CN107418567B - Biomass-based carbon quantum dot and preparation method thereof - Google Patents
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Abstract
The invention discloses a biomass-based carbon quantum dot and a preparation method thereof, and belongs to the technical field of carbon quantum dot preparation. The preparation method comprises the following steps: mixing the shell material and the activating agent with water, and drying to obtain a dipping sample; carbonizing the impregnated sample to obtain a carbonized sample; soaking the carbonized sample in water, filtering, adjusting the pH value of the filtrate to be less than or equal to 3, filtering again, dialyzing the filtrate, and freeze-drying to obtain the biomass-based carbon quantum dots; wherein the activating agent is KOH, NaOH or K2CO3、KHCO3、Na2CO3And NaHCO3One or more of them. The preparation method has the advantages of simple preparation process, green and environment-friendly raw materials, low price and easy obtainment, and the prepared carbon quantum dots have small sizes and uniform particle size distribution.
Description
Technical Field
The invention belongs to the technical field of carbon quantum dot preparation, and particularly relates to a biomass-based carbon quantum dot and a preparation method thereof.
Background
The practical application of the traditional semiconductor quantum dots is limited due to self-generated toxicity and harm to the environment. Compared with the prior art, the emerging fluorescent carbon quantum dot not only inherits the excellent optical performance of the traditional semiconductor quantum dot, but also has the characteristics of excellent biocompatibility, low toxicity, chemical inertness and the like, so that the fluorescent carbon quantum dot has important application potential in the aspects of in vivo and in vitro living body biological imaging, fluorescent labeling, drug delivery, environmental metal ion fluorescent probes, organic pollutant degradation and photocatalytic water splitting hydrogen production photocatalysts, biosensors, photoelectric devices and the like.
The reported methods for preparing carbon quantum dots can be divided into two major categories, top-down and bottom-up. From top to bottom, the method is to treat carbon-based materials with larger sizes, such as graphene, carbon nanotubes, activated carbon, candle burning ash and the like, by means of arc discharge, laser ablation, electrochemical oxidation, chemical oxidation and the like, and then strip out the small-sized carbon quantum dots. From bottom to top, the carbon quantum dots are prepared from small molecule precursors such as saccharides, organic acids, alcohols and the like through a polymerization carbonization process by means of a hydrothermal method, thermal decomposition, microwave heating, electrochemical carbonization and the like.
At present, most of raw materials used in the methods are non-renewable resources, and the raw materials are obtained by a complex process and have high cost. Therefore, more and more people pay attention to the preparation of the carbon quantum dots by using the biomass which is cheap, easy to obtain, natural, non-toxic and environment-friendly as the raw material.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of biomass-based carbon quantum dots, so as to solve the problems of complex process, high cost and environmental pollution in the prior art.
The invention also aims to provide the biomass-based carbon quantum dot which is small in size, uniform in particle size distribution, simple in preparation process, low in cost, green and pollution-free.
The technical scheme for solving the technical problems is as follows:
a preparation method of biomass-based carbon quantum dots comprises the following steps:
mixing the shell material and the activating agent with water, and drying to obtain a dipping sample;
carbonizing the impregnated sample to obtain a carbonized sample; and
soaking the carbonized sample in water, filtering, adjusting the pH value of the filtrate to be less than or equal to 3, filtering again, and dialyzing the filtrate to obtain the biomass-based carbon quantum dots;
wherein the activating agent is KOH, NaOH or K2CO3、KHCO3、Na2CO3And NaHCO3One or more of them.
Before carbonization, the preparation method adds water to the shell material and the activator to mix and prepare the mixture into an impregnation sample, so that the activator enters the lignocellulose of the shell in advance, thereby being beneficial to forming uniform activation point positions in the subsequent carbonization stage and being beneficial to generating carbon quantum dots. In particular, due to the activators KOH and NaOH, and the activator K2CO3、KHCO3、Na2CO3And NaHCO3The hydrolysis product can generate KOH and NaOH after hydrolysis, so that part of the structure of the lignin is damaged, and more activating agents penetrate into the shell material to react with cellulose and hemicellulose. K+(Na+) Or CO3 2-Can weaken molecular action between polymers, reduce activation energy of pyrolysis reaction and promote the decomposition of polymers into small molecules. At the same time, KOH or NaOH can further react with the hydroxyl of lignocellulose to obtain active functional groups such as "-OK (Na)". And the active groups can react with benzene ring and' -CH2The hydrogen atoms of the-groups react to form a "C-C" cross-linked structure. Therefore, the introduction of the activating agent changes the carbonization behavior of the shell material, thereby reducing the reaction temperature of carbonization and shortening the reaction time.
Before dialysis, the pH value of the filtrate obtained after soaking the carbonized sample in water is adjusted to be less than or equal to 3, so that the lignin in the filtrate is removed, and the purity of the subsequent carbon quantum dots is improved.
Further, in a preferred embodiment of the present invention, the mass ratio of the shell material to the activator is (0.5-5): 1.
further, in the preferred embodiment of the present invention, the impregnated sample is carbonized at 150-350 ℃ for 1-5h in the preparation of the carbonized sample.
Further, in a preferred embodiment of the invention, the filtrate is dialyzed using a dialysis bag with a molecular weight cut-off of 300-.
Further, in the preferred embodiment of the invention, the preparation method further comprises cleaning the fruit shell material, pulverizing, sieving, and drying the undersize product at 80-110 deg.C to obtain the fruit shell material, before mixing the fruit shell material with the activating agent in water.
The biomass-based carbon quantum dot prepared by the preparation method is adopted.
Further, in a preferred embodiment of the present invention, the particle size of the biomass-based carbon quantum dot is 1 to 5 nm.
The invention has the following beneficial effects:
the invention uses reproducible fruit shell as raw material, is cheap and easy to obtain, has low whole reaction temperature, simple preparation process and short reaction time, and the prepared carbon quantum dots have small size and uniform particle size distribution.
Drawings
FIG. 1 is a Transmission Electron Microscope (TEM) image of a carbon quantum dot obtained in example 1;
FIG. 2 is a high-resolution transmission electron microscope (HRTEM) image of the carbon quantum dots obtained in example 1;
FIG. 3 is fluorescence spectra of carbon quantum dots obtained in example 1 at different excitation wavelengths;
FIG. 4 is a photograph of the carbon quantum dots obtained in example 1 under 365nm ultraviolet light irradiation.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
Cleaning, crushing and sieving the peanut shells, and drying the peanut shells at 85 ℃ according to the mass ratio of the peanut shells: k2CO35: 3 adding a proper amount of water, mixing, and drying at 105 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 300 ℃ for 2h to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, and filteringFiltering, adding acid into the filtrate to adjust pH to 1, filtering, and dialyzing the filtrate for 24h with a dialysis bag of 1000Da to obtain light yellow carbon quantum dot aqueous solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
FIG. 1 is a Transmission Electron Microscope (TEM) image, and it can be seen from FIG. 1 that the carbon quantum dots prepared in this example have uniform particle size ranging from 1nm to 5 nm. Fig. 2 is a High Resolution Transmission Electron Microscope (HRTEM) image of the carbon quantum dot of the present embodiment, which has a lattice stripe texture and a interplanar spacing of about 0.21nm, and illustrates that the carbon quantum dot has a certain crystallinity and belongs to a graphite type. FIG. 3 is a graph showing fluorescence spectra at different excitation wavelengths, with features that change as the excitation wavelength changes. FIG. 4 is a photograph of the carbon quantum dot of this example under 365nm UV light, from which it can be clearly seen that the aqueous solution of the prepared carbon quantum dot exhibits blue fluorescence.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 2
Cleaning, crushing and sieving the peanut shells, and drying the peanut shells at 85 ℃ according to the mass ratio of the peanut shells: k2CO35: 1, adding a proper amount of water, mixing, and drying at 105 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 250 ℃ for 3h to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 1, filtering, and dialyzing the filtrate with 1000Da dialysis bag for 24 hr to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 3
Cleaning, crushing and sieving the peanut shells, and drying at 105 ℃, wherein the peanut shells are prepared from the following raw materials in percentage by mass: k2CO35: 10, adding a proper amount of water, mixing, and drying at 105 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 350 ℃ for 1h to obtain a carbonized sample. Soaking carbonized sample in appropriate amount of water, stirring, filtering, and filteringAdding acid into the solution to adjust pH to 1, filtering, and dialyzing the filtrate for 24h with a dialysis bag of 1000Da to obtain light yellow carbon quantum dot aqueous solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 4
Cleaning, crushing and sieving the peanut shells, and drying at 105 ℃, wherein the peanut shells are prepared from the following raw materials in percentage by mass: k2CO35: 4 adding a proper amount of water, mixing, and drying at 105 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 150 ℃ for 5 hours to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 1, filtering, and dialyzing the filtrate with 1000Da dialysis bag for 24 hr to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 5
Cleaning, crushing and sieving the peanut shells, and drying the peanut shells at 85 ℃ according to the mass ratio of the peanut shells: NaOH 5: 2 adding a proper amount of water, mixing, and drying at 105 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 250 ℃ for 3h to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 1, filtering, and dialyzing the filtrate with 1000Da dialysis bag for 24 hr to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 6
Cleaning, crushing and sieving the peanut shells, and drying the peanut shells at 85 ℃ according to the mass ratio of the peanut shells: KHCO35: 2 adding a proper amount of water, mixing, and drying at 105 ℃ to obtain a dipping sample. Placing the impregnated sample in a reaction furnace, and carbonizing at 250 deg.C for 3 hr to obtain carbonAnd (6) sample preparation. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 1, filtering, and dialyzing the filtrate with 1000Da dialysis bag for 24 hr to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 7
Cleaning, crushing and sieving the peanut shells, and drying the peanut shells at 80 ℃, wherein the peanut shells are prepared from the following raw materials in percentage by mass: na (Na)2CO31: 2 adding a proper amount of water, mixing, and drying at 110 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 210 ℃ for 3.5 hours to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 2, filtering, and dialyzing the filtrate with 300Da dialysis bag for 25 hr to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 8
Cleaning, crushing and sieving the oil-tea camellia shells, and drying at 110 ℃, wherein the oil-tea camellia shells are peanut shells according to the mass ratio: NaHCO 231.25: 1, adding a proper amount of water, mixing, and drying at 100 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 280 ℃ for 4h to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 3, filtering, and dialyzing the filtrate with 500Da dialysis bag for 24.5h to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
Example 9
Cleaning, crushing and sieving chestnut shells, drying at 110 ℃, and preparing the peanut shells according to the mass ratio: (Na)2CO3+NaHCO3)＝2.5: 1, adding a proper amount of water, mixing, and drying at 90 ℃ to obtain a dipping sample. And (3) putting the impregnated sample into a reaction furnace, and carbonizing at 320 ℃ for 1.2h to obtain a carbonized sample. Soaking the carbonized sample in appropriate amount of water, stirring, filtering, adding acid into the filtrate to adjust pH to 0.5, filtering, and dialyzing the filtrate with 500Da dialysis bag for 24 hr to obtain light yellow carbon quantum dot water solution. The carbon quantum dot aqueous solution is kept still for more than 8 weeks, no insoluble substances are separated out, and the fluorescence intensity is basically kept unchanged.
And (3) freeze-drying the carbon quantum dot aqueous solution to obtain the biomass-based carbon quantum dot.
It should be noted that the shell for preparing the carbon quantum dots according to the present invention is not limited to the above-mentioned examples, and may be a shell of a fruit or a seed of a nut, a vegetable, and a fruit, and the present invention is not limited thereto.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. A preparation method of biomass-based carbon quantum dots is characterized by comprising the following steps:
mixing the shell material and the activating agent with water, and drying to obtain a dipping sample; the mass ratio of the shell material to the activating agent is (0.5-5): 1;
carbonizing the impregnated sample to obtain a carbonized sample; and
soaking the carbonized sample in water, filtering, adjusting the pH value of the filtrate to be less than or equal to 3, filtering again, dialyzing the filtrate, and freeze-drying to obtain the biomass-based carbon quantum dots;
wherein the activating agent is KOH, NaOH or K2CO3、KHCO3、Na2CO3And NaHCO3One or more of the above; when preparing the carbonized sample, carbonizing the impregnated sample at 150-350 ℃ for 1-5 h.
2. The method for preparing biomass-based carbon quantum dots according to claim 1, wherein the filtrate is dialyzed by a dialysis bag with a molecular weight cut-off of 300-1000 Da.
3. The biomass-based carbon quantum dot prepared by the preparation method of any one of claims 1-2.
4. The biomass-based carbon quantum dot of claim 3, wherein the biomass-based carbon quantum dot has a particle size of 1-5 nm.
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| CN110194953A (en) * | 2019-06-27 | 2019-09-03 | 上海大学 | Biomass-based fluorescent carbon quantum dot, preparation method and application |
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| CN110437830A (en) * | 2019-08-26 | 2019-11-12 | 济南大学 | It is a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot |
| CN110437829A (en) * | 2019-08-26 | 2019-11-12 | 济南大学 | A kind of preparation method of polynary nonmetalloid codope carbon quantum dot |
| CN113289581B (en) * | 2021-06-16 | 2022-10-25 | 华南理工大学 | Lignin-based hierarchical porous carbon for rapidly purifying dye wastewater and preparation method thereof |
| CN113247882B (en) * | 2021-06-25 | 2022-11-18 | 赣南医学院 | Preparation and application of oil-tea meal-based carbon dots |
| CN114604870A (en) * | 2022-02-24 | 2022-06-10 | 南京智汇环境气象产业研究院有限公司 | Method for preparing foam carbon material from wood block |
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