CN115029715A - Preparation method of carbon quantum dot, carbon quantum dot and application - Google Patents
Preparation method of carbon quantum dot, carbon quantum dot and application Download PDFInfo
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Abstract
The invention provides a preparation method of a carbon quantum dot, the carbon quantum dot and application, and particularly relates to the technical field of nano materials. The preparation method takes aniline with substituent groups as electrolyte, and carbon quantum dots are obtained after electrolysis. The aniline having a substituent includes at least one of sulfanilic acid, p-aminobenzoic acid, p-aminobenzamide, p-aminobenzenesulfonamide, sodium p-aminobenzenesulfonate, sodium p-aminobenzoate and sodium p-aminosalicylate. The invention provides a carbon quantum dotThe preparation method has simple process and easily obtained raw materials, the carbon quantum dots can be prepared by one-step electrolysis, and the aniline electrolyte with substituent groups endows the carbon quantum dots with rich surface functional groups in the preparation process, so that the carbon quantum dots have excellent temperature resistance and salt resistance, are stably dispersed in high-temperature high-salt solution, and are 1.5 multiplied by 10 at the temperature of 90 DEG C 5 Under the condition of mg/L mineralization degree, the carbon quantum dot solution can be uniformly and stably dispersed for more than 30 days, and can be used as a drag reduction and injection enhancement agent in the low-permeability oilfield exploitation.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a carbon quantum dot, the carbon quantum dot and application.
Background
As a novel low-permeability reservoir rock surface modification technology, the nano material anti-drag injection-increasing technology has huge application potential in the aspects of depressurization injection-increasing, profile control plugging, molecular membrane oil displacement, catalysis viscosity reduction and the like. The nano material drag reduction injection augmentation technology generally disperses nano particles in water to obtain water-based nano fluid injection augmentation liquid to be injected into a stratum, so that the nano particles are adsorbed on the surface of a pore, the wettability and microstructure of the inner surface of the pore of a rock are changed, the oil-water interfacial tension is reduced, the water-oil fluidity ratio is changed, and the injection pressure and the water-flooding efficiency of subsequently injected water in the stratum are effectively reduced. Silicon-based nanoparticles (e.g. SiO) 2 ) The water flow resistance of a stratum pore channel can be effectively reduced, the injection pressure is reduced, the injection volume is increased, and the pressure reduction and injection enhancement effects are generated, so that the nano material is the most widely researched anti-drag and injection enhancement nano material at present. However, SiO 2 The particle size of the nano particles is generally between 10 and 100nm, the size is relatively large, and the permeability is less than 10 multiplied by 10 -3 μm 2 The ultra-low permeability and ultra-low permeability oil field is easy to cause throat blockage, and the application range of the oil field is limited. In addition to this, SiO 2 High density, easy settlement, and more diesel oil as carrying medium in field application, not only increasingThe operation cost is reduced, and the environmental pollution is easily caused.
The carbon quantum dots have the advantages of small particle size (<10nm), low cost, stable structure, environmental friendliness and the like, and are reported to be used as novel anti-drag injection-increasing nano materials, but the currently reported carbon quantum dot materials are difficult to stably exist under the conditions of underground high temperature and high salt in the actual oil-gas flooding process, so that the actual application effect of the carbon quantum dot materials as the nano anti-drag injection-increasing agent is limited.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the present invention is to provide a method for preparing carbon quantum dots, so as to alleviate the technical problem that the prepared carbon quantum dots in the prior art are difficult to be stable under high temperature and high salt conditions.
In order to solve the technical problems, the invention adopts the following technical scheme:
the first aspect of the invention provides a preparation method of a carbon quantum dot, which comprises the steps of taking aniline with a substituent group as an electrolyte, and electrolyzing to obtain the carbon quantum dot.
Optionally, the substituted aniline comprises at least one of sulfanilic acid, p-aminobenzoic acid, p-aminobenzamide, p-aminobenzenesulfonamide, sodium p-aminobenzenesulfonate, sodium p-aminobenzoate, and sodium p-aminosalicylate.
Optionally, the concentration of the electrolyte is 0.1 wt.% to 5 wt.%.
Preferably, the concentration of the electrolyte is 1.5 wt.% to 3 wt.%.
Optionally, the voltage of the electrolysis is 10V-50V.
Preferably, the voltage of the electrolysis is 20V-40V.
Optionally, the time of the electrolysis is 6h-24 h.
Preferably, the time of the electrolysis is 12h-18 h.
Optionally, the electrolytic electrode material comprises graphite rods and/or petroleum coke.
Optionally, filtering after electrolysis to obtain the carbon quantum dots.
Preferably, the filtration is performed using a microfiltration membrane.
Optionally, the method further comprises dialyzing after the filtration to obtain the carbon quantum dots.
The second aspect of the present invention provides the carbon quantum dots prepared by the preparation method of the first aspect.
The third aspect of the invention provides the application of the carbon quantum dot in the drag reduction and injection enhancement agent.
Compared with the prior art, the invention has at least the following beneficial effects:
the preparation method of the carbon quantum dots provided by the invention has the advantages that the process is simple, the raw materials are easy to obtain, the carbon quantum dots can be prepared through one-step electrolysis, the surface modification of the carbon quantum dots is realized in the preparation process, aniline with substituent groups is electrolyzed and then endowed with surface functional groups of the carbon quantum dots, the repulsive force among particles is increased, the carbon quantum dots have excellent temperature resistance and salt resistance, the carbon quantum dots are stably dispersed in high-temperature high-salt water solution, and the carbon quantum dots are 1.5 multiplied by 10 at the temperature of 90 DEG C 5 Under the condition of mg/L mineralization degree, the carbon quantum dot solution can be uniformly and stably dispersed for more than 30 days.
The carbon quantum dots provided by the invention have controllable sizes, the particle size is less than 10nm, and the carbon quantum dots have excellent high-temperature resistance and salt water resistance.
The carbon quantum dots provided by the invention are used as the anti-drag injection agent and are easily dispersed in water to form nanofluid, and the obvious pressure reduction and injection enhancement effects are achieved under the conditions of high temperature and high salt.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a diagram of an electrolytic apparatus used in example 1;
FIG. 2 is a transmission electron micrograph of a carbon quantum dot provided in test example 1;
FIG. 3 is a distribution diagram of the particle diameters of carbon quantum dots provided in test example 1;
FIG. 4 is a graph of the drag reduction and injection enhancement performance of the carbon quantum dot nanofluid provided in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The components of embodiments of the present invention may be arranged and designed in a wide variety of different configurations.
Currently, most medium-high-permeability oil reservoirs with better development conditions in China enter the middle and later stages, and in newly explored oil reservoirs, the low-permeability/extra-low-permeability reserves account for the vast majority of the total explored reserves, so that exploitation of low-permeability/extra-low-permeability oil reservoirs becomes the main direction of oil development. The exploitation effect is not ideal, the recovery efficiency is low, which is the main bottleneck in the development of low-permeability/ultra-low-permeability oil reservoirs, and the exploration of new exploitation modes and the improvement of exploitation technologies are the key points for improving the recovery efficiency of low-permeability oil reservoirs at present.
Commonly used nano SiO 2 The particles are used as a nontoxic and environment-friendly material, can effectively reduce the flow resistance of formation pore water, reduce the injection pressure, increase the injection volume, obviously increase the overall flow rate and flow, and have obvious pressure reduction and injection increase effects. However, except for the conventional difficult problems of difficult large-scale synthesis, uncontrollable particle size, high surface modification cost and the like, the nano SiO has 2 The dispersion stability of the material in a solvent is poor due to poor temperature resistance and salt resistance and easy agglomeration; and when the device is applied on site, diesel oil is mostly adopted as a carrying medium, so that the operation cost is increased, the environmental pollution is easily caused, and the risks of storage and transportation are increased.
Therefore, an environment-friendly water-based ultra-small-size nano material which is simple to prepare, strong in dispersibility, good in stability, temperature-resistant and salt-tolerant is researched and developed, and the development of the oil field depressurization and injection increasing technology can be effectively promoted.
The carbon quantum dot is a dispersed quasi-spherical carbon nano-particle with the size less than 10nm,has the advantages of wide raw material source, low cost, friendly synthetic environment, rich surface functional groups, easy modification, small particle size and being smaller than that of nano SiO 2 The nano-material has the characteristics of uniformity, controllability, good dispersibility and the like, has great potential in the development of low-permeability/ultra-low-permeability oil reservoirs, is expected to be used as a novel nano-material to realize resistance reduction and flow increase, reduce the injection resistance of a super-infiltration interface, relieve the problems of high injection pressure, difficult water injection and the like in the subsequent water injection and oil displacement process and promote the injection-production balance.
According to the preparation method of the carbon quantum dot provided by the first aspect of the invention, aniline with a substituent group is used as an electrolyte, and the carbon quantum dot is obtained after electrolysis.
Because the carbon quantum dots have small particle size and high surface energy, the repulsive force between particles is often destroyed under high temperature and high salt, so that the energy is reduced by agglomeration. The preparation method of the carbon quantum dots provided by the invention has the advantages that the process is simple, the raw materials are easy to obtain, the carbon quantum dots can be prepared through one-step electrolysis, the surface modification of the carbon quantum dots is realized in the preparation process, aniline with substituent groups is electrolyzed and then is endowed with surface functional groups of the carbon quantum dots, the particle size of the carbon quantum dots is small, the repulsive force among particles is large, the carbon quantum dots have excellent temperature resistance and salt resistance, the carbon quantum dots are stably dispersed in high-temperature high-salt water solution and are 1.5 multiplied by 10 at the temperature of 90 DEG C 5 Under the condition of mg/L mineralization degree, the carbon quantum dot solution is uniformly and stably dispersed for more than 30 days.
Optionally, the aniline having a substituent includes at least one of sulfanilic acid, p-aminobenzoic acid, p-aminobenzamide, p-aminobenzenesulfonamide, sodium p-aminobenzenesulfonate, sodium p-aminobenzoate, and sodium p-aminosalicylate.
Optionally, the concentration of the electrolyte is 0.1 wt.% to 5.0 wt.%.
When the concentration of electrolysis is less than 0.1 wt.%, the functional groups for surface modification of the carbon quantum dots are less, the electrolysis efficiency is low, and the temperature resistance and the salt tolerance are poor; when the concentration of electrolysis is more than 5.0 wt.%, the size of the exfoliated carbon material is too large due to excessive electrolysis current, and the yield of carbon quantum dots is low.
In some embodiments of the invention, the concentration of the electrolyte is typically, but not limited to, 0.1 wt.%, 0.5 wt.%, 1 wt.%, 1.5 wt.%, 2 wt.%, 2.5 wt.%, 3 wt.%, 3.5 wt.%, 4 wt.%, 4.5 wt.%, or 5 wt.%.
Preferably, the concentration of the electrolyte is 1.5 wt.% to 3.0 wt.%.
In some preferred embodiments of the present invention, the concentration of the electrolyte is 1.5 wt.% to 3.0 wt.%, the carbon quantum dots can be subjected to abundant surface functional group modification in situ during the electrolysis process, the yield of the carbon quantum dots is high, and the carbon quantum dots exhibit good temperature resistance, salt resistance, resistance to drag reduction and injection enhancement.
Optionally, the voltage of the electrolysis is 10V-50V.
When the electrolysis voltage is less than 10V, the electrolysis efficiency is low, and the graphite electrode or the petroleum coke-based electrode is difficult to effectively strip to prepare the carbon quantum dots; when the voltage of electrolysis is more than 50V, the size of the exfoliated carbon material is too large due to excessive electrolysis current, and the yield of carbon quantum dots is low.
In some embodiments of the invention, the voltage of electrolysis is typically, but not limited to, 10V, 15V, 20V, 25V, 30V, 35V, 40V, 45V, or 50V.
Preferably, the voltage of the electrolysis is 20V-40V.
In some preferred embodiments of the present invention, the electrolysis voltage is 20V-40V, the yield of carbon quantum dots is high, the size is uniform, and the particle size distribution is uniform.
Optionally, the electrolysis time is 6h-24 h.
When the electrolysis time is less than 6h, the yield of carbon quantum dots is low; when the electrolysis time is longer than 24 hours, the electrode consumption is large, the current is unstable, the carbon material peeling particle size is not uniform, and the electrolysis cost is high.
In some embodiments of the invention, the time of electrolysis is typically, but not limited to, 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, or 24 h.
Preferably, the time of the electrolysis is 12h-18 h.
In some preferred embodiments of the invention, the electrolysis time is 12h-18h, the yield of carbon quantum dots is high, the size is uniform, the particle size distribution is uniform, and the comprehensive preparation cost is low.
Optionally, the electrolytic electrode material comprises graphite rods and/or petroleum coke.
In some embodiments of the invention, the petroleum coke and pitch are bonded to press calcined wafers as electrodes.
Optionally, filtering after electrolysis to obtain the carbon quantum dots.
Preferably, the filtration is performed using a microfiltration membrane.
Optionally, the method further comprises dialyzing after the filtration to obtain the carbon quantum dots.
According to a second aspect of the present invention there is provided a carbon quantum dot.
The carbon quantum dots provided by the invention have controllable sizes, the particle size is less than 10nm, and the carbon quantum dots have excellent high-temperature resistance and salt water resistance.
The carbon quantum dots provided according to the third aspect of the invention are used in drag reduction and injection enhancement agents.
The carbon quantum dots provided by the invention are used as the anti-drag injection-increasing agent and are easily dispersed in water to form a nano fluid, and the pressure-reducing injection-increasing effect is obvious under the conditions of high temperature and high salt, so that the oil displacement recovery rate is obviously improved.
Some embodiments of the present invention will be described in detail below with reference to examples. The embodiments described below and the features of the embodiments can be combined with each other without conflict.
Example 1
The embodiment provides a carbon quantum dot, which is carried out by using the device shown in figure 1 and comprises a power supply and an electrolytic cell, wherein the power supply is provided with positive and negative wiring ports, the electrolytic cell consists of internal electrolyte, an anode and a cathode, and the positive and negative wiring ports of the power supply are respectively connected with the anode and the cathode in the electrolytic cell through leads. The anode and the cathode are both made of graphite rods or electrodes formed by bonding, pressing and calcining petroleum coke and asphalt.
The preparation method of the carbon quantum dot comprises the following steps:
(1) sodium sulfanilate was prepared into an electrolyte having a concentration of 2.5 wt.%, and poured into the electrolytic cell of the apparatus shown in fig. 1, wherein the volume of the electrolyte was 10 mL.
(2) Two graphite rods are taken as a working electrode and a counter electrode to connect the whole device.
(3) The voltage was set to 30V and electrolysis was started for 12 h.
(4) And after the electrolysis is finished, carrying out suction filtration by using a microporous filter membrane with the aperture of 0.22 mu m, and putting the solution obtained by suction filtration into a dialysis bag for dialysis for 3 days to obtain the carbon quantum dots.
Example 2
This example provides a carbon quantum dot, which is different from example 1 in that the electrolyte concentration is 0.1 wt.%, and the remaining raw materials and steps are the same as those in example 1, and are not repeated herein.
Example 3
This example provides a carbon quantum dot, which is different from example 1 in that the electrolyte concentration is 1.5 wt.%, and the remaining raw materials and steps are the same as those in example 1, and are not repeated herein.
Example 4
This example provides a carbon quantum dot, which is different from example 1 in that the electrolyte concentration is 3.5 wt.%, and the remaining raw materials and steps are the same as those in example 1, and are not repeated herein.
Example 5
This example provides a carbon quantum dot, which is different from example 1 in that the electrolyte concentration is 5.0 wt.%, and the remaining raw materials and steps are the same as those in example 1, and are not repeated herein.
Example 6
The present embodiment provides a carbon quantum dot, which is different from embodiment 1 in that the electrolyte is a p-aminobenzamide solution, and other raw materials and steps are the same as those in embodiment 1, and are not described herein again.
Example 7
The present embodiment provides a carbon quantum dot, which is different from embodiment 1 in that the electrolyte is a sulfanilamide solution, and the rest of the raw materials and steps are the same as those in embodiment 1, and are not repeated herein.
Example 8
The present embodiment provides a carbon quantum dot, which is different from embodiment 1 in that the electrolyte is a sodium p-aminosalicylate solution, and the rest of the raw materials and steps are the same as those in embodiment 1, and are not described herein again.
Comparative example 1
This comparative example provides a carbon quantum dot, which is different from example 1 in that the electrolyte is pure water, and the remaining raw materials and steps are the same as those in example 1, and are not described again.
Comparative example 2
The comparative example provides a carbon quantum dot, which is different from example 1 in that the electrolyte is ammonia water, the concentration of the ammonia water is 5 wt.%, and other raw materials and steps are the same as those in example 1 and are not repeated.
Comparative example 3
This comparative example provides a carbon quantum dot, which is different from example 1 in that the electrolyte is a NaOH solution, the concentration of the NaOH solution is 0.1 wt.%, and the remaining raw materials and steps are the same as those in example 1 and are not described again.
Comparative example 4
This comparative example provides a carbon quantum dot, which is different from example 1 in that the electrolyte is an aniline solution, the concentration of the aniline solution is 2 wt.%, and the rest of the raw materials and steps are the same as those in example 1 and are not described again.
Test example 1
The carbon quantum dots obtained in example 1 were subjected to a transmission electron microscope to obtain an image as shown in fig. 2, and the particle size distribution of the carbon quantum dots was counted as shown in fig. 3.
As can be seen from FIG. 3, the carbon quantum dots have a particle size <5nm and a uniform size distribution, centered at 2-4 nm.
Test example 2
The carbon quantum dots obtained in examples 1 to 8 and comparative examples 1 to 4 were used to measure particle diameters and yields, the particle diameters were measured by atomic force microscopy, and the results are shown in table 1.
TABLE 1 data sheet for particle size and yield of carbon quantum dots
| Average particle diameter/nm | Yield/(%) | |
| Example 1 | 2.5 | 92 |
| Example 2 | 5.3 | 85 |
| Example 3 | 3.1 | 89 |
| Example 4 | 5.6 | 95 |
| Example 5 | 8.4 | 80 |
| Example 6 | 5.8 | 88 |
| Example 7 | 5.4 | 90 |
| Example 8 | 4.6 | 82 |
| Comparative example 1 | 23.6 | 42 |
| Comparative example 2 | 5.2 | 60 |
| Comparative example 3 | 4.0 | 56 |
| Comparative example 4 | 6.8 | 68 |
As can be seen from Table 1, the particle sizes obtained in 8 examples are all below 10nm and the yield is more than 80% compared with comparative examples 1, 2, 3 and 4. The results show that the carbon quantum dot obtained by using aniline with the substituents as an electrolyte has smaller particle size and higher yield.
Test example 3
The carbon quantum dots obtained in examples 1 to 8 and comparative examples 1 to 4 were subjected to a temperature resistance and salt tolerance test by placing the carbon quantum dots in an aqueous solution environment at a certain temperature and a certain degree of mineralization, and detecting the maximum temperature and degree of mineralization that the carbon quantum dots can withstand when uniformly and stably dispersed for 30 days, and the obtained results are shown in table 2.
TABLE 2 data sheet of the temperature and salt resistance of carbon quantum dots
As can be seen from Table 2 above, the 8 examples all have a degree of mineralization tolerated at 90 ℃ of greater than 1.5 x 10 5 mg·L -1 The carbon quantum dot material is far higher than the carbon quantum dot materials prepared in comparative examples 1, 2, 3 and 4, and shows that the carbon quantum dot prepared by taking aniline with substituent groups as electrolyte has better temperature resistance and salt resistance.
Test example 4
The carbon quantum dots obtained in examples 1-8 and comparative examples 1-4 were tested for resistance reduction and filling performance, tap water was used as a control, the permeability of the core was 20mD, and the porosity was 15-17%. The testing method comprises the steps of injecting tap water into the rock core at the flow rate of 0.2mL/min, and recording the equilibrium pressure (P1); next, a carbon quantum dot dispersion with a concentration of 0.03 wt.% was injected into the core as a displacement agent at the same flow rate until the pressure stabilized and recorded (P2). The drag reduction ratio was (P1-P2)/P1, and the results obtained are shown in table 3.
TABLE 3 data sheet of carbon quantum dot resistance-reducing and injection-increasing performance
| Drag reduction ratio/(%) | |
| Example 1 | 36.5 |
| Example 2 | 21.3 |
| Example 3 | 29.0 |
| Example 4 | 32.3 |
| Example 5 | 24.4 |
| Example 6 | 30.7 |
| Example 7 | 25.5 |
| Example 8 | 22.6 |
| Comparative example 1 | 3.9 |
| Comparative example 2 | 7.6 |
| Comparative example 3 | 8.9 |
| Comparative example 4 | 11.0 |
| Tap water | - |
As can be seen from the above Table 3, the drag reduction ratio of 8 examples is 20% or more compared with 4 comparative examples, which shows that the drag reduction of carbon quantum dots obtained by using the aniline solution with substituent groups as the electrolyte has excellent drag reduction and injection enhancement performance.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the carbon quantum dot is characterized in that aniline with substituent groups is used as electrolyte, and the carbon quantum dot is obtained after electrolysis.
2. The method for producing a carbon quantum dot according to claim 1, wherein the aniline having a substituent comprises at least one of sulfanilic acid, p-aminobenzoic acid, p-aminobenzamide, p-aminobenzenesulfonamide, sodium p-aminobenzenesulfonate, sodium p-aminobenzoate, and sodium p-aminosalicylate.
3. The method for producing a carbon quantum dot according to claim 1, wherein the concentration of the electrolyte is 0.1 wt.% to 5.0 wt.%;
preferably, the concentration of the electrolyte is 1.5 wt.% to 3.0 wt.%.
4. The method for preparing a carbon quantum dot according to claim 1, wherein the voltage of the electrolysis is 10V to 50V;
preferably, the voltage of the electrolysis is 20V-40V.
5. The method for preparing the carbon quantum dot according to claim 1, wherein the electrolysis time is 6h to 24 h;
preferably, the electrolysis time is 12h-18 h.
6. The method of claim 1, wherein the electrolytic electrode material comprises graphite rod and/or petroleum coke.
7. The method for preparing the carbon quantum dot according to claim 1, further comprising obtaining the carbon quantum dot by filtering after electrolysis;
preferably, the filtration is performed using a microfiltration membrane.
8. The method of claim 7, further comprising dialyzing the filtered carbon quantum dot.
9. A carbon quantum dot produced by the production method according to any one of claims 1 to 8.
10. Use of the carbon quantum dot of claim 9 in a drag reducing and injection enhancing agent.
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