CN112499616B - Method for synthesizing fluorescent carbon quantum dots by taking marine product deep processing wastewater as raw material - Google Patents
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Abstract
The invention discloses a method for synthesizing fluorescent carbon quantum dots by taking marine product deep processing wastewater as a raw material, which comprises the steps of taking marine product deep processing wastewater as a raw material, adding deionized water or ultrapure water into a reaction container, carrying out microwave reaction in a microwave oven, adding deionized water and carrying out ultrasonic dispersion to obtain a fluorescent carbon quantum dot crude product; filtering the crude product by a filter membrane, and dialyzing by a dialysis bag to obtain a purified product of the fluorescent carbon quantum dots; the marine product deep processing wastewater is rich in protein and amino acid. The method takes the deep processing wastewater of the biomass waste marine products as a carbon source, does not need to add other reagents, and fully utilizes the NH rich in the deep processing wastewater 3 And the-N and the like realize the doping of the carbon quantum dots by the heteroatoms, so that the fluorescent carbon quantum dots are prepared. The method is simple to operate, green and environment-friendly, and the obtained carbon quantum dots are uniformly dispersed and controllable in morphology. In a word, the method has low cost, is convenient and quick, is easy for industrial production, can be used in various fields, and also solves the problem of deep processing wastewater of marine products.
Description
Technical Field
The invention belongs to the technical field of carbon quantum dot synthesis, and particularly relates to a method for synthesizing fluorescent carbon quantum dots by taking marine product deep processing wastewater as a raw material.
Background
The deep processing of marine products is one of sustainable development marine resource utilization modes implemented in China. The deep processing of marine products not only solves the problem of deep processingThe problems of short storage, transportation and quality guarantee period of the fresh marine products are solved, the added value of the marine products is improved, and the income of local fishermen and similar enterprises is increased. However, the deep processing of seafood is a high wastewater industry, and the deep processing of seafood is accompanied by the generation of large amounts of wastewater containing high concentrations of organic matter. The protein and amine content of these wastewaters is so abundant that the Chemical Oxygen Demand (COD), biological Oxygen Demand (BOD) and NH in the wastewaters are responsible 3 The concentration of main pollutants such as N, solid suspended matters and the like is increased rapidly, and the water body is stinky. With the continuous development and growth of the seafood processing industry, the generated wastewater poses serious threat to the ecological environment. At present, the waste water generated in the deep processing process of marine products is usually discharged after being treated by some purification technologies, but the purification process has great technical difficulty and high cost due to the complex components of the waste water. The researchers not only reduce the concentration of the waste water but also recycle the waste by extracting useful substances such as protein, astaxanthin and the like contained in the waste water. These techniques are still limited and are relatively costly to implement.
Carbon quantum dots are a young member of a family of carbon nanomaterials, have excellent photoelectric properties, and have been widely applied in the fields of photoelectric sensors, catalysts, cell imaging, photoelectric devices and the like. In addition, carbon is a main element constituting a living body, and carbon quantum dots composed of it have good biocompatibility. The biomass material has wide sources, low price, easy obtaining, regeneration and rich functional groups, and is an ideal material for synthesizing the carbon quantum dots. However, the unmodified carbon quantum dots have low fluorescence efficiency and single physicochemical property, so that the gaps are often introduced by doping some heteroatoms, the defects of the carbon quantum dots are increased, and the photoelectric properties of the carbon quantum dots are regulated. At present, the heteroatom is usually realized by adding a compound containing related elements, which undoubtedly increases the operation and cost of the experiment.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for synthesizing fluorescent carbon quantum dots by taking marine product deep processing wastewater as a raw material, which is simple to operate and low in energy consumption.
In order to solve the technical problems, the invention adopts the following technical scheme:
the method for synthesizing the fluorescent carbon quantum dots by taking marine product deep processing wastewater as a raw material comprises the steps of taking the marine product deep processing wastewater as a raw material, adding deionized water or ultrapure water into a reaction container, carrying out microwave reaction in a microwave oven, adding deionized water, and carrying out ultrasonic dispersion to obtain a fluorescent carbon quantum dot crude product; filtering the crude product by a filter membrane, and dialyzing by a dialysis bag to obtain a purified product of the fluorescent carbon quantum dots; the wastewater from deep processing of marine products is rich in protein and amino acid.
The method for synthesizing the fluorescent carbon quantum dots by taking the marine product deep processing wastewater as the raw material comprises the following steps:
step S1: marine product deep processing wastewater and deionized water are added into a (clean) conical flask simultaneously;
step S2: placing the conical flask (100 mL) in the step S1 into a microwave oven for microwave reaction;
and step S3: adding deionized water into the conical flask reacted in the step S2 and performing ultrasonic dispersion to obtain a fluorescent carbon quantum dot crude product;
and step S4: and (4) passing the fluorescent carbon quantum dot crude product obtained in the step (S3) through a 0.22-micron filter membrane, and then dialyzing through a dialysis bag to obtain a fluorescent carbon quantum dot purified product solution.
3-10 mL of deep processing wastewater of the marine product in the step S1 and 0-7 mL of deionized water, wherein the microwave reaction in the step S2 is carried out for 1-4 min under 390-650W, 10mL of deionized water is added in the step S3 and ultrasonic dispersion is carried out for 10-30 min, and the dialysis is carried out for 12-36 h by adopting a 500-1000 Da dialysis bag.
9mL of deep-processing wastewater of the marine product in the step S1 and 1mL of deionized water, wherein in the step S2, the microwave reaction is carried out for 3.5min under 585W, 10mL of deionized water is added in the step S3, ultrasonic dispersion is carried out for 10min, and dialysis is carried out for 24h by adopting a dialysis bag of 1000 Da.
The fluorescent carbon quantum dot obtained by the method.
The fluorescent carbon quantum dots show bright blue-white fluorescence under the irradiation of a 365nm ultraviolet lamp.
The fluorescent carbon quantum dots have an excitation peak at 226nm,294nm and 344nm respectively, and the fluorescence emission centers of the fluorescent carbon quantum dots are positioned at about 425nm.
The fluorescent carbon quantum dots are used for visual detection of chromium (VI).
Aiming at the problems in the preparation of the current marine product deep processing wastewater and carbon quantum dots, the inventor establishes a method for synthesizing the fluorescent carbon quantum dots by taking the marine product deep processing wastewater as a raw material, the method takes the marine product deep processing wastewater as a raw material, deionized water or ultrapure water is added into a reaction container, microwave reaction is carried out in a microwave oven, and the deionized water is added and ultrasonic dispersion is carried out to obtain a fluorescent carbon quantum dot crude product; filtering the crude product by a filter membrane, and dialyzing by a dialysis bag to obtain a purified product of the fluorescent carbon quantum dots; the marine product deep processing wastewater is rich in protein and amino acid. The method takes the deep processing wastewater of the biomass waste marine products as a carbon source, does not need to add other reagents, and fully utilizes the NH rich in the deep processing wastewater 3 And the heteroatom such as-N realizes the doping of the heteroatom to the carbon quantum dot, so that the fluorescent carbon quantum dot is prepared. The method is simple to operate, green and environment-friendly, and the obtained carbon quantum dots are uniformly dispersed and controllable in morphology. In a word, the invention has low cost, is convenient and quick, is easy for industrialized production, can be used in various fields, and also solves the problem of deep processing wastewater of marine products.
Compared with the prior art, the invention has at least the following advantages:
1. by using the rich protein and NH 3 the-N marine product deep processing wastewater is used as a raw material to synthesize the carbon quantum dots, so that the environmental pressure is reduced, and a green and environment-friendly way is provided for resource recycling of the marine product deep processing wastewater.
2. The raw materials can be synthesized in a few minutes by a microwave method without other pretreatment steps, and the method is simple, convenient and quick to operate.
3. Abundant protein, amino acid and NH in marine product deep processing wastewater 3 N provides a heteroatom source for the carbon quantum dots, and can be synthesized without adding heteroatoms, so that the experimental steps are shortened.
4. The fluorescent carbon quantum dot prepared by the invention shows selective quenching, and can be applied to visual detection of hexavalent chromium.
Drawings
FIG. 1 is a graph showing the effect of microwave power on the fluorescence intensity of fluorescent carbon quantum dots (examples 1-5).
FIG. 2 shows the effect of microwave time on the fluorescence intensity of fluorescent carbon quantum dots (examples 1, 6 to 9).
FIG. 3 shows the effect of the concentration of wastewater from further processing of seafood on the fluorescence of carbon quantum dots.
Fig. 4 is a fluorescence excitation spectrum and a fluorescence emission spectrum of a carbon quantum dot, in which: the upper right inset is a fluorescence plot of carbon quantum dots under a 365nm ultraviolet lamp.
Fig. 5 is an ultraviolet absorption spectrum of the carbon quantum dot (example 1).
FIG. 6 is a transmission electron micrograph of a carbon quantum dot (example 1).
FIG. 7 is a graph of the change in fluorescence of the carbon quantum dot strip in the presence of different ions (365 nm UV lamp).
Detailed Description
The detection proves that the deep processing wastewater of the marine products used in the embodiment is rich in protein and amino acid, wherein the protein content is 2.41g/100g, and the total amount of 16 amino acids is 1.86g/100g.
Example 1
9mL of the seafood deep processing wastewater and 1mL of deionized water were added to a 100mL clean Erlenmeyer flask and subjected to microwave reaction at a power of 585W for 3.5min. And then, adding 10mL of deionized water for ultrasonic extraction for 10min to obtain a fluorescent carbon quantum dot crude product. And (3) filtering the obtained crude product with a 0.22-micron filter membrane, and dialyzing in a dialysis bag of 1000Da for 24h to obtain the purified fluorescent carbon quantum dots.
Example 2
Example 2 was operated the same as example 1, except that the microwave had a power of 650W.
Example 3
Example 3 operates the same as example 1, except that the microwave power is 520W.
Example 4
Example 4 operates the same as example 1, except that the microwave has a power of 455W.
Example 5
Example 5 was operated the same as example 1, except that the microwave power was 390W.
Example 6
Example 6 was the same as example 1 except that the microwave time was 1min.
Example 7
Example 7 was conducted in the same manner as in example 1 except that the microwave time was 2min.
Example 8
Example 8 was the same as example 1 except that the microwaving time was 3min.
Example 9
Example 9 was the same as example 1 except that the microwave time was 4min.
As shown in FIG. 1, the fluorescence intensity of carbon quantum dots with different microwave powers at 343nm measured by a fluorescence photometer showed that the fluorescence intensity of the prepared CQDs was gradually increased as the microwave power was increased, the microwave power reached a maximum at 585W, and then the fluorescence intensity of the CQDs was decreased as the microwave power was increased. It is presumed that when the microwave power is too high, the carbonaceous organic matter in the raw material may react violently to coke, thereby reducing the generation of the fluorescent nanoparticles. The fluorescence intensity is strongest when the microwave power is 585W.
As shown in FIG. 2, the results of measuring the fluorescence intensity of the carbon quantum dots at different microwave times at the excitation wavelength of 343nm using a fluorescence spectrophotometer showed that the fluorescence intensity did not change significantly between the reaction times of 1min and 2min, and the fluorescence intensity of the carbon quantum dots increased significantly when the reaction time was increased to 3min. When the reaction time is 3.5min, the fluorescence intensity reaches the peak value, and the reaction time is continuously increased to 4min, so that the fluorescence intensity is weakened. Therefore, the optimal reaction time for preparing the carbon quantum dots by the microwave method is 3.5min.
As shown in FIG. 3, the amount of the wastewater from the marine product processing was controlled to be 3,4,6,8, 10mL, corresponding to 7,6,4,2,0mL of distilled water. The fluorescence intensity of the carbon quantum dots is enhanced along with the increase of the consumption of the seafood processing wastewater, when the consumption of the seafood processing wastewater is 8mL, the fluorescence intensity is the maximum, and when the consumption of the seafood processing wastewater is continuously increased, the fluorescence is reduced. Therefore, the amount of seafood processing wastewater used is optimally 8mL.
As shown in FIG. 4, each of 226nm,294nm and 344nm has one excitation peak, and the 3 excitation peaks have fluorescence centers around 425nm, so that the synthesized carbon quantum dot solution shows bright blue-white fluorescence under the irradiation of a 365nm ultraviolet lamp.
As shown in FIG. 5, the carbon quantum dots obtained in example 1 have a distinct ultraviolet absorption peak around 270 nm.
As shown in FIG. 6, the carbon quantum dots obtained in example 1 were uniformly dispersed and spherical, and had a particle size distribution of 3 to 12nm and an average particle size of 6.5nm.
Application example carbon quantum dot test paper
The fluorescent carbon quantum dots prepared in example 1 were coated on paper and air-dried naturally to obtain carbon quantum dot test paper. Next, 10. Mu.g/mL of S was added 2- ，NH 4 + ，Cl - ，Na + ，NO 2 - ，Bi 3+ ，K + ，Cr 6+ Coating the test paper on the obtained carbon quantum dot test paper, naturally drying, and observing the fluorescence change condition of the carbon quantum dot test paper under an external lamp of 365 nm.
As shown in fig. 7, at S 2- ，NH 4 + ，Cl - ，Na + ，NO 2 - ，Bi 3+ ，K + In the presence of the test paper, the fluorescence of the carbon quantum dot test paper is not obviously changed under a 365nm ultraviolet lamp, and when Cr is contained 6+ When the fluorescent probe exists, the obvious fluorescence quenching phenomenon of the carbon quantum dot test paper can be observed under a 365nm ultraviolet lamp. Illustrating the fluorescent carbon quantum in Cr prepared in example 1 6+ The method has potential application value in rapid visual detection.
Claims (7)
1. A method for synthesizing fluorescent carbon quantum dots by taking marine product deep processing wastewater as a raw material is characterized by comprising the following steps: taking marine product deep processing wastewater as a raw material, adding deionized water or ultrapure water into a reaction container, carrying out microwave reaction in a microwave oven, adding deionized water, and carrying out ultrasonic dispersion to obtain a fluorescent carbon quantum dot crude product; filtering the crude product by a filter membrane, and dialyzing by a dialysis bag to obtain a purified product of the fluorescent carbon quantum dots; the marine product deep processing wastewater is rich in protein and amino acid; the microwave reaction is carried out for 1-4 min under 390-650W.
2. The method for synthesizing the fluorescent carbon quantum dots by using the marine product deep processing wastewater as the raw material according to claim 1, which is characterized by comprising the following steps of:
step S1: adding marine product deep processing wastewater and deionized water into a conical flask simultaneously;
step S2: placing the conical flask in the step S1 in a microwave oven for microwave reaction;
and step S3: adding deionized water into the conical flask reacted in the step S2 and performing ultrasonic dispersion to obtain a fluorescent carbon quantum dot crude product;
and step S4: and (4) passing the fluorescent carbon quantum dot crude product obtained in the step (S3) through a 0.22-micron filter membrane, and then dialyzing through a dialysis bag to obtain a fluorescent carbon quantum dot purified product solution.
3. The method for synthesizing fluorescent carbon quantum dots by using marine product deep processing wastewater as a raw material according to claim 2, wherein the deep processing wastewater of the marine product is 3-10 mL and the deionized water is 0-7 mL in step S1, the microwave reaction is performed for 1-4 min at 390-650W in step S2, 10mL of deionized water is added in step S3 and ultrasonic dispersion is performed for 10-30 min, and dialysis is performed for 12-36 h by using a 500-1000 Da dialysis bag.
4. The method for synthesizing fluorescent carbon quantum dots by using seafood deep processing wastewater as a raw material according to claim 3, wherein the amount of the seafood deep processing wastewater in step S1 is 9mL, the amount of deionized water in step S2 is 1mL, the microwave reaction in step S2 is performed at 585W for 3.5min, 10mL of deionized water in step S3 is added and ultrasonic dispersion is performed for 10min, and dialysis is performed for 24h by using a 1000Da dialysis bag.
5. The fluorescent carbon quantum dot obtained by the method of claim 1, which is characterized by having an excitation peak at 226nm,294nm and 344nm, and the fluorescence emission centers of which are located at 425nm.
6. The fluorescent carbon quantum dot according to claim 5, characterized by exhibiting bright blue-white fluorescence under 365nm ultraviolet lamp irradiation.
7. The fluorescent carbon quantum dots of claim 5 for visual detection of chromium (VI).
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