CN109135686B - Graphene-based modified nano fluid heat transfer working medium and preparation method thereof - Google Patents
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Abstract
The invention discloses a graphene-based modified nano fluid heat transfer working medium and a preparation method thereof, which comprises the following steps of firstly, preparing graphene oxide through two times of oxidation, then reducing to obtain graphene, mixing the graphene, glycerol, ketone or aldehyde, then reacting at 80-150 ℃ for 2-12 hours, removing unreacted ketone or aldehyde through reduced pressure distillation after the reaction is finished, and then placing the obtained suspension in an ultrasonic cell crusher for ultrasonic treatment for 1-5 hours to obtain modified graphene: ketone/aldehyde glycerol acetal nanofluids. The method skillfully combines the traditional method for preparing the nanofluid by a two-step method with organic synthesis chemical reaction, the preparation process is simple and easy to operate, the heat conductivity coefficient of the prepared nanofluid is improved by 92 percent on the basis of base liquid, the viscosity is reduced by 98 percent, the working temperature range is expanded to-18-300 ℃, the preparation process is simple, the material source is wide, the process is easy to control, the repeatability is good, and the technology is easy to popularize and apply.
Description
Technical Field
The invention belongs to the technical field of heat transfer, relates to a nano fluid heat transfer working medium, and particularly relates to a graphene-based modified nano fluid heat transfer working medium and a preparation method thereof.
Background
The heat transfer process relates to all industries in the industry. With the increasing heat load of the heat transfer system and the complicated structure of the heat transfer system, higher requirements are put on heat transfer technologies, such as cooling of an insulating superconductor, heat control in thin film deposition, heat management of a power battery, heat dissipation of a high-power electronic element, heat management of an aerospace plane and the like. Improving the performance of heat transfer media is one of the primary ways to enhance heat transfer.
In 1995, professor Choi of Argonne laboratory in the united states proposed the concept of Nanofluid (Nanofluid), i.e., nanoparticle suspension formed by adding nanoparticles to a liquid, as a new approach to break through the low thermal conductivity characteristics of conventional working fluids. The base fluid, as a major component of the nanofluid, plays a crucial role in the thermal conduction of the dispersed nanoparticles and the nanofluid. The base fluid is selected primarily for its thermal stability, viscosity, thermal conductivity, heat capacity, freezing point and boiling point. In cold regions, such as the northern region of China, the lowest temperature can reach-30 ℃; in hot areas, the maximum temperature of the solar energy collecting system can reach 270 ℃, and the traditional water-based working medium can not work normally due to the limitation of a higher freezing point and a lower boiling point.
The glycerol is a main byproduct in the industrial biodiesel and soap making industry, and has wide source and low price. It is used as heat transfer medium due to its high thermal conductivity, thermal stability, safety and wide working temperature range (18-230 ℃), but its wide use is limited due to its high viscosity resulting in high pump consumption.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene-based modified nano fluid heat transfer working medium, which solves the problems of poor heat transfer capability and narrow working temperature range of the traditional liquid heat transfer medium.
The invention also aims to provide the graphene-based modified nano fluid heat transfer working medium prepared by the method, which has a wide working temperature range, and has a higher heat conductivity coefficient and a lower viscosity compared with the nano fluid of the glycerol base liquid.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a graphene-based modified nano fluid heat transfer working medium comprises the following steps:
(1) mixing graphite, phosphorus pentoxide, potassium permanganate and concentrated sulfuric acid, reacting at 10-50 ℃ for 1-8 hours, wherein the mass ratio of the phosphorus pentoxide to the potassium permanganate is 1:1, the mass ratio of the graphite to the total mass of the phosphorus pentoxide and the potassium permanganate is 1: 1-2: 1, and the mass ratio of the graphite to the concentrated sulfuric acid is 3: 1-5: 1, and filtering, washing and vacuum drying after the reaction is finished to obtain pre-oxidized graphite;
(2) mixing the pre-oxidized graphite obtained in the step (1), potassium permanganate and concentrated sulfuric acid, reacting at 0-50 ℃ for 2-5 hours, wherein the mass ratio of the pre-oxidized graphite to the potassium permanganate is 1: 3-1: 5, the mass ratio of the pre-oxidized graphite to the concentrated sulfuric acid is 1: 30-1: 50, neutralizing unreacted oxidant with 30% aqueous hydrogen peroxide solution by mass percent after the reaction is finished, centrifuging, washing precipitates for 3-5 times by taking the aqueous solution of a water-soluble organic solvent as a washing solvent, and drying in vacuum to obtain graphene oxide;
(3) mixing the graphene oxide obtained in the step (2) with a reducing agent in a mass ratio of 1: 30-1: 50 in a solvent environment, adjusting the pH of the solution to 9-10, reacting at 80-120 ℃ for 12-24 hours, and filtering, washing and vacuum drying after the reaction is finished to obtain graphene, wherein the mass volume ratio of the graphene oxide to the solvent is 1: 1-1: 3 (g/L);
(4) mixing the graphene, glycerol, ketone or aldehyde obtained in the step (3), reacting at 80-150 ℃ for 2-12 hours, wherein the mass ratio of the graphene to the glycerol is 0.216-1.264%, the molar ratio of the glycerol to the ketone or aldehyde is 1: 3-1: 5, removing unreacted ketone or aldehyde through reduced pressure distillation after the reaction is finished, and then placing the obtained suspension in an ultrasonic cell crusher for ultrasonic treatment for 1-5 hours to obtain modified graphene: ketone/aldehyde glycerol acetal nanofluids.
Preferably, in the steps (1) to (3), the temperature of the vacuum drying is 35-60 ℃, and the drying time is 12-24 hours.
Preferably, in the step (2), the centrifugal rotation speed is 2000-4000 rpm.
Preferably, in the step (3), the reducing agent is any one of sodium borohydride, formic acid, hydrazine hydrate, formaldehyde and sodium citrate; the solvent is any one of water, ethanol and methanol.
Preferably, in step (3), the pH is adjusted using a saturated sodium carbonate solution.
Preferably, in the step (4), the ketone is one of acetophenone, cyclohexanone and acetone.
Preferably, in the step (4), the aldehyde is one of benzaldehyde, phenylacetaldehyde, acetaldehyde and butyraldehyde.
Preferably, in the step (4), the power of the ultrasound is 30-60 KW.
Compared with the prior art, the invention has the following beneficial effects:
the method skillfully combines the traditional method for preparing the nanofluid by a two-step method with organic synthesis chemical reaction, the preparation process is simple and easy to operate, the heat conductivity coefficient of the prepared nanofluid is improved by 92 percent on the basis of base liquid, the viscosity is reduced by 98 percent, and the working temperature range is expanded to-18-300 ℃ (the glycerol has a temperature of 18-230 ℃). Research shows that the glycerol which is not completely reacted acts as a dispersing agent so that the nanofluid has better stability. The preparation method has the advantages of simple preparation flow, wide material source, easy process control, good repeatability and easy popularization and application of the technology.
Drawings
Fig. 1 is a scanning electron microscope image of 10 μm of graphene prepared in the present invention.
Fig. 2 is an X-ray diffraction pattern of graphene prepared in the present invention.
FIG. 3 shows the acetone glycerol prepared in example 1 of the present invention: transmission electron microscopy of graphene nanofluids; a: 1 μm; b: 500 nm.
FIG. 4 shows the acetone glycerol prepared in example 1 of the present invention: graph of graphene nanofluid and glycerol viscosity as a function of temperature.
FIG. 5 shows the glycerol ketals prepared in examples 1-3 of the present invention: graph of thermal conductivity of graphene nanofluid and acetone glycerol base liquid along with temperature change.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
The reagents and starting materials used in the following examples are all commercially available reagents unless otherwise specified.
Example 1: the nanometer fluid is prepared by taking glycerol, acetone and graphene as raw materials.
Putting graphite, phosphorus pentoxide, potassium permanganate and concentrated sulfuric acid into a reactor provided with a magnetic stirrer, wherein the mass ratio of the phosphorus pentoxide to the potassium permanganate is 1:1, the mass ratio of the graphite to the total mass of the phosphorus pentoxide and the potassium permanganate is 2:1, and the mass ratio of the graphite to the concentrated sulfuric acid is 4:1, mixing the materials, reacting for 6 hours at 30 ℃, filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol in sequence, and then drying in a vacuum drying oven at 50 ℃ for 18 hours to obtain pre-oxidized graphite.
Putting pre-oxidized graphite, potassium permanganate and concentrated sulfuric acid into a reactor provided with a magnetic stirrer, wherein the mass ratio of the pre-oxidized graphite to the potassium permanganate is 1:4, the mass ratio of the pre-oxidized graphite to the concentrated sulfuric acid is 1:40, mixing the materials, reacting for 3 hours at 30 ℃, neutralizing unreacted oxidant with 30% aqueous hydrogen peroxide solution by mass percent after the reaction is finished, centrifuging by using a 3000rpm centrifuge, centrifuging and washing for three times by using 50% ethanol aqueous solution as a washing solvent, and then drying for 18 hours in a 50 ℃ vacuum drying oven to obtain the graphene oxide.
Putting graphene oxide, hydrazine hydrate and deionized water into a reactor with a magnetic stirrer, adjusting the pH of the solution to 9 by using a saturated sodium carbonate solution, wherein the mass ratio of the graphene oxide to the hydrazine hydrate is 1:40, the mass volume ratio of the graphene oxide to a solvent is 1:2g/L, mixing the materials, reacting at 100 ℃ for 18 hours, filtering and washing after the reaction is finished, and vacuum drying at 50 ℃ for 18 hours to obtain the graphene.
The prepared graphene is observed under a scanning electron microscope (model: FEI Quanta 250), as shown in figure 1, the graphene mainly has a lamellar structure, has the edge fold characteristic specific to the graphene prepared by a chemical oxidation-reduction method, and has the appearance consistent with that reported in the literature.
The results of an X-Ray diffractometer (XRD) (model: Bruker X-Ray Diffraction, D8Advance) show that the characteristic peak of the 002 crystal face of about 26.4 degrees 2 theta of graphite completely disappears after the graphite is acted by a strong oxidant, and the characteristic peak of the 001 crystal face of graphene oxide appears at about 10.1 degrees, which shows that the graphite is completely converted into graphene oxide under the condition of two times of oxidation (figure 2A). After the graphene oxide is reduced, the characteristic peak of the 001 crystal face of the graphene oxide at about 10.1 degrees disappears, the diffraction peak is widened, and the intensity is very weak, because the size of the reduced graphite is reduced, the structural integrity of the crystal is reduced, the disorder degree is increased (fig. 2B), and the XRD spectrogram of the graphene is consistent with that reported in the literature.
Putting 12.5g (0.136mol) of glycerol, 39.3g (0.679mol) of acetone and 79mg of graphene into a reactor provided with a magnetic stirrer, mixing the materials, reacting at 120 ℃ for 12 hours, distilling under reduced pressure after the reaction is finished to remove unreacted acetone, and then carrying out ultrasonic treatment in an ultrasonic cell crusher with the power of 50KW for 4 hours to obtain the glycerol ketal: a graphene nanofluid.
The nanofluid was tested to have the following properties, viscosity: 20.9 mPas (25 ℃), thermal conductivity: 0.2988W/(m.K) (32 ℃ C.), temperature working range: -18 to 298 ℃.
As can be seen from FIG. 4, the viscosity of the nanofluid is reduced by 98% (25 ℃) relative to pure glycerol, and the practicability of the nanofluid as a heat transfer working medium is greatly enhanced.
Example 2: the nanometer fluid is prepared by taking glycerol, acetone and graphene as raw materials.
The graphene was prepared as in example 1.
Putting 12.5g (0.136mol) of glycerol, 31.6g (0.544mol) of acetone and 54mg of graphene into a reactor provided with a magnetic stirrer, mixing the materials, reacting at 120 ℃ for 12 hours, distilling under reduced pressure after the reaction is finished to remove unreacted acetone, and then carrying out ultrasonic treatment in an ultrasonic cell crusher with the power of 50KW for 4 hours to obtain the glycerol ketal: a graphene nanofluid.
The nanofluid was tested to have the following properties, viscosity: 20.9 mPas (25 ℃), thermal conductivity: 0.2442W/(m.K) (32 ℃ C.), temperature working range: -18 to 298 ℃.
Example 3: the nanometer fluid is prepared by taking glycerol, acetone and graphene as raw materials.
The graphene was prepared as in example 1.
Putting 12.5g (0.136mol) of glycerol, 39.4g (0.679mol) of acetone and 27mg of graphene into a reactor provided with a magnetic stirrer, mixing the materials, reacting at 120 ℃ for 12 hours, distilling under reduced pressure after the reaction is finished to remove unreacted acetone, and then carrying out ultrasonic treatment in an ultrasonic cell crusher with the power of 50KW for 1 hour to obtain the glycerol ketal: a graphene nanofluid.
The nanofluid was tested to have the following properties, viscosity: 20.2 mPas (25 ℃), thermal conductivity: 0.2278W/(m.K) (32 ℃ C.), temperature working range: -18 to 298 ℃.
As can be seen from fig. 5, the thermal conductivity of the graphene nanofluids prepared in examples 1 to 3 is greatly improved, wherein the thermal conductivity of the 0.6% graphene nanofluids is increased to 92%, the thermal conductivity of the 0.3% graphene nanofluids is increased to 54%, and the thermal conductivity of the 0.15% graphene nanofluids is increased to 43%. The results show that the effect of improving the heat conductivity coefficient of the base liquid by the graphene is very obvious.
Example 4
Putting graphite, phosphorus pentoxide, potassium permanganate and concentrated sulfuric acid into a reactor provided with a magnetic stirrer, wherein the mass ratio of the phosphorus pentoxide to the potassium permanganate is 1:1, the mass ratio of the graphite to the total mass of the phosphorus pentoxide and the potassium permanganate is 1:1, and the mass ratio of the graphite to the concentrated sulfuric acid is 3:1, mixing the materials, reacting for 8 hours at 10 ℃, filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol in sequence, and then drying for 24 hours in a vacuum drying oven at 35 ℃ to obtain pre-oxidized graphite.
Putting pre-oxidized graphite, potassium permanganate and concentrated sulfuric acid into a reactor provided with a magnetic stirrer, wherein the mass ratio of the pre-oxidized graphite to the potassium permanganate is 1:3, the mass ratio of the pre-oxidized graphite to the concentrated sulfuric acid is 1:30, mixing the materials, reacting for 2 hours at 50 ℃, neutralizing unreacted oxidant with 30% aqueous hydrogen peroxide solution by mass percent after the reaction is finished, centrifuging by using a 2000rpm centrifuge, centrifuging and washing for three times by using 50% methanol aqueous solution as a washing solvent, and then drying for 24 hours in a 35 ℃ vacuum drying oven to obtain the graphene oxide.
Putting graphene oxide, hydrazine hydrate and deionized water into a reactor with a magnetic stirrer, adjusting the pH of the solution to 10 by using a saturated sodium carbonate solution, wherein the mass ratio of the graphene oxide to the hydrazine hydrate is 1:30, the mass volume ratio of the graphene oxide to a solvent is 1:1g/L, mixing the materials, reacting at 80 ℃ for 24 hours, filtering and washing after the reaction is finished, and vacuum drying at 35 ℃ for 24 hours to obtain the graphene.
Putting 12.5g (0.136mol) of glycerol, 81.5g (0.679mol) of acetophenone and 158mg of graphene into a reactor provided with a magnetic stirrer, mixing the materials, reacting at 150 ℃ for 4 hours, distilling under reduced pressure after the reaction is finished to remove unreacted acetophenone, and then carrying out ultrasonic treatment in an ultrasonic cell crusher with the power of 60KW for 1 hour to obtain the acetophenone glycerol: a graphene nanofluid.
The nanofluid was tested to have the following properties, viscosity: 35.3 mPas (25 ℃), thermal conductivity: 0.3305W/(m.K) (32 ℃ C.), temperature working range: -10 to 330 ℃.
Example 5: the nanometer fluid is prepared by taking glycerol, phenylacetaldehyde and graphene as raw materials.
Putting graphite, phosphorus pentoxide, potassium permanganate and concentrated sulfuric acid into a reactor provided with a magnetic stirrer, wherein the mass ratio of the phosphorus pentoxide to the potassium permanganate is 1:1, the mass ratio of the graphite to the total mass of the phosphorus pentoxide and the potassium permanganate is 2:1, and the mass ratio of the graphite to the concentrated sulfuric acid is 5:1, mixing the materials, reacting for 1 hour at 50 ℃, filtering after the reaction is finished, washing with deionized water and absolute ethyl alcohol in sequence, and then drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain pre-oxidized graphite.
Putting pre-oxidized graphite, potassium permanganate and concentrated sulfuric acid into a reactor provided with a magnetic stirrer, wherein the mass ratio of the pre-oxidized graphite to the potassium permanganate is 1:5, the mass ratio of the pre-oxidized graphite to the concentrated sulfuric acid is 1:50, mixing the materials, reacting for 5 hours at 0 ℃, neutralizing unreacted oxidant with 30% aqueous hydrogen peroxide solution by mass percent after the reaction is finished, centrifuging by using a 4000rpm centrifuge, centrifuging and washing for three times by using 50% methanol aqueous solution as a washing solvent, and then drying for 12 hours in a 60 ℃ vacuum drying oven to obtain the graphene oxide.
Putting graphene oxide, hydrazine hydrate and deionized water into a reactor with a magnetic stirrer, adjusting the pH of the solution to 9 by using a saturated sodium carbonate solution, wherein the mass ratio of the graphene oxide to the hydrazine hydrate is 1:50, the mass volume ratio of the graphene oxide to a solvent is 1:3g/L, mixing the materials, reacting at 120 ℃ for 12 hours, filtering and washing after the reaction is finished, and vacuum drying at 60 ℃ for 12 hours to obtain the graphene.
Putting 12.5g (0.136mol) of glycerol, 81.5g (0.679mol) of phenylacetaldehyde and 158mg of graphene into a reactor provided with a magnetic stirrer, mixing the materials, reacting at 80 ℃ for 2 hours, distilling under reduced pressure after the reaction is finished to remove unreacted phenylacetaldehyde, and then carrying out ultrasonic treatment in an ultrasonic cell crusher with the power of 50KW for 3 hours to obtain the phenylacetaldehyde glycerol: a graphene nanofluid.
The nanofluid was tested to have the following properties, viscosity: 33.2 mPas (25 ℃), thermal conductivity: 0.3411W/(m.K) (32 ℃ C.), temperature working range: -12 to 305 ℃.
Example 6: preparing the nanofluid by using glycerol, cyclohexanone and graphene as raw materials.
The graphene was prepared as in example 4.
Putting 12.5g (0.136mol) of glycerol, 66.5g (0.679mol) of cyclohexanone and 103mg of graphene into a reactor provided with a magnetic stirrer, mixing the materials, reacting at 100 ℃ for 8 hours, distilling under reduced pressure after the reaction is finished to remove unreacted cyclohexanone, and then carrying out ultrasonic treatment in an ultrasonic cell crusher with the power of 30KW for 5 hours to obtain cyclohexanone glycerol: a graphene nanofluid.
The nanofluid was tested to have the following properties, viscosity: 28.2 mPas (25 ℃), thermal conductivity: 0.2906W/(m.K) (32 ℃ C.), temperature working range: -18 to 287 ℃.
Claims (7)
1. A preparation method of a graphene-based modified nano fluid heat transfer working medium is characterized by comprising the following steps:
(1) mixing graphite, phosphorus pentoxide, potassium permanganate and concentrated sulfuric acid, and making it pass through a mixer at 10 ~ 50oC, reacting for 1 ~ 8 hours, wherein the mass ratio of phosphorus pentoxide to potassium permanganate is 1:1, the mass ratio of graphite to the total mass of phosphorus pentoxide and potassium permanganate is 1:1 ~ 2:1, and the mass ratio of graphite to concentrated sulfuric acid is 3:1 ~ 5:1, filtering, washing and vacuum drying after the reaction is finished to obtain pre-oxidized graphite;
(2) mixing the pre-oxidized graphite obtained in the step (1), potassium permanganate and concentrated sulfuric acid, and then adding the mixture to 0 ~ 50oReacting for 2 ~ 5 hours under the condition of C, wherein the mass ratio of pre-oxidized graphite to potassium permanganate is 1:3 ~ 1:1, and the mass ratio of pre-oxidized graphite to concentrated sulfuric acid is 1:30 ~ 1:50, neutralizing unreacted oxidant with 30% aqueous hydrogen peroxide solution after the reaction is finished, centrifuging, washing precipitate for 3 ~ 5 times by taking the aqueous solution of a water-soluble organic solvent as a washing solvent, and drying in vacuum to obtain graphene oxide;
(3) mixing the graphene oxide obtained in the step (2) with a reducing agent according to a mass ratio of 1:30 ~ 1:50 in a solvent environment, wherein the mass volume ratio of the graphene oxide to the solvent is 1:1 ~ 1:3(g/L), adjusting the pH of the solution to 9 ~ 10, and adjusting the pH to 80 ~ 120oReacting for 12 ~ 24 hours under the condition of C, and filtering, washing and vacuum drying after the reaction is finished to obtain graphene;
(4) mixing the graphene, glycerol, ketone or aldehyde obtained in the step (3) and then carrying out 80 ~ 150oReacting for 2 ~ 12 hours under the condition of C, wherein the ketone is one of acetophenone, cyclohexanone and acetone, the aldehyde is one of benzaldehyde, phenylacetaldehyde, acetaldehyde and butyraldehyde, and the mass ratio of graphene to glycerol is 0.216% ~ 1.264.264%, the molar ratio of glycerol to ketone or aldehyde is 1:3 ~ 1:5, after the reaction is finished, the unreacted ketone or aldehyde is removed by reduced pressure distillation, and then the obtained suspension is placed in an ultrasonic cell crusher for ultrasonic treatment for 1 ~ 5 hours to obtain the modified graphene ketone/aldehyde condensed glycerol nanofluid.
2. The preparation method of the graphene-based modified nanofluid heat transfer working medium according to claim 1, wherein in the step (1) to the step (3), the temperature of vacuum drying is 35 ~ 60oC, drying time is 12 ~ 24 hours.
3. The preparation method of the graphene-based modified nanofluid heat transfer working medium according to claim 1, wherein in the step (2), the centrifugal rotation speed is 2000 ~ 4000 rpm.
4. The preparation method of the graphene-based modified nanofluid heat transfer working medium according to claim 1, wherein in the step (3), the reducing agent is any one of sodium borohydride, formic acid, hydrazine hydrate, formaldehyde and sodium citrate; the solvent is any one of water, ethanol and methanol.
5. The preparation method of the graphene-based modified nanofluid heat transfer working medium according to claim 1, wherein in the step (3), a saturated sodium carbonate solution is used for adjusting the pH.
6. The preparation method of the graphene-based modified nanofluid heat transfer working medium according to claim 1, wherein in the step (4), the power of the ultrasound is 30 ~ 60 KW.
7. The preparation method of the graphene-based modified nanofluid heat transfer working medium according to claim 1, wherein in the step (2), the water-soluble organic solvent is one or more of methanol, ethanol and acetone, and the volume fraction of the water-soluble organic solvent is 50%.
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