CN111960399A - Oxidized glassy carbon microsphere with electrochemiluminescence activity and preparation method thereof - Google Patents
Oxidized glassy carbon microsphere with electrochemiluminescence activity and preparation method thereof Download PDFInfo
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- 239000004005 microsphere Substances 0.000 title claims abstract description 69
- 229910021397 glassy carbon Inorganic materials 0.000 title claims abstract description 66
- 230000000694 effects Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000012043 crude product Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 238000004020 luminiscence type Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000002096 quantum dot Substances 0.000 description 6
- 238000007865 diluting Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000002186 photoelectron spectrum Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- -1 bipyridyl ruthenium Chemical compound 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910002567 K2S2O8 Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000002717 carbon nanostructure Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000001362 electron spin resonance spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- HWYHZTIRURJOHG-UHFFFAOYSA-N luminol Chemical compound O=C1NNC(=O)C2=C1C(N)=CC=C2 HWYHZTIRURJOHG-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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- 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
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses an oxidized glassy carbon microsphere with electrochemiluminescence activity and a preparation method thereof. The method comprises the following steps: adding the crude product of the glassy carbon microsphere into a concentrated nitric acid solution, stirring and refluxing for a period of time, cooling to room temperature, adding water for washing, centrifuging or filtering until the washing liquid is neutral, and drying the obtained solid precipitate to obtain the oxidized glassy carbon microsphere with the electrochemiluminescence activity. The method for preparing the oxidized glassy carbon microspheres with electrochemiluminescence activity is simple, low in cost, green and environment-friendly, and the obtained oxidized glassy carbon microspheres have good electrochemiluminescence activity.
Description
Technical Field
The invention relates to an oxidized glassy carbon microsphere with electrochemiluminescence activity and a preparation method thereof.
Background
Electrochemiluminescence is the phenomenon of a substance that produces luminescence during electrochemiluminescence. The electrochemiluminescence technology is a relatively new technology developed by crossing an electrochemical technology and a chemiluminescence technology, has the advantages of good controllability of electrochemistry and good sensitivity of chemiluminescence, and has wide application prospects in modern analytical chemistry, life analysis and clinical examination. The most central problem of the electrochemiluminescence analysis technology is how to obtain the electrochemiluminescence material with high sensitivity, low cost and environmental friendliness. There are two main classes of electrochemiluminescent materials in common use today: one is a molecular electrochemiluminescence material, such as luminol and bipyridyl ruthenium, which has the advantages of high luminous efficiency and commercial application, but has the disadvantages of difficult modification, expensive product price and high use cost; the other is a nano electrochemiluminescence material, mainly comprising semiconductor quantum dots containing heavy metals of cadmium and lead, such as CdS, PbS and the like, which have electrochemiluminescence activity, and is characterized by high electrochemiluminescence activity, easy preparation and modification, low cost, large toxicity of the material, harm to operators and the environment, and great limitation on the application of the material. In more than ten years, carbon-based quantum dots including carbon quantum dots and graphene quantum dots are found to solve the problems of high toxicity and difficult modification of heavy metal semiconductor quantum dots, but the carbon-based quantum dots still have too good water solubility and are difficult to fix on the surface of an electrode, so that the construction of an electroluminescence luminescence sensing interface is not facilitated. Therefore, the prepared electrochemiluminescence micron material has the advantages of low cost, low toxicity, high electrochemiluminescence activity, easy modification, easy separation and fixation, and has important significance for the development of electrochemiluminescence technology.
Disclosure of Invention
The invention aims to provide the oxidized glassy carbon microsphere with electrochemiluminescence activity and the preparation method thereof, the method is simple to operate and low in cost, and the prepared oxidized glassy carbon microsphere has good electrochemiluminescence activity.
The invention is realized by the following technical scheme:
a. adding the crude product of the glass-carbon microspheres into a nitric acid solution, and stirring and refluxing;
b. cooling to room temperature, diluting with water, filtering or centrifuging, washing with water for several times, and separating to obtain filtrate or centrifuging to obtain clear solution;
c. and collecting the precipitate, and drying to obtain the oxidized glassy carbon microsphere with electrochemiluminescence activity.
Wherein the concentration of the nitric acid in the step a is 1-98%, and the preferable concentration is 68%.
Further, the dosage ratio of the glassy carbon microsphere crude product and the nitric acid solution in the step a is that 0.001-50 g of the glassy carbon microsphere crude product is added to every 100mL of nitric acid, and preferably 0.5g of the carbon nanotube crude product is added to every 100mL of nitric acid.
Further, the reflux temperature in the step a is 20-200 ℃, and the reflux time is 0.1-100 h. The reflux time is preferably 8 h.
Further, the separation method in step b can be vacuum filtration or centrifugal ultrafiltration or centrifugal separation. Preferably, the filtration is carried out with a 0.2 um filter membrane.
The invention takes the industrial prepared crude product of the glassy carbon microsphere as a raw material, adopts simple and cheap acid oxidation treatment, and ensures that the surface of the glassy carbon microsphere generates rich defects, surface states and proper oxidation degree on the basis of keeping the spherical structure of the glassy carbon microsphere by researching and controlling the acid oxidation condition, the reaction temperature, the reaction time and the acid concentration of the glassy carbon microsphere, thereby preparing the oxidized glassy carbon microsphere with electrochemiluminescence activity.
According to the invention, graphene-like and fullerene-like carbon nanostructures of the glassy carbon microsphere are oxidized by nitric acid and are crushed, so that graphene-like quantum dots and fullerene-like quantum dots which are small in size, rich in carbon edge and provided with a plurality of oxygen-containing groups and carbon dangling bonds are formed on the surface of the glassy carbon microsphere, and the oxidized glassy carbon microsphere with strong electrochemical luminescence activity is prepared. The reaction mechanism of the invention is how to prepare the oxidized glassy carbon microspheres with electrochemiluminescence activity from the crude products of the glassy carbon microspheres by acid.
The invention has the following remarkable advantages:
the preparation method has the characteristics of cheap raw materials, low preparation cost, simple process, high yield and the like. The electrochemiluminescence functionalized oxidized glassy carbon microspheres prepared by the method have the advantages of easy separation and purification of products, good electrochemiluminescence performance and easy implementationFixing and decorating the lines and the like. The prepared electrochemiluminescence functionalized oxidized glassy carbon microsphere has good hydrophilicity and water dispersibility (figure 1 a), and is obviously superior to a glassy carbon microsphere raw material (figure 1 b). Scanning electron microscopy (see fig. 2) shows that the surface of the oxidized glassy carbon microsphere (fig. 2 a) has a wrinkled oxide layer, which is clearly different from the glassy carbon microsphere raw material having a smooth surface (fig. 2 b). Fig. 3 shows that the electrochemiluminescent functionalized oxidized glassy carbon microspheres (fig. 3 (a)) have a more abundant defect state (graphitic edges) compared to the glassy carbon microsphere crude product (fig. 3 (b)). The photoelectron spectrum of fig. 4 shows that the oxygen content of the electrochemiluminescence functionalized oxidized glassy carbon microspheres (curve 1) is obviously improved compared with the oxygen content of the crude products of the glassy carbon microspheres (curve 2), and the main oxygen-containing groups on the surfaces of the microspheres are carboxyl (-COOH). The paramagnetic resonance spectrum (fig. 5) shows that the electrochemiluminescence functionalized oxidized glassy carbon microspheres (curve (a)) have many dangling bonds closely related to the electrochemiluminescence activity while the crude products of the glassy carbon microspheres (curve (b)) have almost no dangling bonds. FIG. 6 is a measurement of the electrochemical activity of the prepared carbon nanotubes, in coreactant K2S2O8In the presence of the carbon nano tube, the prepared carbon nano tube shows good cathode electrochemiluminescence activity.
Drawings
FIG. 1 is a photograph of dispersions of electrochemiluminescence functionalized oxidized glassy carbon microspheres (a) and crude glassy carbon microspheres (b) in pure water; the more uniform the dispersion, the better the hydrophilicity of the material;
FIG. 2 is a scanning electron micrograph of electrochemiluminescence functionalized oxidized glassy carbon microspheres (a) and crude glassy carbon microspheres (b); the white part is an organic matter with poor conductivity;
FIG. 3 Raman spectra of electrochemiluminescence functionalized oxidized glassy carbon microspheres (a) and crude glassy carbon microspheres (b); i isD/IGThe larger the ratio, the more defective states (graphitic edges) of the material;
FIG. 4 is a photoelectron spectrum of electrochemiluminescence functionalized oxidized glassy carbon microspheres (1) and a crude product of the glassy carbon microspheres (2); the total photoelectron spectrum in the graph (a) and the high resolution photoelectron spectrum in the graph (b) of C1S;
FIG. 5 EPR spectra of electrochemiluminescent functionalized oxidized glassy carbon microspheres (a) and a crude product of glassy carbon microspheres (b); the EPR signal is ultra strong, and more carbon dangling bonds are arranged on the surface of the material;
fig. 6 is an electrochemiluminescence response curve of an electrochemiluminescence functionalized oxidized glassy carbon microsphere, wherein:
(a) oxidizing the electrochemiluminescence response of the glassy carbon microsphere in the absence of a coreactant; (b) electrochemiluminescence response of persulfate coreactants per se; (c) and (3) performing electrochemiluminescence response on the oxidized glassy carbon microspheres in the presence of a persulfate coreactant.
Detailed Description
For a better understanding of the present invention, it is further illustrated by way of example, but the present invention is not limited thereto.
Example 1
Weighing 0.15 g of crude glassy carbon microsphere powder, adding the crude glassy carbon microsphere powder into a round-bottom flask, adding 30 mL of 68% concentrated nitric acid, refluxing for 8 hours under the condition of 140 ℃ oil bath, naturally cooling to room temperature, diluting suspension with water to 100mL, washing and centrifuging, discarding clear liquid, continuously washing and centrifuging precipitate with water until the clear liquid is neutral, and drying the obtained black solid precipitate in a 100 ℃ oven to obtain the oxidized glassy carbon microsphere with the electrochemiluminescence property.
Example 2
Weighing 0.15 g of crude powder of glassy carbon microspheres, adding the crude powder into a round-bottom flask, adding 30 mL of 98% concentrated nitric acid, refluxing for 4 hours under the condition of oil bath at 20 ℃, naturally cooling to room temperature, diluting suspension to 100mL with water, carrying out vacuum filtration with a 0.2-micrometer filter membrane, repeatedly washing and carrying out vacuum filtration on the obtained filter flask with water until filtrate is neutral, drying the obtained black solid precipitate in an oven at 100 ℃, and obtaining the oxidized glassy carbon microspheres with electrochemiluminescence performance.
Example 3
Weighing 0.05g of crude glassy carbon microsphere powder, adding the crude glassy carbon microsphere powder into a round-bottom flask, adding 30 mL of 68% concentrated nitric acid, refluxing for 6 hours under the condition of 200 ℃ oil bath, naturally cooling to room temperature, diluting suspension with water to 100mL, washing and centrifuging, discarding clear liquid, continuously washing and centrifuging precipitate with water until the clear liquid is neutral, and drying the obtained black solid precipitate in a 100 ℃ oven to obtain the oxidized glassy carbon microsphere with the electrochemiluminescence property.
Example 4
Adding 0.10 g of dried crude powder of the single-walled carbon nanotube into 30 mL of 20% nitric acid, refluxing for 30 h under the condition of oil bath at 140 ℃, naturally cooling to room temperature, diluting the suspension to 100mL by using water, carrying out centrifugal ultrafiltration by using a 10 kDa ultrafiltration tube, removing the nitric acid, and washing by using water until the filtrate is neutral. And collecting the purified black solid, and drying at 70 ℃ under reduced pressure to obtain the oxidized glassy carbon microsphere with the electrochemiluminescence property.
Claims (7)
1. A preparation method of oxidized glassy carbon microspheres with electrochemiluminescence activity is characterized in that: the preparation method comprises the following steps:
a. adding the dried crude product of the glass-carbon microspheres into a nitric acid solution, and stirring and refluxing;
b. cooling to room temperature, washing with water, filtering or centrifuging until the filtrate or clear liquid is neutral, and collecting solid precipitate;
c. and drying the solid precipitate to obtain the oxidized glassy carbon microspheres with electrochemiluminescence activity.
2. The method for preparing the oxidized glassy carbon microsphere with the photoactivity of the electrochemiluminescence carbon nano-tube as claimed in claim 1, wherein: the oxidized glassy carbon microspheres have electrogenerated chemical luminescence activity, namely, the phenomenon of luminescence is generated by self or in the presence of a coreactant through electrolysis.
3. The method for preparing oxidized glassy carbon microspheres with electrochemiluminescence activity according to claim 1, wherein: the mass concentration of the nitric acid in the step a is 1% -98%.
4. The method for preparing oxidized glassy carbon microspheres with electrochemiluminescence activity according to claim 1, wherein: the dosage ratio of the glassy carbon microsphere crude product and the nitric acid solution in the step a is that 0.001-50 g of carbon nanotube crude product is added to every 100mL of nitric acid.
5. The method for preparing oxidized glassy carbon microspheres with electrochemiluminescence activity according to claim 1, wherein: the reflux temperature in the step a is 20-200 ℃, and the reflux time is 0.1-100 h.
6. The method for preparing oxidized glassy carbon microspheres with electrochemiluminescence activity according to claim 1, wherein: the filtration method in the step b can be vacuum filtration or centrifugal separation.
7. An oxidized vitreous carbon microsphere with electrochemiluminescence activity prepared by the preparation method of any one of claims 1 to 6.
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