridyl group porphyrins are completely dissolved in acetic acid again, are made 5,10,15,20- tetra-
(4- pyridyl groups) porphyrin acetic acid solution；
S2）First copper acetate monohydrate solution and dodecyl metabisulfite solution are uniformly mixed, are then added dropwise 5,10,
15,20- tetra- (4- pyridyl groups) porphyrin acetic acid solutions are stirred to uniformly mixed；
S3）By the mixed liquor of step S2 20oConstant temperature under C stands reaction 5h-24h to get to metalloporphyrin organic frame quantum
Point aqueous solution；
S4）The metalloporphyrin organic frame quantum dot aqueous solution of step S4 is dropped on copper mesh, is spontaneously dried, metal is made
Porphyrin organic frame quantum dot.
4. the preparation method of metalloporphyrin organic frame quantum dot according to claim 3, it is characterised in that：Step S2 is mixed
Close copper acetate monohydrate solution, dodecyl metabisulfite solution and the 5,10,15,20- tetra- in solution（4- pyridyl groups）Porphyrin
The concentration ratio of acetic acid solution is 1mM-2mM:3.5mM-4mM:0.01mM-0.04mM.
5. the preparation method of metalloporphyrin organic frame quantum dot according to claim 3, it is characterised in that：In step S2
Copper acetate monohydrate solution, dodecyl metabisulfite solution and 5,10,15,20- tetra-（4- pyridyl groups）Porphyrin acetic acid solution
Volume ratio be 15:15:1.
6. the preparation method of metalloporphyrin organic frame quantum dot according to claim 3, it is characterised in that：Step S4's
Copper mesh is that copper mesh carbon supports film.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109575299A (en) * | 2018-11-15 | 2019-04-05 | 三明学院 | A method of synthesis conduction MOF material |
| CN110105582A (en) * | 2019-05-08 | 2019-08-09 | 南京邮电大学 | The preparation method of metalloporphyrin frame nanocrystalline structure |
| CN110124714A (en) * | 2019-05-08 | 2019-08-16 | 南京邮电大学 | A kind of Cu-N-C base carbon nanosheet and the preparation method and application thereof |
| WO2021223317A1 (en) * | 2020-05-07 | 2021-11-11 | 青岛大学 | Preparation method for ratio fluorescent lactic acid probe based on novel nanocomposite system and enzyme catalytic reaction |
| CN113737152A (en) * | 2021-09-02 | 2021-12-03 | 黑龙江八一农垦大学 | Preparation method of graphene/metal organic framework composite photoresponse device |
| CN113831544A (en) * | 2021-09-22 | 2021-12-24 | 同济大学 | Non-linear nano hybrid material of titanium carbide quantum dots and vanadium metal organic framework and preparation method thereof |
| CN115382581A (en) * | 2022-09-22 | 2022-11-25 | 吉林大学 | Construction method and application of two-dimensional double-layer metal organic framework material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109575299A (en) * | 2018-11-15 | 2019-04-05 | 三明学院 | A method of synthesis conduction MOF material |
| CN110105582A (en) * | 2019-05-08 | 2019-08-09 | 南京邮电大学 | The preparation method of metalloporphyrin frame nanocrystalline structure |
| CN110124714A (en) * | 2019-05-08 | 2019-08-16 | 南京邮电大学 | A kind of Cu-N-C base carbon nanosheet and the preparation method and application thereof |
| CN110105582B (en) * | 2019-05-08 | 2021-08-27 | 南京邮电大学 | Preparation method of metalloporphyrin framework nanocrystalline structure |
| CN110124714B (en) * | 2019-05-08 | 2022-08-30 | 南京邮电大学 | Cu-N-C-based carbon nanosheet and preparation method and application thereof |
| WO2021223317A1 (en) * | 2020-05-07 | 2021-11-11 | 青岛大学 | Preparation method for ratio fluorescent lactic acid probe based on novel nanocomposite system and enzyme catalytic reaction |
| CN113737152A (en) * | 2021-09-02 | 2021-12-03 | 黑龙江八一农垦大学 | Preparation method of graphene/metal organic framework composite photoresponse device |
| CN113737152B (en) * | 2021-09-02 | 2022-04-05 | 黑龙江八一农垦大学 | Preparation method of graphene/metal organic framework composite photoresponse device |
| CN113831544A (en) * | 2021-09-22 | 2021-12-24 | 同济大学 | Non-linear nano hybrid material of titanium carbide quantum dots and vanadium metal organic framework and preparation method thereof |
| CN115382581A (en) * | 2022-09-22 | 2022-11-25 | 吉林大学 | Construction method and application of two-dimensional double-layer metal organic framework material |
| CN115382581B (en) * | 2022-09-22 | 2024-03-19 | 吉林大学 | Construction method and application of two-dimensional double-layer metal organic framework material |
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