CN115710487A - Method for preparing graphene nanofluid through microwave coupling ultrasonic one-step method - Google Patents
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Abstract
The invention discloses a method for preparing graphene nanofluid by a microwave-coupled ultrasonic one-step method. The method has the advantages of good graphene stripping effect, avoidance of the use of chemical reducing agents in the preparation process, shortening of the preparation period of the whole graphene nanofluid, high efficiency, energy conservation, simplicity in operation, greenness, no pollution and capability of meeting the environmental protection requirement under the double-carbon background.
Description
Technical Field
The invention relates to the technical field of nanofluids, in particular to a method for preparing graphene nanofluids by a microwave-coupled ultrasonic one-step method.
Background
The nanometer fluid is a colloid suspension containing a complex multiphase system of nanometer particles, is a novel functional fluid which is gradually developed in nearly 20 years, has the characteristics of high heat transfer, high mass transfer and strong lubrication, and can effectively strengthen the chemical reaction and the transfer process between multiphase flows. Compared with the traditional pure liquid heat exchange working medium, the heat exchange working medium is more expected to meet the heat transfer and cooling requirements under special environments such as high heat transfer strength, microchannel heat dissipation and the like, such as the cooling of a high-temperature superconductor, the cooling of a strong laser mirror, the heat dissipation of a high-power electronic element and the like. The heat exchanger has great significance for improving the economy, reliability and miniaturization of a heat exchange system, and has become a leading-edge scientific field with high attention of scientists in various countries. In addition, the nano particles contained in the system also have unique properties of heat, light, electricity, magnetism and the like, so that the nano particles have very wide application prospects and potential economic values in the fields of aerospace, energy and power, mechano-electronics, nuclear energy systems, biomedicine and the like, and are called as 'future cooling and heat dissipation technologies'.
The graphene has extremely high thermal conductivity and excellent thermal conductivity. In addition, the graphene also has the characteristics of ultrahigh mechanical strength, special low-dimensional layered structure, larger specific surface area, good tribological performance, chemical inertness and the like. The thermal conductivity of the graphene powder is obviously higher than that of Cu, znO and Al 2 O 3 And common high-thermal-conductivity nanoparticles such as SiC. In addition, the carbon material has the unique antifriction and lubricating characteristics, has the potential of becoming a molecular ball (shaft) lubricating additive, and can be used as the lubricating additive to obviously reduce the friction factor. Compared with other nanoparticles, the graphene serving as a heat exchange medium of the nano dispersoid has the following advantages: one is that the thermal conductivity is significantly enhanced; secondly, the phenomena of erosion, corrosion, blockage and the like in the micro-channel, the heat pipe and other systems are reduced; thirdly, the friction coefficient is reduced, so that excellent lubrication is obtained; fourthly, the requirement of pumping power and pressure drop are reduced, and the cost is saved. Therefore, the research on the novel preparation technology of the high-thermal conductivity graphene nanofluid has important scientific significance and application value.
However, the preparation of graphene nanofluid generally adopts a two-step dispersion method, that is, prepared graphene is added according to a required proportion and is dispersed into a liquid phase medium by using dispersion means such as ultrasound, mechanical stirring, pH adjustment, shearing force application and the like. For example, chinese patent publication No. CN103588197A discloses a method for preparing a graphene nanofluid, which comprises oxidizing graphite, ultrasonically dispersing the graphite in a dispersion medium to obtain a graphene oxide solution, stirring the graphene oxide solution at a high speed, and mechanically reducing the graphene oxide in situ to form the graphene nanofluid. Also, for example, chinese patent publication No. CN114574168A discloses a carbide graphene nanofluid heat dissipation material and a preparation method thereof, in which silicon carbide graphene, a base liquid, and a surfactant are mixed, ground, ultrasonically dispersed, and centrifuged to obtain a silicon carbide graphene nanofluid. Therefore, the synthesis and dispersion of the method are carried out step by step, the drying, transfer and dispersion of the nano material cannot be avoided (the operations of the two-step method are necessary and cannot be avoided), the operation is complicated, and the graphene is more prone to agglomeration in the drying process and is not beneficial to the stability of the nanofluid.
Disclosure of Invention
In order to overcome the defects of long preparation period, low efficiency, complex operation, poor stability of the nanofluid and the like existing in the preparation of the graphene nanofluid by the traditional two-step dispersion method, the invention aims to provide a method for preparing the graphene nanofluid by a microwave coupling ultrasonic one-step method.
Microwaves are a form of energy that can be converted to heat in a medium. Different from other conventional heating modes, in the microwave heating process, heat is generated from the inside of the material instead of absorbing a heat source from the outside, the whole material is heated at the same time, the heat energy utilization rate is high, and the whole temperature gradient of the material is very small, so that the heating time is effectively shortened, and the energy is saved. When the ultrasound is transmitted in the liquid, the physical processes of generation, growth, compression, closing, breaking and the like of the liquid hollow cavity can be caused, the breaking of the cavitation bubbles can generate micro jet flow in a small space around the cavitation bubbles, cavitation noise is radiated outwards, particle aggregate is effectively broken, and the dispersion of the graphene in the base liquid is strengthened. According to the invention, chemical reaction is directly initiated in the base liquid to prepare graphene through a microwave one-step method, the surface charge of particles is changed by adjusting pH to form an electric double layer structure, and graphene particles are uniformly dispersed in the base liquid under the assistance of ultrasound.
The method comprises the steps of simultaneously putting a solvent mixed with a graphene precursor into a microwave reactor with an ultrasonic function, absorbing microwaves by using the graphene precursor, converting microwave energy into heat energy through the movement of pi electrons in a graphitized structure, and rapidly decomposing oxygen-containing functional groups and doped substances in the graphene precursor into CO 2 And H 2 And (4) O gas. When the pressure generated by these gases exceeds the van der waals force between the sheets, the graphite layers are exfoliated to obtain graphene. And then adjusting the proper pH value and further promoting the particle dispersion under the action of intermittent ultrasonic cavitation effect, and breaking particle aggregates to obtain the stable graphene nanofluid.
The invention provides a method for preparing graphene nanofluid by a microwave coupling ultrasonic one-step method, which comprises the following specific steps:
(1) Immersing a graphene precursor into a solvent for premixing to obtain a mixture;
(2) Placing the mixture obtained in the step (1) in a microwave reactor with an ultrasonic function, carrying out microwave heating under the power condition of 300-2000W to liquid phase strip graphene for 90s-60min, then closing the microwave, and cooling to room temperature to obtain a suspension of graphene particles;
(3) And (3) adjusting the graphene particle suspension obtained in the step (2) by using a pH regulator, starting an ultrasonic mode, controlling the ultrasonic working frequency to be 20-40kHz, controlling the temperature to be below 50 ℃ during ultrasonic treatment, and carrying out ultrasonic treatment for 10 min-2h in a mode of intermittent 3 min-10min every 10 min-30min, so as to finally obtain the stable graphene nano fluid.
Further, in the step (1), the graphene precursor is one of carbon-based materials such as graphene oxide, expanded graphite and natural graphite, and the concentration of the precursor in a mixture obtained by premixing the precursor and a solvent is 0.1 to 50 mg/mL.
Further, the solvent is one or more of mixed liquid such as N-methylpyrrolidone, ethanol, hydrogen peroxide and the like.
Further, the pH regulator is sodium hydroxide, ammonia water or the like, the concentration is 0.1 to 1.5 mol/L, and the pH is regulated to 7 to 9.
Further, the average thickness of the prepared graphene powder is 1 to 5 nm.
Furthermore, the prepared graphene nanofluid does not delaminate or precipitate within 3 months, and the zeta potential absolute value is more than 25 mV.
The invention discloses a device for preparing graphene nanofluid by adopting a microwave-coupled ultrasonic one-step method, which comprises an ultrasonic microwave chemical reactor, wherein the ultrasonic microwave chemical reactor comprises an ultrasonic probe and a built-in microwave radiation device, the left side wall of a shell is provided with a heat dissipation window, the right end of the shell is provided with a control panel, the front part of the shell is provided with a cover body, the bottom of the shell is provided with a microwave rotary base, a reactor liner is arranged above the microwave rotary base, precursor powder and a solvent are arranged in the reaction container, a temperature measurement probe and a system regulating valve extend into the reactor liner to realize real-time temperature measurement, and the control panel can control the independent control and synergistic combination functions of microwave, ultrasonic wave and microwave ultrasonic wave.
The invention has the beneficial effects that:
the method has the advantages of good graphene stripping effect, avoidance of the use of a chemical reducing agent in the preparation process, shortening of the preparation period of the whole graphene nanofluid, high efficiency, energy conservation, simplicity in operation, greenness, no pollution and better accordance with the environmental protection requirement under the double-carbon background.
Drawings
Fig. 1 is a schematic diagram of an apparatus for preparing graphene nanofluid by a microwave-coupled ultrasonic one-step method;
in the figure: 1-an ultrasonic probe; 2-precursor powder; 3, a microwave radiation device is arranged in the shell; 4-a control panel; 5-a shell; 6-temperature measuring probe and system regulating valve; 7-a solvent; 8-rotating the base by microwave; 9-inner container of reactor; 10-a heat dissipation window; 11-cover body.
Detailed Description
For a better understanding of the present invention, the contents of the present invention will be further explained below with reference to the drawings and examples, but the contents of the present invention are not limited to the following examples.
As shown in fig. 1, a device for preparing graphene nanofluid by a microwave coupling ultrasonic one-step method comprises an ultrasonic microwave chemical reactor, wherein the ultrasonic microwave chemical reactor comprises an ultrasonic probe 1 and a built-in microwave radiation device 3, the left side wall of a shell 5 is provided with a heat dissipation window 10, the right end of the shell is provided with a control panel 4, the front part of the shell is provided with a cover body 11, the bottom of the shell is provided with a microwave rotating base 8, a reactor liner 9 is arranged above the microwave rotating base, precursor powder 2 and a solvent 7 are arranged in a reaction container, a temperature measurement probe and a system regulating valve 6 extend into the reactor liner 9 to realize real-time temperature measurement, and the control panel 4 can control independent control and synergistic combination functions of microwave, ultrasonic wave and microwave ultrasonic wave.
Comparative example:
the method for preparing the graphene nanofluid by adopting a two-step method in the prior art specifically comprises the following steps:
firstly, 10mg of graphite powder and 50mL of concentrated sulfuric acid are mixed for primary reaction for 30min, and 50mL of MnO is added 4 Reacting at 35 ℃ for 6h, adding 100mL of 30% hydrogen peroxide, filtering to obtain a graphite oxide filter cake, and washing with hydrochloric acid, ethanol and distilled water in sequence. And ultrasonically stripping the filter cake in distilled water for 2 hours, drying the filter cake in an oven, and grinding the filter cake to obtain graphene oxide powder. And finally, mixing 20mg of graphene oxide powder with 50mL of water, adjusting the pH to 8 by using ammonia water, and ultrasonically dispersing for 2h at normal temperature to obtain graphene oxide nanofluid with a zeta potential absolute value of 30mV, wherein the graphene oxide nanofluid can stably exist for more than 2 months without sedimentation, and the thermal conductivity coefficient is 0.75W/(m k).
Example 1:
a method for preparing graphene nanofluid by a microwave coupling ultrasonic one-step method comprises the following specific steps:
mixing 10mg of graphene oxide and 100mL of N-methylpyrrolidone, placing the mixture in a microwave reactor with an ultrasonic function, carrying out microwave heating for 30min under the power condition of 600W to strip graphene in a liquid phase, cooling to room temperature, and adjusting the pH value to 8 by adopting 0.1 mol/L sodium hydroxide solution. And (3) starting an ultrasonic mode, controlling the ultrasonic frequency to be 30kHz, and controlling the ultrasonic time to be 30min to finally obtain the graphene nanofluid with the zeta potential absolute value of 45mV, wherein the graphene nanofluid can stably exist for more than 3 months without sedimentation, the time is saved by 92% compared with the two-step method for preparing the graphene nanofluid, and the heat conductivity coefficient of the graphene nanofluid is improved by 8% compared with the two-step method for preparing the graphene nanofluid.
Example 2:
a method for preparing graphene nanofluid by a microwave coupling ultrasonic one-step method comprises the following specific steps:
mixing 3 mg of expanded graphite with 100mL of ethanol, placing the mixture in a microwave reactor with an ultrasonic function, performing microwave heating for 10min under the power condition of 800W to perform liquid-phase graphene stripping, cooling to room temperature, and adjusting the pH to 8 by adopting 0.1 mol/L ammonia water. And (3) starting an ultrasonic mode, controlling the ultrasonic frequency to be 40kHz, and controlling the ultrasonic time to be 50min to finally obtain the graphene nanofluid with the zeta potential absolute value of 40mV, wherein the graphene nanofluid can stably exist for more than 3 months without sedimentation, time is saved by 91% compared with the method for preparing the graphene nanofluid by using a two-step method, and the thermal conductivity coefficient of the graphene nanofluid is improved by 6% compared with the method for preparing the graphene nanofluid by using a two-step method.
Example 3:
a method for preparing graphene nanofluid by a microwave coupling ultrasonic one-step method comprises the following specific steps:
mixing 5 mg of natural graphite with 100mL of mixed solution of ammonium persulfate and hydrogen peroxide, placing the mixture in a microwave reactor with an ultrasonic function, and carrying out microwave heating for 5 min under the power condition of 900W. Ammonium persulfate is decomposed under microwave to generate oxygen free radicals, under the induction of the oxygen free radicals, the graphite nanosheets are cut open, then hydrogen peroxide is decomposed and inserted into the graphite nanosheet layers, and graphite uniformly expands along the circumference c to obtain graphene. After cooling to room temperature, the pH was adjusted to 9 with 0.2 mol/L ammonia. And (3) starting an ultrasonic mode, controlling the ultrasonic frequency to be 40kHz, and controlling the ultrasonic time to be 60min to finally obtain the graphene nanofluid with the zeta potential absolute value of 35mV, wherein the graphene nanofluid can stably exist for more than 3 months without sedimentation, the time is saved by 90% compared with the two-step method for preparing the graphene nanofluid, and the heat conductivity coefficient of the graphene nanofluid is improved by 5% compared with the two-step method for preparing the graphene nanofluid.
Claims (8)
1. A method for preparing graphene nanofluid by a microwave coupling ultrasonic one-step method is characterized by comprising the following steps: immersing a graphene precursor into a solvent for premixing to obtain a mixture, then placing the mixture into a microwave reactor with an ultrasonic function, carrying out microwave heating liquid phase stripping to obtain a suspension of graphene particles, adjusting a proper pH value, and further promoting the particles to disperse under the action of an intermittent ultrasonic cavitation effect to obtain a stable graphene nanofluid.
2. The method for preparing graphene nanofluid according to the claim 1 by using the microwave-coupled ultrasonic one-step method, is characterized by comprising the following specific steps:
(1) Immersing a graphene precursor into a solvent for premixing to obtain a mixture;
(2) Placing the mixture obtained in the step (1) in a microwave reactor with an ultrasonic function, carrying out microwave heating under the power condition of 300-2000W to liquid phase strip graphene for 90s-60min, then closing the microwave, and cooling to room temperature to obtain a suspension of graphene particles;
(3) And (3) adjusting the graphene particle suspension obtained in the step (2) by using a pH regulator, starting an ultrasonic mode, controlling the ultrasonic working frequency to be 20-40kHz, controlling the temperature to be below 50 ℃ during ultrasonic treatment, and carrying out ultrasonic treatment for 10 min-2h in a mode of intermittent 3 min-10min every 10 min-30min, so as to finally obtain the stable graphene nano fluid.
3. The method for preparing the graphene nanofluid according to the claim 2, wherein in the step (1), the graphene precursor is one of graphene oxide, expanded graphite and a natural graphite carbon-based material, and the concentration of the precursor in a mixture obtained by premixing the precursor and a solvent is 0.1-50 mg/mL.
4. The method for preparing graphene nanofluid according to claim 2, wherein in the step (1), the solvent is one or more of N-methylpyrrolidone, ethanol and hydrogen peroxide.
5. The method for preparing the graphene nanofluid according to the claim 2, wherein in the step (3), the pH regulator is one of sodium hydroxide and ammonia water, the concentration is 0.1 to 1.5 mol/L, and the pH is adjusted to 7 to 9.
6. The method for preparing graphene nanofluid according to claim 2, wherein the method comprises the following steps: the average thickness of the prepared graphene powder is 1 to 5 nm.
7. The method for preparing graphene nanofluid according to claim 2, wherein the method comprises the following steps: the prepared graphene nanofluid does not delaminate or precipitate within 3 months, and the zeta potential absolute value is more than 25 mV.
8. A device for preparing graphene nanofluid by a microwave-coupled ultrasonic one-step method is used for the method for preparing the graphene nanofluid by the microwave-coupled ultrasonic one-step method according to any one of claims 1 to 7, and is characterized in that: including supersound microwave chemical reaction ware, supersound microwave chemical reaction ware includes ultrasonic probe, built-in microwave radiation device, and the casing left side wall is equipped with the heat dissipation window, and the right-hand member is equipped with control panel, and the front portion is equipped with the lid, and the bottom is equipped with microwave rotating base, and microwave rotating base top is the reactor inner bag, is equipped with precursor powder and solvent in the reaction vessel, and temperature probe and system control valve realize real-time temperature measurement in stretching into the reactor inner bag, and the steerable microwave of control panel, ultrasonic wave, microwave ultrasonic wave independent control and synergistic combination function.
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