CN114634815B - Preparation method of lignin carbon quantum dots - Google Patents
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Abstract
The application provides a preparation method of lignin carbon quantum dots, which takes waste biomass resources to carry out enzymolysis on lignin as a carbon source, introduces different types of organic acids to catalyze and modify on the basis of preparing lignin-based carbon quantum dots by an original hydrothermal method, and effectively improves the fluorescence intensity and fluorescence quantum yield of the lignin carbon quantum dots. Compared with the unmodified lignin-based carbon quantum dot, the carbon quantum dot obtained by using different types of organic acid to catalyze and hydrolyze lignin by adopting the technology can improve the fluorescence intensity by 3-9 times, the fluorescence quantum yield is improved to 14.9%, and the particle size of the carbon quantum dot is reduced to 1.9nm. In addition, the application adopts the design concept of replacing traditional resources with waste biomass, thereby not only reducing the use of harmful chemicals such as strong acid, strong alkali and the like, but also realizing the full utilization of waste biomass resources, reducing the preparation cost of the carbon quantum dots and having strong competitiveness in the market.
Description
Technical Field
The application belongs to the field of carbon materials, and particularly relates to a preparation method of lignin carbon quantum dots.
Background
With the development of science, a sufficient research is provided to understand the existence of different forms of carbon, and some novel carbon materials are continuously developed, and recently, in the nanotechnology era, carbon-based nanomaterials have also been developed. The emerging carbon quantum dots are novel zero-dimensional photoluminescent fluorescent carbon nano materials with diameters smaller than 10nm and quasi-spherical. Carbon quantum dots are currently of particular interest because of their excellent water solubility, low toxicity, unique photoluminescent properties, and ease of surface functionalization. The unique photoluminescence characteristics of the carbon quantum dots enable the carbon quantum dots to be widely applied to the fields of biosensing, ion detection, photoelectrocatalysis, food quality analysis, anti-counterfeiting and the like, and the carbon quantum dots are considered as a very promising substitute material.
Biomass renewable resources widely existing in nature are used as precursors for preparing biomass carbon quantum dots, so that the raw material cost in the preparation process of the carbon quantum dots can be effectively reduced, the high-quality recycling of waste resources is realized, and the biomass carbon quantum dots generally have excellent biocompatibility and stable fluorescence emission. At present, preparation of various types of biomass carbon quantum dots has been realized, but compared with carbon quantum dots synthesized by traditional small molecular compounds (such as citric acid, ethylenediamine, glucose and the like), most biomass carbon quantum dots have the problems of weak fluorescence intensity and low fluorescence quantum yield, so that application of the biomass carbon quantum dots is limited. Therefore, the realization of efficient preparation and deep functional application of the high-yield biomass carbon quantum dots is a key problem to be solved in the development process of the biomass carbon quantum dots at present.
Disclosure of Invention
The application aims to provide a preparation method of lignin carbon quantum dots, which improves the fluorescence intensity and fluorescence quantum yield of the carbon quantum dots.
The technical scheme for realizing the purpose of the application comprises the following steps:
the preparation method of the lignin carbon quantum dot comprises the following steps:
(1) Purifying waste enzymatic hydrolysis lignin residues, uniformly mixing the purified enzymatic hydrolysis lignin powder with deionized water according to the mass ratio of 1:10-40, adding organic acid accounting for 10-40 wt% of the enzymatic hydrolysis lignin powder, uniformly stirring by ultrasonic waves, and then carrying out hydrothermal reaction on the mixed solution in a reaction kettle, wherein the hydrothermal time is 8-24 h, the hydrothermal temperature is 180-260 ℃, and the organic acid is one or more than two kinds of carboxylic acid such as citric acid, DL-malic acid, oxalic acid, palmitic acid, tartaric acid and the like; the organic acid not only provides acidic conditions for the hydrothermal system, but also effectively promotes the hydrolysis of biomass resources; meanwhile, the synergistic effect among a plurality of organic acids is superior to that of one organic acid. In addition, the organic acid can also serve as a second carbon source to provide a part of carbon source for hydrothermal carbonization, so that the fluorescence intensity of the carbon quantum dots is improved.
(2) Filtering the mixed solution after the hydrothermal reaction to remove insoluble carbon;
(3) Dialyzing the filtrate after suction filtration in a dialysis bag with the molecular weight cut-off of 400-600 Da for 40-60 hours, and changing deionized water every 5-8 h to remove unreacted micromolecules;
(4) And (3) pre-freezing the dialyzed solution at-20 to-25 ℃ for 10-15 hours, then placing the solution in a vacuum freeze dryer for compression of 15-25 MPa and freeze drying at-55 to-70 ℃ for 2-4 days, and finally obtaining lignin-based carbon quantum dot powder.
Preferably, the organic acid is citric acid, tartaric acid and DL-malic acid, and the mass ratio is 1:1: 1. The surface of the carbon quantum dot modified by the mixed acid has rich carboxyl functional groups, and the carboxyl functional groups can generate more defect sites on the surface of the carbon quantum dot to play a role of excitation energy traps, and fluorescence emission is from radiation recombination of excitons captured by defects.
Preferably, the organic acid accounting for 10 to 20 weight percent of the mass of the enzymolysis lignin powder is added. And a proper amount of organic acid accelerates hydrolysis of enzymolysis lignin, promotes hydrothermal reaction, and produces the carbon quantum dots with good water solubility, uniform size distribution and high yield. And excessive addition of the organic acid can cause agglomeration of part of carbon quantum dots, so that the fluorescence intensity is reduced.
Preferably, the enzymatic hydrolysis lignin residue in the step (1) is enzymatic hydrolysis residue of poplar, oak, fir or corn stalk biomass waste. The present application is not limited to these types of biomass as biomass is widely found in nature and is largely discarded as waste. The components such as cellulose and hemicellulose in the biomass can be efficiently utilized after hydrolysis, and the hydrolyzed lignin can be further utilized as a carbon precursor, so that high-value utilization of wastes is realized.
Preferably, the purification is carried out by an alkali-based acid precipitation method. The alkali dissolution and acid precipitation method is used for purifying lignin, and has simple operation and high extraction rate.
Preferably, the mass ratio of the enzymatic hydrolysis lignin powder to the deionized water is 1:20-30.
Preferably, the hydrothermal time is 10-15 h, and the hydrothermal temperature is 200-240 ℃.
Preferably, the molecular weight cut-off is 500Da and the dialysis time is 48 hours, during which the water is changed every 6 hours.
Preferably, the solution after dialysis is pre-frozen at-22 ℃ for 12 hours, and then is placed in a vacuum freeze dryer under the pressure of 20MPa, and the temperature is-60 ℃ for freeze drying for 3 days.
According to the application, waste biomass enzymolysis lignin is used as a carbon precursor, different types of organic acids are added for modification, and the carbon quantum dots with bright blue fluorescence are synthesized by a one-step hydrothermal method. The particle size distribution of the unmodified lignin carbon quantum dots is wider, and the fluorescence intensity is weaker. The particle size of the carbon quantum dots prepared by modifying lignin with organic acid is reduced, the size distribution is narrow, and the fluorescence intensity and fluorescence quantum yield are also improved to a great extent.
The application has the advantages and positive effects that:
according to the application, waste biomass is adopted to replace traditional carbon resources, and one or more organic acids are directly introduced to modify and prepare the carbon quantum dots on the basis of synthesizing lignin carbon quantum dots by an original one-step hydrothermal method. The fluorescence intensity of the carbon quantum dot prepared by the method can be improved by 3-9 times, the quantum yield is improved to 14.9% from 0.8%, and the particle size is reduced to 1.9nm from 6.2nm. The technology realizes the efficient utilization of waste biomass, and the modification method is simple, convenient and effective.
Drawings
FIG. 1 is a flow chart of the method of the present application;
FIG. 2 (a) is a photograph of an aqueous lignin-based carbon quantum dot solution under sunlight;
FIG. 2 (b) is a photograph of an aqueous lignin-based carbon quantum dot solution under ultraviolet irradiation;
FIG. 3 is a transmission electron microscope image of lignin-based carbon quantum dots;
FIG. 4 is a graph showing fluorescence spectra of carbon quantum dots modified with different organic acids.
Detailed Description
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The application will be described in detail below with reference to the drawings in connection with embodiments.
Comparative example 1:
the purified biomass enzymolysis lignin powder and deionized water are uniformly mixed according to the mass ratio of 1:25 (raw materials: 2g, 50mL of deionized water), and are ultrasonically stirred for 30min. And then placing the uniformly stirred mixed solution into a 100mL high-pressure reaction kettle, and placing the mixture into a 240 ℃ oven for hydrothermal reaction for 12 hours. And filtering the mixed solution after the hydrothermal reaction is finished to remove insoluble carbon. The filtrate after suction filtration was dialyzed in a dialysis bag with a molecular weight cut-off of 500Da for 48 hours, with water being changed every 6 hours. And then, placing the dialyzed carbon quantum dot solution into a vacuum freeze dryer for pre-freezing for 12 hours at the temperature of minus 22 ℃, placing the carbon quantum dot solution into the vacuum freeze dryer for freeze drying for 3 days at the vacuum pressure of 20MPa, and finally obtaining lignin-based carbon quantum dot powder (EHL CQDs).
The prepared EHL CQDs can emit short-wavelength blue fluorescence at 453nm under excitation of 360nm, and have certain excitation dependence and good water solubility. The image under the transmission electron microscope can observe that the carbon quantum dots are spherical, and the average particle size is 6.2nm. However, the fluorescence intensity and fluorescence quantum yield were not high, and the quantum yield of EHL CQDs was only 0.8%.
The preparation flow of lignin-based carbon quantum dots is shown in figure 1; the aqueous solution of the carbon quantum dots has obvious blue fluorescence under the irradiation of ultraviolet light, and is shown in the figure 2 (b); and a transmission electron microscope image of the lignin-based carbon quantum dot is shown in fig. 3.
Example 1
Uniformly mixing the purified biomass resource enzymolysis lignin powder with deionized water according to a mass ratio of 1:25 (raw materials: 2g, deionized water 50 mL), adding 0.3g of citric acid, and stirring for 30min by ultrasonic. And then placing the uniformly stirred mixed solution into a 100mL high-pressure reaction kettle, and placing the mixture into a 240 ℃ oven for hydrothermal reaction for 12 hours. And filtering the mixed solution after the hydrothermal reaction is finished to remove insoluble carbon. And (3) putting the filtrate after suction filtration into a dialysis bag with the molecular weight cut-off of 500Da for dialysis for 48 hours, and changing deionized water every 6 hours to remove unreacted micromolecules. And then, placing the dialyzed carbon quantum dot solution into a vacuum freeze dryer for pre-freezing for 12 hours at the temperature of minus 22 ℃, and then, placing the dialyzed carbon quantum dot solution into the vacuum freeze dryer for freeze drying for 3 days at the temperature of minus 60 ℃ under the vacuum pressure of 20MPa, thereby finally obtaining the citric acid modified carbon quantum dots (CA-EHL CQDs).
The prepared CA-EHL CQDs can emit short-wavelength blue fluorescence at 452nm under excitation of 360nm, and have certain excitation dependence and good water solubility. The average particle diameter was 3.5nm, and the size distribution was narrow. The fluorescence intensity of the CA-EHL CQDs is obviously improved, which is 3.3 times of that of the EHL CQDs, and the quantum yield is 4.1 percent.
Example 2
Uniformly mixing the purified biomass resource enzymolysis lignin powder with deionized water according to a mass ratio of 1:25 (raw materials: 2g, deionized water 50 mL), adding 0.15g of citric acid and 0.15g of tartaric acid, and stirring for 30min by ultrasonic. And then placing the uniformly stirred mixed solution into a 100mL high-pressure reaction kettle, and placing the mixture into a 240 ℃ oven for hydrothermal reaction for 12 hours. And filtering the mixed solution after the hydrothermal reaction is finished to remove insoluble carbon. The filtrate after suction filtration is put into a dialysis bag with the molecular weight cut-off of 500Da for dialysis for 48 hours, and water is changed every 6 hours. And then, the dialyzed carbon quantum dot solution is placed in a vacuum freeze dryer for pre-freezing for 12 hours at the temperature of minus 22 ℃, and then is placed in the vacuum freeze dryer for freeze drying for 3 days at the temperature of minus 60 ℃ under the vacuum pressure of 20MPa, so that the carbon quantum dots (CA/TA-EHL CQDs) modified by the combined action of citric acid and tartaric acid are finally obtained.
The prepared CA/TA-EHL CQDs can emit blue fluorescence with the short wavelength of 454nm under the excitation of 360nm, and have certain excitation dependence and good water solubility. The average particle diameter was 2.8nm, and the size distribution was narrow. The fluorescence intensity of the CA/TA-EHL CQDs is obviously improved, 5.3 times of that of the EHL CQDs, and the quantum yield is 7.8%.
Example 3
Uniformly mixing the purified biomass resource enzymolysis lignin powder with deionized water according to a mass ratio of 1:25 (raw materials: 2g, deionized water 50 mL), adding 0.1g of citric acid, 0.1g of tartaric acid and 0.1g of gDL-malic acid, and ultrasonically stirring for 30min. And then placing the uniformly stirred mixed solution into a 100mL high-pressure reaction kettle, and placing the mixture into a 240 ℃ oven for hydrothermal reaction for 12 hours. And filtering the mixed solution after the hydrothermal reaction is finished to remove insoluble carbon. The filtrate after suction filtration was dialyzed in a dialysis bag having a molecular weight cut-off of 500Da for 48 hours, with water being changed every 6 hours. And then, the dialyzed carbon quantum dot solution is placed in a vacuum freeze dryer for pre-freezing for 12 hours at the temperature of minus 22 ℃, and then, the dialyzed carbon quantum dot solution is placed in the vacuum freeze dryer for freeze drying for 3 days at the temperature of minus 60 ℃ and the vacuum pressure of 20MPa, so that the three organic acid modified carbon quantum dots (CA/TA/MA-EHL CQDs) are finally obtained.
The prepared CA/TA/MA-EHL CQDs can emit 448nm short-wavelength blue fluorescence under excitation of 360nm, and have certain excitation dependence and good water solubility. The average particle diameter was 1.9nm, and the size distribution was narrow. The fluorescence intensity of the CA/TA/MA-EHL CQDs is obviously improved, which is 8.73 times that of the EHL CQDs, and the quantum yield is 14.9%.
Example 4
The purified biomass resource enzymatic hydrolysis lignin powder is uniformly mixed with deionized water in a ratio of 1:25 (raw materials: 2g, deionized water 50 mL), and then 0.1g of citric acid, 0.1g of oxalic acid and 0.1g of palmitic acid are added, and the mixture is ultrasonically stirred for 30min. And then placing the uniformly stirred mixed solution into a 100mL high-pressure reaction kettle, and placing the mixture into a 240 ℃ oven for hydrothermal reaction for 12 hours. And filtering the mixed solution after the hydrothermal reaction is finished to remove insoluble carbon. The filtrate after suction filtration was dialyzed in a dialysis bag with a molecular weight cut-off of 500Da for 48 hours, with water being changed every 6 hours. And then, the dialyzed carbon quantum dot solution is placed in a vacuum freeze dryer for pre-freezing for 12 hours at the temperature of minus 22 ℃, and then, the dialyzed carbon quantum dot solution is placed in the vacuum freeze dryer for freeze drying for 3 days at the temperature of minus 60 ℃ and the vacuum pressure of 20MPa, so that three organic acid modified carbon quantum dots (CA/OA/PA-EHL CQDs) are finally obtained.
The prepared CA/OA/PA-EHL CQDs can emit blue fluorescence with the short wavelength of 455nm under the excitation of 360nm wavelength, and have certain excitation dependence and good water solubility. The average particle diameter was 2.4nm, and the size distribution was narrow. The fluorescence intensity of the CA/OA/PA-EHL CQDs is obviously improved, 6.32 times of that of the EHL CQDs, and the quantum yield is 10.7%.
As shown in FIG. 4, compared with unmodified lignin-based carbon quantum dots, the carbon quantum dots prepared by catalyzing and hydrolyzing lignin with different organic acids have obviously improved fluorescence intensity and quantum yield. The organic acid not only provides an acidic condition for the hydrothermal system to effectively promote the hydrolysis of biomass resources, but also can serve as a second carbon source to provide a part of carbon source for hydrothermal carbonization, so that the fluorescence intensity of the carbon quantum dots is improved. In addition, the synergistic effect among a plurality of organic acids is superior to that of one acid. The synergistic effect between the mixed acids can effectively promote the hydrolysis of biomass materials and the hydrothermal reaction, so that the fluorescence intensity of the carbon quantum dots is further improved. Wherein, CA/TA/MA-EHL CQDs prepared by jointly catalyzing and hydrolyzing lignin by citric acid, tartaric acid and DL-malic acid have smaller particle size, better fluorescence effect and higher fluorescence quantum yield. This is because the three organic acids have better synergistic effect, can promote the hydrolysis of biomass materials, and the carbonization degree of the carbon quantum dots is improved. In addition, the CA/TA/MA-EHL CQDs surface has rich carboxyl functional groups, the carboxyl functional groups can generate more defect sites on the surface of the carbon quantum dots to play a role of excitation energy traps, and fluorescence emission is recombined from radiation of excitons captured by the defects. In conclusion, citric acid, tartaric acid and DL-malic acid together catalyze and hydrolyze lignin to prepare the carbon quantum dot with high fluorescence intensity and high quantum yield.
While the application has been described in detail with respect to the general description and specific embodiments thereof, it will be apparent to those skilled in the art that various modifications and improvements can be made thereto. Accordingly, all such modifications and improvements may be made without departing from the spirit of the application as set forth in the following claims.
Claims (8)
1. The preparation method of the lignin carbon quantum dot comprises the following steps:
(1) Purifying waste enzymolysis lignin residues, uniformly mixing the purified enzymolysis lignin powder with deionized water according to the mass ratio of 1:10-40, adding organic acid accounting for 10-40 wt% of the mass of the enzymolysis lignin powder, carrying out hydrothermal reaction on the mixed solution in a reaction kettle after ultrasonic stirring uniformly, wherein the hydrothermal time is 8-24 h, the hydrothermal temperature is 180-260 ℃, and the mass ratio of the organic acid to the citric acid, the tartaric acid and the DL-malic acid is 1:1: 1;
(2) Filtering the mixed solution after the hydrothermal reaction to remove insoluble carbon;
(3) Dialyzing the filtrate after suction filtration in a dialysis bag with the molecular weight cut-off of 400-600 Da for 40-60 hours, and changing deionized water every 5-8 hours to remove unreacted micromolecules;
(4) And (3) pre-freezing the dialyzed solution at-20 to-25 ℃ for 10-15 hours, then placing the solution in a vacuum freeze dryer for compression of 15-25 MPa and freeze drying at-55 to-70 ℃ for 2-4 days, and finally obtaining lignin-based carbon quantum dot powder.
2. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: adding organic acid accounting for 10-20wt% of the mass of the enzymolysis lignin powder.
3. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: the enzymatic hydrolysis lignin residues in the step (1) are enzymatic hydrolysis residues of poplar, oak, fir or corn straw biomass waste.
4. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: the purification adopts an alkali-dissolution and acid-precipitation method.
5. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: the mass ratio of the enzymatic hydrolysis lignin powder to the deionized water is 1:20-30.
6. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: the hydrothermal time is 10-15 h, and the hydrothermal temperature is 200-240 ℃.
7. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: the molecular weight cut-off was 500Da and the dialysis time was 48 hours, during which water was changed every 6 hours.
8. The method for preparing lignin carbon quantum dots according to claim 1, wherein the method comprises the following steps: the solution after dialysis is placed at the temperature of minus 22 ℃ for pre-freezing for 12 hours, and then placed in a vacuum freeze dryer for freeze drying for 3d at the temperature of minus 60 ℃ under the pressure of 20 MPa.
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| CN103756675A (en) * | 2014-01-17 | 2014-04-30 | 西安亚博生物技术有限公司 | Nitrogen doped carbon quantum dot as well as preparation method and application thereof |
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| CN110437826A (en) * | 2019-07-26 | 2019-11-12 | 华南理工大学 | A kind of lignin-base carbon dots of high-fluorescence quantum yield and preparation method thereof |
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