CN115124027A - Preparation method and application of carbon dots with high yield and resistance reduction function - Google Patents
Preparation method and application of carbon dots with high yield and resistance reduction function Download PDFInfo
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- 230000009467 reduction Effects 0.000 title claims abstract description 41
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 26
- 239000004202 carbamide Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- 238000000967 suction filtration Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 description 29
- 239000000243 solution Substances 0.000 description 26
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 25
- 238000002347 injection Methods 0.000 description 25
- 239000007924 injection Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a preparation method of carbon dots with high yield and resistance reduction function and application thereof.
Description
Technical Field
The invention belongs to the technical field of carbon dot preparation, and particularly relates to a carbon dot preparation method with high yield and a resistance reduction function and application thereof.
Background
The micro-nano pore throat of the hypotonic/ultra-hypotonic oil reservoir is developed, the permeability is low, the heterogeneity is serious, the conditions of a complex reservoir are complicated, the yield of natural energy production is reduced rapidly, and the energy supplement is difficult. Water injection is the most economical and feasible mode for supplementing formation energy for a long time, but the pore throat water injection with fine matrix can cause hydration expansion and scaling of reservoir clay, so that throat blockage is caused, the water injection pressure is too high, and the problem of serious high-pressure short injection is caused, so that the development effect of the low-permeability/ultra-low-permeability reservoir in China is not ideal, and the average recovery ratio is lower than 15% depending on the prior art. Therefore, the method solves the problem of 'high-pressure under-injection', and is the key for ensuring the water injection development effect of the low-permeability/ultra-low-permeability oil reservoir and greatly improving the recovery ratio; the gripper is the most realistic gripper which practices the basic national policy of saving and reasonably using mineral resources and ensures the realization of high benefit and high quality development of the petroleum upstream industry. Nanomaterials are the vision scheme most likely to address such problems due to their superior properties. And aiming at the micro-nano pore throat, the wall surface roughness of the pore throat can be effectively improved only by the ultra-small nano material to achieve the resistance reduction effect.
The nanometer material drag reduction and injection enhancement technology is characterized in that nanometer particles are dispersed in water to prepare water-based nanometer injection enhancement liquid to be injected into a stratum, and the wettability and microstructure of the inner surface of the wall of a rock hole are changed through the adsorption of the nanometer particles on the surface of a pore micro-channel, so that the injection pressure of subsequently injected water in the stratum is effectively reduced. The technology can effectively realize resistance reduction and flow increase, reduce water injection resistance, further solve the problems of high injection pressure, difficult water injection and the like in the water injection process, and promote injection-production balance (namely resistance reduction performance).
The invention closely combines the characteristics and development characteristics of a hypotonic/ultra-hypotonic reservoir layer, aims at providing a preparation process of the carbon-based nano material which has wide sources, low price and easy obtaining and can obtain products with multiple active sites, preferably selects a carbon source with mild reducibility, optimizes synthesis conditions, and has the advantages of simple construction process, environmental protection and controllable reaction kinetics. How to prepare the carbon dots with resistance reduction performance and improve the yield of the carbon dots by synthesizing the uniformly dispersed nano material with small particle size (less than 10nm), good uniformity and good stability is an urgent problem to be solved.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments.
According to one aspect of the invention, citric acid and urea are sequentially added into deionized water, fully dissolved and then placed into a microwave reactor, reaction is carried out for 20-40 min under the microwave power of 2000-4500W, a carbonized product is obtained after the reaction is finished, deionized water is added into the carbonized product, the carbonized product is dispersed in the deionized water to obtain a solid-liquid mixture, and the solid-liquid mixture is obtained through suction filtration and drying to obtain the carbon dots.
As a preferred scheme of the preparation method of the carbon dots with high yield and the resistance reduction function, the method comprises the following steps: the mass ratio of the citric acid to the urea is 1: 5-5: 1.
as a preferred scheme of the preparation method of the carbon dots with high yield and the drag reduction function, the invention comprises the following steps: the mass ratio of the citric acid to the urea is 1: 4.5 to 5.
As a preferred scheme of the preparation method of the carbon dots with high yield and the resistance reduction function, the method comprises the following steps: sequentially adding citric acid and urea into deionized water, wherein the mass ratio of the citric acid to the deionized water is (0.1-1.5): 1.
as a preferred scheme of the preparation method of the carbon dots with high yield and the resistance reduction function, the method comprises the following steps: sequentially adding citric acid and urea into deionized water, wherein the mass ratio of the citric acid to the deionized water is (1-1.5): 1.
as a preferred scheme of the preparation method of the carbon dots with high yield and the resistance reduction function, the method comprises the following steps: the microwave power is 3000-4000W.
As a preferred scheme of the preparation method of the carbon dots with high yield and the resistance reduction function, the method comprises the following steps: and dispersing the carbonized product in deionized water to obtain a solid-liquid mixture, wherein ultrasonic dispersion is adopted, the ultrasonic power is 90-120 Hz, and the ultrasonic time is 5-30 min.
As a preferred scheme of the preparation method of the carbon dots with high yield and the resistance reduction function, the method comprises the following steps: the drying is freeze drying, and the time is 24-36 h.
The invention has the beneficial effects that: the invention unexpectedly discovers that under the high microwave power, the carbon dots with very high resistance reduction performance can be prepared by using citric acid and urea as raw materials, and meanwhile, the carbon dots also have very strong high-temperature high-salt stability, low carbon cost, simple and rapid preparation process, suitability for batch production and very good application prospect in the field of actual oil exploitation.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below, and for those skilled in the art, other drawings can be obtained according to the drawings without any creative effort. Wherein:
FIG. 1 is a HRTEM image of a carbon dot prepared in example 1;
FIG. 2 is an XPS spectrum of carbon dots prepared in example 1;
FIG. 3 is a FT-IR spectrum of the carbon dots prepared in example 1;
FIG. 4 is a photograph showing that 0.05 wt% of CDs-1, CDs-2, CDs-3, CDs-4, CDs-5 and CDs-6 are stably present in a saline solution at 135 ℃ and 20 wt% NaCl concentration for 3 weeks;
FIG. 5 is a PL spectrum of a carbon dot prepared in example 1 at 375nm incident light.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein, and it will be appreciated by those skilled in the art that the present invention may be practiced without departing from the spirit and scope of the present invention and that the present invention is not limited by the specific embodiments disclosed below.
Example 1:
sequentially adding 525g of citric acid and 2400g of urea into 500mL of deionized water, fully dissolving, then placing into a microwave reactor, reacting for 30min at 4000W, obtaining a carbonized product after the reaction is finished, adding 3L of deionized water into the obtained carbonized product, dispersing the carbonized product in water, carrying out ultrasonic treatment for 15min under the power of 100Hz to obtain a solid-liquid mixture, then carrying out suction filtration by using qualitative filter paper, then carrying out suction filtration by using a 0.22-micrometer inorganic filter membrane, carrying out freeze drying on the obtained filtrate for 24-36 h, obtaining solid yellow-green powder which is CDs-1, weighing the obtained product, and calculating the yield to be 65.42%.
Testing temperature resistance and salt tolerance: firstly, a sodium chloride solution with the mass fraction of 20% is prepared, the carbon dots CDs-1 obtained in example 1 are added into the 20% sodium chloride solution, the mass concentration of the CDs-1 is 0.05 wt%, the mixture is kept stand at 135 ℃ for 3 weeks without obvious precipitation, the PL strength test result is shown in figure 5, and the PL strength is not obviously changed from figure 5, which shows that the carbon dots CDs-1 have strong temperature and salt resistance.
And (3) testing the resistance reduction performance: preparing an aqueous solution of CDs-1 with the mass concentration of 0.05%, injecting the solution into a core, wherein the injection speed is 0.2ml/min, the injection volume is 1PV, the adsorption time is 36h, and the drag reduction rate is 40.34%.
The invention unexpectedly discovers that under the high microwave power, the carbon dots with very high resistance reduction performance can be prepared by using citric acid and urea as raw materials, and meanwhile, the carbon dots also have very strong high-temperature high-salt stability, low carbon cost, simple and rapid preparation process, suitability for batch production and very good application prospect in the field of actual oil exploitation.
In the invention, the proportion of citric acid and urea can influence the resistance reduction performance of the prepared carbon dots, and the mass ratio of citric acid to urea is 1: 4.5-5 is optimal, and the addition of excessive citric acid and excessive urea can affect the functional group proportion and the lattice structure of carbon points, so that the resistance reduction performance is reduced.
Study example 1:
weighing 525g of citric acid and 2400g of urea, dissolving in 500mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid and urea, placing the solution in a microwave reactor to react for 30min under 3500W power, obtaining a carbonized product after the reaction is finished, adding 3L of deionized water into the obtained carbonized product to disperse the carbonized product in water, performing ultrasonic treatment for 15min under 100Hz power to obtain a solid-liquid mixture, performing suction filtration by using qualitative filter paper, performing suction filtration by using an inorganic filter membrane of 0.22 mu m, performing freeze drying on the obtained filtrate for 24-36 h to obtain solid yellowish green powder, namely CDs-2, and weighing the obtained product to obtain the yield of 49.46%.
And (3) testing temperature resistance and salt tolerance of CDs-2: firstly, a sodium chloride solution with the mass fraction of 20% is prepared, the carbon dots CDs-2 obtained in the research example 1 are added into the sodium chloride solution with the mass fraction of 20%, the mass concentration of the CDs-2 is 0.05 wt%, and no obvious precipitation phenomenon exists after the mixture is kept for 3 weeks at 135 ℃, which shows that the carbon dots show high stability under the conditions of high temperature and high salt.
Drag reduction testing of CDs-2: preparing a CDs-2 aqueous solution with the mass concentration of 0.05%, injecting the solution into a rock core, wherein the injection speed is 0.2ml/min, the injection volume is 1PV, the adsorption time is 36h, and the drag reduction rate is 34.26%.
Study example 2:
weighing 525g of citric acid and 2400g of urea, dissolving in 500mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid and urea, placing the solution in a microwave reactor to react for 30min under 3000W of power, obtaining a carbonized product after the reaction is finished, adding 3L of deionized water into the obtained carbonized product to disperse the carbonized product in water, performing ultrasonic treatment for 15min under 100Hz of power to obtain a solid-liquid mixture, performing suction filtration by using qualitative filter paper, performing suction filtration by using a 0.22 mu m inorganic filter membrane, performing freeze drying on the obtained filtrate for 24-36 h to obtain solid yellow-green powder which is CDs-3, weighing the obtained product, and calculating the yield to be 40.43%.
And (3) temperature resistance and salt tolerance test:
firstly, a sodium chloride solution with the mass fraction of 20% is prepared, the CDs-3 prepared in research example 2 is added into the sodium chloride solution with the mass fraction of 20% to ensure that the mass concentration of the CDs-3 is 0.05 wt%, and no obvious precipitation phenomenon exists after the mixture is kept stand at 135 ℃ for 3 weeks, which shows that the carbon dot shows high stability under the conditions of high temperature and high salt.
And (3) testing the resistance reduction performance:
preparing a CDs-3 aqueous solution with the mass concentration of 0.05 percent, injecting the solution into the rock core, wherein the injection speed is 0.2ml/min, the injection volume is 1PV, the adsorption time is 36h, and the drag reduction rate is 26.86 percent.
Study example 3:
weighing 525g of citric acid and 2400g of urea, dissolving in 500mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid and urea, placing the solution in a microwave reactor to react for 30min at 2500W power, obtaining a carbonized product after the reaction is finished, adding 3L of deionized water into the obtained carbonized product to disperse the carbonized product in water, performing ultrasonic treatment for 15min at the power of 100Hz to obtain a solid-liquid mixture, performing suction filtration by using qualitative filter paper, performing suction filtration by using an inorganic filter membrane of 0.22 mu m, performing freeze drying on the obtained filtrate for 24-36 h to obtain solid yellowish green powder, namely CDs-4, and weighing the obtained product to obtain the yield of 35.43%.
And (3) temperature resistance and salt tolerance test:
firstly, a sodium chloride solution with the mass fraction of 20% is prepared, the CDs-4 prepared in research example 3 is added into the sodium chloride solution with the mass fraction of 20% to ensure that the mass concentration of the CDs-4 is 0.05 wt%, and no obvious precipitation phenomenon is generated after the mixture is kept stand at 135 ℃ for 3 weeks, which shows that the carbon dot shows high stability under the conditions of high temperature and high salt.
And (3) testing the resistance reduction performance:
preparing a CDs-4 aqueous solution with the mass concentration of 0.05%, injecting the solution into a rock core at the injection speed of 0.2ml/min, the injection volume of 1PV and the adsorption time of 36h, and measuring the drag reduction rate to be 23.65%.
Study example 4:
weighing 525g of citric acid and 2400g of urea, dissolving in 500mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid and urea, placing the solution in a microwave reactor to react for 30min under 2000W of power, obtaining a carbonized product after the reaction is finished, adding 3L of deionized water into the obtained carbonized product to disperse the carbonized product in water, performing ultrasonic treatment for 15min under 100Hz of power to obtain a solid-liquid mixture, performing suction filtration by using qualitative filter paper, performing suction filtration by using a 0.22 mu m inorganic filter membrane, performing freeze drying on the obtained filtrate for 24-36 h to obtain solid yellow-green powder, namely CDs-5, weighing the obtained product, and calculating the yield to be 30.23%.
And (3) temperature resistance and salt tolerance test:
firstly, a sodium chloride solution with the mass fraction of 20% is prepared, the CDs-5 obtained in research example 4 is added into the sodium chloride solution with the mass fraction of 20%, so that the concentration of the CDs-5 is 0.05 wt%, and the carbon dots do not have obvious precipitation phenomenon after standing for 3 weeks at 135 ℃, which indicates that the carbon dots show high stability under the conditions of high temperature and high salt.
And (3) testing the resistance reduction performance:
preparing a CDs-5 aqueous solution with the mass concentration of 0.05%, injecting the solution into a rock core at the injection speed of 0.2ml/min, the injection volume of 1PV and the adsorption time of 36h, and measuring the drag reduction rate to be 17.96%.
Study example 5:
weighing 525g of citric acid and 2400g of urea, dissolving in 500mL of deionized water, performing ultrasonic treatment to fully dissolve the citric acid and urea, placing the solution in a microwave reactor to react for 30min under 1500W power, obtaining a carbonized product after the reaction is finished, adding 3L of deionized water into the obtained carbonized product to disperse the carbonized product in water, performing ultrasonic treatment for 15min under 100Hz power to obtain a solid-liquid mixture, performing suction filtration by using qualitative filter paper, performing suction filtration by using an inorganic filter membrane of 0.22 mu m, performing freeze drying on the obtained filtrate for 24-36 h to obtain solid yellowish green powder, namely CDs-6, and weighing the obtained product to obtain the yield of 23.75%.
Testing temperature resistance and salt tolerance:
firstly, a sodium chloride solution with the mass fraction of 20% is prepared, the CDs-6 prepared in research example 5 is added into the prepared salt solution, so that the concentration of the CDs-6 is 0.05 wt%, and no obvious precipitation phenomenon is generated after the mixture is kept stand at 135 ℃ for 3 weeks, which shows that the carbon dot shows high stability under the conditions of high temperature and high salt.
And (3) testing the resistance reduction performance:
preparing CDs-6 aqueous solution with mass concentration of 0.05%, injecting the solution into the rock core at an injection speed of 0.2ml/min, an injection volume of 1PV, an adsorption time of 36h, and measuring the drag reduction rate to be 14.56%.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. A method for preparing carbon dots with high yield and resistance reduction function is characterized by comprising the following steps: sequentially adding citric acid and urea into deionized water, fully dissolving, then placing into a microwave reactor, reacting for 20-40 min under the microwave power of 2000-4500W to obtain a carbonized product after the reaction is finished, adding deionized water into the carbonized product to disperse the carbonized product in the deionized water to obtain a solid-liquid mixture, performing suction filtration, and drying to obtain the carbon dots.
2. The method for preparing carbon dots with high yield and drag reduction function according to claim 1, characterized in that: the mass ratio of the citric acid to the urea is 1: 5-5: 1.
3. the method for preparing carbon dots with high yield and drag reduction function according to claim 1, characterized in that: the mass ratio of the citric acid to the urea is 1: 4.5 to 5.
4. The method for preparing carbon dots with high yield and drag reduction function according to claim 1 or 2, wherein: sequentially adding citric acid and urea into deionized water, wherein the mass ratio of the citric acid to the deionized water is (0.1-1.5): 1.
5. the method for preparing carbon dots with high yield and drag reduction function according to claim 1 or 2, wherein: sequentially adding citric acid and urea into deionized water, wherein the mass ratio of the citric acid to the deionized water is (1-1.5): 1.
6. the method for preparing carbon dots with high yield and drag reduction function according to claim 1 or 2, wherein: the microwave power is 3000-4000W.
7. The method for preparing carbon dots with high yield and drag reduction function according to claim 1 or 2, wherein: and dispersing the carbonized product in deionized water to obtain a solid-liquid mixture, wherein ultrasonic dispersion is adopted, the ultrasonic power is 90-120 Hz, and the ultrasonic time is 5-30 min.
8. The method for preparing carbon dots with high yield and drag reduction function according to claim 1 or 2, wherein: the drying is freeze drying for 24-36 h.
9. Use of the carbon dots produced by the method of claim 1 for the production of carbon dots with high yield and drag reduction function.
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