CN105670617A - Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots - Google Patents
Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots Download PDFInfo
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Abstract
The invention belongs to the field of petrochemical industry and carbon nanomaterial science and relates to a simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots. Ammonia water is creatively and directly used as an electrolyte so as to raise conductivity of an aqueous solution and simultaneously realize one-step nitrogen-doping. After electrolysis, complex steps of dialysis, desalting, purification and the like are not required, and nitrogen-doped carbon quantum dots with uniform particle size, stable fluorescence property and good water solubility are directly prepared. The method for preparation of carbon quantum dots has advantages of low time consumption and high yield. Efficient and large-scale preparation of the carbon quantum dots and synchronous doping are realized. The invention is mainly characterized in that low-cost petroleum coke is used as a carbon source and ammonia water is used as an electrolyte to prepare the nitrogen-doped petroleum coke-based carbon quantum dots by an electrochemical oxidation method in one step without dialysis desalting purification, the method is efficient and environmentally friendly and yield of the product is high. By the method, carbon quantum dots with stable fluorescence can be rapidly prepared in batch, and the maximum bottleneck of carbon quantum dot application limit is solved. Extensive application of carbon quantum dots in many fields of photoelectric device, ion detection, photocatalysis and the like will be promoted.
Description
Technical field
The invention belongs to petrochemical industry and carbon nanomaterial scientific domain, be specifically related to a kind of simple method that efficiently batch prepares N doping petroleum coke base carbon quantum dot. This method is because eliminating the dialysis step of time-consuming and contaminated environment, therefore the petroleum coke base carbon quantum dot with stable fluorescence can be prepared quickly, in bulk, thus such as the field such as photoelectric device, ion detection, photocatalysis has wide practical use in a lot of fields. The raw material of selection is cheap to be easy to get, and simple to operation, preparation process is environment friendly and pollution-free, has highly important using value.
Background technology
In recent years, the research about quantum dot (Quantumdots is abbreviated as QDs) is very active, particularly in biological and medicine aspect applied research. Traditional QDs is usually to extract from the mixture of plumbous, cadmium and silicon and obtains, and has high toxicity, and the hazardness of environment is very big. Therefore, people are seeking to the QDs substitution material that toxicity is relatively low.
2004, the researcher of South Carolina, USA university synthesizes a kind of novel QDs carbon quantum dot (Carbonquantumdots first, it is abbreviated as CQDs) (JournaloftheAmericanChemicalSociety, 2004,126 (40): 12736-12737). Compared to traditional QDs, CQDs is except the luminescent properties with traditional Q Ds and small size property, also maintain the advantages such as material with carbon element toxicity low, environmental friendliness, good biocompatibility, also have that two photon absorption cross section is big, light emitting region is adjustable simultaneously, good light stability, be prone to extensive preparation and functional modification and the unrivaled advantage such as cheap and easy to get.
Prepare at present the method for CQDs mainly to include laser and corrode method, chemical oxidization method, electrochemical process, ultrasonic method, microwave method etc., the carbon source chosen mainly has that graphite, Graphene, CNT, combustion of natural gas are grey, wax candle is grey and little molecule organic carbon source etc. But, there is the raw material adopted and the defect such as experiment equipment is expensive, preparation flow is consuming time, operating process is complicated or product yield is low in the method reported, and need to carry out desalting purifying, the preparation cost making CQDs remains high and is difficult to prepare a large amount of samples, limits large-scale production and the application of CQDs.Therefore, find raw material cheap and easy to get, eco-friendly, utilize simple efficient method rapid batch to prepare CQDs and there is highly important theory significance and actual application value.
Summary of the invention
Simple High-efficiency one-step batch prepares N doping petroleum coke base carbon quantum dot, it is primarily characterized in that: with petroleum coke for carbon source, ammonia is electrolyte, adopt electrochemical oxidation process, one step prepares nitrogen-doped carbon quantum dot (N-CQDs), and without carrying out the CQDs that desalting purifying, high-efficiency environment friendly and product yield are prepared far above Conventional electrochemical method. With this seminar in 2014 used by chemical oxidization method prepare the method (Carbon, 2014,78 (11): 480-489) of petroleum coke base CQDs and compare, this method clean environment firendly more, simple to operate and reaction temperature and. Compared with the patent of invention (application number: 201510612800.3) of this seminar application in 2015; this method is more rapidly and efficiently; without strong electrolytes such as NaOH; course of reaction generates without salt; therefore without carrying out numerous and diverse dialysis desalination; significantly reduce preparation cost and shorten the operating time, it is possible to realizing scale and prepare. In addition, the present invention is first creatively directly using ammonia as electrolyte, method (the DaltonTrans. of CQDs is relatively prepared using pure water as electrolyte, 2012,41,9526 9531), it is possible to while improving electrolyte conductivity, realize nitrating and response time shortening decades of times.
Concrete preparation method comprises the following steps:
(1) with petroleum coke for carbon source, asphalt is binding agent, and proper proportion mixes, hot-forming, calcines, obtain circular electrode sheet under high temperature.
(2) using prepared electrode slice as working electrode and to electrode, with ammonia spirit for electrolyte, electrolysis 80～480min under 20～40V constant-pressure conditions, obtain the electrolyte containing N-CQDs.
(3) membrane filtration removes big particle diameter carbon granule, then excess of ammonia water is evaporated off, and can obtain the N-CQDs solution of brownish black.
The fluorescence quantum yield (QY) of the made N-CQDs of the present invention adopts conventional reference method to measure, namely under identical shooting condition, record the absorbance of incident illumination under the integrated fluorescence intensities of the reference fluorescent standard substance of testing sample and known QY and same excitation wavelength respectively, substitute into below equation:
In formula, Q is the integration luminous intensity that QY, I are sample of sample, and A is the absorptance of sample, and n is the refractive index of solvent in sample, and R represents standard substance quinine sulfate, uniformly, and QR=54%. IR=635102, AR=0.05925,
The N doping petroleum coke based quantum dot prepared by the present invention has good water solublity, in water dispersed, can directly use, it is also possible to use after preparing into solid by the method such as cold drying, lyophilization, can be widely applied to prepare the field such as C-base composte material, photoelectric device. The present invention realizes scale application for carbon quantum dot and has important value.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure (a) and the grain size distribution (b) of the made petroleum coke base N-CQDs of embodiment 3.
Fig. 2 is ultraviolet-visible absorption spectroscopy (UV-Vis) and the fluorescence emission spectrum under different excitation wavelengths of embodiment 3 made petroleum coke base N-CQDs.
Fig. 3 is UV, visible light UV-Vis spectrum and the fluorescence emission spectrum under different excitation wavelengths of embodiment 5 made petroleum coke base N-CQDs.
Fig. 4 is made petroleum coke base N-CQDs PL comparison diagram under 350nm excitation wavelength when being differential responses.
Detailed description of the invention
It is described as follows according to the detailed description of the invention that technical scheme of the present invention is taked:
Embodiment 1
With petroleum coke for carbon source, Colophonium is as binding agent, and 4:1 ratio mixes, hot-forming, 700 DEG C of calcining 4h, obtains circular electrode sheet. Using prepared electrode slice as working electrode and to electrode, with 150mL2wt% ammonia spirit for electrolyte, electrolysis 480min under 20V constant-pressure conditions, obtain the electrolyte containing N-CQDs. Filtering with microporous membrane is evaporated off excess of ammonia water, can obtain N-CQDs dark brown solution after removing big particle diameter carbon granule. The fluorescence quantum yield (QY) of made CQDs is 0.85%, and yield is 11.4%.
The maximum emission wavelength of the N-CQDs that reaction prepares, at 437nm, demonstrates strong blue-green fluorescent under ultraviolet light.
Embodiment 2
With petroleum coke for carbon source, Colophonium is as binding agent, and 9:1 ratio mixes, hot-forming, 1000 DEG C of calcining 1h, obtains circular electrode sheet. Using prepared electrode slice as working electrode and to electrode, with 150mL8wt% ammonia spirit for electrolyte, electrolysis 360min under 25V constant-pressure conditions, obtain the electrolyte containing N-CQDs. Membrane filtration is evaporated off excess of ammonia water, can obtain N-CQDs dark brown solution after removing big particle diameter carbon granule. The QY of made CQDs is 1.01%, and yield is 7.2%.
The maximum emission wavelength of the N-CQDs that reaction prepares, at 438nm, demonstrates strong blue-green fluorescent under ultraviolet light.
Embodiment 3
With petroleum coke for carbon source, Colophonium is as binding agent, and 7:3 ratio mixes, hot-forming, 900 DEG C of calcining 2h, obtains circular electrode sheet. Using prepared electrode slice as working electrode and to electrode, with 150mL10wt% ammonia spirit for electrolyte, electrolysis 240min under 30V constant-pressure conditions, obtain the electrolyte containing N-CQDs. Membrane filtration is evaporated off excess of ammonia water, can obtain N-CQDs dark brown solution after removing big particle diameter carbon granule. The fluorescence quantum yield (QY) of made CQDs is 1.33%, and yield is 20.0%.
The maximum emission wavelength of the N-CQDs that reaction prepares, at 435nm, demonstrates strong blue-green fluorescent under ultraviolet light. Its TEM figure is as it is shown in figure 1, made N-CQDs spherical, the mono-dispersed nano granule that is class, and between particle size distribution 1.1～2.8nm, mean diameter is 1.66nm. PL under uv-visible absorption spectra figure (UV-Vis) and different excitation wavelength schemes as shown in Figure 2.
Embodiment 4
With petroleum coke for carbon source, Colophonium is as binding agent, and 5:2 ratio mixes, hot-forming, 800 DEG C of calcining 2h, obtains circular electrode sheet. Using prepared electrode slice as working electrode and to electrode, with 150mL5wt% ammonia spirit for electrolyte, electrolysis 180min under 35V constant-pressure conditions, obtain the electrolyte containing N-CQDs. Membrane filtration is evaporated off excess of ammonia water, can obtain N-CQDs dark brown solution after removing big particle diameter carbon granule. The fluorescence quantum yield (QY) of made N-CQDs is 1.47%, and yield is 8.4%.
The maximum emission wavelength of the N-CQDs that reaction prepares, at 443nm, demonstrates strong blue-green fluorescent under ultraviolet light.
Embodiment 5
With petroleum coke for carbon source, Colophonium is as binding agent, and 3:1 ratio mixes, hot-forming, 800 DEG C of calcining 3h, obtains circular electrode sheet. Using prepared electrode slice as working electrode and to electrode, with 150mL15wt% ammonia spirit for electrolyte, electrolysis 80min under 40V constant-pressure conditions, obtain the electrolyte containing N-CQDs.Membrane filtration is evaporated off excess of ammonia water, can obtain N-CQDs dark brown solution after removing big particle diameter carbon granule. The fluorescence quantum yield (QY) of made CQDs is 1.69%, and yield is 14.7%.
The maximum emission wavelength of the N-CQDs that reaction prepares, at 443nm, demonstrates strong blue-green fluorescent under ultraviolet light. PL under uv-visible absorption spectra figure (UV-Vis) and different excitation wavelength schemes as shown in Figure 3. When differential responses, made N-CQDs PL comparison diagram under 350nm excitation wavelength is as shown in Figure 4.
Claims (3)
1. the simple method that efficiently batch prepares N doping petroleum coke base carbon quantum dot, it is characterized in that: first directly using ammonia as electrolyte, electrochemical oxidation process is utilized to prepare nitrogen-doped carbon quantum dot, only with cheap ammonia for electrolyte, a step nitrating can be realized while improving aqueous electrolyte electric conductivity, the maximum feature of the present invention is without carrying out numerous and diverse dialysis desalting purifying and can obtain batch sample, raw material is cheap and easy to get, prepare simple and quick, high-efficiency environment friendly, prepared by the batch that can realize carbon quantum dot, its concrete preparation method is as follows:
(1) with petroleum coke for carbon source, asphalt is binding agent, and proper proportion mixes, hot-forming, calcines, obtain circular electrode sheet under high temperature;
(2) using prepared electrode slice as working electrode and to electrode, with ammonia spirit for electrolyte, electrolysis 80～480min under 20～40V constant-pressure conditions, obtain the electrolyte containing N-CQDs;
(3) membrane filtration removes big particle diameter carbon granule, then excess of ammonia water is evaporated off, and can obtain the N-CQDs solution of brownish black.
2. a kind of simple method that efficiently batch prepares N doping petroleum coke base carbon quantum dot according to claim 1, it is characterized in that: in step (1), petroleum coke is 9:1～3:2 with the mass ratio of asphalt, calcining heat is 700～1000 DEG C, and calcination time is 1～4h.
3. a kind of simple method that efficiently batch prepares N doping petroleum coke base carbon quantum dot according to claim 1, it is characterised in that: in step (2), the concentration of ammonia used is 2～15wt%.
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Cited By (7)
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| CN108996492A (en) * | 2018-08-31 | 2018-12-14 | 中国石油大学(北京) | A kind of petroleum liquid product base graphene quantum dot and its preparation method and application |
| CN110589813A (en) * | 2019-10-08 | 2019-12-20 | 杭州高烯科技有限公司 | Preparation method of three-dimensional graphene |
| CN110660593A (en) * | 2019-10-08 | 2020-01-07 | 浙江大学 | Preparation method of capacitor |
| CN110655829A (en) * | 2019-10-08 | 2020-01-07 | 浙江大学 | Preparation method of graphene carbon dot-based ink |
| CN112569997A (en) * | 2019-09-30 | 2021-03-30 | 中国石油化工股份有限公司 | Nano nitrogen-carbon material, preparation method thereof and catalytic oxidation method of cycloparaffin |
| CN113372895A (en) * | 2021-06-23 | 2021-09-10 | 中国石油大学(华东) | Crude oil expansion oil displacement agent and preparation method and application thereof |
| CN114256420A (en) * | 2021-12-24 | 2022-03-29 | 华荣照明有限公司 | Preparation method of carbon quantum dot, carbon quantum dot and application of carbon quantum dot in OLED |
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Cited By (11)
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| CN112569997A (en) * | 2019-09-30 | 2021-03-30 | 中国石油化工股份有限公司 | Nano nitrogen-carbon material, preparation method thereof and catalytic oxidation method of cycloparaffin |
| CN112569997B (en) * | 2019-09-30 | 2023-03-10 | 中国石油化工股份有限公司 | Nano nitrogen-carbon material, preparation method thereof and catalytic oxidation method of cycloparaffin |
| CN110589813A (en) * | 2019-10-08 | 2019-12-20 | 杭州高烯科技有限公司 | Preparation method of three-dimensional graphene |
| CN110660593A (en) * | 2019-10-08 | 2020-01-07 | 浙江大学 | Preparation method of capacitor |
| CN110655829A (en) * | 2019-10-08 | 2020-01-07 | 浙江大学 | Preparation method of graphene carbon dot-based ink |
| CN113372895A (en) * | 2021-06-23 | 2021-09-10 | 中国石油大学(华东) | Crude oil expansion oil displacement agent and preparation method and application thereof |
| CN113372895B (en) * | 2021-06-23 | 2022-06-28 | 中国石油大学(华东) | Crude oil expansion oil displacement agent and preparation method and application thereof |
| CN114256420A (en) * | 2021-12-24 | 2022-03-29 | 华荣照明有限公司 | Preparation method of carbon quantum dot, carbon quantum dot and application of carbon quantum dot in OLED |
| CN114256420B (en) * | 2021-12-24 | 2022-08-30 | 华荣照明有限公司 | Preparation method of carbon quantum dot, carbon quantum dot and application of carbon quantum dot in OLED |
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Application publication date: 20160615 |